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Chapter 1 Introduction

Chapter 1 Introduction
Chapter 1. 1 Overview
This thesis describes improvements to the Shape Deposition Process (SDM) for the development of tool steels die inserts. SDM is a rapid prototyping process, which is used at Stanford University and Carnegie Mellon University to develop metallic parts by rapid fusion of powder metal by laser deposition or by plasma melting of metal wire. The approach given here was to develop an understand the microstructure produced by the laser deposition of tool steels. This understanding is essential to building die inserts. Die inserts have stringent material requirements because of the intense service conditions to cast aluminum parts. The presented research developed three signicant outcomes: 1. The microstructual and morphological characterization of laser layered deposition of carbon steels. 2. A set of design rules which one must consider when depositing carbon steels with laser based layered manufacturing processes. 3. A methodology for using phase transformation and other microstructual knowledge to design improved parts, Designing for Microstructural Manipulation (DFM2) was also developed. The benets of characterizing carbon steel microstructure and cataloging the morphological evolution are the application of this knowledge to reduce part deection and enhance part properties. Also, the carbon steel deposition methodology will increase building throughput, reduce part failure, and extend the range of the applications that can use laser layered manufacturing. The benets to DFM2 are the ability to leverage the transient heating patterns of laser layered manufacturing to manipulate phase percentage, grain size, and phase location to enhance wear

Chapter 1. 1 Overview

Chapter 1 Introduction

resistance, deformation, and strength. Conventional Shape Deposition Manufacturing techniques do not leverage knowledge of the deposited microstructure to create improved parts or improved designs.

Chapter 1. 2 Thesis Outline


Chapter 2 provides a detailed background material on rapid tooling processes, the SDM process, and other laser deposition processes. Chapter 3 describes the experimental procedures used to analyze microstructure and material properties. Chapter 4 describes the initial investigation into using tool steels with the SDM process to make small die casting inserts (less than 25 mm in thickness) and low aspect ratios. Chapter 5 details the characterization of SDM deposited 400 series Martensitic Stainless steels and other carbon steels. Chapter 6 discusses utilizing the characterization to select die cast insert material and to reduce part deection. Chapter 7 describes design rules for laser depositing carbon steels in a new process which focuses on depostion microstructure, Designing for Microstructural Manipulation. Chapter 8 provides a short conclusion to this thesis. Additional information is included in the appendix.

Chapter 1. 3 Individual / Group Work Statement


Part of the work presented here represents group work. The Stanford Rapid Prototyping Lab is an environment in which teamwork and collaboration of ideas is encouraged for the purpose of enriching and progressing the pace of research. All of the work presented was developed under this environment. The idea, testing and use of the martensitic expansion to reduce CTE shrinkage deection, and the development of Designing for Microstructural Manipulation process are completely my own work. The parametric modelling of this phenomena in laser deposited martensitic steels is also my own work. Most of the analysis by X-ray diffraction, transmission electron microscope, electron microbeam analysis, and pixel-phase color analysis are also my own work. The development of Blue, the pixel color intensity matching program, was designed by Rudolph Leitgeb. Many samples were etched, polished, and analyzed by Monikka Mann, Tony Nguyen and Tonya Huntley. Ms. Mann helped to perfect the

Chapter 1. 2 Thesis Outline

Chapter 1 Introduction

electron backscattering probe technique for bulk carbon steel samples. Finite element modelling was performed by Alexander Nickel. Many of the 316L SDM tooling efforts were built by John Fessler, Alexander Nickel, and Xiochun Li. The laser SDM process was perfected by John Fessler and Alexander Nickel. Any errors presented in this work are my responsibility.

Chapter 1. 3 Individual / Group Work Statement

Chapter 2 Background

Chapter 2 Background
Chapter 2. 1 Tooling Industry
The prototype tooling industry is about 300 Billion dollar a year industry. Prototype parts are often used by designers to test alternative designs. Prototype parts can range from conceptual to functional. Barkan and Iansiti developed a detail study of the levels a prototyping stages which can occur during the design process (2.1). Simple models or mockups are conceptual parts which can be made from the simplest materials and processes. They can be made of plastics, paper, etc. They can be formed by gluing, simple machining, or blade shaping. Mock up parts do not have to necessarily t tight tolerances. The primary purpose for conceptual parts are look and feel attributes. They are typically used in the early part of the design cycle. Subsystem and mechanical prototypes have a wide range of model classes which very in level of integration and tolerances. Parts in these two subclass range from moderate to highly tight tolerances. They can also be semi-functional to functional. These parts are used for design validation. Often these parts are used to determine part t within packaging requirements. These parts made be made from traditional prototyping techniques or rapid prototyping techniques. Show parts are subsystem prototypes which high accuracy but are used primarily for display or review purposes. These parts are not typically made of conventional engineering materials, but are often painted or decaled to have show quality nishes. These parts are typically made very quickly from foams, ren board, and epoxy plastics. They often require manual nishing to insure tight tolerances and part dimensions.

Chapter 2. 1 Tooling Industry

Chapter 2 Background

Breadboards are subsystem prototypes which are very simple with low tolerances but exhibit part function. These types of are typically used for testing concept function or local part/subsystem function. The ability to make changes to these systems rapidly is a prime feature of breadboards. Tooling to build such prototypes is relatively simple, typically glue, solder, simple linkages, etc. Mechanical prototypes are functional prototypes which typically support all the functions of the nal model but do not necessarily represent the nal size or shape of the actual part. These prototypes may include several breadboard prototypes, Tooling for these types of prototypes, typically consists of off the shelf technology. For examples, standard housing may be used for prototype printers. Non standard metal and plastic parts may be machined from simple stock materials. Engineering prototypes are classes of models which are functional prototypes like the mechanical prototypes but are typically made out the same engineering material as the nal part. The size or footprint of the prototypes match the nal design. These prototypes are used as nal design checks or limited eld testing. Low volume prototype casting processes are used for exotic parts as opposed to machining them out of stock. Metal parts may be sand cast or gravity poured. Even though parts may be made from the design intent engineering material, quality may still differ from the production run parts. Production prototypes are prototype parts which are made from the same engineering material that the nal part will be made and manufactured from similar processes. The purpose of these parts is to test the manufacturing process and production part quality. These prototypes will have the material characteristics of production intent manufacturing. Therefore, early cycle time scenarios and production volumes can be forecasted from these prototypes. Also, reliability or failure studies on the actual part can be run with prototypes. Unlike many engineering prototypes, the parts could be included within validation cycles. Tooling for these prototypes are very expense and usually require long lead times because actual tooling inserts are required. As the Figure 2.1 below shows, changes to prototype design at this point is very expense.

Chapter 2. 1 Tooling Industry

Chapter 2 Background

Production 100K

Engineering Mechanical Subsystem 10K Computer Simulation 1K Models, Mock-Ups Timing


Figure 2.1 Adapted from Barkan and Iansiti (1993)

Chapter 2. 2 Conventional Tooling Process


To build prototype parts many conventional tooling processes are used. There are two approaches which are usually taken to make prototypes parts: part simulation and process simulation. Part simulation typically involves using simple processes like material removal to just get prototype parts made. Similar stock material may be machined to get a model. Other part simulations includes the models, mock-ups, and low level simulations. Prototypes built with process simulation are cast, drawn forged, stamped, etc. to build parts which will be similar to the production intent pieces. Process simulations include the mechanical, engineering, and production prototypes. The two types of tooling processes are common to both part and process simulations are material-removal processes and casting. Joining processes are also common but will not be described explicitly. Chapter 2. 2.1 Material-Removal Processes Traditional tooling processes for building parts typically encompasses material

Chapter 2. 2 Conventional Tooling Process

Chapter 2 Background

removal process. These processes include cutting, abrading, burning, and eroding. Cutting processing involve single or multiple point cutting tools such as milling or drilling bits. Abrading processes involve grinding, polishing or sanding. Burning and eroding processes involve utilizing electricity, chemicals, heat, or hydrodynamics to shape or remove material. Milling and drilling processes remove material by using a single point or multipoint tool to shear material (chips) away from the workpiece, the material being formed into the part. The workpiece is typically xtured so that the cutting tool can remove material by rotating the tool while feeding the workpiece toward the cutters tool face. High tolerances and sharp corners can be achieved by these processes. These processes are typically coupled with other conventional tooling processes. Similar processes include lathing, turning, planing and reaming. Grinding, polishing and sanding processes are very similar to milling and drilling operations in that it is a chip removal process with the cutting tool being the individual abrasive grain. More chip deformation occurs with highly abrasive processes because of the highly negative rake angles of the grains. When grinding, high temperatures can be reached at the surface. These raised temperatures can cause tempering, burning or heat-checking at the surface of the workpiece. Heat checking is cracking at the surface which leads to low toughness and low fatigue and corrosion resistance. The temperature gradients within the workpiece. Similar processes include lapping, Electrical discharge machining is a material removal process which erodes metals by spark discharges. A shaping tool called the electrode delivers DC power to the workpiece. The workpiece is submerged in dielectric uid. When the voltage potential difference between the electrode and workpiece is sufciently high, a transient spark discharges through the uid, removing a small amount of the workpiece. Even though EDM has a localized effects on the workpiece, the rst 500 m of a tool steel workpiece may have undergone signicant phase changes. The average rate of removal is 10-6 to 10-4 mm3 with discharges repeating between 50kHz to 500kHz. Electrochemical machining is another material removal process which unlike electroplating deposits or build up material, erodes material. The workpiece is submerged in an electrolytic uid which is a current carrier. As the electrolyte moves over the workpiece, metal ions are washed away. This constant owing of electrolyte keeps the ions from plating on to the tool. The tool serves as a cathode and the
Chapter 2. 2 Conventional Tooling Process

Chapter 2 Background

workpiece serves as a anode. This process does have a tendency of eroding sharp corners, developing uneven at sections, loosing tight tolerances. Another similar material removal process is electrochemical grinding. Thermally assisted machining or hot machining uses a heat input to lower local yield strength to allow for easier or more efcient machining requiring lower cutting forces. The heat input can be a torch, electron beam, laser, or plasma arc. Because high temperatures are involved and uniform workpiece temperatures are hard to achieve, the microstructure of the full workpiece may be affected. If the high energy beams sources and machining conditions are well regulated, only local microstructure will be affected. Hydrodynamic machining or abrasive water jet machining is a material removal process which uses a jet of water to remove material. The water pressure can be as high as 1600 MPa. Up to a depth of 7.5 m/min of material can be removed. This process also has a localized temperature and deformation on the workpiece. These processes are needed because they typically can provide higher dimensional accuracy and smoothness of surface nish than casting, forming, or other shaping processes. Also, they can produce features with sharp corners or atness which cannot be formed by other shaping processes. Material removal process typically have a localized inuence on the workpiece or part. Phase transformation, plastic deformation, and surface residual stress resulting from removal processes, typically occur very close to the cutting surface and not within the bulk inuence. The chips or material removed absorb most of the heat.

Chapter 2. 2 Conventional Tooling Process

Chapter 2 Background

Tool E n e r g y
(%)

pi Work

ece

Chip

Removal Speed
Figure 2.2 Percentage of heat generated which is absorbed by workpiece, tool and chip as a function of removal speed. (Adapted from Manufacturing Engineering and Technology,2.3)

Chapter 2. 3 Casting
Casting is one of the oldest methods of manufacturing dating back to 4000 B.C. Casting is not limited to metals, but can also be used with plastics, glasses, and ceramics. Casting is most often used because it can produce very complex shapes. These shapes may also have cast features like internal cavities and hollow sections. Large parts can be produced by casting. Many hard to work with materials can be shaped much more easily with casting than other processes. Metal casting processes are of most interest to the topic presented and will be discussed in detail in this section. Casting processes for other materials will not be discussed. Metal casting processes can be divided into two categories expendable and permanent. Chapter 2. 3.1 Sand Casting One of the earliest forms of casting metal is sand casting. Sand casting consists of using a pattern shaped like the nal cast shape to make an imprint in sand. This imprint or cavity will be lled with molten metal. The sand will also having gating or ow systems for the metal to enter the cavity of the sand mold. Many large parts are cast with this method like engine blocks and pump housings.

Chapter 2. 3 Casting

Chapter 2 Background

The sand used for these molds are typically have a silica base making them have high resistance to temperature. When the casting cools, they shrink, and the sand mold collapses around the part. If the sand did not collapse hot tears or cracks would form in the casting. The sand is molded into the cope (the top of the mold and the drag (the bottom of the mold. Cores which are used to represent interior surfaces like hollows or cylinders can also be made out of sand. They are held in place in the sand mold to cast these features. All types of metals can be sand cast. Shape complexity of sand cast parts can be quite complex. There is no limit on part size, but small size parts are very hard to cast because of the difcult of maintaining gating and regulating metal ow into these cavities. The accuracy of tolerances of sand cast parts is lowest when compared to all other methods of casting. Typical surface nishes range from 5-25m. Lastly, one sand mold is usually made for one part. As an expendable mold, the sand mold is destroyed after casting. The sand material is typically reusable. The grain development in sand casting has dendrite grains and must be heat treated. Core (sand)

Open riser Cope

Vent

Pour basin (cup) Blind Riser Flask Sand Parting Line Choke

Drag

Mold Cavity Runner


Figure 2.3 Sand Casting Mold System

Gate

Chapter 2. 3.2 Shell Casting Shell-mold casting was developed in the 1940s. A ne sand is coated and red upon a mounted pattern made of ferrous or aluminum material. The red ne sand is now a highly accurate mold. It is removed from the metal pattern. The shell is removed and often supported by sand, and gated. The shell is from 5-10 mm thick.
Chapter 2. 3 Casting

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Chapter 2 Background

High precision gears and other precision small parts. With proper gating, multiple parts can be cast at one time. Most metals can be cast by shell casting. Although, the these molds have high tolerances, the ne grain sand does not permit much venting. Trapped gasses can cause improper lling of the mold. These molds are also susceptible to porosity and tears. Casting weight should not exceed a few hundred kilograms. Shape complexity is limited. Achievable surface nish is in the range of 1-3 m. Chapter 2. 3.3 Lost Foam Casting An aluminum or metal die is formed to replicate a mold for a casting. Polystyrene beads are placed in the mold and heated. The polystyrene expands to ll the mold. The polystyrene casting is then placed in a sand lled container with gating. The inowing metal evaporates the foam. The dissolving foam causes the metal to solidify faster than in sand casting leading to directional solidication of the metal. Because of the sand, the vaporizing polystyrene vents easily. Unlike the other processes no parting lines, cores, or riser systems are needed. The process for the most part is inexpensive with the polystyrene, sand and containing units being relatively inexpensive. Only the aluminum shaping die can be costly. Therefore, low volume runs can be expensive. Lost foam castings have no size limit. Casting from this process can have surface nishes from 5- 20 m. Dimensional accuracy from this process are better than sand castings.

A.

B. Figure 2.4 Lost foam casting of a (A.) water pump housing and a (B) bearing plate. (Courtesy of Diversa Cast Tech.)

Chapter 2. 3.4 Plaster Mold Castings A plaster made of gypsum or calcium sulfate with talc and silica our is poured
Chapter 2. 3 Casting

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Chapter 2 Background

over a pattern and set. The pattern is then removed and baked at 120C. Molten metal is poured into the mold. The maximum metal temperature is 1200C so only aluminum, magnesium and other non-ferrous metals can be cast. Patterns for this process have to be of ne quality. Wood patterns cannot be used because the liquid plaster will cause swelling to pattern ruining the mold. Also the plaster does not permit much venting of gases. Thus, the part must be poured in vacuum or under pressure. The high strength of these molds allow them to maintain good dimensional accuracy much higher than sand or lost foam casting. Surface nishes from this process are 1-2 m.These molds have very low thermal conductivity. Therefore the casting cools more slowly yielding a much more uniform grain structure and less warpage. The maximum size limit is about 50 kg. This process is best suited for low production runs because of the expense of producing patterns. Also, the time to make these molds as well as the entire molding process is quite lengthy.

C. A.

B.

Figure 2.5 A. Plaster Molds drying in an oven. B. The drag portion of a plaster mold for an air compressor housing. C. Aluminum 356 air compressor housings from a plaster mold.

Chapter 2. 3 Casting

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Chapter 2 Background

Chapter 2. 3.5 Ceramic-Mold Casting Ceramic Mold Casting is very similar to Plaster Castings except that refractory high-temperature materials like zircon or aluminum oxide instead of gypsum or calcium sulfate. This is a cope and drag technique. A ceramic slurry covers a pattern which has been put in a ask, holding container. Once the slurry is set, the pattern is removed. The slurry is then dried and burnt to remove volatile matter. It is then baked. Often, to improve strength of mold, reclay is added to the backings of the mold. This additional processing is called the Shaw process. These high temperature molds can be used with all metal including ferrous alloys. Parts cast in these molds can weigh as much as 700 kg. Castings can have surface nishes of 1-2 mm. Dimensional accuracy is also very high. This process is very expensive. Typical parts made with this method are impellers, cutters, dies for metal working, or molds for plastic parts. Parting Line

Cope

Fireclay Backup Ceramic Facing

Drag

Figure 2.6 A Ceramic Mold made with the Shaw Process

Chapter 2. 3.6 Investment Casting Investment casting or the lost wax process is an old process dating back to 4000 B.C. First a metal die is made which is used to cast a pattern of the intended part. Wax and plastic is injected into the die. Several wax pattern are created. Special care in handling patterns must be done in order keep them from breaking or distorting. The patterns are then attached to a pattern assembly or tree. The tree will help develop

Chapter 2. 3 Casting

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Chapter 2 Background

gating in the future investment molds. The tree is then invested with refactory materials by dipping the tree into a ceramic slurry. This dipping is repeated over and over to build up thickness of the coating. This mold is now dried in air and then heated to about 100C in an inverted position to melt out the wax. This may take up to 12 hours. Four additional hours are spent ring the mold to 650 -1050 C to drive off any remaining water.

Slurry Coating

Injecting Wax or Plastic Pattern Tree

Figure 2.7 Steps 1-3 of the investment casting process

Detaching of Castings Pattern Melt out Pouring Shakeout


Figure 2.8 Steps 4-7 of the investment casting process

The mold can now be lled with molten metal. Once the metal has solidied, the mold can be broken up to remove the castings. Highly accurate and complex castings can be made. Surface nishes will range from 1-3 mm. Parts cast in this method should be under 100 kg. The development of patterns and the use of labor throughout the process can be very expensive. Investment castings are most cost effective at high production volumes.

Chapter 2. 3 Casting

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Chapter 2 Background

Chapter 2. 3.7 Hard Mold Casting For hard mold casting, a metal mold made from cast iron, steel, bronze, graphite, or refractory metal alloys. The mold is machined with gating. Internal cavities are maintained by cores made from metal, plaster or sand and placed in the mold prior to casting. Various parts of the mold which are sensitive to high wear can have inserts. To increase the life of the mold, the surfaces of the mold is coated with a ceramic slurry like sodium silicate. These coatings serve as a parting agents or thermal barriers to control the rate of cooling of the casting. Ejector pins may also be placed in these molds. The mold halves are clamped together and then heated to 150200C to aid metal ow through the mold and reduce thermal damage to the mold. The molten metal is then poured through the gating system to ll the mold. Once the casting solidies, the mold is opened and the casting is removed. The mold may be water cooled or cooled by ns. All metals can be cast in this method, but high metaling point metals like steels need dies built or heat resistant materials. Surface nishes range from 2-3 m. Maximum part weight made in this method is about 300 kg. Achievable shape complexity is from moderate to low. Typical parts made in this method are kitchenware, connecting rods and gear blanks. Accuracy of castings is very high. Minimum part thicknesses allowable is 2 mm. Machinery costs and labor can make this process quite expensive. This process is most economical for high volume runs.

Chapter 2. 3.8 Low Pressure Casting Low pressure casting or pressure pouring is a process similar to hard mold casting. The process involve mold haves which are clamped together and lled by molten metal forced upward by gas pressure. The mold may be made from graphite or metal. The pressure is maintained until the metal has completely solidied in the mold. The metal may also be driven upward to ll the mold by a vacuum. The vacuum helps remove dissolved gases lowering porosity. Very high quality casting are made with this process. Surface nishes range from 1-3 mm. All metals can be cast in this process. Castings have very high accuracy, but moderate to low complexity. The process is very expense because of equipment. Typical parts made by this process are railroad wheels.

Chapter 2. 3 Casting

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Chapter 2 Background

Casting Mold

Air Tight Chamber Ladle


Figure 2.9 Low Pressure Casting Systems

Air Pressure Refractory Tube Molten Metal

Chapter 2. 3.9 Die Casting Die casting was developed in early 1900s. Molten metal is forced into a die cavity by pressure ranging from .7 -700 MPa. In order to achieve, to die cast a special machine is required. Two basic types of die cast systems are available: hot-chamber and cold chamber systems. The hot chamber process involves using a piston which traps a specic volume of molten metal and injects it into a die cavity. The shot chamber or piston path way is heated. The die cavity is formed by two die halves called an ejector die and cover die. The ejector die is movable. The die halves clamp together to receive the shot of metal. The cavity is kept under pressure until the metal solidies. The dies are cooled by circulating water or oil through various cooling channels in the die blocks. This cooling aids in improving die life and in rapid cooling of metals. Usually cycle times can reach up to 900 shots per hour. Zinc, tin and other low metaling point alloys are cast using the hot chamber process.

Chapter 2. 3 Casting

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Chapter 2 Background

Nozzle Die Cavity Hydraulic Shot Cylinder

Furnace Ejector Die Cover Die

Molten Metal Pot

Figure 2.10 Hot Chamber Die Casting System

The cold chamber process involves molten metal which is placed in an injection cylinder. The injection cylinder or shot chamber is not heated. The metal is then forced into a two part die cavity. The cavity is very similar to the ones used in the hot chamber process. The metal injection pressures average about 20-150 MPa. Aluminum, magnesium and copper are commonly cast in this process. Other high melting temperature metals can also be cast in this manner. Ejector Platen (moves) Ejector Box Stationary Platen Cavity

Ladle

Hydraulic Cylinder Shot Sleeve Plunger Rod

Ejector Die Half

Figure 2.11 Cold Chamber Die Casting System

Dies are typically made from H13 or other hot working steels. Wear on dies increases with the temperature of the molten metal. Surface cracking from repeated heating and cooling of dies, heat checking, is a major result of die wear. Conventional die cast dies can last for more than 500,000 shots before signicant wear occurs. Die cast parts have high accuracy and can maintain tight tolerances. Bearing surfaces can be produced by die casting. Surface nishes are between 1-2 mm. Maximum casting weigh from less than .05 kg to 50 kg. The minimum thickness of

Chapter 2. 3 Casting

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Chapter 2 Background

sections can be a thin as .5 mm. Volume production for die casting is typically high. The expense of making die inserts, getting needed equipment and the time to produce die inserts makes only large volume runs economical.

Chapter 2. 3.10 Centrifugal Casting Centrifugal casting process has been used since the 1800s. The process uses spins a mold about an axis of rotation. Molds are typically made of graphite, steel or iron. All types of metals can be cast in this method. Often the inside of the mold cavity is coated with a refactory lining to reduce mold wear. Typical parts cast in this method are pipes, gun barrels and street posts. Centrifugal cast parts have high degree of accuracy and very little porosity. The surface nish will range from 2-10 m. Maximum part weight is above 5000 kg. The cost of the mold and equipment is quite expensive so only large volume runs are economically feasible.

Mold

Molten Metal Mold Spout Drive Shaft Rollers

Drive Roller
Figure 2.12 Centrifugal Casting

Free Roller

Chapter 2. 3.11 Crystal Growing Casting Crystal Growing casting processes originate from the 1960. The has a corkscrew gate into the cavity chamber. The corkscrew constriction is designed so that only favorably oriented grains can grow. The die cavity is contained on a moving platform. The die cavity is heated by heat bafes which radiate heat. As the constriction only permits a single favorably oriented crystal to grow.
Chapter 2. 3 Casting

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Chapter 2 Background

As the platform lowers, the radiant heat of the bafes causes the single to grow and ll the die cavity. All other grains are stopped at the walls of the constriction. When the mold is complete, a single crystal casting in the shape of the die cavity The parts have a high degree accuracy, good surface nish. Equipment is and the die cavity is very expensive. Part strength is higher than conventional castings because it is a single crystal.

Radiant Heat

Growing Single Crystal


Chill Plate
Figure 2.13 Single Crystal Casting

Constriction to orient and grow 1 preferred grain

Chapter 2. 4 The Use of Conventional Tooling to Make Prototype Parts


To produce simple models or mockups which to progress the design process, stock, material can be machined to produce prototypes. When material removal processes are used to make prototypes, the grain structure of the metal prototypes resembles that of the stock material. If the stock material is rolled, then the prototype will have a rolled grain structure. Parts made in this manner typically will not have the strength or yield characteristics of the production part. For example, an aluminum valve cover machined from wrought stock will not have the structure of a die cast valve cover. Prototype parts for shell or investment casting can be cheaply done with sand castings. The grain structures will be very similar. Validation or other lifecycle testing could occur on these prototypes because of the similarity of the grain structure. It is more difcult to develop prototyping techniques which will yield similar grain structure and size that the conventional metal mold process produce. However, to simulate die cast prototypes, special heat treatment must be used to gain microstructure similar from any other type of casting or stock machined material.
Chapter 2. 4 The Use of Conventional Tooling to Make Prototype Parts

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Chapter 2 Background

Producing prototype die cast parts is a tradeoff between time, money, and material properties. The heat treatment of stock materials will be costly and time consuming. Using sand casting technology to produce one die cast prototype would be relatively inexpensive. However, the additional processes needed to attain similar microstructures and material properties will consume design lead time. Figure compares the average yield strength of die cast parts to cast S. Crystal

Increasing Grain Size

Sand

Ceramic

Shell Inv Casting

Cutting EDM Milling ECM Drilling Hydro Lost Foam Thermal

Permanent Mold

Centrifugal

Die Casting Cost to Produce 1 Part -Without Heat Treatment


Figure 2.14 The Cost to Produce 1 Part versus the as cast or produced grain size

Die Castings

Plaster Casting Grain-Refined

Plaster Castings Grain Refined Chilled-cast Sand Castings

50

100 Yield Strength (MPa)

150

200

Figure 2.15 Comparison of Yield Strength for various types of Castings .

Chapter 2. 4 The Use of Conventional Tooling to Make Prototype Parts

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Chapter 2 Background

Chapter 2. 5 The Need for Rapid Tooling.


As the preceding Figure 2.1 shows, the ability to make design changes is most cost effective during the early stages of the design cycle. Today, concurrent or simultaneous engineering that have multi-discipline design teams can now design manufacturing processes along with new parts (2.2). The ability to test part features and function in engineering materials and at the same time closely prototype the manufacturing processes can occur under these new design paradigms with rapid tooling. Conventional tooling methods are too costly and require too much lead time to practically use them to construct prototype parts. A typical die cast insert can take up to 4 months to build and heat treat. Testing preliminary designs with conventional tooling methods would eventually reduce the number of prototypes possible during limited design times. An alternative method is required to produce functional prototyping tooling, rapid prototyping. Rapid tooling is the needed alternative process. Rapid tooling is the use of solid froufrou processes to rapidly construct die insert or other forming tools to build actual parts in simulated manufacturing rigs. Rapid tooling methods are typically faster and less expensive than conventional tooling methods.

Chapter 2. 6 Solid Freeform Fabrication


Solid freeform fabrication is a process of building three dimensional objects in a layered fashion. The three dimensional object is built in 2 dimensional layers typically in an automated fashion. Therefore, complex parts can be built quite when resolved in to two dimensional structures. Objects which cannot be built with conventional manufacturing paradigms like high speed milling can not make conformal cooling passages. Solid freeform fabrication techniques can build cooling passages which follow intricate part surfaces because of the 2D layering approach. For solid freeform fabrication a computerized model typically represented by CAD (computer aided modelling) is then divided into layers by a hierarchical algorithm. This algorithm divides the part by prioritizing layer order with shaping and depositing precedences. The part is then built in the z direction, layer by layer with a rapid prototyping process. The Figure 2.16 models the process.

Chapter 2. 5 The Need for Rapid Tooling.

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Chapter 2 Background

CAD System Automated Process Planner

Rapid Fabrication Process Automated Prototyping Machine

data exchange format

motion control trajectories

Computerized Solid Model

Physical Object

Figure 2.16 A CAD model is divided into layers and then programed and built by a rapid prototyping process.

Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tooling


Several commercial process have been used in rapid tooling. Stereolithography, selective laser sintering, and laminate object manufacturing are all primarily polymeric in nature and have been either used as a tool to create an insert or have been used directly as the tooling insert. Chapter 2. 7.1 Stereolithography Stereolithography is a polymer based process which uses a laser or ultaviolet light to cure an epoxy or plastic resin. This process was commercialized by 3D Systems in and Beta tested by General Motors in . The part substrate or starting point is a movable elevator platform which rests on the surface a large vat of curable resin. The laser draws a pattern in the epoxy resin which solidies and acts as bonded supports on the platform. The supports are between 5 mm -10 MS thick which is about 20 to 100 layers. With each drawn layer the elevator submerges the part to rewet the surface. Once the support layers are drawn, the rst layer of the part is then scanned. The scanning process begins with the laser curing the outline of a 2D cross section of
Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool22 ing

Chapter 2 Background

the part. The inside of the cross sections are then rastered or weaved scanned. The platform and scanned layers are then rewet by resin with the submerging of the part beneath the liquid resin surface. After a 30 second (or shorter) wait time, the part is raised to just below the surface the distance of one layer. Next the laser begins scanning of the next layer. This process continues until the part is completed. Once the part is completed, it is drained and then removed from the vat. The part is then rinsed in a solvent to remove any uncured resin from the part surface. It is then detached from the platform and placed in an ultraviolet curing oven for a post cure. This process insures part strength and rigidity. UV Light Source Formed Part

Liquid Surface

Vat UV Curable Liquid Platform


Figure 2.17 Stereolithography

Figure 2.18 SLA Part building on platform

Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool23 ing

Chapter 2 Background

Chapter 2. 7.2 Stereolithography Rapid Tooling This process can be used for undercut and novel overhanging features which cannot be easily produced with conventional machining. Thus, this process has been used to advance rapid tooling in several ways: as EDM electrodes, the negative blank to form the tool or as the positive insert. Researches have begun using Stereolithography patterns to make investment cast die inserts. Electrical discharge machining (EDM) is a tooling process which expends high amounts to shape metal by burning or vaporization. Tool steel die inserts often used EDM to build complex shapes and contoured surfaces. By plating Stereolithography electrodes with copper, these electrodes have been used successfully to rough, semirough and nish metal parts (2.4). Prototype vacuum casting molds have been made with stereolithograhy (2.5). These type of molds are ideal for stereolithography because pressure requirements and casting temperatures are low. This process typically uses pressure to have the material ow to all parts of the mold cavity. Rapid pressure changes typically do not occur. Polyurethane plastic parts have been made with these stereolithography rapid tooled molds. In addition to vacuum casting stereolithography rapid prototyping technology was used to create injection molding inserts, These insert unlike the vacuum casting require much higher cycle pressures. Thermoplastic parts have been built with these tooling inserts. Thermo-plastic specimens made using epoxy inserts and steel inserts were compared in tensile strength, impact strength, and bifringence stress. The epoxy tooled specimens had properties within 5 -10% of the parts molded with steel inserts. These epoxy tooled parts had greater tensile strength, lower impact strength and lower birefringence stress levels than there steel tooled parts (2.6). Polyurethane and thermoplastic materials seem to perform well in stereolithography tooling. Experiments have shown that as many as 500 parts have been shot from a single epoxy die (2.7) . However, more demanding plastics like ABS, polycarbonate and glass lled nylons have not fared as well because of the higher melting temperatures have caused warping or galling of the parts. Thin walled features like ribs and bosses are very vulnerable. One research investigation using vapor deposited metal coating of nickel, copper, and zirconium nitride upon stereolithography epoxy insert set. Regardless of the coating wear damage was evident fairly quickly. The maximum number of parts, 14 parts were produced with the copper coated tool before tool failure (2.8).
Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool24 ing

Chapter 2 Background

B.

A. Figure 2.19 A, Vacuum Casting Using a SLA Models B. Injection Molds made with SLA Technology

The ability to use stereolithograpy inserts seems to be a tradeoff analysis between timing, tolerances, temperature(2.9), material, and volume. Stereolithography tooling can produce prototype plastic parts quickly, giving the designers the ability to get near-production parts quickly. However, the designer ability to sufcient cool the part will dictate the materials and volume which can be successfully produced via these inserts. Although more research is occurring, currently, the best option to produce tightly tolerances parts in materials like ABS or nylon still require metal inserts.

Chapter 2. 7.3 Selective Laser Sintering Selective laser sintering is a SFF process which sinters powered material in a layer by layer automated fashion to produce a part. Metal and plastic powders can be used in this process. The powder is coated with a polymer binder and laser intensity is used to melt the binder and fuse the powder together. The process pioneered by University of Texas was commercialized by DTM Corporation. The commercial process has a powder bed with a roller which spreads a thin layer of material on to a platform. The laser then scans the outline and rasters the

Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool25 ing

Chapter 2 Background

interior of a 2 D layer. Once the layer is completed the platform indexes downward. The roller then once again spreads a thin and even layered of material across the top of the last layer. The laser then draws the next layer. This process of lowering, spreading, and scanning continues until the part is completed. The part must be removed from the platform and surrounding powder bed and shaken or air blown to remove excess powder. Unlike the stereolithography process the build chamber is heated to just below the glass-transition temperature or melting point of the material or binder. This reduces the amount of laser power energy needed to consolidate the part. It also reduced part stress because local part temperature is only raised slightly above the bulk part. The chamber is also lled with nitrogen to make sure that chemical reactions do not occur. Typically this process builds parts from polymer materials. ABS, nylon, glasslled nylon, and polycarbonate plastics have been used in this process. Metals, like low carbon steel have also been used. However, these parts have to undergo additional sintering and inltration processes. Metal powder used in this process are simply not heated enough to attain fusion. Only the polymer powder coating the powders is melted. Additional heat treatment is needed to sinter the metal material and vaporize out polymer binder. Once this done, the process must be inltrated to ll pores. The circular powder when lased simply cannot fuse or shrink together enough to eliminate pores because of the spherical nature of the powders. Copper inltration is used to ll pores and produce a dense part. The nal metal part is a hybrid or composite with reasonable strength and thermal conductivity (2.10, 2.11).

Figure 2.20 SLS Parts Being shaken out of Powder Support Bed.

Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool26 ing

Chapter 2 Background

Chapter 2. 7.4 SLS Rapid Tooling Most rapid tooling activity have developed from the non-metal SLS process. Part masters in wax have been used to make rapid investment casting molds for General Motors. The SLS master is dipped into a ceramic slurry and coated. The slurry coated part is then heated in a furnace, fusing and solidify the ceramic slurry while burning or vaporizing the original SLS master. The surviving slurry is now a perfect pattern to produce cast metal Injection molding inserts have been built using the metal SLS process (2.12). Cavity inserts and mold components have been successfully made with SLS for low part volume injection molding. Fixturing methods have to be considered when using these inserts. Good contact must be established so that these inltrated molds will dissipate heat well and reduce residual stress from thermal cycling. Surface nish in inltrated dies needs to be improved. Currently a lot of post processing is required nish the cavities to acceptable levels. Over fty polypropylene injection molded parts have been in one of these inltrated die sets (2.13). Die casting molds have also been built for magnesium applications. Aluminum die casting, because of metal reactivity can not be used in copper composite inserts. Accuracy problem have limited the development of tooling insert using this approach. Varying part geometries and wall thicknesses of die inserts lends themselves to nonuniform shrinkage during the sintering process. Tooling for injection molding or die casting need to have accurate tolerancing or simpler modelling techniques could be used to build the prototypes. Sandcasting for metals and direct SLA parts for plastics can built parts with higher accuracies than using SLS tooled inserts.

Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool27 ing

Chapter 2 Background

Figure 2.21 Rapid Steel Inltrated SLS Injection Molding Inserts

Chapter 2. 7.5 Laminate Object Manufacturing Laminate object manufacturing (LOM) is the process of building prototypes by assembling 2 dimensional sections of adhesive material together. The material is typically long sheets of adhesive backed paper. During preprocessing, the part is divided into 2-D layers which are the thickness of the paper. The part is built upon a wooden substrate which is screwed on to a steel plate. The plate is supported in the LOM machine for stability. A few layers are adhered to the substrate by the machine advancing the paper on to the board. A heated roller then presses the paper on to board melting the adhesive to it. A laser then scans the outline of the paper and hatch a pattern over the interior of the outline. The paper is then advanced forward. The outline acts a separation so that only the unused paper, everything in the exterior of the outline advances. This is repeated for a few layers to aid with part removal. Now 2D part cross sections are scanned by the laser over the substrate. The exterior of the cross section is hatched by additional laser scans. This continues until the part is completed. When the part is completed, it surrounded by excess paper composite which is similar to a type of sacricial material. It was needed to support the part during the building cycle. It is removed in a process called decubing. The hatching process allows the sacricial material to be removed as cubes. This process can be very time consuming. When the part is nally decubed and removed from the
Chapter 2. 7 Commercial Rapid Prototyping Processes used in Rapid Tool28 ing

Chapter 2 Background

substrate, it must be sealed to prevent swelling from humidity and moisture. Epoxy or wood sealants are typically applied to the LOM parts.

Laser

Part in Cube Paper Support Roll of Paper or Material


Figure 2.22 Laminate Object Manufacturing

Used Paper Roll

Chapter 2. 7.6 LOM Tooling LOM paper material parts are most often used with investment or sand casting. This type of tooling is often used to make cores or patterns. These paper parts look like wood parts which is similar to traditional pattern parts. LOM is excellent for tooling applications, because it can build very large tooling beds. Where the SLA and SLS have size constraints, LOM has a build size of 50.8 cm x 50.8 cm x 50.8 cm. Also, the paper parts are combustible and are quite suitable for investment casting because they can be burned out during the ring of the investment shell. LOM inserts have been used in blow molding, hydroforming, and injection molding. LOM inserts have been used successfully to die cast magnesium inserts (2.15).

Chapter 2. 8 Adapted Rapid Tooling Processes


Many rapid tooling processes have arisen from the combination of traditional prototyping methods and commercial rapid prototyping processes. The most advanced of these are the Nickel Transfer Molding and Keltool Process.
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Chapter 2. 8.1 Nickel Transfer Molding Nickel Transfer Molding is a process which has been commercialized by CEMCOM corporations. From the CAD le of the part an SLA master is developed to simulate the die insert set top and bottom faces needed to build the part. The SLA is then placed in a nickel plating bath and plated. Several millimeters are plated on to the model. The plated model is then suspended into a supporting frame box. The box is then lled with a ceramic slurry which solidies around the model. The SLA model itself establishes the parting line. Once the slurry has hardened the two halves formed by the SLA parts parting line. The newly formed die set is removed from the SLA model. The interiors of each halve are polished. The completed inserts can now be used in standard injection molding frames. Part is translated into an SLA part which represent negatives of mold cavities.

SLA part is supported in Nickel plating bath. When plating has finished, The SLA part is fixtured in a supporting frame. The SLA nickel plated part form a parting line within support

The cavities are filled on both sides with a ceramic slurry.

Figure 2.23 Nickel Plating Transfer Process: (Courtesy of CEMCOM)

Although these molds wear faster than soft tooling P20 molds, die sets made in this manner have made over 45,000 glass lled nylon parts.

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Once the slurry has hardened, the two halves are demolded, leaving 2 die inserts.

Figure 2.24 NPTP Demolding Process: (Courtesy of CEMCOM)

Ejector pins and other die cavity utilities are drilled or inserted. A complete die set is now ready for injection molding.

Figure 2.25 NPTP: Ejector Pins are Placed in Die Cavities

Chapter 2. 8.2 Keltool Keltool is a process commercialized by 3D Systems, which also uses a SLA model as a master. Keltool is a sintering technology which creates die inserts from powdered material. The cavity and core of the tool to create the prototype part are designed from the 3D CAD le. These core and cavity is then built by stereolithography. These SLA parts are typically highly detailed. These SLA parts are now called the master patterns. Next these SLA masters are used with Room Temperature vulcanized silicone rubber molding process. Molds of these cavities and cores are created by suspending them in a frame and lling the frame silicone rubber. The SLA masters are removed from the newly formed silicone molds. These molds are then lled with a mixture of
Chapter 2. 8 Adapted Rapid Tooling Processes

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A6 tool steel powder, tungsten carbide powder, and epoxy binder. When the epoxy binder mixture has cured within the mold, a green part is made. The green part is then de-molded and sintered. The part which is the insert is sintered in a hydrogenreduction furnace. During the sintering process, the binder material is burned off leaving a brown part which is a composite of A6 steel and tungsten carbide. The composite insert now has voids from the burned out binder. The insert is then inltrated with copper to make the part fully dense. The nal insert is 70% steel and tungsten carbide and 30% copper. The insert is heat treatable and can achieve hardness of 40-44 Rc.

Keltool Insert

SLA Cavity & Core Models Injection Molded Parts


Figure 2.26 The Keltool Process (Courtesy of 3D Systems)

Chapter 2. 8.3 Metal Spray Tooling Early in the 1900s, Dr. M.U Schoop found that by pouring molten metal into a high pressure gas stream found that the metal would particulate into drops and deposit in coatings. Schoop found similar results by passing metallic powder through ame. Both of theses experiments led to the development of equipment to spray metal in wire form. Common object sprayed in the 1930s were dental light bulbs, refrigeration cold plates, turbine wheels, and brake drums with soft metals like zinc, lead, or copper. Most metal spraying had been accomplished by electric arc or ame from

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oxyacetylene torches. By the early 1960s, a similar process is plasma spraying of coatings began depositing hard metal or ceramic coatings. Thermal barriers and oxidation or corrosion resistant coatings are the most common uses of metal spraying. These coatings can also be designed to reduce wear and friction. Surfacing of die inserts can be accomplished with spray processes. In addition to now surfacing pumps with wear resistant coatings, heat and corrosion resistant coating on electrical boards, massive depositions of spraying have been attempted.

Chapter 2. 9 Other Rapid Tooling Processes


In addition to Stanford University, other academic or national lab researchers have been developing processes to produce tooling inserts. The most advance of these processes are the 3D Printing Process and LENS. Chapter 2. 9.1 3D Printing The 3D Printing process was developed by Massachusetts Institute of Technology in 19 . The process is very similar to inkjet printing technology. To build a metal tooling insert, liquid binder is selectively secreted on powdered material. On a layer by layer basis, the binder is applied in a process very similar to the way ink is ejected on to the paper from an inkjet printer. The liquid hardens binding the powder to the part. When the part is completed, it now a matrix of metal and binder. The part is then sintered removing the binder. The part is then inltrated with a metal or epoxy to make a dense part (2.16). Molding inserts have been built with this process. A ceramic mold made from alumina powder and colloidal silica binder was built using the 3D Printing process. The mold was made up of 100 powder binder layers. The mold was used to create a bras casting in a gravity poured process. For the gravity poured process, the brass is heated to melting temperature and poured in to the mold set under atmospheric pressure (2.17). This tooling process has been licensed by Extrude-Hone company Chapter 2. 9.2 LENS Process Laser Assisted Net Shaping process is a direct metal fabrication process which can produce fully dense parts which can be used as die inserts, patterns, or metal casting. A ND:YAG lase is used to melt metallic powder or powder mixtures. This is an additive process building the part layer by layer.
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The LENS process uses a computer model to develop a laser deposition path which represent the part in 2D cross-sections. The sections are deposited successively in Z direction. The laser paths are changed with each layer. Alternative layers are deposited at 90-degree angles to the previous layer. The part is built on a moving platform which can move in X-Y translation. The powder injection nozzle moves upward to compensate for the building of part height in the z direction. The process has been used to make fully functional metal parts and metal molds for injection molding. The LENS process has even been used to repair injection molding molds. However surface nish and dimensional accuracy are a problem for this technology. A LENS mold may require manual processing to produce good surface nished and dimensional accuracy. Optomec is attempting to commercialize the process.

Laser Beam

Powder Delivery Y Translation

X Translation
Figure 2.27 LENS Process (Courtesy of Optomec)

Chapter 2. 10 Shape Deposition Manufacturing


Shape Deposition Manufacturing is an SFF process which was started at Carnegie Mellon University and developed by Stanford University to produce laser

Chapter 2. 10 Shape Deposition Manufacturing

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deposited structures. Unlike other SFF processes like stereolithography and laser sintering, Shape Deposition Manufacturing is a layered manufacturing process which builds fully dense metal parts by incremental deposition and CNC shaping of material layers (2.18, 2.19). First, a computer aided design model of a part is sliced into layers. The layers are in the z-direction and derived by custom planning software. Next a layer is deposited. The layer is deposited as near-net shape. This near-net shaped layer is then milled to nal dimensions by a 5-axis CNC mill. Support material is then deposited around the layer to protect the features of this layer and provide a base for overhanging features in following layers. The next layer of the part material is then deposited, and the process continues.

Deposit Deposit
Metal With Laser

Shape Remove

Deposit Part with and Shape Support Support Material Material

Remove Remove Support Support Material Material

Figure 2.28 The Shape Deposition Manufacturing

The combination of layered manufacturing and sacricial support material enables the production of complex features such as undercuts or conformal cooling channels (2.20). Also this technique lends itself to the production of multi-material structures. For instance, an insert can be produced which is primarily a hard ferrous alloy with copper deposits for enhanced thermal conductivity. Using the multimaterial strategy, sensors can also be embedded in the die during the build sequence to develop smart dies. A laser / powder deposition system was used to deposit material for testing and for construction of a test die (2.21). The system uses a 2.4 kW Neodymium YAG Laser to fuse metallic powders into fully dense material. The laser is delivered by ber optics to an end effector mounted on a four-degrees-of-freedom robotic arm. The end

Chapter 2. 10 Shape Deposition Manufacturing

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effector focuses the light on the substrate, creating a melt pool. Metal powder is added to the melt pool via a powder feed tube and a bead of deposited metal is created as the robot transverses the substrate. This technique, which is similar to laser cladding, has been very effective in forming fully dense metal layers. Nitrogen gas shrouds the deposition to help prevent oxides from forming during the deposition process.

laser direction of travel

powder

deposited layer

substrate

Figure 2.29 Powder placement during the SDM Process

Chapter 2. 11 SDM Tooling Efforts


Several tooling inserts have been built using the SDM process. The GM injection molding insert, the Alcoa tool injection molding insert were built for industry partners of the Stanford Rapid Prototyping Lab.

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end effector

nitrogen shroud

powder feed tube

Figure 2.30 Equipment Setup for the SDM process

Chapter 2. 11.1 GM Injection Molding Tool The SDM process was used to produce an injection mold for an electronics compartment cover with snap t tabs. The part was split into three main elements a support level, cooling channel level, and a feature level. The support level is simply the base of the injection molding insert. This level has no distinct features and merely needed to allow the insert to t into the molding base. The cooling channel level contains the concentric cooling channel design needed to control temperature within the insert and reduce warpage of the insert. The feature level is the top part of each insert which will serve to mold and eject the part. By segmenting the insert design in this manner, one can plan the deposition and shaping of the part to enhance build time and reduce tool wear. The support level of the insert 15 mm thick plate of 316L stainless steel. As described above a substrate is deposited upon to build parts with the SDM method. Thus the support level and part substrate are combined. Next, 316L stainless steel powder is then deposited and fused to form the channel level of the part. After, a thickness of 10 mm is deposited, cooling
Chapter 2. 11 SDM Tooling Efforts

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channels are then machined in the deposit. The passages are then lled with microcast copper to preserve the integrity of the channels as the next layers of the part are deposited. The feature level was laser deposited and near net-shaped by CNC on layer by layer basis. Layer thickness averaged .25 mm. When the structure was completed, the copper channels where etched, removing the copper so that channels could be used. many features because of size or taper angle had to be EDM. The inserts where placed in a 10 ton injection molding machine. The inserts were prepped to t into the mold base. About 20 nylon parts were run to see if the inserts worked. As expected with such a short run, no visible die wear occurred.

Sinker EDM Feature

Zone 3 Zone 2 Zone 1 Wire EDM Feature


Figure 2.31 GM Tool

Chapter 2. 11.2 Alcoa Injection Molding Tool A set of injection molding inserts were made for Alcoa using the SDM process. The inserts are a composite stainless steel tool. Residual stresses caused warpage or deformation to the GM tool during the deposition process. This warpage added additional machining and heat treating hours to the deposition process. To combat this during the deposition of the Alcoa inserts, the interior of the insert is deposited with invar instead of 316L stainless. Because of the intricacy of the inserts, only two planning levels are available: the channel level and the feature level. Microcast copper is deposited into cooling channels.
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Once the bulk shape of the insert had been deposited and shaped, the copper channels are etched out of the insert. Next specic tapers and part level features that cannot be CNC machined were electro-discharge machined. The molding inserts where completed and sent to Alcoa in December of 1998. Because of budget cuts the tool was never tested.

Figure 2.32 Alcoa Injection Molding Inserts

Legend Stainless Steel Invar Copper

Figure 2.33 The Interior of the Alcoa Tool

Chapter 2. 12 Other Developing Laser Deposition Technologies There are other laser based technologies which could potentially be used to

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build die casting prototype inserts and other forms of rapid tooling. Some of the outcomes of this research will be able to benet not only SDM laser process but other laser technologies as well. Chapter 2. 12.1 Laser-induced Vacuum Arc Deposition Laser-induced vacuum arc deposition is a process which combines the controllability of pulsed laser deposition with vacuum arc technology (2.22). This allows for very small droplets which produces a ne lms. Typically amorphous carbon lms are made. These lms are very hard and have excellent wear resistance and low friction. This method has been used to deposit hard lms on metallic substrates. This technology could potentially be used to face die inserts to make them more wear resistant yielding longer insert die life. Potentially could allow softer steels like 316L to become more wear resistant so they could potentially be used to prototype die casting or glass-lled nylon injection molding.

Chapter 2. 12.2 CO2 Laser Deposition This process uses a CO2 laser to solidify metallic powder (2.23). The substrate translate in the X,Y, and Z directions as powder is fed into the interaction zone on the substrate. The laser power ranges between 300-400W and is focussed on to the substrate in a donut shape with a 600 mm diameter. Helium gas is used as a shield gas. Stainless steel 304L parts have been built with this method. Tool steel inserts may also be able to be made with this process.

Chapter 2. 12.3 Pulsed Laser Deposition Excimer Nd:YAG or CO2 lasers are used to produce vapor of plasma states to deposit or grow thin lms (2.24). Ceramic thin lms have been grown by pulsed lasers on stainless steel, hard metal, Si, SrTiO3, and ZrO2. This technology can be used for hardfacing tools. If multiple layer lms can be built without of loss of adhesion or delamination, this technology may be able to build feature level of die inserts. A similar process called laser implant deposition uses a KF excimer laser to deposit and incorporate silicon on the surface of stainless steel.

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Chapter 2. 12.4 Laser Direct Casting Laser Direct Casting is a laser cladding process which uses a coaxial nozzle to deposit and laze metal powders (2.25). Metal powder is injected into a laser generated melt pool. The substrate translates in the X, Y, and Z directions in order to build 3D parts. The laser power used in this process 400 W - 1400W and speeds of 500 - 1000 mm/min. Fully dense parts have been built with this process.

Chapter 2. 12.5 Laser Cladding Laser cladding is a process very similar to Laser direct casting (2.26). With this process CAD.CAM systems are uses to develop the laser path also known as cladding tracks. AISI 1045 steel plate and steel rollers have been deposited upon with this process. In addition to metal depositions, metal matrix composites with ceramics have been made. Cutting dies and stamping dies have been made with this process. A similar process was developed at Los Alamos National Laboratory called Direct Laser Fabrication (2.27). It is a near-net shape technology which uses CAD/CAM with a high energy laser beam to produce fully dense parts. Another laser cladding technique used powder blowing to place metallic powder in the path of the laser for fusion to the substrate (2.33). A 5 KW CO2 laser is used to solidify the powder. This process allows for very ne microstructure, no porosity, uniform layer thickness and little dilution of material into substrate. The HAZ produced is very small while the interface between cladding and substrate is very sharp.

Chapter 2. 12.6 Laser induced Chemical Vapor Deposition An argon ion laser beam is used to grow lms of titanium nitride (2.28). These lms arise from direct laser pyrolysis of TiCl/4N/2/H/2 gas at atmospheric pressure. These deposited lms are hard, rough, and porous. Tool steel substrates have been used in this process. The porosity of these coating may lend it unsuitable for tool facing or build tool inserts. Other laser-induced chemical vapor deposition process are at elevated pressures of 40 mbar and pulses at 100 to 600mW for nickel-iron lms (2.29). A similar process using an ArF excimer laser and low power CO2 laser to produce pyrolytic laser chemical vapor deposition (2.32). This process has been used to coat tool steels as well as small industrial tools.

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Chapter 2. 12.7 Laser Fused Spray Tooling Molybdenum powder is predeposited on a steel surface by plasma spraying. This coating is then fused by a continuous wave Nd:YAG laser (2.31). In addition to densication of the predeposited molybdenum, alloying with the steel substrate occurs. Surfaces treated by this method have excellent wear properties. The process is monitor for sound emissions to determine crack intensity during alloying to evaluate laser and coating parameters as well as process quality. As long as deformation of the substrate or die can be controlled, this process could be used to face die inserts. Another process similar to the molybdenum spray process, is laser-surface melting (2.30). A 3KW CO2 laser is used melt plasma spray surfaces of ceramics or metal. These surfaces are produced by transferred plasma jet technology. The laser is used to improve the homogeneity of plasma sprays which inherently contains voids, cracks or pores. Plasma oatings100-200 m thick have been homgenitized with laser surface melting.

Chapter 2. 12.8 Hot wire laser deposition A laser beam is used to melt a hot wire electrode (2.34). Two millimeter thick coatings have been built by this system. The high temperature gradients and intensity of the laser interaction with the wire and substrate causes limited dilution and limited penetration into the substrate. Corrosion resistant coatings have been made using this technology. This technology could be used to hard face metal injection molding or die casting inserts.

Chapter 2. 13 Requirements for Die Cast Inserts


To rapid tool die cast inserts, a designer must understand the material and functional requirements that the inserts must have in order to successfully produce castings. Understanding the service requirements of the environments in which the inserts will be used is essential to designing viable parts. Die casting results in abrupt thermal and pressure changes on the insert during the injection of the molten aluminum. An insert for aluminum die casting may encounter temperature changes from 150oC to 670oC and pressure changes from ambient to 142 MPa in a cycle time as short as 20 seconds. To cycle through these changes in temperature and pressure, die casting inserts must be made of material

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which possess the following characteristics: Low Coefcient of Expansion for high thermal fatigue resistance High hardness (44-48 Rc) for wear resistance (2.35) High modulus of elasticity or impact resistance to avoid deformation from galling and heat checking Moderate thermal conductivity to produce castings of similar microstructures as H13 production inserts (on the order of 24 W/mK) When designing die cast inserts, the material used must be able to survive these conditions. Also, the material characteristics must have similar thermal properties to insure proper microstructual development of castings produced by the inserts. Additional requirements may be added because of processing requirements of laser based deposition, particularly requirements of the SDM process. Initially the only additional requirement is high corrosion resistance. SDM deposits sacricial material to support undercut features or preserve cooling channels shaped within the die. Utilizing the 400 series martensitic stainless steel materials, will also add requirement to insure the production of sound inserts with minimal deformation.

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2.1 Barkan, P and Iasiti, M. (1993). Prototyping: A tool for Rapid Learning in Product Development. Concurrent Engineering: Research and Applications 1: 125134. 2.2 Barkan, P. (1991). Strategic and Tactical Benets of Simultaneous Engineering. Design Manufacturing Journal (Spring): 39-41. 2.3 Kalpakjian, Manufacturing Engineering & Technology, 1995 2.4 Leu, Ming C., Feasibility study of EDM tooling using metallized stereolithography models, Technical Paper - Society of Manufacturing Engineers, Proceedings of the NAMRX XXVI Conference Atlanta, GA, USA 2.5 Kai, Chua Chee, Integrating rapid prototyping and tooling with vacuum casting for connectors, International Journal of Advanced Manufacturing Technology, v14 n 9 1998. pp. 617-623. 2.6 Polosky, Quentin F., Mechanical property performance comparison for plastic parts produced in a rapid epoxy tool and conventional steel tooling, Annual Technical Conference - ANTEC, Conference Proceedings. Special Areas Annual Technical Conference - ANTEC, Conference, Proceedings v 3 1998, p 2972-2976. 2.7 Rahmati, Sadegh and Dickens, Philip, Stereolithography for injection mould tooling Rapid Prototyping Journal. Rapid Prototyping Journal v 3 n 2,1997. p 5360. 2.8 Burns, David T., Malloy, Robert A, McCarthy, Stephen P., Analysis of metal coating effects on stereolithography tooling for injection molding, Annual Technical Conference - ANTEC, Conference Proceedings, Proceedings v 1 1998, p 888-892. 2.9 Janczyk, M., Rapid stereolithography tooling for injection molding: The effect of cooling channel geometry, Journal of Injection Molding Technology. Journal of Injection Molding Technology v 1 n 1 Mar 1997. pp. 72-78. 2.10 Lakshminarayan, U., McAlea, K., Girouard, D., and Booth, R., Manufacture of iron-copper composite parts using selective laser sintering (SLS**T**M), Advances in Powder Metallurgy and Particulate Materials, v. 3, p 13/77-13/85. 2.11 Klocke, F.,Celiker, T., and Song, Y.-A., Rapid metal tooling, Rapid Prototyping Journal. Rapid Prototyping Journal v 1 n 3, 1995. pp. 32-42. 2.12 Hornig, C. and Lohner, A., Direct laser sintering of metal powder, Kunststoffe Plast Europe. Kunststoffe Plast Europe v 87 n 11, Nov 1997. pp. 72. 2.13 Killander, Lena Apelskog, Rapid Mould: Epoxy-inltrated, laser-sintered inserts, Rapid Prototyping Journal. Rapid Prototyping Journal v 2 n 1,1996. pp. 34-40. 2.14 Pak, Sung S, Prototype tooling and manufacturing through Laminated Object Manufacturing (LOM), International SAMPE Symposium and Exhibition (Proceedings), v43 n 1 1998. SAMPE, Covina, CA, USA. pp. 685-692. 2.15 Warner, Merlin C., Rapid prototyping for die casting: today's applications and future developments, Die Casting Engineer. Die Casting Engineer v 40 n 2 Mar-Apr.,1996. 4pp.
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2.16 Sachs, E, Williams, P., Brancazio, D., Cima, M., and Kremmin, K., Three-Dimensional Printing. Rapid tooling and prototypes directly from a cad model, Proceedings of Manufacturing International '90. Part 4:, 1990, p 131-136. 2.17 Sachs, Emanuel, Cima, Michael, Brancazio, David, Curodeau, Alain, and Shalon, Tidhar, Three dimensional printing. Rapid fabrication of molds for casting, American Society of Mechanical Engineers, Production Engineering Division (Publication) PED. Advances in Integrated Product Design and Manufacturing American Society of Mechanical Engineers, Production Engineering Division (Publication) PED v 47. Publ by ASME, New York, NY, USA. pp. 95-10. 2.18 Rahmati, Sadegh, Rapid Prototyping Journal, Vol. 3, No .2, p. 53, (1997) 2.19 Pintat, M. and Greulich, M., Proceedings Solid Freeform Fabrication Symposium, The University of Texas at Austin, pp. 74 (1995). 2.20 Merz, R., Prinz, F. B., Ramaswami, K., Terk, M., and Weiss, L. E, Proceedings Solid Freeform Fabrication Symposium, The University of Texas at Austin, p. 1, (1994). 2.21 Fessler, J. R., Merz, R., Nickel, A. H., and F. B. Prinz, Proceedings Solid Freeform Fabrication Symposium, The University of Texas at Austin, p.117, (1996). 2.22 Rebholz, C.,Scheibe, H.-J., Schultrich, B., and Matthews, A. Mechanical and tribological properties of hard aluminium-carbon multilayer lms prepared by the laser-arc technique, Surface & Coatings Technology v107 n 2-3 Sep 10 1998. pp. 159-167,1998. 2.23 Kahlen, Franz-Josef,Kar, Aravinda, Watkins, Tom, and Burl, C., Stress analysis in rapid manufacturing, Laser Institute of America, Proceedings. Laser Institute of America, Proceedings v 83 n 2 1997. Laser Inst of America, Orlando, FL, USA. pp. E76-E83. 2.24 Kreutz, E.W., Pulsed laser deposition of ceramics - fundamentals and applications, Applied Surface Science. Applied Surface Science v 127-129 May1 1998. pp. 606-613. 2.25 McLean, Mark A, Shannon, Geoff J., and Steen, William M., Laser Direct Casting high nickel alloy components, Advances in Powder Metallurgy and Particulate Materials v 3, 1997. Metal Powder Industries Federation, Princeton, NJ, USA. pp. 21-3-21-16. 2.26 Hu, Y.P., Chen, C.W., and Mukherjee, K., Analysis of powder feeding systems on the quality of laser cladding,Advances in Powder Metallurgy and Particulate Materials, Advances in Powder Metallurgy and Particulate Materials v 3, 1997. Metal Powder Industries Federation, Princeton, NJ, USA., p 21-17-21-31. 2.27 Lewis, Gary K., Lyons, Peter, Direct laser metal deposition process fabricates near-net-shape components rapidly, Materials Technology. Materials Technology v 10 n 3-4 Mar-Apr. 1995. pp. 51-54 2.28 Reisse, Guenter and Ebert, Robby, Titanium nitride thin lm deposition by laser CVD, Applied Surface Science. Applied Surface Science v 106 Oct 2, 1996. pp. 268-274. 2.29 Maxwell, J.L., and Pegna, J., Deangelis, D.A., and Messia, D.V., Three-dimen-

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sional laser chemical vapor deposition of nickel-iron alloys, Materials Research Society Symposium Proceedings. Advanced, Laser Processing of Materials - Fundamentals and Applications, Materials Research Society Symposium Proceedings v 397 1996.,Materials Research Society, Pittsburgh, PA, USA. pp. 601-606. 2.30 Pujar, M.G., Dayal, R.K., and Singh Raman, R.K., Microstructural and aqueous corrosion aspects of laser-surface-melted type 304 SS plasma-coated mild steel, Journal of Materials Engineering and Performance v 3 n 3 June 1994. pp. 412-418. 2.31 Haferkamp, H., Gerken, J., Toenshoff, H.K., and Marquering, M., Laser alloying of molybdenum on steel surfaces to increase wear resistance, , Proc 1995 9 Int Conf Surface Modif Technol 1996. Minerals, Metals & Materials Soc (TMS). pp. 547-564. 2.32 Zergioti, I.Zervaki, A., Hatziapostolou, A., Haidemenopoulos, G., and Hontzopoulos, E., Deposition of refractory coatings by LCVD, Optical and Quantum Electronics. Optical and Quantum Electronics v 27 n 12 Dec 1995. pp. 13771383. 2.33 Yellup, J.M., Laser cladding using the powder blowing technique, Surface & Coatings Technology. Surface & Coatings Technology v. 71 n 2 Mar 1995. pp. 121-128. 2.34 Bouai, Belkacem and Bartzsch, Jorg, Surface protection by laser beam deposition with hot wire addition, Welding Research Abroad. Welding Research Abroad v 40 n 8, Aug-Sept 1994. pp. 31-33,1994.
2.35 Skoff, J. V., Die Casting Engineer, Vol. 31, n. 1 , p. 58, (1987)

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Chapter 3 Testing Procedures

The investigative approach to designing successful carbon steel inserts or any parts using SDM laser technology has been to understand, at a fundamental level, microstructural development. Microstructure and processing conditions have been shown to be highly correlated to material properties like strength and hardness. Residual stress development has also been correlated to the microstructure.

Figure 3.1 Microstructure and grain growth.

To begin to understand the microstructure, a number of procedures had to be 47

Chapter 2. 13 Requirements for Die Cast Inserts

Chapter 3 Testing Procedures

used to analyze SDM processed microstructure. Measurements of grain size, phase volume, and material properties were studied to characterize SDM parts. Both manual and automated processes were used.

Chapter 3. 1 Grain Size As Figure 3.1 illustrates, grain size inuences material properties. With increasing grain size, strength and hardness decrease. ASTM standard E112-96 describes procedures for measuring average grain size. These procedures characterize two dimensional grain size which is exposed by sectioning test samples. Manual and automated methods exist to measure grain size. Both methods were used to measure grain sizes as well as verify technique accuracy.
Chapter 3. 1.1 Point Intercept Method Three to ve horizontal lines are placed across a metallographic image. The length of the lines calibrated to the same scale as features within the image are drawn. Next the number of times a grain boundary intersects one of the lines is summed. The line intercept count (PL) is the number of intersections counted divided by the total length of the lines. PL = counts / total length PL = 5/ (3*100m) =.016 counts /m SV = 2* PL = .032 counts / m D = 8/(3SV ) = 83m
Figure 3.2 Point Intercept Method

The PL is used to calculate the surface area in a unit volume. It is needed to estimate the grain diameter. This method can also be accomplished with the use of a circle. The circle must be larger than the largest grain. Total length is simply the circumference of the circle. This method, also known as the Hillard method, and reduces directional bias when counting intercepts. Chapter 3. 1.2 Automated Point Intercept using Photoshop Plug In A program written by Reindeer Inc. uses pixel value measurements of grain
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boundary images to measure the equivalent diameter and shape of grains in a metallograph. The metallograph is prepared by thresholding the RGB (Red-GreenBlue) image so that black represents the grain and white represents grain boundaries. Depending on how the image is etched and photographed, the image may be inverted so that the grain will be thresheld as black and the grain boundaries are white. Other aspects of this program can measure grain perimeter, grain center of gravity in x and y coordinates.

10m

Inverted and Thresholded Image

Figure 3.3 Grains of SDM Tool Steel Analyzed by Photoshop Plug In

Chapter 3. 2 Volume Measurement and Phase Conrmation


Chapter 3. 2.1 Point Intercept Method The ASTM E562-1995 procedure uses a grid of 36 points area to measure phase volume fraction. The grid is a 6 x 6 square area which is placed over a metallograph. The phase or features of interest which intersect grid lines are counted. The number of intercepted grid points divided by the total number of grid points (36) is an estimate of the volume fraction. The volume fraction of a phase or constituent is the fraction of the volume of the structure that it occupies. Accuracy depends upon selecting several grids. For 10% relative accuracy, 625 elds would need to be analyzed for a 2% volumetric phase and 63 elds would be needed for a 20% volumetric phase using a 32 point grid. Chapter 3. 2.2 X-ray Diffraction X-ray diffraction was used in two ways: Phase Identication and Stress analysis. For randomly oriented samples, quantitative measurements of volume fraction of constituents like martensite, or austenite can be made from X-ray diffraction patterns because the total integrated intensity of all the diffraction peaks for
Chapter 3. 2 Volume Measurement and Phase Conrmation

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Point Count, Pp Pp = 3/36 = 1/12 = 8% of

Figure 3.4 Point Intercept Method for Volume Analysis

each phase is proportional to the volume fraction of that phase. Moreover, if the crystalline phases or grains of each phase are oriented randomly then the integrated intensity of any single diffraction peak is proportional to the volume of the fraction of that phase. Copper A radiation was used for most of the quantitative measurements. Because of background emissions or limited penetration depth of copper, the beam count time was extended 30 sec. per .25o. As gure 3.5 shows characteristic peaks of austenite and martensite existed

C%austenite +C%martensite + C%carbides =1


400 350

R * C% I austenite austenite = austenite I R * C% martensite martensite martensite


Where:
1+cos 2 R = ( v12 )[F 2 * p * ( sin 2 *cos )(e 2 M )
2

X Ray Diffraction Counts

300 110 Martensite Plane 250 200 150 100 50 0


41 42 43 44 45 46 47 48

111 Austenite Plane

v = volume of cell unit p=multiplicity factor F = structure factor, F=f(f) e-2M =temperature factor
Assumptions: polycrystalline specimens, form of flat plate of effectively infinite thickness, randomly oriented grains, making equal angles with incident and diffracted beams completely filling the incident beam at all angles.

Two Theta Angle

Figure 3.5 Analysis of Integrated X-ray Intensity for Phase Volume Analysis.

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with in an x-ray scan of the SDM tool steel samples. For peak separation, higher angles were used to calculate integrated intensities to determine phase percentages. X-ray stress measurements were also made. X-ray methods permit the determination of the surface stress components which characterize the existing stress system. X-rays measure biaxial stress within the surface because no stress exists at the free surface.
150

111111 Martensite Martensite 002 002 AusteniteAustenite

112 Martensite 112Martensite 211 Martensite 211 Martensite

200 Martensite 200 Martensite

100
Counts

022 Austenite 020 Austenite

Counts
5 0

0
30

90% Martensite 5.3% Austenite

22theta

Figure 3.6 Full X-ray diffraction Pattern

The relation of stress and strain are shown in Figure 3.7 . Using this formula we can determine x by nding the difference of strain in two angle in plane xz, and y can be found by measuring strain in yz plane. Strain can be measured by x-ray diffraction of lattice parameters by the use of Braggs Law as shown in Figure 3.8. Lastly, stress can be approximated by measuring strain at number of angles in a particular plane and plotting the strain versus the square of the sines of each angle. From the slope of the line the stress can be attained as shown in Figure 3.9. This method is often called the Sin2 method.

110

50

70

90

30

50

210 Austenite

70

311 Austenite 311Austenite

90

220 Martensite 220 Martensite

110

310 Martensite 310 Martensite

Austenite 111 Austenite

111

Chapter 3. 2 Volume Measurement and Phase Conrmation

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Chapter 3 Testing Procedures

E = Youngs Modulus v = Poissons Ratio

=Strain in xz plain x = stress in x direction y = stress in y direction

Y X
Figure 3.7 Relation of Stress and Strain

2 = 1/E x[(1+v)sin -v]-v y) ( 2 -sin }] 2-1 = 1/E x[(1+v){sin 21 ( 2

2 -sin 2 x = (E/(1+v))[1/{sin1})(2-1) 2

= (d-do)/do 2-1 = (d2-d1)/do


If 1 = 0 then:
2 )]*(d x = (E /(1+v))[1/{sin -d1)/do 2 2

d = 2 sin l =Bragg Law d = lattice spacing 2 = diffraction Angle of X-ray = X-ray wavelength employed

Figure 3.8 Braggs Law of X-ray Diffraction and Strain

slope = x (1+v)/E

sin2

1, 2, 3 ...

Figure 3.9 Stress Approximation by Sines.

Another method of determining stress measurements is called Fastress. A Fastress machine was used to determine stress and retained austenite. This system uses
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two chromium targets and four counters. The two x-ray beams are positioned so that two incident beams strike the xed specimens at 0o and 45o for simultaneous measurement. When the counters are centered on the lines of diffraction, a voltage proportional to the difference of the angular positions is recorded. Since the voltage is a linear function of (2 1-2 2) the stress can be measured directly. The Fastress acts as , a stress gauge which must be calibrated with known stresses. It has been designed to measure stresses in ferritic and martensitic material. If 1 = 0 then: 2 )]*(d x = (E /(1+v))[1/{sin -d1)/do 2 2 y x
With negligible error replace do with d2 or d1[] 2 x = (E /(1+v))[1/{sin -d1)/d1 2)]*(d2

differentiate Bragg Law : d/d= - cot 2/2

2 )]} x = (E (2(2 -2 2))/{2(1+v))[1/sin cot 1 2

Figure 3.10 Equations of Stress for Fastress Machine

Cross sections of laser deposited tool steels where analyzed by the Fastress technique to gain a stress prole of the material in the as-deposited condition. The Sin2 method was used to measure the average stress of a 316L stainless steel deposit and the average stress of the substrate for the 316L deposit. All measurements were made with the substrates still attached to the laser deposit. Chapter 3. 2.3 Scanning Electron Microscope Scanning Electron Microscopes (SEM) were patterned after light microscopes and yield similar information about topography, morphology, and composition. SEM can relay topographical information about the surface features of an object, its texture or other detectable features limited to a few manometers. SEM can relay morphological information about the shape, size and arrangement of the particles making up the object that are on the surface or have been exposed by grinding or chemical etching. All detectable morphological features are limited to a few nanometers. Lastly, SEM can relay compositional information about elements and compounds making up the sample relative to the surface can be determined but limited to 1 micrometer in diameter area. Light microscopes can also be used for topographical and morphological

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information. However, the SEM has a much higher resolution. Resolution with a light microscope is 0.0002 mm while with a scanning microscope it is 0.000000001 mm. SEM can attain higher magnications. A light microscope can magnify and object up to 1,000X, while the scanning microscope may go up to 400,000X. The SEM images are obtained by using a very small electron probe (or electron spot) scanning over the surface of the specimens and by mapping the detected electron signals from each specimen pixel onto the corresponding pixel of the Cathode Ray Tube (CRT) or Charge Coupled Device (CCD), i.e. the screen. Typically a device called an electron gun at the top of the apparatus produces a stream of monochromatic electrons. The stream is condensed by the rst condenser lens which is usually controlled by the coarse probe current knob. This lens is used to form the beam and limit the amount of current in the beam and works with aperture of the condenser to eliminate the high-angle electrons from the beam. A second condenser lens focuses the electrons into a thin, tight, coherent beam and is controlled by the ne probe current knob The aperture of the second condenser again eliminates high-angle electrons from the beam. A set of coils then scans the beam The dwell time is typically microseconds. The nal lens which is the Objective, focuses the scanning beam onto specimen. When the beam strikes the sample, electrons scatter or excited within the specimen. These electrons are detected with various instruments and counted. A pixel value corresponding to the number of counts is displayed on the CRT /CCD. The pixel intensity corresponds to the counts: (the higher the count the brighter the pixel). This process is repeated until the grid scan is nished and then repeated, the entire pattern can be scanned 30 times per second. For this research, SEM was used to examine fracture surfaces such as solidication and stress cracks. The ease of specimen preparation, high resolution, and extensive eld of depth make the SEM an invaluable analysis tool. The emissive mode of SEM which utilizes low-energy secondary electrons emitted from the specimen surface produces high resolution images contrasting surface roughness or height of topographic features making the examination of cracks or fracture to within 4 nm. Samples are mounted in bakelite or conductive SEM plastic mount. If a nonconductive mount is used, carbon leads are painted from sample to the backside of the mount to allow for charging of sample for imaging. Sample are polished up to .05 m silicate slurry nish.

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Chapter 3. 2.4 Transmission Electron Microscopy Transmission Electron Microscopy (TEM) was used to conrm crystalline structures of martensite and austenite. In the standard mode, bright eld and dark eld images were taken. A bright eld image is produced when only the direct beam is used for image formation. A dark eld image is formed when the diffracted beam is used for image formation. Lattice images were also taken. These images were used to index diffraction patterns to conrm the existence of phases. Double diffraction patterns were differentiated based upon intensities. Angles are measured from the intensity of the patterns to determine poles and stereographic projects of planes. Bases on determined planes fcc, bct, and bcc phases were found. Images in transmission electron microscope form when incident electrons are scattered by the specimen and focused by one or more electromagnetic lenses. Electrons scatter elastically, without energy loss (velocity and wavelength remain unchanged) if they hit the nuclei of specimen atoms. Electrons scatter inelastically with loss of energy (velocity decreases and wavelength increases), when the orbital electrons of the specimen atoms are hit. Inelastic events generally involve deections through small angles (<10-4 radians) and cause specimen damage . The amount of scattering is proportional to the thickness of the specimen or atomic number. Thick specimens, or those with large number atomic numbers, scatter more electrons than thin specimens or ones with low average atomic number. TEM specimens are typically thinner than 50 nm. This reduces the number of collisions because most electrons pass through the specimens without scattering. However, the electrons that do scatter are sufcient to produce images but without causing specimen damage. TEM differs from light microscopy techniques in different ways. Optical lenses are generally made of glass with xed focal lengths. TEM uses magnetic lenses which are constructed with ferromagnetic materials and windings of copper wire producing a focal length which can be changed by varying the current through the coil. Magnication in the light microscopes is generally changed by switching between different power objective lenses mounted on a rotating turret above the specimen. or by changing to different power oculars (eyepieces). The magnication of TEM arises changing focal lengths but the objective remains xed. While light microscopes have small depth of elds, the TEM have large depth of elds allowing for the full sample to be in focus simultaneously. A bright eld image is produced when only the direct beam is used for image
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formation. In other words, unscattered electrons of the incident beam combine with scattered electrons which have been modied or refocus by passage through objective aperture. Dark areas in the bright eld image arise from specimen regions which scatter electrons widely and into the objective aperture. A dark eld image is formed when the diffracted beam is used for image formation. If only scattered electrons are used (unscattered electrons are removed), t a dark eld image is produced. The viewing screen is dark unless there is a specimen present to scatter electrons. Dark eld images typically have higher contrast than bright eld images. However, since the intensity is greatly reduced, longer photographic exposures required. The objective aperture can be displaced sideways to intercept the main unscattered electrons. To study specic crystallographic orientations the apertures may be placed off-axis or the beam may be tilted. This dark eld image may be of poor quality because the aperture accepts off-axis electrons subject which are subject to larger aberrations (spherical and chromatic) than those on the optic axis. However, if the incident electron beam is tilted at such an angle that it is intercepted by the aperture and the diffracted beam of interest travels down the objective lens axis, only minimum aberrations exist. These aberrations are similar to those suffered by a bright eld image. However, both of these methods allow only certain diffraction spots/rings to be transmitted so only specic crystallographic orientations will be highlighted in the image. These crystallographic or lattice images expose crystal lattices. Crystals are composed of groups of atoms repeated at regular intervals in three dimensions with the same orientation. This group of atoms or the collection of points form is the space lattice or lattice of the crystal. A crystal lattice can be indexed so that material phases can be identied. Chapter 3. 2.5 Electron Microbeam Probe Electron microprobe analysis (EMPA) is a non-destructive method for determining the chemical composition. EPMA allows one to quantitatively determine the chemical composition of nearly all solids on the micron scale. This is achieved by collecting x-rays that are emitted from atoms which have become excited by a primary beam of electrons. Localized specimen chemistry can be achieved which can provide insight into the degree of chemical homogeneity which will affect bulk mechanical, electrical and thermodynamic qualities.

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EMPA uses a high-energy focused beam of electrons to generate X-rays characteristic of the elements within a sample from a volumes as small as 3 micrometers diameter. The resulting X-rays are diffracted by analyzing crystals and counted by detectors. Chemical composition is determining by comparing the intensity of X-rays from standards of known composition with those from the unknown materials. The measurements are corrected for the effects of absorption and uorescence within the sample. EMPA uses an electron beam current from 10 to 200 nanoamps to excite Xrays. This beam current is about 1000 times greater than the beam used in SEM analysis. These higher beam currents produce more X-rays from the sample and improve both the detection limits and accuracy of the resulting analysis. Analysis locations upon the specimen can be selected by using a transmitted-light optical microscope mode or SEM mode, which allows positioning accurate to about 1 micrometer. The resulting data can yield quantitative chemical information in a textural context. Variations in chemical composition within a material, such as a mineral grain or metal, can be determined. In this research, EMPA was used to measure chemical composition of material interfaces and areas with graded material transitions. EMPA was very important in determining the sharpness of interfaces within the micrometer range. Chapter 3. 2.6 Etching TEM and X-ray diffraction are very timely/expensive operations to perform phase identications. TEM samples may take weeks to prepare. With one martensitic stainless steel sample, to dimple the sample for TEM took 2 weeks in the ion mill. Because of very low penetration in ferrous based samples, when using X-ray diffraction, a sample must run for about 1 week for a full scan from 40-120o to gather enough counts to differentiate peaks. The analysis which has gone into this research has spanned over 300 samples. Samples were mechanically polished to .05 micron with an AlO3 slurry. The following etchants were used to analyze the samples to determine phase compositions. Light microscopy techniques were used to take picture of the samples.

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Etchants Picral Reagent Sodium Meta-Bisulte Potassium Meta-Bisulte Muramakis Reagent Klemms Reagent

Application Technique Swabbed Immersed Swabbed Boiling Etched Swabbed

Phase Exposure Exposes Grain Boundaries Darkens as Quenched martensite Darkens All Martensite Blue-Sigma Ferrite, Brown-Delta Ferrite Blue - Ferrite, BrownMartensite

Table 3.1 Etchants Used to Analyze Laser Material

Chapter 3. 2.7 Blue: Automated Volume Analysis A program called BLUE was developed to quantify material phases in steel samples. These steel samples were etched in different reagents which colored different crystalline structures with specic colors. Optical light microscope photographs were taken at 125X magnication to 200X magnication. These photographs were all taken at similar cyan, magenta, and yellow levels and similar contrast, brightness and sharpness levels as well. By standardizing the parameters used during the light microscopy photographs, automated analysis is able to be completed. This technique allows one to compare the amounts of the different phases among all the samples. This automation can occur by using a pixel value analysis technique. An earlier form of Blue assigns different ranges of grayscale pixel value to martensite and other two austenite. Calibrated samples which have all ready been categorized for phases were analyzed. This earlier form of blue is able to predict the amount of martensite and austenite to within 2% of values reported values. However, to resolve or separate colored phases of brown (light brown and dark), blue and red, full RGB color pixel values must be used. Thus, Blue was created. It is designed to allow the user to standardize an input le to represent all pixel values of a specic phase. For example, a lter called blue209 contains all pixel values which correspond to sigma ferrite, which have been revealed by potassium metabisulde
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Chapter 3 Testing Procedures

reagent. The optical photomicrograph and the lter are saved as xpm les, which is a text format of the graphic values. The xpm format allows for programming logic to analyze the lter and the optical photo . The accuracy of blue is once again within 2% of X-ray diffraction measurements.

Technique X-ray Diffraction Blue Analysis

Martensite 90% 89%

Austenite 5.3 7%

Table 3.2 Comparison of X-ray Diffraction and Blue results for SDMT Steel Sample

In addition to just matching pixels, the beauty of BLUE is that it is able identify additional area of the phase of interest by identifying a pixels proximity to that of a given phase. This searching parameter is controlled by user inputs, so the program can be told how far to deviate from dened pixel values.

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Color Image

Sigma Ferrite Filter

Delta Ferrite Filter


Figure 3.11 Color Separtion of Blue Technique

Chapter 3. 2.8 Electron Backscattering Probe In the nal stages of this research, a new technique was discovered which can used by others in the future who want to understand the material phases within bulk deposits. Electron Backscattering Probe (EBSP) is a technique similar to SEM. This technique enables crystal orientation to be determined on thicker surfaces than TEM. To produce measurements, a stationary beam interacts with the surface of the crystal. The electrons backscatter in a direction opposite the incoming beam and are captured by on a phospor screen with a low intensity video camera. Orientations can be determined by Braggs law. Unlike TEM which takes large amounts of time to prepare carbon steel samples, preparation of EBSP samples are quite simple. Bulk samples are polished by mechanical means to a .05 m silica nish. They are etched and then

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polished again by only the .05 m solution. Samples can also be quite large (over These 1cm2 in area) giving maximum localized orientation information. measurements can be automated to get a complete surface mapping of crystalline information. However, special lters have to be written for BCT formation. Further testing of this technique for use with carbon samples is undergoing.

37.7 57.6 [211] BCT

Beam = [011] TEM Index Pattern

BCC/BCT EBSP Pattern

Figure 3.12 Comparison of TEM and EBSP

Chapter 3. 3 Material Property Test


To determine the material properties of tools steels deposited by laser deposition, testing had to occur. Three types of tests which were preformed: tensile testing, Charpy Impact testing and hardness testing. Tensile testing are able to measure yield and ultimate tensile strength. Impact resistance a property which is very necessary for dies inserts can be measured by Charpy Impact testing. Hardness testing can give information on a more localized area. Microhardness testing was used to yield layer by layer information or even interfacial informations.

Chapter 3. 3.1 Tensile Testing ASTM E8-1998 describes methods for producing samples for tensile testing. Tensile specimens, when tested, are able to yield material property information like, yield strength, yield point elongation, tensile strength, elongation and reduction of area.
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Chapter 3. 3.2 Charpy Impact Testing ASTM E23-1998 describes the method of using notched-bar impact testing of metallic materials by using a Charpy apparatus. It is used to test impact resistance. Chapter 3. 3.3 ASTM E18-1998 describes Rockwell Hardness testing. ASTM E10-1998 describes Brinell hardness testing. Also, ASTM E92-1982 describes Vickers hardness testing.

Chapter 3. 4 Part Functionality Testing


To determine if a part can actually be used in service or if the part possess functionality. For this research three characteristic of functionality were tested: deection, wear resistance and thermal resistance. Deection is an indication of whether a part is able to meet geometrical requirements. Wear and thermal resistance are indications of whether a part was able to meet service or environmental requirements. Chapter 3. 4.1 Deection Testing One measure of part integrity is surface warp or deection. When layered manufacturing parts exhibit deection, it is a symbol of residual stress or shrinkage imbedded to the part during the deposition or building sequence. A part with low warpage tends to have low residual stress conditions or has built in a manner to compensate for shrinkage. Currently, the shape manufacturing process has deection measured from the curvature of the substrate on the order of 1-2 mm. Warpage or deection is also a concern for the silicon processing industry. Warp can signicantly affect the yield of semiconductor device processing. Producers and consumers of silicon products use the measurement of warp to determine if dimensional characteristics of a silicon wafer will satisfy geometrical requirements. Likewise, warp in layered manufacturing parts, will mean that additional processing is required to insure that outer part dimensions are within required tolerances. Although additional processing steps like machining may bring outer dimension back in to specications, internal geometry cannot be repaired very easily. Silicon warpage is measured by ASTM F657-1992. A granite plate is used to dene a surface indexing 3 points on the bottom of the silicon wafer. The maximum
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Chapter 3 Testing Procedures

radius of curvature is measured using this plane as a base. Deection of beam deposits is measured in a similar way to silicon warpage. For manual measurements, the substrate and deposit are positioned on xture which supports the substrate level to granite plate. The deposit is now pointing towards the granite plate. The now exposed surface of the substrate is used to take measurements. The edge of the exposed surface of the substrate is grounded at zero. A height gauge is then moved across the substrate in a grid with measurements taken every 6 mm. The largest absolute deviation in height from zero is dened as the maximum deection. A coordinate measuring machine at the Stanford Linear Accelerator Center was used to measure deection. The beam deposit was again xtured with the deposit point down toward a granite plate. A 3 x 24 point grid was used to measure deection. This method was very fast and very accurate.

D=Deflection

Figure 3.13 Measurement of Deection

Chapter 3. 4.2 Dunk Test Specimen The Jack Wallace Dunk test is a die casting simulation. This test has been calibrated so that one cycle is equivalent to 100 die casting shots. A cycle consists of lowering a prefabricated xture into molten aluminum (667 oC) while cold water (20
oC) is injected into the interior cavity of the xture.

This test is also a measurement of

the thermal fatigue of the material.

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Chapter 3 Testing Procedures

50.8 mm

50.8 mm

50.8 mm

177.8 mm

177.8 mm

38.1 mm

Figure 3.14 Thermal Dunk Test Specimen

Chapter 3. 4.3 Die Casting Die Casting was described in Chapter 2. 3.9. Die casting was used to test an insert built by Shape Deposition Manufacturing. This is the ultimate test of insert viability.

Chapter 3. 5 Modelling of Results A problem as complex as modeling phase transformation in laser deposition can be attacked in many ways each with limitations. Laser deposition is a 3D dimensional problem which involves many variables: laser scanning speed, laser focal length, laser spot size, laser path, the number of laser scans, nitrogen shroud gas ow rate, cooling rate, material properties, material combinations, substrate material and thickness, bolting conditions, layer thickness, machining parameters, subsequent processing steps, process step order, etc. Design of experiments like the Taguchi approach can be used if judgements can be made to simplify the system components to key parameters which can be stringently manipulated to plan experiments [3.8, 3.9]. Parameters like scanning speed and laser power can be manipulated for a planned experiment. It is more difcult and at times impossible to regulate levels of certain variables like the chromium content of a stock alloy for a planned experiment. For the laser deposition system, it is at times, difcult to separate endogenous (input) variables or exogenous (output) variables. Sometimes effects can be masked because it may take several endogenous variable to produce one exogenous response. Often DOEs require a basic understanding of the system relationships to produce accurate results. Because of these problems: the inability to control certain variable
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inputs and the daunting inability to separate variables, typical DOE methods may be inadequate. When a judgment about the magnitude of inuence and interelationship of variables is needed other non-traditional methods may need to assessed. In cases like the laser deposition system, it may be impossible to make such judgement calls. Laser deposition is a complex problem which can be looked at as an ill-dened system because there is insufcient knowledge to throughly dene the systems and key interactions. At present no theory exists which can account for all of the primary relationships or interaction of variables to dene system responses such as phase formations or grain sizes. Therefore, modeling the system based on a theory driven approach is difcult and can often lead to errors because of inappropriate assumptions. Often, when building the model, one has to know things about the system that are generally impossible to know without extensive testing. These unknowns may not only cause the inappropriate selection of key controls or variables, but the model structure can be compromised by the insufencient knowledge about interference factors or inuencing factors. This uncertainty can confuse the modeling in several ways: 1. The selection of variables as endogenous variables or exogenous variables. 2. The functional form of the relationships between variables and system dynamics. 3. Proper understanding of the origin or description of error. A data driven approach can overcome some or all of the problems associated with ill-dened systems. Often data is analyzed by statistical means for model formation. However, this type of dening process typically needs to have priori knowledge about the structure of the system to produce the mathematical model [3.10]. Data mining techniques can be implemented to gain system knowledge and modelling information. Data mining techniques include data visualization, tree-based methods and methods of mathematical statistics like multivariate regressions as well as those for knowledge extraction from data using self-organizing modelling [3.13, 3.13]. Data mining is an interactive and iterative process of numerous subtasks and decisions-making steps such as data selection and pre-processing, choice and application of data mining algorithms and analysis of the extracted knowledge. Many automated data mining programs try to limit the involvement of users in the overall data mining process and the inclusion of existing a priori knowledge. Thus, the process becomes more automated and more objective. To tackle the phase transformation element of the laser deposition problem
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which is complex and expense (in time, operations, etc.) to solve and to ascertain primary inuences of parameters the Group Method of Data Handling (GMDH) procedure was used [3.11]. GMDH looks for simple relationships in multiple level systems. The goal of GMDH and other similar tools are to predict behavior by means of parametric or nonparametric models. Parametric models are adaptively created from data by the Group Method of Data Handling (GMDH) in the form of networks of optimized transfer functions (Active Neurons). Nonparametric models are selected from a set of variables analyzing one or more patterns of a trajectory of past behaviors which are analogous to a chosen reference pattern. Both approaches of self-organizing modeling include not only core data mining algorithms but also an iterative process of generation of alternative models with growing complexity, their evaluation, validation and selection. At present, GMDH algorithms present a method to identify and forecast relationships in cases of noisy and short input sampling. In contrast to neural networks, the results are explicit mathematical models, obtained in a relatively short time. KnowledgeMiner is a software tool which uses GMHD. It is an easy-to-use modelling tool which realizes twice-multilayered neuronets and enables the creation of time series, multi input/single output and multi input/multi output systems (system of equations). Successful applications are shown in the eld of analysis and prediction of characteristics of stock markets in nancial risk control modelling [3.10].

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3.1 Kalpakjian, Manufacturing Engineering & Technology, 1995 3.2 Norton, John T., Review of Methods of X-ray Stress Measurement, 3.3 Kocks, U.F., Tome,C. N. and Wenk H.-R., Texture and Anisotropy, New York: Cambridge University Press, 1998, pp. 167 -177. 3.4 E. Beraha and B. Shpigler, Color Metallography, (1977). 3.5 B. L. Averbach, L. S. Castleman, and M. Cohen, Measurement of Retained Austenite in Carbon Steels, Transactions of the ASM, (1949) Vol. 42, pp112-120. 3.6 N. Williams and C. Carter, Transmission Electron Microscopy - Diffraction, Vol 2, (1996), pp.267-288. 3.7 Burgman, Patrick, Design of Experiments The Taguchi Way, Manufacturing Engineering, May 1985, pp. 44-46. 3.8 Ross, Philip J., Taguchi Techniques for Quality Engineering, McGraw Hill, New York: 1996. 3.9 Ranjit, R. A Primer on the Taguchi Method, Van Nostrand Reinhold, New York, pp. 145-155, (1990). 3.10 Lemke, F.; Mueller, J.A. (1997): Self-Organizing Data Mining for a Portfolio Trading System. Journal for Computational Intelligence in Finance, 5(1997) pp. 3 3.11 Farlow, S.J. (ed.) (1984): Self-organizing Methods in Modeling. GMDH Type Algorithms. Marcel Dekker. New York, Basel 3.12 Madala, H.R.; Ivakhnenko, A.G. (1994): Inductive Learning Algorithms for Complex Systems Modelling,CRC Press Inc., Boca Raton, Ann Arbor, London, Tokyo 3.13 Sarle, W.S. (1995): Neural Networks and Statistical Models. in: Proceedings of 19th Annual SAS User Group International Conference. Dallas. pp. 15381549.

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

Chapter 4 Material Selection and Design of Small Scale Die Inserts


Chapter 4. 1 The Need for A New Material As described in Chapter 2. 10, the SDM process is an additive and subtractive process which involves the deposition and shaping of material. When used with metals, part material is deposited by laser deposition and shaped by CNC machining. A sacricial material is often used to support over-hanging features or to maintain the integrity of hollow internal geometries within the part. For example support features are often used to ll cooling channel passages as well as to support undercut surfaces. To remove sacricial material, an etching process is used. This removal process requires that part materials have high corrosion resistance and sacricial material to have low corrosion resistance. Common materials used to produce parts in Shape Deposition Manufacturing (SDM) have been 316L stainless steel, copper, copper bronze, and invar. Stainless steel-316L is a soft machinable material with high corrosion resistance. It is often used as part material. However, it has a very high coefcient of thermal expansion (CTE). When 316L is deposited, the melted powder upon solidication shrinks. This shrinkage cause 316L parts to deform. Copper is used as a support material. It is often plasma deposited and shaped to support 316L parts. The low corrosion resistance of copper allows, exposed surfaces of copper to be etched away and removed. The high thermal conductivity makes it an attractive option for depositing within multimaterial parts to improve heat transfer. Copper bronze can also be used as a sacricial material, and it can be deposited

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by laser. Its low corrosion resistance make it ideal for this etching process. It also soluble with 316L. Thus, for depositing gradient structures, copper bronze is a good candidate. However, the thermal conductivity is very similar to 316L so no thermal advantage is gained by using copper bronze within the deposited part. Invar is used as part material and for graded structures. Functionally graded parts have been researched by the Stanford Rapid Prototype Lab. Two materials are blended in the power feeding unit by allowing material mixing in situ by changing powder feed ow rates. For example, Invar has a low CTE from 400C to room temperature. It is during this temperature range when most residual stress develops which causes part deformation. Therefore, invar has been used in graded structures called functionally gradient parts. The powder feeding system used for SDM consists of 3 automated powder feeders. Each can be lled with different material and controlled individually. Figure 4.1 shows the results of depositing both invar and stainless in over a 48 mm span. The measurements for this graph were taken by electron microprobe analysis. As one material decreases the other increased. A smooth compositionally graded structure is created. This technique has been used to build multi-material parts. The invar is deposited on the interior of the part while stainless steel is deposited on exterior surfaces or as barriers near low corrosion resistant materials.
Percent Compositon of Stainless-Invar Bar %316L
1

%Invar

Percent Composition

0.8

0.6

0.4

0.2

0 0 8 100% Stainless Steel 16 24 32 40 48

mm 100% Invar Variation within 95% confidence Level is + .6%

Figure 4.1 Graded Structure of Invar and 316L - Measured by Microprobe

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As graded material with 316L, Invar has been used to build many parts. However, Invar has low corrosion resistance and low machineability. Because of these two properties, production of parts completely from invar is limited. While each of these materials have been successfully used to produce parts, each is inadequate to produce die cast inserts. Stainless 316L, Invar, copper, and copper bronze are not wear resistant enough to survive molten injection of aluminum. Nickel in 316L and Invar are soluble in molten aluminum. Alloying and precipitation of die material with casting material produces an unusable material combination. Copper and copper bronze in addition to solubility, have melting temperatures in the range of molten aluminum. Mold deformation or dissolution would occur if used in aluminum die casting. Also none of these materials attain the hardness needed for wear resistance specied for die casting.

C% Copper Copper Bronze Invar 316L 0 0 .03 .02

Mn% 0 0 .3 1.74

Si% 0 0 .2 .73

Cr% 0 0 0 17.3

Ni% 0 .5 40 13.1

Mo% 0 0 0 2.66

Cu% 99.9 86.5 0 0

Al% 0 6 0 0

Sn% 0 .2 0 0

Table 4.1 Current SDM Materials: Balance Iron

Also, in addition to the requirements needed for die casting listed in Chapter 2. 13, the material needs to meet requirements of laser deposition in SDM. Also, any new material should yield more applicability than just aluminum die cast inserts. The process to nd new materials should attempt incorporating materials which have properties that would lower part deformation, or improve deposition characteristics, etc. For example, if it is possible, the new material should have a low CTE or have improved wetting characteristics so that additional materials can be used with SDM.

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Melting Temperature (C) Copper Copper Bronze Invar 316L 1083 1053 1427 1385

CTE (m/mK)
300oC -20oC

16.9 16.2 1.6 17.5

Table 4.2 Typical Materials used with SDM

Therefore the requirements of materials incorporated in the SDM process to build aluminum die casting inserts can be divided into to camps, Tier I and II. Tier one requirements cannot be compromised. Tier II. requirements are additional requirements which are to be sought but are not decision limiting criteria: Tier I. Requirements Low Coefcient of Expansion for high thermal fatigue resistance High hardness (44-48 Rc) for wear resistance (2.35) High modulus of elasticity for high resistance to deformation to avoid galling and heat checking Moderate thermal conductivity to produce castings of similar microstructures as H13 production inserts (on the order of 24 W/mK) Minimal to trace amounts of Nickel to reduce the potential alloying or dissolution. Corrosion Resistance or the ability to alloy with corrosion resistant materials Tier II. Requirements Good Machineability Low CTE Commercially available from reliable source

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Chapter 4. 2 Initial Selection of Tool Steels


The hardness and strength requirements were the guiding criteria to select materials. The typical tool building material for SDM was 316L stainless steel. This is an austenitic steel which has the crystal lattice structure of face-centered cubic (FCC). A FCC alloy has many good characteristics, low-temperature toughness and excellent weldability, and typically good corrosion resistance. However, they are often susceptible to stress-corrosion cracking. However, the main problem is that the relatively low yield strength allows that these FCC alloys can only be hardened by coldworking, precipitation, or solid solution strengthening. Precipitation and solution hardening involve special heat treatment processes to either change the bulk to one phase or cause precipitation of a second phase in the part matrix. All three treatments, would be difcult to perform on a SDM 316L part especially if it were a multi-material part (with Invar and copper) because of the multiple melting point /thermal phase characteristics or deformation to nal part dimensions. The low yield strength was actually one of the guiding principles for choosing 316L. When one looks at beam deformation, maximizing R or the radius of curvature would minimize the amount of warp or deection which the deposited structure would have. Stainless-316L has a high E/ ratio.

R
y

Maximize R by Maximizing

Figure 4.2 Maximizing R to Minimize Deection

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

E x104 MPa Copper Copper Bronze Invar Low Carbon Steel 316L 110.4 96.5 14.1 20.0 19.3

MPa
(Annealed)

E/ 15977 4660 511 358 825

69 207 276 558 234

Table 4.3 Comparison of E/ with Common SDM Metals

This criteria though does not seem to help when trying to nd hardenable material for build die inserts. Two types of materials which did meet the hardness criteria were the 400 series martensitic stainless steel and tool steels. The 400 series martensitic stainless steels stainless. Theses material have high modulus, can attain high hardnesses. They have moderate to high corrosion resistance. The high hardnesses does pose a challenge for machining, but it has similar machining characteristics to 316L. Therefore, the expertise of depositing and machine stainless could be exploited for these new materials. Tool steels will also be able to attain the hardnesses required for die casting inserts. However, the corrosion resistance of these materials was questionable. Chromium which forms carbides that reduces corrosion susceptibility is low in many tool steels. Also many allowing agents are also included in the composition of tool steels. Eight materials were originally tested. The alloys consisted of two high speed tool steels T15 and M2, H13 a hot working steel and ve industrial alloys similar in carbon and chromium compositions to the 400 series stainless: Polar, Cryotherm, Pyro 1, Pyro 2, Spraco 2.

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C% T15 M2 Polar Cryo1 Pyro1 Pyro2 H13 316L 1.6 .8 .01 .01 .01 .01 .4 .02

Mn% 0 .3 0 0 0 0 0 1.74

Si% 0 .3 0 0 0 0 1.05 .73

Cr% 4 4 10.5 15 12 14 5 17.3

Ni% 0 0 0 0 0 0 0 13.1

Mo% 1 0 0 0 0 0 0 2.66

Co% 5 0 0 0 0 0 0 0

W% 13 6 0 0 0 0 0 0

P% 0 0 0 0 0 0 0 0

V% 5 2 0 0 0 0 1.1 0

Table 4.4 Initial Tool Steel Selection for SDM Processing

The materials were tested for hardness, deposition quality and corrosion resistance. The material was SDM deposited in samples measuring 30 mm x 35 mm x 4 mm were deposited from each of the metal powders. Each sample was produced using standard deposition parameters of 100% laser power, 25 mm/sec laser scanning rate, and 30 g/min. powder feed rate. Each sample was evaluated on the basis of deposition quality, hardness, surface wetting and acid etch resistance. Deposition quality was evaluated through visual observation of cracking and surface oxidation. Hardness testing was performed with a Rockwell Hardness Indenter (ASTM E181995) and 10 individual tests per sample. Etch resistance testing was determined in accordance to ASTM A262-93a-1996 by placing the sample in 65o C nitric acid for 30 minutes. After an etch test, the microstructure of each sample was analyzed for corrosion susceptibility based on etch structure classication (ASTM A262-93a1996).

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

Alloy T15

Composition

Hardness

Deposition Pitted

Etching Fast

4% Cr, 5% Co, 13%W 1.6% C, 5% V, 1% Mo 63 Rc 4% Cr, .3% Si, 6% W .8% C, 2% V, .3% Mn Industrial Alloy 10.5% Cr Industrial Alloy 15% Cr 58 Rc 42 Rb

M2

Good

Fast

Polaris

Good Visible Cracking Cracking

Slower Etching Slower Etching Slow

Cryo 1

40 Rb 30 Rc

Pyro 1

12% Cr, 0% Co <1% C 14% Cr, 0% Co <1% 44 Rc C 16% Cr, 0% Co <1% 40 Rc C 5% Cr. 0% Co .4%C 50 Rc Good (Cracked during cooling) Good Good Slight, Very Slow

Pyro 2

Spraco 2 H13

None Etching

Table 4.5 Testing Results of Tool Steel in SDM Processing

Spraco 2 was the only alloy to successfully meet all the requirements of hardness, etch resistance and deposition quality. This alloy was selected as the SDM Tool Steel. Analysis of photomicrographs of the Spraco 2 deposit after the nitric bath showed no ditch structures or end grain pits which would indicate susceptibility to intergranualar corrosion. M2 and H13 steels can only be considered if they can be used with corrosion resistant functionally graded structures such as a structure with H13 on the outside and 316L deposited upon faces of etchable surfaces.
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Spraco tool was selected as the new SDM tool steel. Metallographic analysis showed that using the deposition parameters, as for 316L were not sufcient because some deposits had many voids. To reduce the voids and create an efcient deposition routine, the deposition parameters had to be optimized. Chapter 4. 2.1 Optimization of Deposition Parameters A Taguchi based design of experiment was used to nd optimal deposition parameters for SDM Tool steel. The optimal parameters should provide the maximum material deposition rate which produces fully dense deposits and material within the acceptable hardness range. Remelting of the substrate should also be kept to a minimum to preserve the geometry of previous layers. Three factors were investigated: laser power, laser scan speed, and powder feed rate. A Latin square array of 8 experiments varying the three factors at two levels was completed.

Parameter Laser Power Laser Scanning Rate Material Feed Rate


Table 4.6

Level 1 100% 25 mm/sec 30 g/min

Level 2 90% 35 mm/sec 15 g/min

Experimental Parameters

The full factorial design was chosen to directly characterize the two factor and three factor interactions. Tool steel samples of 30 mm x 10 mm x 5 mm were deposited at each of the 8 experimental settings. Hardness was measured as described in Chapter 3. Metallographs were taken at optical magnication from 50-1000x. From these photomicrographs, the laser penetration depth, porosity and pore density were calculated. D. Gentry, et al. (4.1). showed that optical measurements of porosity were within 93% of the accuracy of traditional porosimetry methods. A Taguchi function for maximizing the outcome, F was chosen to correlate the observed measurements with the optimal condition (4.2). The optimal setting is found when F is maximized with the following equation : F = .4 H* + .4(1- P) +.2 D*
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Chapter 4 Material Selection and Design of Small Scale Die Inserts

where H* is the Hardness normalized by 48 Rc, Pi is the porosity, D* is the depth of penetration normalized by 100 m. Once the optimized results were obtained, tensile specimens were deposited. ASTM Standard E8-1995 was used for the tensile testing of specimens. The factors, (A = Laser Power, B = Laser Scanning Rate, and C = Powder Feed Rate) contribute to the optimal deposit conditions as described in . Using the optimizing function, (equation 1), the following deposition parameters were selected: 100% laser power, 35 mm/sec scan rate, and a powder feed rate of 15 g/min. According to the data, the laser scan rate is the single most important factor in the optimizing function, as well as for controlling hardness, penetration depth, and porosity individually. Specically, the faster the scanning rate within the limits examined, the harder the material, the lower the porosity and the lower the penetration depth. Laser power independent of the other factors made little contribution to the outcome.

Degree of Freedom A B C AxBxC AxB AxC BxC Total ERROR 1 1 1 1 1 1 1 15 0

Sum Squares

of

Mean Squares (Variance) 0.0006 0.07 0.00007 0.05 0.004 0.02 0.004 0.0000 0.0005

Variance Ratio

Pure Sum of Squares S'

Percent Contribution

0.0006 0.07 0.0001 0.05 0.004 0.02 0.004 0.2 0.004

1.23 143.27 0.13 96.72 7.23 36.19 7.45

0.0001 0.07 -0.0004 0.05 0.003 0.02 0.003

Pooled 47.39 Pooled 31.88 2.08 11.72 2.15

1.00

0.008

4.78

Table 4.7 Analysis of Variance Table for Optimal Response: A = laser power, B = scan rate, C = powder feed rate

The signal to noise ratio of the data is 37.9 and mean squared deviation is .0002. These value indicate a minimal scatter of data and a highly reliable optimum (4.1).

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

Chapter 4. 2.2 Material Properties At this optimized level, the material structure and properties were analyzed. Metallographs were made of cross sections of the SDM tool steel deposits made at the optimum conditions. The metallograph shown below shows a cross section of SDM Tool steel etched with prical acid. The material structure is primarily martensite (dark, ne regions) with retained austenite (light bands) . The material exhibited a hardness of 45 Rc. and was found to be 99.9 % dense. The pore density is .002 pores/ mm2 with an average pore diameter of 29 m (4.3). The mechanical properties from tensile testing are shown in Table 4.8 compared with standard H13 tool steel.

Mechanical Property Ultimate Tensile Strength .2% Offset Yield Strength Reduction of Area Modulus of Elasticity

SDM Tool Steel 879 MPa 510 MPa 2% 254 MPa

H13 1482 MPa 1344 MPa 38% 210 MPa 14 % (50 cm gage length)

Elongation (in 25 cm gage 2% length)


Table 4.8

SDM Tool Steel (as deposited) Vs. H13 (tempered)

As compared to H13 which has been heat treated , SDM tool steel has a lower yield and tensile strengths and less elongation (4.4). However, these properties for the SDM Tool steel are in the as deposited condition. For prototype inserts, these property levels may be sufcient. The high modulus of the SDM tool steel is a result of the martensitic matrix. The retained austenite should add increased toughness and reduce the possibility of cracking or galling (4.5).

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

100 m

Figure 4.3 Metallograph of Austenite (light) and Martensite (dark) in SDM Tool Steel

Chapter 4. 3 Building A Small Scale SDM Die Cast Insert To test the SDM process and the new SDM tool steel, a die cast insert needed to be built. To minimize the possibility of failure within a die casting machine, a small scale insert was built. To design the insert a set of guidelines was imposed. The both the part thickness and feature depth would be minimized while maximizing the ratio between the two specications. These constraints accomplish two things, the deposition time would be minimized and the complexity of the die insert would also be simplied. A ratio of 4 to 1, part thickness to feature depth was maintained. An insert was built using the optimal parameters for SDM Tool steel and cycled in an overow of a production die set in a 600 ton die casting machine. The insert, the Stanford paper clip (Figure 4.4) had outer dimensions of 6.4 cm x 6.4 cm x 1.9 cm. By using the SDM additive and subtractive processes, the insert was deposited and fabricated in layers. A pocket of aluminum bronze, 1 cm x 1 cm x.32 cm, was deposited in layers .32 cm below the S feature of the paper clip. The aluminum bronze was added to illustrate the multi-material capability of SDM.

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

Figure 4.4 SDM Tool Steel Insert

A number of tests were performed on the insert prior to die casting. Melted wax was poured in the die to test part removal. Thermal fatigue testing was performed. The insert was thermally cycled by pouring molten aluminum 380 alloy at 670oC into the insert, allowing the casting and insert to air cool to about 100oC and removing the casting. The insert was then air cooled to room temperature. This would be repeated seven times with different amounts of insert preheat. The original 5o taper was found to be insufcient for the removal of the wax from the insert. Ejector pins, gating, and venting were added to facilitate material removal (Figure 4.7). The insert was tested for thermal fatigue resistance with gravity poured aluminum. Figure 4.5 shows the thermal cycling history of the insert. Aluminum 380 castings without warpage or dimensional shifts, proper surface nish and low porosity, were produced with an insert preheat of 660oC and a 5 minute dwell time in the closed stand. Figure 5 compares the microstructures of the gravity poured insert and a die cast part from a traditional H13 insert. The gravity poured parts showed more columnus structure due to dwell times on the order of 25 times longer. However, the hardness of the castings from the SDM insert and H13 insert are similar (55 Rb and 57 Rb, respectively).

Chapter 4. 3 Building A Small Scale SDM Die Cast Insert

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

730 630

Temperature (C)

530 430 330 230 130 30 0 50 100 150 200 250

Time (Min.)
Figure 4.5 Gravity Casting produced Thermal Cycling

The die casting machine parameters used to produce castings are listed in Table 4.9. Castings were evaluated microstructural homogeneity under the optical microscope and compared to castings produced by an H13 insert. The average grain diameter was calculated by the intercept method in accordance with ASTM Standard E112-1995.

Parameter Shot Pressure (No Intensier) Intensier Pressure

Setting 103 MPa 27.6 MPa

Die Preheat (2 hours) Die Temperature while running


Table 4.9 Die Casting Parameters

121oC 82oC

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

60 m

60 m

A. Figure 4.6 A. Die Casting of Aluminum B. Gravity Cast Structure

B.

For actual die casting, the features were remachined with a 15o taper to facilitate easy removal of the part without ejector pins. The insert was positioned in an overow of a valve body die set where ejector pins could not be used. The increased taper angle resulted in sharp thin edges in the S feature as shown in Figure 4.7.

10 mm

1 mm b

o Taper Figure 4.7 Remilled Insert: 15 added to all walls (a) and close up of ne f

Figures 4.8 and 4.9 show, the position of the insert in an overow section of a production H13 die casting tool. The cycle time for producing the casting shown in Figure 4.10, from injection of the aluminum to ejection of the casting was 70 seconds. The SDM insert was run in the die cavity for over 150 shots with no visible evidence of wear, fatigue, or cracking. Both the castings from the SDM insert and H13 overow sections had a hardness of 57 Rb. Metallographs of a castings from the two sections are shown in Figure 4.10.

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

10 mm

Figure 4.8 SDM Insert in Overow

Figure 4.9 SDM Insert placed in overow of Saturn Valve Body

have a similar structure with agglomerated cell patterns. The ASTM E112-1995 intercept method was used to calculate average grain diameter. The average grain diameters for the castings from the SDM insert and the H13 insert were 8.5 m and 8.6 m, respectively. Chapter 4. 3.1 SDM Tool Steel use for small inserts The SDM tool steel used for the die casting insert exhibited higher hardness than expected for this material. This material deposited through ame spray or conventional welding operations will have a hardness in the range of 20-28 Rc. The material experienced rapid quenching during air cooling which initiated a martensitic transformation without going through the other diffusion limited phases. The martensitic phase is responsible for the high hardness of this low carbon alloy. Alloys with higher carbon content should produce material with even higher hardnesses, but

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

such materials would be difcult to mill. The low carbon content in SDM tool steel will allow the SDM process to produce structures within the range of 35-45 Rc. The corrosion resistance of the SDM tool steel assures that the rapid transformation is not causing sites for intergranular corrosion (4.6). Certain heating conditions can allow chromium to be depleted from the alloy matrix and form chromium carbides on the grain boundaries. This depletion weakens corrosion resistance. This condition is corrected by tempering and other heat treatments. The rapid cooling does not allow this precipitation to occur. This is one reason that SDM tool steel artifacts could be used without heat treatments. In addition to giving good corrosion resistance, the high chromium content will also give the insert high heat resistance up to 1000oC (4.7). These experiments show that SDM is a viable method for rapidly producing die casting inserts. SDM die cast inserts can produce time savings over conventional tool and die methods. Multi-material dies with better heating properties can be used to shorten dwell times and still attain proper cell structures. Moreover, the possibilities of producing small prototype die inserts as deposited, without heat treatment, can reduce die production lead times further.

Cast from SDM Insert


Figure 4.10 Die Cast Part from the SDM Mold.

30 m

Cast from H13 Insert

Chapter 4. 4 Deection Vs. SDM Tool Steel


An interesting observation was made with beams deposited with SDM tool steel. One beam was built at 20 mm/s and another at 30 mm/s. The beams were 127 mm x 4 mm x 12.5 mm on a 152 mm x 52,4 x 6.25 mm substrate. The beam built at 20 mm/s had an average hardness of 46 Rc, and the beam built at 30 mm/s had an average hardness of 38 mm/s. The beam seemed to possess less deection with increasing

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

hardness. This is exactly the opposite effect seen in 316L beams. Increasing hardness in 316L beams seamed to increase deection.

0.8

0.6 1.5

Deflection (mm)

0.4 1.0

0.5
0 0.0 SDM Tool Steel (46 R c ) SDM Tool Steel (38 R c)

0.2

-0.2 20 40

Distance Along Beam (mm)

60

80

100

120

140

Figure 4.11 Increasing Hardness reduced deection in SDM Tool Steel

The test suggests that increasing hardness may have inuence upon deection. Further testing would have to help calibrate whether the change in deection was truly the result of hardness or whether it can be attributed to smaller grain size, phase percentage or other factors which can contribute to increased hardness.
0.8 Stainless Steel (316L) (90 R b) Stainless Steel (316L) (86 R b)

1.5 0.6

Deflection (mm)

deflection (mm)

1.0 0.4

0.2 0.5

Increasing Hardness

0 0.0

-0.2 20 40

Distance Along Beam (mm)


distance (mm)

60

80

100

120

140

Figure 4.12 Increased Hardness increased deection in 316L beams

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

Chapter 4. 5 Attempting to Build Larger Scale Inserts


The unheat treated SDM die insert made from the alloy known as SDM tool steel work well with the small scale die insert, producing over 150 parts without any signs of wear or cracking. However, when the a much larger insert was attempted, the Dunk test specimen, catastrophic failure occurred. This insert has a part thickness to feature level thickness of 177 mm to 171 mm. In an attempt to minimize the build or deposition time, the insert was deposited on its side, changing the deposition part thickness to feature ratio to 55 mm to 40 mm. A dunk test specimen was being built in 1mm thick layers at the optimized setting for SDM tool steel. Every 10 layers, the part was allowed to cool before more deposition occurred. With only 5 mm left to be built the 50 mm part fractured during deposition.

Figure 4.13 Cracked Deposit: 50 layers of SDM Tool Steel Deposited

Metallographic examinations were performed upon crack surfaces. Etchants were used to determine the amounts of martensite, austenite, and ferrite were located in the area of the crack. The rst interesting nding was the stridation of the regions of tempered to as-quenched martensite. The grain size of the tempered martensite was on average 3 times larger than grains within the as-quenched region. The tempered region has cementite precipitation on the former austenitic boundaries of the tempered martensite. The larger tempered martensite packets are an indication of extended reheat temperatures or extended heating times. Very close to the crack sigma ferrite stringers were found. Also along the crack face sigma ferrite seemed to be propagated. The metallographic examination helped us to determine that the heating characteristics of layers is retained as the deposit is built. Tempering of layers occurs but is not complete. Grain size differences is quite apparent. The initiating crack surface started in area of brittle martensite. Moreover, sigma ferrite was found along the crack interface. It is difcult to determine if sigma ferrite existed before crack

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failure. However, the appearance of sigma ferrite does indicate under certain deformation or heating conditions sigma ferrite can develop. It became quite obvious that by building parts with tools steels, new designing or planning rules are required. Unlike our experience with austenitic material, these carbon steels can develop multiple phases. Our understanding of these phases and phase development would also need to be challenged.

Dark regions represent as-quenched martensite. Light regions represent tempered martensite and other phases.

1 mm
Figure 4.14 Microstructure of the cracked layers of SDM tool steel deposit

Delta Ferrite formed on crack interface.

Delta Ferrite Stringer within deposit. 100m

Figure 4.15 Sigma Ferrite has developed along crack edge

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Chapter 4 Material Selection and Design of Small Scale Die Inserts

100 m

As-Quenched Martensite Tempered Martensite and Other phases

Figure 4.16 Close up of tempered and as-quenched layers of SDM deposit.

When examining the crack surface in the interior of the part, voids were also discovered. This void growth had not been encountered before. Smaller samples were then built at the previously optimized levels. Void growth was now at 30%. When samples of the original powder was tested at the optimal settings, void percentage was under 1%. The powder characteristics or composition had changed.

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40 m

20 m

20 m 40 m
Figure 4.17 500 and 1000 X Views of Cracked SDM Deposit.

Chemical analysis showed that the silicon content of the powdered alloy had changed from initial specications. Also, the particle size had become coarser. When rening the powder mesh to between 90 m-120 m, the void percentage reduced or was eliminated. However, instability of the powder source and cleanliness of powder was now questionable. A new material for carbon steel deposition would have to be developed. However, the profoundly different microstructure of carbon steels, required that a more fundamental understanding of the deposition process needed to developed.

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. 4.1 Gentry, D., Humbert, L., and Burlot, Rene, C. R. Academy of Science, Paris, Vol 309:II, p. 1481, (1989) 4.2 Ranjit, R. A Primer on the Taguchi Method, Van Nostrand Reinhold, New York, pp. 145-155, (1990). 4.3 Homand-Etienne, F., and Houper, R., International Journal of Rock Mechanics and Mining Sciences and Geomechanics, p. 125, (1989) 4.4 ASM Engineering Property of Steel, ASM, pp. 458-461, (1982). 4.5 Wayman, Michael, The Metals Black Book: Ferrous Metals, Vol. 1., 2nd Edition, Cast 1 Publishing Inc., Edmonton, Alberta, pp. 14-37, (1995). 4.6 Metals Handbook, ASM, Vol 2, pp. 253-254, (1974). 4.7 Metals Handbook, Lyman, Taylor, Vol. 2, 8th Edition, American Society of Metals, Metals Park, Ohio, pp. 221-283, (1964).

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Chapter 5 Characterization Tool Steels

In this chapter, the characterization of carbon steels on a layer by layer basis was preformed to understand the cell and layer morphology of depositing tools steels. A generalization of carbon steel (>.05%C) morphology in layer manufacturing is made which can be aid in designing and building carbon steel parts. The term carbon steel is used to designate the set of steels characterized. The austenitic steel 316L is also characterized to serve as a comparison. New tools for determining microstructural phases are adapted for layered manufacturing with laser deposition: Shaefer Welding Diagram and the Solidication Modes Diagram. When originally attempting to deposit carbon steels, the same optimization strategy designed for laser deposition of 316L stainless steel and aluminum bronze was used. This strategy emphasizes trying to maximize layer thickness and minimize the build completion time. Using this laser deposition strategy which emphasized maximizing throughput was simply inadequate for depositing carbon steels because of phase transformations. Phase transformations of materials had not been encountered before. In order to improve tool steel deposition a more fundamental understanding of the deposition of tools steels from a microstructual level needed to occur. Also, since SDM Tool (SDMT) steel was no longer the most reliable powder choice, more materials had to be tested. The opportunity to investigate higher carbon materials would be benecial to the quest to understand the affect of parameters on material phases and layered deposition microstructure.

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Chapter 5. 1 The Addition of 400 Series Stainless Steels and Other Carbon Steels With the quality of SDMT alloy now in question, the opportunity to change or add materials to the characterization search was now presented. Martensitic stainless steel alloys can attain the hardnesses need for die cast tooling, and were readily available. Multiple sources of powder could be found. The 400 series stainless can possess several different quantities of carbon, so the possibility of developing a understanding of the relationship of material constituents to factors like hardness or strength now existed. For conventional processes, like quenching and tempering, correlations currentlt exist to quantify the effects of material composition upon hardness levels. Thus, by using the 400 series, one could develop a more meaningful understanding of carbon steel deposition than just developing a carbon steel for die casting. The composition of tested martensitic steels are compared against the other carbons steels investigated and 316L in the table below:

C%

Mn % .17 .49 .69 1

Si% .53 .54 .57 1.23

Cr% 12.5 13.6 15.6 21.5

Ni% .07 0 1.78 2.8

Mo % 0 0 0 0

Nb % 0 0 0 .84

Al% 0 0 0 0

P% .017 .017 .016 0

S% .007 .007 .003 0

410 420 431 SDM Tool Steel I


H13 M2

.06 .45 .18 .01

.4 .8 .15 .02

0 .3

1.05 .3

5 4 16

0 0 1 13.1

0 0

0 0

0 0

0 0

0 6

1.1 2

0 0

Rock 316L

1.74

.73

17.3

2.66

Table 5.1 Carbon Steels: Martensitic, Hot Working, Tool Steels, and Commercial Alloys

When one looks at the E/ ratio for these steels, we can see that only one has a ratio higher than 316L stainless. However, most are much worse:

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E x104 MPa 410 420 431 M2 H13 SDM Tool Steel 316L 21 25.4 19.3 22 20 20

(annealed) 241 345 665 913 580 301

MPa

E/

1250 510 234

168 498 825

Table 5.2 Comparison of E/ of Tool Steels

The coefcient of thermal expansion of these materials are lower than 316L but not lower than Invar in the 20oC - 400oC range. It is during this range the residual stress begin to develop. At temperatures above this range, the yield strength of the material has been exceeded so the plastic deformation of the material relieves any additional stress accumulation. SDM tool steel is similar in composition to 440C. Thus, 440C is included to approximate SDM tool steels coefcient of thermal expansion. The corrosion resistance of most of the 400 series stainless is a bit lower than 316L. From the initial tooling search, a criteria of at least 12% chromium had been designated to insure corrosion resistance. However, since SDM has the capability of building gradient structures, the ability to deposit a high corrosion resistant material next to a low corrosion resistant material, this concern was removed.

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20 15

Coefficient of Thermal Expansion


316 410 420 440C 414 430

CTE m/(m K)

10 5

Invar (Fe -36Ni)

0 0 200 400 600 800 1000 1200 1400 Temperature (K)

Figure 5.1 Comparison of the Coefcient of Thermal Expansion of Tool Steels and SDM Materials

For example, suppose cooling channels need to be deposit in a tooling insert. Typically, the part would be planned with copper (the sacricial material) being deposited as the cooling channel and the hard carbon steel deposited around the copper, forming the walls of the cooling channel. However, during the etch removal of the copper, some of the low corrosion resistant carbon steel would also be etched. However, if 316L stainless is deposited as a barrier between the copper and carbon steel interface, the carbon steel interior of the die insert would be protected. Figure 5.2 shows the cooling channel arrangement. Figure 5.3 shows that it is possible to achieve smooth gradients by changing the percentage of each metal during deposition. The gure shows a graded deposition with SDM tool steel and 316L by laser deposition. The dotted line represents the composition as detected by electron microprobe measurements and calibrated to represent the increasing carbon content. The solid line represents the hardness of carbon steel alloys with similar compositions. The smooth transition enables the use of martensitic stainless or even lower corrosion resistant carbon steels, like H13.

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Copper 316L Carbon Steel A A Cooling Channel


Figure 5.2 Graded Structure with Cooling Channel

Die Insert

Section A

50
Hardened Stainless SS-Tool Steel Deposition

40

Rockwell C

30

20

10

100% 316L
0 0 0.05 %C 0.1

100% Carbon Steel


0.15

Figure 5.3 Graded Deposition of 316L and a .15% Carbon Steel

Chapter 5. 2 Differences in Depositing Carbon Steels Our understanding of deformation, grain size, cell morphology, and other aspects of laser layered manufacturing had developed over many years of laser depositing invar, aluminum bronze, and 316L. However, none of these materials undergo solid state phase transformation during laser deposition. These materials remain face centered cubic or body centered cubic.
Chapter 5. 2.1 Stress States of Carbon Steels Two noticeable aspects of deposition changed: stress state and hardness. In 316L, tensile stresses, measured by X-ray diffraction, were located within the deposit and compressive stresses were measured within the substrate. This is predominantly from solidication shrinkage. The melted 316L powder will shrink upon solidication and cooling. The coefcient of thermal expansion insures that the shrinkage will be
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upon the order of the thermal gradient. However, since the deposit is constrained by the substrate it is placed in tension. The substrate is simultaneously placed in compression.

As the material shrinks the molecules of the deposit are placed in tension because it is constraint by substrate. These tension forces cause the molecules of the substrate to be in compression.
Figure 5.4 Material Shrinkage

However, in carbon steels, some solid-state phase transformations can induce either tension or compression within the laser layered deposits. Stress measurments of cross sections of laser deposited 316L stainless steel and carbon steels were taken by use of the Sin2 and Fastress methods, respectively [Section 3. 2.2]. Figure 5.5 shows the results for the stress testing. Steels with percentage weight carbon between .2-.8% can impose compressive stresses within the deposit and tensile stresses within the zz
Stress (MPA)

400

.2% C -Stainless Steel .8% C - M2 1.7% C - Grey Cast Iron .1% C 316L

200

zz

Cross Section of Layers

-200

-400 4 3 2 1 0 - 1 - 2 - 3 - 4 Depth (mm) - Note: 0 is substrate-deposit interface

Figure 5.5 Stress development in SDM Deposits

substrate. When considering multiple phase depositions, one can consider it having a

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Chapter 5 Characterization Tool Steels

matrix phase and inclusion phases. The balance between hydrostatic pressure arising from the inclusion phase upon the matrix and stress from thermal contraction of the matrix will dictate the magnitude and sign of the stress [6.17]. Figure 5.5 is a graph of residual stress measured at different points within the bulk of a deposit which is still constrained by the substrate. The austenitic 316L stainless steel deposit exhibits tension, while the substrate is in compression which is common to single phase depositions. The austenite (20%) and martensite deposition of a .2%C martensitic stainless steel has the deposit in compression and the substrate displaying both compression and tension at different points. The two phase (matrix and inclusion) deposit has changed the stress prole exhibited by the deposit. The high carbon steel (.8% C) also displays mixed modes. At the top of the deposit (the last deposited layer) the material is primarily austenite and martensite and the material exhibits compression. The middle and bottom layers consist of 3 phases, austenite, martensite and ferrite. The middle and lower regions of the deposit exhibit tension. The possibility of different stress states causes our current understanding of laser deposition to be challenged. However, these different stress states could be benecial. The possibility of compression in the deposited layers could benecially affect layered deposition by improving crack resistance but it could also be detrimental by reducing fatigue strength. Chapter 5. 2.2 Hardness of Laser Deposited Carbon Steels Hardness for 316L and Invar were 90-96 Rb (200-230 HK) and 80-90Rb (175200 HK). This level of hardness indicates typically soft and reasonably ductile material. Hardnesses for the carbon steels deposited by SDMs 2400 W Nd:YAG laser was now in the range of 35-65 Rc (350-700 HK). The higher the carbon content, the
600

Microhardness (HK)

500 400 300 200 100

410-Left Side 410-Middle

Deposit

Substrate

8 6 4 2 0 -2 -4 -6 -8 Distance (mm) Note: O is Deposit Interface

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Figure 5.6 Microhardness of a 410 (SP) deposit on a low carbon steel cold roll substrate

higher the hardness ranked. Figures 5.6-5.9 are microhardness graphs of 410 and 420 martensitic stainless steels. Each structure is from 5-6 layers thick. The measurements are taken in two places: 2 mm on the left edge of a deposit and in the middle of the deposit. Each deposit is about 20 mm wide. Different build styles were used to try to increase hardness by creating more martensite within the bulk structure. A single pass style (SP) occurs when each layer is built with powder rst being placed on the substrate or previously deposited layer and then scanned by the laser. This sequence continues over and over until the part is completed. A double pass style (DP) is very
600

Microhardness (HK)

500 400 300 200 100 Deposit

410R Left 410R-Middle

Substrate

8 6 4 2 0 -2 -4 -6 -8 Distance (mm) Note: O is Deposit Interface

Figure 5.7 Microhardness of a 410 (DP) deposit on a low carbon steel cold roll substrate
600 420-Left 420-Middle

Microhardness (HK)

500 400 300 200 100 Deposit

Substrate

8 6 4 2 0 -2 -4 -6 -8 Distance (mm) Note: O is Deposit Interface

Figure 5.8 Microhardness of a 420 (SP) deposit on a low carbon steel cold roll substrate

isimilar with one important difference. Powder is preplaced upon the substrate or previously deposited structure and then scanned by the laser. Immediately, the laser scans the part again, a double pass. No additional powder is placed on the newly deposited layer before the double pass occurs. This procedure of a powder-laser scan combination followed by a powderless-laser scan is continued to produce each layer of

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the part. It was hoped that the second scan would reduce the retention of secondary retained phases or extend the heat affected zone of the laser pass to harden the material. The left side of deposits seem to have much more variability in hardness than the middle of the deposit. The bottom layers of the SP deposits in the middle of the deposits are typically harder than the top layers of the same area. In 410, the DP sequence hardened the deposit signicantly, while the 420 DP deposit seems to have soften a bit.
600 Microhardness (HK) 500 400 300 200 100 Deposit Substrate 420R-Left 420R-Middle

8 6 4 2 0 -2 -4 -6 -8 Distance (mm) Note: O is Deposit Interface

Figure 5.9 Microhardness of a 420 (DP) deposit on a low carbon steel cold roll substrate

Chapter 5. 3 Changes in Solidication Modes When building parts or die inserts by using a layer laser manufacturing technique, there are two steps which should dictate the resultant phases: Solidication and Layering. Solidication or the solidify of molten metal particles into a solid deposit is a signicant affect. With our laser deposition process, we are able to attain
solidication rates between 104 and 105 K/s. This is rapid solidication. By undergoing rapid solidication, metastable phases can now exist at room temperature. Austenite, martensite, and even sigma ferrite may exist. Under slower cooling processes, martensite will not form, austenite should not be retained, and sigma ferrite may not exist in iron based steels. If we can understand the solidication modes produces by rapid solidication, then we may be able to predict in advance phases produced in the deposition process and begin to prescribe processing changes or even heat treatments for minimal layer deposits (1-3 layers). Tools have been developed by Shaefer (5.1) and Delong (5.2) to aid in predicting solidication modes. These tools are dependent upon knowing the

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composition of the metals. The solidication diagram is based upon the fact that as most iron based metals solidify from the liquid state, the will either solidify as austenite or ferrite. Typically , the determining factor resides within the composition. The amount of nickel or chromium within the metal is typically the determinant. Nickel is an austenite stabilizing element and chromium is a ferrite-stabilizing element. The ratio of Chromium to nickel is a good indication of which phase the melt will solidify rst. If the Cr/Ni ratio is higher than 1.5 the melt will solidify as ferrite. If the Cr/Ni ratio is lower than 1.5 it will solidify as austenite (5.3). Other elements may also be classied as austenite or ferrite-stabilizing. Carbon and manganese are strong austenite stabilizing elements. Molybdenum, silicon, and niobium are strong ferrite stabilizing elements. Austenite forming element may extend the austenite range on the Fe-C phase diagram to lower temperatures. Ferrite stabilizing element may extend the ferrite zone or shrink the austenitic phase eld (5.1). The solidication diagram displays four modes of solidication which are quantied by the calculation of nickel (Ni-Eq) and (Cr-Eq) chromium equivalence. The nickel equivalence (Ni-Eq = Ni + 30 C + .5 Mn) and the chromium equivalence (Cr-Eq = Cr + Mo + 1.5 Si + .5 Nb) attempt to incorporate the effects of the strongest ferrite or austenite-stabilizing elements.

Ni-Equivalent = C, NI

40 35 30 25 20 15 10 5 0

A AF
FA F
5 10

Cr-Equivalent = Cr, Nb, Mo

15

20

25

30

Figure 5.10 Solidication Diagram

The Solidication Diagram was designed to be used to determine the solidication modes of weld metal. It uses the nickel and chromium equivalents to determine the mode preference. Four solidication modes are represented on the

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Chapter 5 Characterization Tool Steels

diagram: Austenitic (A), Austenitic-ferritic (AF), Ferritic (F) and Ferritic-austenitic (FA). Austenitic solidication is a mode in which austenite solidies as the primary and only mode. No ferrite is present in the structure. Segregation occurs only to grain boundaries. Austenitic-ferritic solidication has austenite solidifying as the primary phase with ferrite forming at grain boundaries. The ferritic second phase may partially transform to austenite at subsolidus temperatures. Ferritic solidication occurs when ferrite solidies at the primary and only phase. Ferritic-austenitic solidication occurs when ferrite is the primary phase but a second phase, austenite grows at grain boundaries. Seven carbon steels were examined. M2, H13, Rock, SDMT, 410, 420, 431 were compared against 316L. Table 5.3 shows the calculated nickel equivalents.

Metal 410-Anval 420-Anval 431-Anval SDMT M2 H13 Rock 316L

Cr-Eq 12.500 13.600 15.600 21.520 4.0000 6.3500 21.000 19.960

Ni-Eq 2.1700 15.750 8.0800 3.1450 28.000 14.000 1.5500 13.905

Table 5.3 Nickel and Chromium Equivalents


40 35
Nickel Equivalent

30 25 20 15 10 5 0 5 10 410 H13 M2

A AF
420 431 SDMT Rock 25 316L

FA F
30

15 20 Cr-Equivalent

Figure 5.11 Solidication Modes as Determined by Nickel and Chromium Equivalents

Chapter 5. 3 Changes in Solidication Modes

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Chapter 5 Characterization Tool Steels

However, rapid solidication of the laser melt pool allows for most of the modes to solidify as austenitic and austenitic-ferritic (Figure 5.12). The rapid solidication seems to suppress the ferritic transformation. When comparing these results against other rapid solidication techniques, the suppression of the ferritic transformation is supported for similarly composed metals especially stainless steel (5.5,5.6).
40 35 30 25 20 15 10 5 0

Ni-Equivalent

M2 H13 410
5 10

A
420

316L

AF

431 RockSDMT F A
15 20 25 30

Cr-Equivalent
Figure 5.12 Redrawn Solidication Diagram

Chapter 5. 4 The Inuence of Layering upon Laser Deposited Carbon Steels A single layer typically is not enough material deposition to build a part. Several layers have to be deposited in order to build parts. Figure 5.13 shows a deposition which has been etched with sodium meta-bisulte to reveal the individual weld passes.

2 mm
N+2 N+1 N
Substrate

T1 T2 T3

Build Platform

Figure 5.13 SDM deposited 410 Stainless steel Vs. a diagram showing layered manufacturing

With each additional layer, prior layers begin to be reheated. The layering process allows for multiple temperature gradient to exist within the deposition. Thus,
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the phases of the solidied structure will change. Solid state phase transformations may occur, grain growth, or tempering may occur. To account for just solidication phases is insufcient. The SDM deposition process is very similar to multipass welding. Tools like the Shaefer welding diagram could be potentially used to benet SDM designers by aiding them to understand phase development. By knowing phase developement,the SDM designer can now make a more informed decision on material selection and potentially gain insight upon necessary heat treatment regimes to remove unwanted phases. However, the Shaefer welding diagram was designed for lower solidication rates. Conventional welding processes like acetylene torches or GMAW solidify between 100 to 102 K/s. Solidication for this application has been calculated to be between 104 to 105 K/s. Other laser based process can be as high as 107. Figure 5.14 is a plot of the test metals on the traditional Shaefer Welding Diagram. The phases that the diagram predicts are only correct in one incident. Using the nickel and chromium equivalents calculated above, one can see the predicted phases are inadequate. For the Shaefer Diagram to be useful for layered manufacturing, it would have to be changed.
The Prediction Actual M2
A+M 420 316L 431 A+M+F SDMT
20 25 30 15

30 25

Actual 431=A+M+F
431 = A+M+F 420 420 = A+M+F = A+M+F 316L = A 316L = A 410 = A+M 410 =A+M SDMT =SDMT =A+M A+M H13 = A+M H13 =A+M M2 = A+M+F

Austenite

Ni-Equivalent

20 15

H13
10

Martensite
5 0 0 5 10

M+F() 410

-Ferrite
35 40

M2 =A+M+F

Cr-Equivalent

A=Austenite, F=Ferrite, M=Martensite

Figure 5.14 Plotting the test metals based on the Nickel and Chromium Equivalents

Other researches investigating rapid solidication have suggested altering the Shaefer diagram. Vitek et. (5.7) al and Katayama et. al. (5.8) have actually proposed modications of the Shaefer Welding diagram to reect rapid solidication. Instead of modify the areas of the diagram, Self et. al (5.9) proposes modifying the denition of the nickel equivalent. This approach seems to be stronger, in that trends to modifying the denitions of nickel equivalents can be accomplished more easily than redening the boundaries of the entire diagram. In this study, the researched focused
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Chapter 5 Characterization Tool Steels

upon the martensitic regions of the Shaefer Diagram. Other researchers data who have looked at other rapid solidication processes or laser multipass welding phenomena have predominantly studied metals falling in the austenitic and ferritic regions. Combining their analysis with this research could provide a more comprehensive revision to the Shaefer welding diagram and a more robust solution. Utilizing the group handling data method (GMDH), the Cr-Eq and Ni-Eq were modied to place the rapid solidication metals in to the correct areas. The GMDH was not only given the compositional elements of the metals to choose from but melting temperatures, thermal conductivities, etc. to nd the relevant modications to the Shaefer Diagram. Also, other researchers data was also included in the pattern recognition search (5.6,5.10,5.11). 30
25 Austenite A+M LS 316L

Ni-Equivalent

20 15 10 5

ST = SDMT

0 0

H13 309A ST 4 3 1 M2 Martensite 410 A+M+F 420 M+F( ) 5 10 15 20 25 30

-Ferrite

35

40

Cr-Equivalent
Figure 5.15 Modied Shaefer for Layered Laser Manufacturing

Figure 5.15 shows the modied Shaefer Welding Diagram. Notice how the the over all trend is to shift down and to the right for the more martensitic and triphase steels and up and left for the more austenitic steels. (Figure 5.17 shows more of the modelled data and includes other researchers data: Katayama (5.8), Vitek (5.7), David(5.6) , Anjos (5.9), Wei (5.10). ) Figure 5.16 shows the proposed New Ni-Eq and Cr-Eq. Both the New Ni-Eq and the New Cr-Eq show a dependence upon the Cr-Eq. This is similar to results found by Self et al (5.9). Self found that the amount of chromium was relevant in the retention of austenite and the formation of martensite . At high chromium the phase change of interest in Selfs work is austenite-ferrite, but at low chromium, it becomes austenite-martensite.
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Chapter 5 Characterization Tool Steels

Researchers have shown that the level of chromium can become an agent to determine how certain phase-stabilizers behave. In addition to the strong austenitestabilizers listed earlier, there are others: Co, Cu, N, Al. There are also additional ferrite-stabilizers: Ta, Ti, W, V, Z. However, during cryogenic solidication or high service temperatures, some of these element along with Mn, Al, Mo, and Si may change and stabilize the opposite modes (5.12, 5.13). At high solidication rates, ferrite-stabilizers may act as austenite-stabilizers and vice-versa. One indicator of this mode change, may be the level of chromium. In low chromium systems, ferritestabilizers act like ferrite-stabilizers and austenite-stabilizers act like austenitestabilizers. In high chromium systems the switching: properties has been shown to occur.

(New Ni-Eq) = 11.977810 -0.368111 [W] + 1.598563 [Mo] + 0.579666 [Ni] - 0.262729 [Cr-Eq] (New Cr-Eq) =0.666030 + 0.578787 [V] +5.386530 [Si] + 2.048034 [W] + 0.811128 [Cr-Eq]
Figure 5.16 The proposed NI-Eq and Cr-Eq

Figure 5.17 shows the limits of the proposed model. The distinctive separation of high ferrite- low austenite content welds from fully ferritic welds is not very clear. 312B was fully ferritic in rapid solidication experiments. However, with the traditional Shaefer diagram. However, Katayamas 100% Ferrite line may be more appropriate for the true boundary line (5.8).
30 25
Ni-Equivalent

Austenite A+M LS MS 316A 316L 316B

20 15 10 5 0 0

Instability in the Model: Model in accurately predicts the austenite ferrite content in this region. 100% Ferrite Line proposed by Katayama, et. al.

H13 304A 309A ST 312B R 4 3 1 M2 Martensite A+M+F 4 4 6 4 1 04 2 0 -Ferrite M+F() 5 10 15 20 25 Cr-Equivalent 30 35 40


Solidification Rate: 104 -106

Figure 5.17 The Extents of the Laser Layered Manufacturing Shaefer Model

Chapter 5. 4 The Inuence of Layering upon Laser Deposited Carbon Steels

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Chapter 5 Characterization Tool Steels

Chapter 5. 5 Phase Location The improved Shaefer Welding Diagram for Layer Manufacturing does not account for the exact percentage of austenite, martensite or ferrite within the deposited material except for 100% single consituency regions. Regions of multiple phases now only account for the existence of a phase as oppose to the quanitity. This exists for two reasons: 1. The data is being t to the Shaefer Welding Diagram thereby eliminating the phase percentage and diagram location relationship. 2. The data is an average of the amount of phases which exist within the bulk deposit. The original Shaefer Welding Diagram was designed to aid designers to not only predict the existence of phases within the welded materials but also to predict the phase percentages. Because data is being t into diagram, it was very difcult to maintain the phase percentages as described by the diagram and successfully redene the Ni & Cr equivalences to accurately describe a wide set of material compositions and encompass the full effects of rapid solidication. To produce a diagram which can acurately describe phases percentage would require redrawing the entire Shaefer Diagram. The model uses the average phase values to position the material within the correct Shaefer zone. A laser deposit which is more than 3 layers thick can be divided into 3 disctinct regions: bottom, middle and top.
A1. Top 420 SS-Single Pass B1. Top 420 SS-Double Pass

50 m 50 m
A2. Middle 420 SS-Single Pass

50 m 50 m

B2. Middle 420 SS-Double Pass

50 m

A3. Bottom 420 SS-Single Pass B3. Bottom 420 SS-Double Pass

50 m

Figure 5.18 Top, Middle, and Bottom sections of carbon steels

Figure 5.18 shows two sets of pictures of microstructural zones of laser


Chapter 5. 5 Phase Location

106

Chapter 5 Characterization Tool Steels

deposited stainless steel. The micrographs labeled A were built with single scans. Single pass scans are a deposition sequence of placing the powder upon the substrate or previously deposited layer and then scanning the powder with the laser heat. The micrographs labeled B were built with double scans. Double pass scans are a deposition sequence of placing the powder upon the substrate or previously deposited layer, scanning it with the laser heat, and then immediately scanning the surface again with laser heat without the addition of new powder. These two samples are included to show how different the microstructure can look if the laser solidication-reheating sequence is changed even with the same lasing conditions (laser power, scanning speed, powder feed rate, etc.). The bottoms of both carbon steel deposits have a signicant amounts asquenched martensite, characterized by dark brown to black because of reactive etching. The lighter brown shown in all 6 photos is tempered martensite. Blue indicates ferrite. The shiny or unreacted boundaries are mixtures of retained austenite and ferrite. Table 5.4 and 5.5 show the average phase percentage for the 420 deposits

Martensite Top Middle Bottom Average 86% 82% 76% 81%

Ferrite 7% 6% 4% 6%

Austenite 5% 9% 12% 9%

Table 5.4 Phase Averages for each location in a 420 Single Pass Laser Deposit

Martensite Top Middle Bottom Average 77% 94% 79% 83%

Ferrite 4% 0% 2% 2%

Austenite 14% 2% 15% 10%

Table 5.5 Phase Averages for each location in a 420 Double Pass Laser Deposit

Chapter 5. 5 Phase Location

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Chapter 5 Characterization Tool Steels

of both conditions (See section 3. 1.1 -3. 2.2 for methodology used to measure phases). The differences in microstructure based upon location can be dramatic and is determined by proximity to substrate ( which acts as a heat sink), the number of layers deposited, and laser conditions. A single tool which could meaningfully characterize all of these effects and still provide quantitative phase percentages is extremely difcult to build. Multiple tools for each region, each lasing condition, and each material would have to be constructed. Also, the regions may not scale as easily to larger builds. When the total thickness of deposited layers extends beyond 25 mm, signicant changes may occur to the phases present. The continual reheating of lower layers begins to form more equilibrium phases like cementite and banite. Therefore, another set of Shafer Diagrams would have to be built. As recounted in Chapter 2, there are several competitive laser deposition processes which can also benet from this knowledge. However, each of the processes uses different deposition sequences, laser conditions, etc. A specic regional tool for SDM could not be leveraged very well for their applications. A universal tool that can inform the designers of potential phases that can arise during laser deposition, is much more useful.

Chapter 5. 6 Grain Size of Laser Deposited Layered Carbon Steels Grain size is indicative of the material properties of the laser deposit. The grain structure of austenitic steels is very different from the laser deposited carbon steels. Austenitic steels formed lenticular shaped cells while the carbon formed from lathe to plate -like structures. No direct correlation could be found between powder size to grain size. However, by using GMDH a relation ship was developed which can predict equivalent diameters of the grains. Equivalent diameters are based on the area of the grain. Using GMDH, a heuristic was developed to predict grain size. The factors included at the beginning of modeling were material composition, powder size, solidication rate, thermal conductivity, and melting point. Figure 5.20 displays the relevant terms. The heuristic will enable designers to get an estimate of the grain size
of the structure if they are using a layering process with solidication rates from 104105 K/s.

Chapter 5. 6 Grain Size of Laser Deposited Layered Carbon Steels

108

Chapter 5 Characterization Tool Steels

Metal 316L 410 SS 431 SS 420 SS H13 SDMT

Phase(s) 100%-A 30%A+M 9%A+M+ 2%F 14%A+M+ 6%F 3%A+M 20%A +M

Powder Size 74 +34 m 55 +32 m 122 +49 m 100 +60 m 45 +20 m 90 +20 m

Equivalent Diameter 9.64 m 10.29 m 5.63 m 5.04 m 4.76 m 4.11 m

Table 5.6 Powder Diameter Vs. Grain Diameter

100 m

100 m

Laser Deposited 431 SS


100 m 100 m

Laser Deposited 410 SS


100 m

100 m

Laser Deposited 420 SS


Figure 5.19 Examples of Grain Sizes

Laser Deposited 316L

Laser Deposited 316L Stainless

The heuristics components seem to be quite applicable. The carbon content will inuence phase formation as well as aid carbide forming elements. Carbide forming element, particularly Mo and V, because they can act as grain size controlling elements. The principal effect of the grain size controlling elements is to extend the recrystallizing time of austenite. The longer time the it takes for austenite to recrystallize, the more nucleation sites for ferrite to form. The more ferrite nucleation site the smaller the ferrite grains will be (5.14). The chromium and Ni-Eq (30*C+Ni+Mn), all aid in determining the phases which exist in the solidify melt. The
Chapter 5. 6 Grain Size of Laser Deposited Layered Carbon Steels

109

Chapter 5 Characterization Tool Steels

melting kinetics related to powder size, thermal conductivity and melting temperature will all inuence grain size.

Average Grain Diameter (m)= 22.8(m) + {0.3 [V] + 3.7 [C] -0.0008/K [Melting Temperature] + 0.6[Cr] -0.1/m [Powder Size] -0.8 [Mo]-0.3 [NI-EQ] -0.5ms/K []}m
Figure 5.20 Equation for Grain Size Predictor

Experimentally Measured Calculated Values 410 420 431 SDMT H13 316L Invar 0 2 4 6 8 10 Equivalent Diameter (m) 12

Figure 5.21 Grain Size Comparison Actual Vs. Heuristic

Chapter 5. 7 Layer Thickness Layer thickness is another characteristic of deposition which needs to be understood. The ability to predict layer thickness will enable designers to accurately forecast the number of layers needed to build a part and predict completion times. Also, understanding the nature of layer morphology will enable more insightful planning. Since SDM is deposited at room temperature and without preheat, much of the energy of the rst layer of deposition is used to bring the substrate and build platform to a steady state temperature with the fresh deposit. The low carbon steel substrate and aluminum build platform act as a heat sink. As more layers are deposited, and the distance from the top layer to the substrate increases, the upper layers of the deposit begin to get warmer. The weld pool can be larger and more powder is able to solidify. Thus layers size increases with z-height. However, the layer thickness does begin to achieve a mean thickness. The last layer of the deposit is about 40-50% larger than
Chapter 5. 7 Layer Thickness

110

Chapter 5 Characterization Tool Steels

mean size thickness. The last layer is not remelted like the prior layer so it maintains the thickness of individual weld passes. Table 5.7 displays layer values for 4 steels used in the research. Five layer structures were built of each material. Two examples of 420 are shown. One was built with single pass layers while 420-DP was built in a double pass condition: Immediately following a powder melting laser pass, the laser scans the part again, this time with no powder. All of the other beams were built with a single pass. The double pass builds seem to slightly thicken the latter layers of the build.

Layer 5th Layer 4th Layer 3rd Layer 2nd Layer 1st Layer

316L (m) 1200 937 899 604 550

SDMT (m) 1286 856 904 647 292

431 (m) 1624 703 797 557 470

420 (m) 732 468 413 442 174

420-DP (m) 755 550 503 470 208

Table 5.7 Layer Thickness for SDM Carbon Steels

Every time a deposit is allowed to cool to room temperature, the layer size starts almost back over, as if it were a brand new deposit instead of a continued build. Figure 5.22 shows a 60 layer (55 mm) structure. Notice how the layer thickness deviates as the build gains in z-height. Figure 5.23 shows the same graph but this time it is identied with every time with the break that was taken during the deposition. The ability to control layer thickness seems to stem from scheduling breaks. If a certain layer size is critical to part strength or critical internal location, like the deposition strategy for the location of internal geometry, a cooling/deposition sequence during the build process need to occur. Lastly, if more than 12 layers are deposited at any point in time, the grain size of bottom layers may grow as well as incur phase transformations.

Chapter 5. 7 Layer Thickness

111

Chapter 5 Characterization Tool Steels

Average Layer Thickness (mm)

1.4 1.2 1 0.8 0.6 0.4 0.2 0


20 0 25 5 35 40 130 0 15 20 Z-Height (mm) 45 25 50 30

Figure 5.22 Sixty Layer Deposition

GHDM was used to determine what the most signicant factors effecting the mean layer thickness. In addition to the material composition, material properties like thermal conductivity, melting point and solidication rate, two addition factors were added: ll rate and thermal diffusivity length.

4 2
A = Overnight Cooling

Layer Thickness (mm)

1 0.8 8 0.6 6 0.4 4 0.2 2 0


20 0

A B B B
25 5

(12-24hr breaks) B = Short Cooling Periods (1-2hr breaks)

A A
40 20 45 25 50 30

130 0

Z-Height (mm)

35 15

Figure 5.23 The Effect of Cooling on Deposition

Chapter 5. 7 Layer Thickness

112

Chapter 5 Characterization Tool Steels

Figure 5.24 shows the results of the model. Metals with various deposition ll rates and scanning speeds were put in the model. However, Figure 5.25 just shows one setting. Figure 5.25 shows a comparison between the model and the actual values of mean layer thickness. Layer (m) = 1176.7m + {80.8 [V] -0.0008s/K [Solidification Rate] +11.1 [Ni] - 40.3 [Ni-EQ + 27.8 min/g [Fill Rate] - 5.5/m [Powder Size]} m
Figure 5.24 Heuristic for Predicting Mean Layer Size

Experimentally Measured Calculated Value 410 420 431 SDMT H13 316L Invar 0 200 400 600 8 0 0 1000 1200

30 mm/s at 23g/min

Thickness (m)
Figure 5.25 Comparison of Mean Layer thickness: Predict Vs. Actual

Even thought the solidication rate does include the effects of the scanning speed, it is the powder ll rate which make more of an impact upon mean layer thickness. As Figure 5.26 shows, from 15 mm/s to 40 mm/s there is an insensitivity to laser scanning speeds. The amount of energy that the SDM puts into weld is so large that regardless of the speed adequate layer solidication is achieved. At speeds higher than 40 mm/s, the 407 W/mm2 is no longer sufcient to get good layer solidication with no porosity or retention or secondary phases. The ll rate is extremely sensitive. Depositions below 23 g/min tend produce too thin of layers and more secondary phases from solid state phase transformations tend to occur. Depositions above 23 g/min produce too thick of layers, secondary phases are retained from the melt.

Chapter 5. 7 Layer Thickness

113

Chapter 5 Characterization Tool Steels

Laser Scan Speed (mm/s)

15

20

25 30

35 40 45 50

55 40 25 30 15 20 35
%Retained Austenite

5 10

Speed Fill Rate

5 10 15

20

25 30 35 40

Fill Rate (g/min)


Figure 5.26 Optimizing Deposition Parameters

Chapter 5. 7 Layer Thickness

114

Chapter 5 Characterization Tool Steels

5.1 Shaefer, A. L., Constitutional Diagram for Stainless Steel Weld Metal, Metal Progress 56(5): 680-680B. 5.2 Delong, W. T. Ferrite in Austenitic Stainless Steel Weld Metal, Welding Journal 53(7):273-s -286-s. 5.3 Suutala, N. Takalo,T.,Moisio, The relationship Between Solidication and Microstructure in Austenitic and Austenitic-Ferrite Stainless Steel Welds, Metallurgical Transactions 10 (A), 512-514 (1979). 5.4 Robert, George, Krauss, George, and Kennedy, Richard, Tool Steels, ASM International, 1998. 5.5 Elmer, Walter, The Inuence of Cooling Rate on the Microstructure of Stainless Steel Alloys, Lawrence Livermore Laboratory, September 1988. 5.6 David, S. A., Vitek, J. M., and Hebble, T. L., Effect of Rapid Solidication on Stainless Steel Weld Metal Microstructures and Its Implications on the Shaefer Diagram, Welding Research Supplement, October 1987, pp. 289-s- 300-s. 5.7 Vitek, J. M. , Dasgupta, A. , and David, S. A., Microstructual Modication of Austenitic Stainless Steel by Rapid Solidication, Metallurgical Transactions 14 (A), 1833-1841 (1983). 5.8 Katayama, S. and Matsunawa, Solidication Microstructure of Laser Welded Stainless Steels, Proc. ICALEO, p. 60, 1984. 5.9 Self, J. A., Matlock, D. K., and Olson, D. L., An Evaluation of Austenitic Fe-MnNi Weld Metal for Dissimilar Metal Welding, WRC Bulletin, September 1984, p 282-s - 288-s. 5.10 Wei, M. Y. and Chen, C., Fatigue Crack Growth Characteristics of Laser-Hardened 4130 Steel, Scripta Metallurgica et Materialia, Vol 31., No. 10, 1994, pp. 1393-1398. 5.11 Rieker, C., D. G. Morris, and Morris, M. A., Microcrystalline Surface Layers Created by Laser Alloying Journal of Less-Common Metals, 145 (1988) 595600. 5.12 Wallace, W., Trenouth, J. M., Daw, J.D., Microstructual Instabilities in An Industrial Engine Vane, Metallurgical Transactions A (Physical Metallurgy and Materials Science), Vol 7A, No 7, Jul 1976 p. 991-997. 5.13 Sakamoto, T., Nakagama, Y., and Yamauchi, I, Effect of Mn on the Cryogenic Properties of High Austenitic Stainless Steels, Advances in Cryogenic Engineering: Materials, Volume 32, 1986, p 65-71. 5.14 Reed-Hill, Robert E. and Abbaschian, Reza, Physical Metallurgy Principles, PWS-Kent Publishing: Boston, pp. 661-685.

Chapter 5. 7 Layer Thickness

115

Chapter 6 Applications of Characterization

Chapter 6 Applications of Characterization


Now that the formation and transformation of carbon steels in layered laser deposition is better understood, one can use this new understanding to solve deposition problems. Knowledge of grain size and phase composition are used to select high impact resistant materials and to reduce part deection. These are just two examples of how understanding the marriage of material microstructure and deposition parameters can benet layered manufacturing

Chapter 6. 1 High Impact Resistant Materials Die cast inserts need high impact resistant materials in order to survive the die casting service environment. Figure 6.1 shows a pressure trace of a 6 ton die casting machine . Dies in this machine will exhibit pressure changes from ambient to 20,000 psi and temperature changes of 150_C to 667_C in 12 seconds or less
20000 19000 18000 Shot 17000 Pressure (PSI) 16000 15000
150m C 667m C

One second after metal injection.

14000

1.0

1.4

1.8 2.2

2.6

Time (Sec)

Figure 6.1 Pressure Trace from a 6 ton Die Casting Machine

Chapter 6. 1 High Impact Resistant Materials

116

Chapter 6 Applications of Characterization

If molten aluminum is injected into a die with low impact resistance, the die will gall or initiate heatchecking. Thin features will degrade, and the die inserts will be rendered useless quickly. Impact resistance is typically measured by charpy impact specimens (see 3. 3.2) at room temperature. Die casting die inserts are typically made out of H13 and are austenitized and tempered. After these heat treatments, charpy specimens can typically endure from 10-20 ft-lb of impact resistance. Chapter 6. 1.1 Engineering Material Selections Our typical engineering understanding would have us select the material by looking at the ratio of the modulous of elasticity to yield strength (Figure 6.2 and Table 6.1). According to this SDMT should have the best results. Although better than most,

Charpy Impact Specimen

mpact Testing

Minimize the Deformation By Toughening the Material *L = h /E Minimize by maximizing E /


Figure 6.2 Maximizing the E / relationship to increase Impact Resistance

E x104 MPa 410 420 431 SDM Tool Steel H13 316L 22 20 20 25.4 21 19.3

MPa (Tempered) 1005 690 738 510 1344 415 219 290 271 498 156 465

E/

Table 6.1 Comparison of E /o Tempered Relationship

Chapter 6. 1 High Impact Resistant Materials

117

Chapter 6 Applications of Characterization

431 was clearly the best. On the half size specimens, it showed almost twice the impact resistance. If E/ is not the appropriate measure to use, perhaps the microstructual information can help.

410 431 420 SDMT H13 0 2 4 6 8 Impact Resistance (ft-lb) 10

Note: H13 was austenitized. All other specimens are in the as deposited condition.

Half Size Charpy Specimens (5mm x 10 mm x 55 mm T x W x L)

Figure 6.3 Results of Charpy Testing

Chapter 6. 1.2 Microstructual Material Selection Impact resistance is a function of grain size just as yield strength and many other properties are. Also, the phases within the deposit will determine, impact resistance. Martensite has a bulk modulus of 17.3 x 104 MPa while austenite has a bulk modulus of 16.4 x 104 MPa and ferrite has a bulk modulus of 17.1 x 104 MPa (6.1). The added toughness of martensite may be swaying the results. However, when compare grain size and phase retention, we see that it is a combined result which gets the best results. A small grain size and the reduction of secondary phases gives the best impact resistance (Figures 6.4 and 6.5).

Grain Size (m)

10.29 5.63 5.04 4.11


0 2

410 431 420 SDMT


4 6 8 10

Impact Resistance (ft-lb)


Figure 6.4 Grain Size (Equivalent Diameters) vs Impact Resistance

The additional heat treatment of H13 did not improve the results. This is a
Chapter 6. 1 High Impact Resistant Materials

118

Chapter 6 Applications of Characterization

trend seen in other metals. A series of experiments were run on the 420 martensitic stainless steels (Figure 6.6). During conventional tempering temperatures between 225- 500 Co the formation of sigma ferrite is quite high. Sigma ferrite is a brittle phase of ferrite . Because it is brittle, it often acts as a crack initiation point in materials or reduce material properties. Typically, sigma transforms from metastable delta ferrite at temperatures of 600-700 Co(6.2). Because conventional heat treatment cycles do not seem to work, each metal will have to be tested to nd appropriate heat treatments.

30

410 420 SDMT 431


0

% 2nd Phase Composition

20 17 11
2

Impact Resistance (ft-lb)

10

Figure 6.5 Secondary Phase Constituents Vs. Impact Resistance


50

Phase Percentage

40 30 20 10 0 0

Delta Ferrite Sigma Ferrite

200 400 600 800 Tempering Temperatures

Dangerous Heat Treatment Zone

1000

Figure 6.6 Sigma Ferrite Formation during Tempering Cycles of 420 Stainless Steel.

The metal 431 had the highest impact resistance. Even though its E/ ratio is not very high, the small grain structure and limited amount of secondary phases cause its material properties to be superior. When comparing the result of 431 with full size specimens, we see that the 431 results are comparable to conventionally rolled or forged H13 which has been tempered (Figure 6.7). The results do suggest that there is

Chapter 6. 1 High Impact Resistant Materials

119

Chapter 6 Applications of Characterization

a possibility to produce die inserts which can work without heat treatment. This would be an additional time savings for the designer and manufacturer.
25

Charpy V-notched

Impact energy ( ftlbf)

20 15 10 5 0 25 420/410

H13 (2 Tem, L)

431
H13 (Tem, L) H13 (Tem, T) H13-VAR (2 Tem, T) H13-ESR (2 Tem, T) 30 35 40 45 50

SDMT 410

H13 (Tem, L)

420

Hardness (Rc)
Figure 6.7 Comparison of Layered Laser Deposited Carbon Steels and Conventionally formed and tempered H13.

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transformation


Laser deposition produces rapid solidication or quenching because of fast heat conduction from the laser melt pool into the base metal. This solidication rate can also be inuenced by changing deposition parameters such as scanning speed and laser power. When depositing carbon steels, rapid solidication can cause metastable phases to occur, primarily martensite. Martensite formation is a diffusionless process which occurs when the deposit cools from high temperatures (like the steel melting point) to below the martensitic start temperature in less than 10 sec. The arrows shown in Figure 6.8 illustrate the isothermal transformation of H13 and 410 stainless steel to martensite by rapidly cooling to room temperature. Cooling slower than this would not produce martensite but result in the production of ferrite and cementite. When the laser melts the powder, the rst solid metal to nucleate within the liquid is austenite. Austenite has a face center cubic structure. The rapid quenching causes the carbon in the austenite phase to transform to body center-tetragonal (BCT) martensite trapping carbon in the BCT lattice which has not had a chance to diffuse.

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma120 tion

Chapter 6 Applications of Characterization

1800 Temperature (C) 1600 1400 1200 1000 800 600 400 200 1

A A+F A+9%F A+>9%F A+F+C F+C F+C

A=Austenite F=Ferrite C=Cementite M=Martensite

A+F+C

410 Ms 10 Time (s) 100 H13

1000

Figure 6.8 Isothermal Transformation Diagram of H13 and 410 steels. Compiled from [6.9].

This transformation results in an expansion in volume. This expansion can be as big as 4%. This is the same order of magnitude as the thermal shrinkage which arises from cooling of the metal. If martensite transformation can be induced and controlled by layered laser deposition, then the potential to balance the solidication shrinkage with phase volumetric expansion may exist. The use of lasers to change part or surface microstructure has been extensively researched for laser cladding and surface hardening. Several researchers have shown a relationship between laser parameters and microstructual evolution for laser cladding and surfacing. Wang et al. [6.5] showed that metastable phases can be produced on material surfaces by laser quenching, a process in which laser melting and quenching of a material occurs by using a very short laser pulses. Yang et. al. [6.6] used a CO2 laser to show that case depth or the depth of phase transformation and morphology of materials can be inuenced by laser power and laser scan rate. Fouquet et. al [6.7] used a continuous wave CO2 laser to transform the surface of grey cast iron from austenite to a mixture of austenite, cementite and martensite by using overlapping multiple laser scan paths. Rieker, et. al [6.8] uses a remelting second pass of the laser to homogenize the chemistry and microstructure of a laser hardened surface on ferritic stainless steel.

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma121 tion

Chapter 6 Applications of Characterization

Once the deposition of the beams was completed, the beams were tested for deection and phase composition. Table 7 lists the average results for each type of material tested. Table 7: Results of Deposition Experiments % As-quenched Martensite (MAQ) % Tempered Martensite (MT) % Austenite

Laser Pass

Deection (mm)

% Ferrite

410 420 431 SDM -Tool 316L 410 420 431

1 1 1 1 1 2 2 2

.97 1.26 .432 .89 .97 1.14 .33 .33

7 16 29 9 0 4 28 30

55 65 62 68 0 88 55 58

34 9 4 20 98 6 10 6

0 6 2.3 0 0 0 2 3

.125 .249 .471 .129 .0 .047 .506 .51

Table 6.2 Phase Analysis and Deection Results

Selective etchants revealed martensitic and austenitic phases in all the metals with the exception of 316L which is only austenitic. Martensitic stainless steel, 420, had three phases: austenite, martensite, and ferrite (Figure 6.9 and Figure 6.10).

1.

100 m

MAQ/MT

A A

Figure 6.9 Pictures of 431 stainless: 1. Optical microscope with light brown reecting tempered martensite, black - as-quenched martensite, white - retained austenite. 2. Brighteld image of TEM with white regions - martensite, black regions - austenite. @30,700 X.

Microhardness for the specimens ranged between 400-540 HK. For each of
Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma122 tion

Chapter 6 Applications of Characterization

the metals, the hardness ranges were typically below the value of typical as-quenched or hardened steel ranges. Figure 6.11 compares the quench/hardness ranges for the martensitic stainless steels used in the experiments. For certain materials increasing the martensite percentage reduced deection while it increased it in others. Figure 6.12 shows that by increasing the ratio of asquenched martensite to tempered martensite, deection is reduced. More as-quenched martensite is found in base layers than in N+1 layers (middle and top layers). This suggests that the quenching rate is much faster near the substrate than for subsequent layers. The double laser pass condition increases the quenching rate for middle sections of the beams than the single pass condition. The inset in gure 6.12 compares middle and bottom layers of 420 in single pass and double pass condition. 20 m 20 m

1.

2.
20 m

3.

4.

20 m MT A MAQ A MAQ MT A F MAQ MT A MT MAQ


4. 420

Figure 6.10 Optical Microscope pictures of :1. 410 - SP, 2. 410 - DP, 3. 420 - SP, - DP.

Chapter 6. 2.1 As-Quenched Martensite Materials Increasing the amount of as-quenched martensite retained in the beams reduced the deection of SDM deposited beams. As-quenched martensite allowed for maximum volumetric expansion. Tempered martensite allowed the carbon to diffuse, shrinking the lattice and reducing the amount of volumetric expansion achieved. SDM laser manufacturing induced as-quenched martensite. However, reheating of layers during the deposition of subsequent layers tempered much of the as-quenched martensite. The addition of a second laser pass increased the quenching rate and helped maintain more as-quenched martensite for most of the metals tested. Attaining a ratio of at least .45 as-quenched to tempered martensite produced a 30-75% reduction in deformation in the SDM deposited beams.
Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma123 tion

Chapter 6 Applications of Characterization

700 650 600 Hardness (HK) 550 500 450 400


410 (2) 431 (1)

Quench/Hardening Range for 420

Quench/Hardening Range for 431 Quench/Hardening Range for 410


420 (2) 420 (1) 431 (2)

350 300 0 5

410 (1)

10

15

20

25

30

35

Percentage of As-Quenched Martensite

Figure 6.11 Comparison of the hardness values for martensitic stainless steel beams: 1 - Single Pass, 2-Double Pass. Quenching range compiled from [6.15].

These tests upon the SDM layered process indicate that continuous deposition of material layers inuences the microstructure of N, N-1, N+1 layers. The layer that is being deposited, N, is obviously affected because of the melting and solidifying of the material. The N-1 microstructure is affected because of the reheating of the layer due to the newly deposited layer. The next layer, N+1 is affected because its grain growth direction is seeded from the prior layer N. As more layers are deposited, more heat is retained in the bulk. Grain growth in both austenitic and martensitic steels increases with each additional layer. Grain size in layer N+1 is larger than in N. However, in martensitic steels, this increased heat retention produces more tempered martensite in the bulk and upper layers than near the interface between substrate and rst layer. The difference in the heat characteristics is an important element to modelling and understanding the phase development within layered metal part.

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma124 tion

Chapter 6 Applications of Characterization

1.4
420 (1) 410 (2)

Deflection (mm)

1
410 (1)

0.8 0.6 0.4 0.2 0 0.1 0.2 0.3 0.4 M /M Ratio


AQ T

MAQ-MT

1.2

MAQ-MT M -M AQ T

(1) SP
MT

(2) DP

431 (2) 420 (2) 431 (1)

N-Layers

20m

0.5

0.6

Substrate Primary Sites for As-Quenched Martensite in 420

Figure 6.12 The effect of increasing MAQ/ MT Ratio on deection.

Multiple phases may be both detrimental and benecial to material properties. A fully martensitic beam that is in the as-quenched phase may be too brittle to use. A beam that has ferritic phases could develop sigma ferrite which is a brittle phase often related to crack initiation points in metal. However, the retention of austenite or delta ferrite has been shown to increase the toughness of martensitic parts [6.16]. Charpy impact specimens show a 20% drop impact resistance at the maximum martensite condition. However, after heat treating a beam with negligible changes in deection at 200Co for 12 hours, the difference was ony 10%. Therefore, if the as deposited condition is not sufcient, this special heat treatment may be enough to give a prototype die insert the impact resistance that it needs. Chapter 6. 2.2 Double Laser Pass Affects the Amount of As-Quenched Martensite The double pass in most cases increased the amount of As-Quench martensite retained in the deposition. As Figure 6.13 shows the double pass seems to improve the ratio of as-quenched to tempered martensite signicantly. The single pass has room temperature powder with air gaps to heat and solidify, limiting the depth of the heat affected zone (HAZ) where most of the as quench martensite populates. The double pass has 250 Co fully solid material (98-99.5% dense with minimal pores) to remelt,

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma125 tion

Chapter 6 Applications of Characterization

extending and densify the depth of the HAZ. Figure 6.14 shows the difference in a single pass and double pass on 410 stainless. The dark brown is as-quenched martensite, lighter brown is tempered martensite and white is retained austenite. Notice the reduction in the amount of retained austenite in the HAZ of the double pass deposition.

Specimen 431-SP 431-DP 431-SP 431-DP

Condition As Deposited As Deposited Heat Treated 12h @ 200Co Heat Treated 12h @ 200Co

Impact Resistance (ft-lb) 9.25 7.5 8.5 8.5

Table 6.3 Heat Treatment of 431 Laser Deposited Steels


Double Laser Scan Single Laser Scan 0.6

Ratio of As-Quenched Martensite /Tempered Martensite

0.5 0.4 0.3 0.2 0.1 0 0 5 10 15

Ratio of Crequ / Niequ

Figure 6.13 Double Pass Vs Single Pass Laser Depositions

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma126 tion

Chapter 6 Applications of Characterization

Single Pass

Double Pass

2 mm

2 mm

200 m

200 m

Figure 6.14 410 Stainless with Single Pass and Double Pass Congurations

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma127 tion

Chapter 6 Applications of Characterization

6.1 Pan, H. H. and Weng, G. J., Thermal Stress and Volume Change During A Cooling Process Involving Phase Transformation, Journal of Thermal Stresses, 15:1-23, 1992, pp. 1-23. 6.2 Gill, T. P. S., Shankar, V., Pujar, M. G., and Rodriguez, P., Effect of Composition on the Formation of d-Ferrite to s In Type 316 Stainless Steel Weld Metals, Scripta Metallurgica Materialia, Vol. 32, No. 10, pp 1595-1600. 6.3 L. Samuels, Metallographic Polishing By Mechanical Methods, 3rd Ed.1982. 6.4 Fourney, Surface Engineering of Tool and Die Steel, ASM Specialty Handbook: Tool Materials, (1995), pp.391-392. 6.5 W. K. Wang, C.J. Lobb, and F. Spaepen, Formation of Metastable Nb-Si Phases by Picosecond and Nanosecond Pulsed Laser Quenching, Materials Science and Engineering, 98, (1988) 325-328. 6.6 L.J. Yang, S. Jana, S. C. Tam, and L. E. N. Lim, The Effects of Process Variables on the Case Depth of Laser Transformation Hardened AISI 01 Tool Steel Specimens 6.7 F. Fouquet and E. Szmatula, Laser Surface Melting of a Pearlitic Grey Cast Iron, Material Science and Engineering, 98 (1988) 305-308. 6.8 C. Rieker, D. G. Morris and M. A. Morris, Microcrystalline surface layers created by laser alloying, Journal of Less-Common Metals, 145 (1988) 595-600. 6.9 Crucible Steel (1949), Rickett, Waltin, Butler (1952), Wang, Lobb, & Spaepen, (1988) 6.10 R. Merz, F.B. Prinz, K. Ramaswani, M. Terk, and L.E. Weiss, Shape Deposition Manufacturing, Proc. of Solid Freeform Fabrication Symposium, The University of Texas at Austin, (1994) pp.1-8. 6.11 J. R. Fessler, Merz, A.H, Nickel and F. B. Prinz, Proceedings of Solid Freeform Fabrication Symposium, The University of Texas at Austin, (1996) pp.117. 6.12 E. Beraha and B. Shpigler, Color Metallography, (1977). 6.13 B. L. Averbach, L. S. Castleman, and M. Cohen, Measurement of Retained Austenite in Carbon Steels, Transactions of the ASM, (1949) Vol. 42, pp112-120. 6.14 N. Williams and C. Carter, Transmission Electron Microscopy - Diffraction, Vol 2, (1996), pp.267-288. 6.15 D. Olson, T. Siewert, S. Liu and G. Edwards, Selection of Wrought Martensitic Stainless Steels, ASM Handbook: Welds, Brazing, and Soldering, Vol. 6, (1993), pp.432-442. 6.16 G. R. Link, J. Fessler, A. Nickel and F. Prinz, Rapid Tooling Die Case Inserts Using Shape Deposition Manufacturing, Material and Manufacturing, Vol 13, No, 2, (1998), pp. 263-274. 6.17 H.H. Pan and G. J. Weng, Thermal Stress and Volume Change During A Cooling Process Involving Phase Transformation, Journal of Thermal Stress, Vol. 15, (1992), pp. 1-23.

Chapter 6. 2 Characterizing Material Composition to Induce Martensite Transforma128 tion

Chapter 7 Designing For Microstructual Manipulation

Chapter 7 Designing For Microstructual Manipulation


This chapter will focus upon designing with microstructure in mind. This approach builds upon the ability of layered manufacturing to inuence microstructure on a localized as well as aggregate basis. Several design rules are introduced to aid designers working with carbon steel deposition to produce viable parts .

Chapter 7. 1 Aggregate and Localized Microstructual Inuence Inuencing or altering the microstructure of a formed object to achieve certain materials properties is a common aspect of producing viable parts. Heat treatment is often used to homogenize the microstructure of newly formed sand castings or machined metal prototypes to attain uniform hardness and reduce residual stress. The surface microstructure of metal parts like gears may be deformed by peening to impose compressive stress to increase wear resistance. Die surfaces may be impregnated with alloying agents to improve die life. Laser hardening has been used on camshafts to improve wear resistance. Layered manufacturing techniques of solid freeform fabrication have the ability to inuence or control the microstructure of the prototype. Like heat treatment and casting processes, laser deposition can affect the microstructure of the part. However, unlike these bulk processes, laser deposition techniques like surface cladding can have a more localized effect (Figure 7.1). Yang et al. [6.6] showed that a CO2 laser hardening process can produce a microstructually altered region near a
parts surface 350 m thick.

Chapter 7. 1 Aggregate and Localized Microstructual Inuence

129

Chapter 7 Designing For Microstructual Manipulation

Laser Deposition Casting Heat Treatment Hacksaw Cutoff Wheel Laser Surface Alloying Laser Welding Laser Cladding EDM Turning Lathe Surface Grinding Abrasive Paper Fine Al2O3 Polish (.1 m) Steel Brass

500

1000

1500

2000

2500

3000

Micrometers of Surface Influence from Deformation or Alloying Thickness


Figure 7.1 Surface effects of processing techniques.

The ability of laser processing to affect both aggregate and localized microstructure as well as the ability of layered manufacturing to affect both aggregate and localized geometry lends itself naturally to begin to think about designing with microstructural constraints or enhancments in mind. Often the designer is limited in her ability to improve her design because they are only focusing upon the feature level of design. They may focus upon the need for a parts surface to be a bearing surface or that two mating parts will rub, and not the underlying microstructure. If one could begin to think about the design on a microstructural level one may nd opportunities to improve the design. For example , a designer is building tensile bars. They need to be stiff but still have good elongation properties. With conventional processes, his choices are limited. With layered laser technique like SDM, one could improve elongation by placing austenitic grains within strategic locations and martensitic in areas requiring stiffness (Figure 7.2). Considering microstrure, or Designing for Microstructual Manipulation (DFM2) adds an additional element of freedom to design. Four thermal fatigue specimens were built without possessing a complete

Chapter 7. 1 Aggregate and Localized Microstructual Inuence

130

Chapter 7 Designing For Microstructual Manipulation

knowledge of the microstructure (Figure 7.3). Each one failed because the deposition strategy was not superior to the effects of the microstructure. However knowledge gained by these experiments, have increased the knowledge of carbon steel deposition 100 fold.

Constrained Designers

Unconstrained Designer

Part Needs Elongation needs elongation more than stiffness. Choose Austenitic Material
Figure 7.2 Freeing Designer with Microstructure SDMT Steel Splity

Interior Section needs Elongation Exterior needs Stiffness Choose Graded Material Deposition: Martensitic Exterior Austenitic Interior

410 Steel Brittle

H13/410 Composite Holey

SDMT Steel Cracky

Figure 7.3 Four Thermal Fatigue Specimens

Chapter 7. 2 Applying DFM2 to Internal Geometry of Die Inserts Copper cooling bars can be deposited in die inserts to improve the thermal conductivity of the dies. With improved conductivity, faster injection cycles can be attained without compromising casting integrity or microstructure. Placing sharp corners in the interior of a part builds in stress concentrations which can induce solidication cracking (Figure 7.4). If the corners could be avoided entirely the

Chapter 7. 2 Applying DFM2 to Internal Geometry of Die Inserts

131

Chapter 7 Designing For Microstructual Manipulation

316L

Solidification crack near sharp Copper Corner.

Copper 500 m 316L


Figure 7.4 Sharp Internal Corner of 316L and Copper

situation would improve, but the difference in thermal conductivity can still produce very sharp thermal gradient differences which can also produce stress concentrations (Figure 7.4). However, inducing delta ferrite near the sharp or thermally divergent interface may be a better way to avoid solidication cracking. Figure 7.5 shows a corner which was removed by the laser only to form to additional corners.

Additional Corner Created

Original Corner

100 m
Figure 7.5 Using laser to eliminate sharp corners is not always successful.

A better way to eliminate solidication cracking is to introduce delta ferrite near the stress concentration. From the carbon steel characterization, we know that 420 forms delta ferrite more easily than any of the other metals tested. The 420 material was applied after an initial powderless pass to warm the copper and insure good bonding. Figure 7.6 shows the etched surface of the interface. Delta ferrite forms near the interface. No cracks were observed.

Chapter 7. 2 Applying DFM2 to Internal Geometry of Die Inserts

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Chapter 7 Designing For Microstructual Manipulation

420
316L

50 m
Cu

50 m 100 m
.

Cu

316L

Figure 7.6 (A.) Corner Solidication crack in SS-CU. (B.) Corner Prep with 420 Stainless

Chapter 7. 3 Applying DFM2 to Part Building Strategy


Chapter 7. 3.1 Part Substrate Interface Good bonding between the parts substrate and rst layers of the part are essential to prevent delamination. As the earlier characterization shows, the rst layer is the thinnest. This thin layer is subject to both residual stress in the substrate as well as stress within the deposit. Plasma spray coatings are applied with pressure and heat to coat a surface. However most of the bonding is purely mechanical than metallurgical. Mechanical bondings are easier to rupture than metallurgical bonding. Figure 7.7 shows the similarities between a plasma coating and a laser layered deposit of H13 on low carbon cold roll steel.

H13 Stainless Steel

Good Bonding

Poor Bonding

Cu 100 m A.

Cold Roll Steel B. 100 m

Figure 7.7 A. Plasma Spray Coating, B. Single Pass interface of H13 and low carbon steel

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133

Chapter 7 Designing For Microstructual Manipulation

H13 Good Bonding

Cold Roll Steel 100 m


Figure 7.8 A prepass before depositing improves substrate and deposit bonding.

One way to get a better bond is by doing a prepass of the laser before deposition. A prepass is a powderless laser scan of the substrate immediately before depositing. The prepass warms the substrate and roughens the surface to further aid in bonding the rst layer of deposition. The bonding region doubles in size making a much stronger bond. This is not the same as doing a double laser pass (a powder scan followed by a second powderless laser scan). The interfacial bonding region of a single pass vs a double pass is about the same, on the order of 100 m. Chapter 7. 3.2 Part Layering Strategy Because carbon steels will continue to transform as multiple layers of laser deposition are attempted no more than 25 mm of layers of continuous deposition should be attempted. If one is trying to design a die insert which is 50 mm in thickness, try to incorporate the substrate within the design. Many die insert designs can be split into a feature level and a bulk part. The feature level includes the casting surface and features beneath the part surface like conformal cooling channels or other internal features. The bulk part is simply the rest of the tool which forms the base. The bulk part should be machined from a similar metal and used as a big substrate for the rest of the deposited features. Special care should be used to insure proper bonding occurs.

Chapter 7. 3 Applying DFM2 to Part Building Strategy

134

Chapter 7 Designing For Microstructual Manipulation

=
Tooling Insert Bulk Part

+
Feature Level

Figure 7.9 Conceptual Splitting of a Die Insert

If this two part build system cannot be done, anneal the part and substrate every 25 mm of deposition. The only way to insure that unwanted phases do not occur within lower parts of the deposition, or that unwanted residual stress arising phase transformations or mismatches in coefcients of thermal expansion, is to anneal the entire deposit. However, annealing is another form of heat treatment. Special care must be taken to characterize the appropriate annealing conditions and procedures. Certain temperatures may cause chromium carbides to form or redistribute upon grain boundaries which can lead to integrannular corrosion during etching procedures or part service. Cooling procedures from the annealing temperatures must also be well characterized. If one does not understand the affects of certain heat treatments upon the particular carbon steel, avoid depositing over 25 mm. In this authors opinion, this caution can be applied not only for SDM but, for any high energy - rapid solidication procedure attempting layered manufacturing of carbon steels. Lastly, the number of layers which are deposited at any given time should be limited to no more than 7-12 layers. The divergence of thicknesses within the deposition can weaken the strength of the part. Uniform grain sizes and layer thicknesses allow parts to have more homogenous properties and attain higher strengths. Continuous deposition beyond these limits cause severe inhomogenity in grain size and layer thicknesses. For example, charpy impact specimens were taken from different positions within a large deposit of SDM Tool Steels (Figure 7.10 and Table 7.1 ). Charpy 1 samples a have a slightly higher value but a very high deviation.

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Chapter 7 Designing For Microstructual Manipulation

4 2

Layer Thickness (mm)

1 0.8 8 0.6 6 0.4 4 0.2 2 0

Charpy 2

Charpy 1

A = Overnight Cooling (12-24hr breaks) B = Short Cooling Periods (1-2hr breaks)

B B B
20 0 25 5

A A
240 0 245 5 350 0 1 30 0 135 5

Z-Height (mm)
Figure 7.10 Charpy impact specimens taken from large deposit

Impact Resistance (ft-lb)

Average Charpy (ft-lb)

Standard Deviation (ft-lb)

Charpy 1-a Charpy 1-b Charpy 1-c Charpy 2-a Charpy 2-b

9.5 6.5 7.5 7.5 7.5

7.83

1.53

7.5

0.00

Table 7.1 Charpy Impact Resistance for variable layer sizes (Sample 1 Area) and consistent layer sizes (Sample 2 Area).

Charpy samples taken from region 2 have much more uniform properties. The slightly lower measurements are probably because they were taken from a lower position within the laser deposition and have been tempered inappropriately by subsequent deposition layers. (The big deposit violates the 25 mm rule.) Chapter 7. 3.3 Deposition Parameters For the 2400 Watt ND:YAG laser which delivers an incident power of about 400 Watt, the speed as was shown earlier is not a signicant factor. With almost all
Chapter 7. 3 Applying DFM2 to Part Building Strategy

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Chapter 7 Designing For Microstructual Manipulation

speeds below 40 mm/sec, SDM is still delivering enough power to insure solidication of the deposit. However, the ll rate is critical. Figure 7.11 shows a graph which compiles at speeds from 15 to 50 mm/sec the effects of changing ll rate. Only one ll rate reduces the amount of 2nd phase constituents at all speeds. Layers Too Thin -Maximum Reheating -Multiple Phase Transformations
35
% Retained Austenite

Layers Too Thick -Maximum Retention of 2nd Phase

30 25 20 15 10 5 0 10 15
Fill Rate (g/min)

20

25

30

35

Figure 7.11 For Laser Deposition, Fill Rate is a Critical Parameter

Therefore, ll rate can be used as a way of reducing or increasing the amount or retained or transformed secondary phases. Depending upon the nature of parts design and ultimate use, ll rate can be an important way of achieving different material characteristics. However, unless one is sure of the affects of secondary phases, one should nd a setting which minimizes the effects. For this research that setting was 23 g/ min.

Chapter 7. 3 Applying DFM2 to Part Building Strategy

137

Chapter 8 Conclusions

Chapter 8 Conclusions
Deposition of carbon steels is feasible and delivers a whole range of potential applications and capabilities to Shape Deposition Manufacturing which cannot be achieved by traditional deposition metals. However, the addition of carbon steels requires a more detail understanding of the microstructure than was necessary for other deposition materials. The added knowledge benets SDM and creates new unique opportunities to improve deposition and more importantly designed objects.

Chapter 8. 1 Characterization of Carbon Steels Knowledge of how phases forms and how grains and layers evolve are essential to develope effective strategies to deposit tools steels. Because SDM involves a high energy deposition source which induces rapid solidication and uses layered manufacturing techniques which induce multiple temperature gradients through out the deposition, traditional designers tools are ineffective. The Shaefer Welding and Solidication Diagrams have been used by low energy welding sources to predict phase evolution. However, for SDM they were highly inaccurate. Proposed in this research are two new modied versions of the Shaefer and Solidication Diagrams which can be used by designers to more accurately select metals for layered high energy deposition. A heuristic for predicting grain size and layer thickness have been proposed for SDM. The heuristic identies the specic variables in composition, and other more process oriented variables like, the ll rate, solidication rate and powder size as determinants for grain and layer size. Although the heuristics are directly applicable to SDM, the parameters may lend incite in to other high energy processes. Also, the
Chapter 8. 1 Characterization of Carbon Steels

138

Chapter 8 Conclusions

understanding of how layer evolve within SDM may also aid others in understanding there own processes.

Chapter 8. 2 Application of Characterization Two applications of using characterization to improve deposition have been highlighted by this research. Choosing high impact resistant materials for building die casting inserts is dependent upon understanding the microstructure in addition to bulk material properties. Because high energy deposition processes produce material which are very different than traditional materials, they will display unusual properties. The small grain sizes of the deposited materials lend to these unique properties. However, knowledge of phase evolution is important. Certain phases in addition to the grain size can improve properties while other may reduce properties. Delta ferrite can help prevent solidication cracking in some metals while serving as a crack initiation point in others. Martensite can add toughness and reduce deection, but can also reduce elongation and yield strength. Therefore, traditional material property knowledge must be supplemented by knowledge of the microstructure when working with nontraditional part forming methods. Chapter 8. 3 Designing with Microstructure
Now that an understanding of how the microstructure of laser deposited carbon steels develops within layered manufacturing techniques has been extracted, and how this knowledge can be used to improve deposition, this knowledge can be further extended to aid designers. Designers can use this knowledge and improve designs intended for layered manufacturing. Improved part strength, wear resistance, and resistance to deformation can be accomplished if one allows the microstructure to guide design decisions. Sooner or later, the microstructure will win, and lesser designs which do take microstructual concerns into account will fail. Design rules which accomplish this have been proposed in this research.

Chapter 8. 4 Leverage of This Knowledge As indicated by Chapter 2, there are several other high energy deposition processes, which are also attempting build structures in a layered fashion. They two can benet from understanding the nature of the microstructure. Metals prototyping has lagged behind its plastic counterparts even though they share many similar problems linked to thermal gradients and shrinkage. Yet, plastics rapid prototyping
Chapter 8. 2 Application of Characterization

139

Chapter 8 Conclusions

has been quite successful in changing the design process for many designers worldwide. Leveraging the nature of metal microstructure may be the key to advancing this technology to every designers door.

Chapter 8. 4 Leverage of This Knowledge

140

Appendix

Appendix

Chapter 8. 4 Leverage of This Knowledge

141

Appendix

Chapter A. 1 Selecting a Laser Scanning Speed


When trying to determine a laser scanning speed knowing the thermal diffusion length is a potential starting point. Thermal diffusion length measures the penetration or diffusion of heat of a laser while it is incident upon a particular material. (t p)

LT = 2

th

To determine the interaction time, or the time a moving laser is incident upon a spot, an approximation is provided by dividing the beam with by the velocity of the beam. An approximation for the interaction time, tp, is spot size divided by scanning speed. The thermal diffusivity, th should be known for each metal. For 2000 W absorbed , into substrate or metal at a 2.8 mm spot size, the calculated thermal diffusion length values are listed in Table : 20 mm/sec 316L SDMT 410 420 431 H13 1.01 mm 1.31 1.33 1.28 1.19 1.31 30 mm/sec .824 mm 1.07 1.08 1.05 .97 1.07

Table A.1 Thermal Diffusion Length for Several Carbon Steels

Select an initial speed which is approximately thickness of layer which you are attempting to deposit. This may not be the most optimized speed but it is good starting point for optimization and characterization.

Chapter 8. 4 Leverage of This Knowledge

142

Appendix

Chapter A. 2 Martensitic Start Temperature


The martensitic start temperature can be calculated with knowledge of the constituents of the materials. Ms=521-350 C-13.6Cr -16.6 Ni -25.1 Mn -30.1Si -20.4 Mo-1.07CR * Ni +21.9(CR+.73Mo)C This formula was developed by Self and Carpenter, Phase Transformations and Alloy Stability, (1986).

Material 410 420 431 H13 SDMT M2 316L

Ms in Co 324 284 214 306 208 240 -298

Table A.2 Martensitic Start Temperature for Materials Used in this Research

Chapter 8. 4 Leverage of This Knowledge

143

Appendix

Chapter A. 3 Theoretical Volumetric Expansion

Dimensional mm per mm

Dimensional mm per mm

Austenite to Martensite Volume Percentage

C%

410 420 431 SDMT H13 1010-low carbon

0.06 0.45 0.18 0.15 0.4 0.1

4.6082 4.4015 4.5446 4.5605 4.428 4.587

0.0154 0.0147 0.0152 0.0152 0.0148 0.0153

4.507 3.646 4.242 4.309 3.756 4.419

0.0144 0.0142 0.0155 0.0155 0.0153 0.0155

Theoretical Percentage of Volume Increase based upon 100% martensitic transformation. Lyman, Metals Handbook, 8th Ed.

Chapter 8. 4 Leverage of This Knowledge

Spherodite - Tempered martensite to eutectoid - FeC3 globules in -4.5074 -3.6455 -4.2422 -4.3085 -3.756 -4.419 144

Austenite to Ferrite and cementite

Appendix

Chapter A. 4 Grain Size Heuristic


For the chosen data basis the following best model was generated: X26= + 9.84e-2z61 + 2.30e+0z62 + 5.82e+0 z61= + 1.00e+0z51 z51= + 1.00e+0z41 z41= + 1.00e+0z31 z31= + 1.00e+0z21 z21= + 1.00e+0z11 z11= + 2.89e+0X14 - 3.54e-1 z62= - 2.40e-1z51 + 1.18e+0z52 z51= + 1.00e+0z41 z41= + 1.00e+0z31 z31= + 1.00e+0z21 z21= + 1.00e+0z11 z11= - 5.14e+0X1 + 1.49e-3X19 - 6.23e-1 z52= - 2.78e-1z41 + 1.26e+0z42 z41= + 1.00e+0z31 z31= + 1.00e+0z21 z21= - 2.24e-1z11 + 8.88e-1z12 z11= + 5.42e+0X1 - 1.30e+0 z12= + 2.91e-1X7 - 4.79e-2X24 + 4.63e-1 z42= - 1.79e-1z31 + 1.09e+0z32 z31= + 1.00e+0z21 z21= + 1.00e+0z11 z11= + 1.94e-1X7 - 2.21e+0 z32= - 1.84e-1z21 + 1.12e+0z22 z21= + 1.00e+0z11 z11= + 1.12e+0X9 - 5.01e-1 z22= + 7.91e-1z11 + 4.42e-1z12 z11= + 2.91e-1X7 - 4.79e-2X24 + 4.63e-1 z12= - 1.52e-1X16 - 2.64e-1X20 + 7.66e+0

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145

Appendix

Mean Absolute Percentage Error (MAPE): Approximation Error Variance: OUTPUT VARIABLE: X26 - avg cell RELEVANT INPUT VARIABLES: X14 - V X1 - C X19 - Melting X7 - Cr X24 - powder X9 - Mo X16 - NI-EQ X20 - K

3.07 % 0.01669

CHOSEN HEURISTICS: Data Length: 9 Number of Input Variables: 20 Max. Lagged Time: 0 Model Type: input-output-model / exclusively linear / static The embraced linear model is: X26 = 22.838715 + 0.284510X14 + 3.738204X1 -0.000820X19 + 0.642496X7 0.125312X24 -0.769774X9 -0.278010X16 -0.483130X20

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146

Appendix

Chapter A. 5 Layer Thickness

For the chosen data basis the following best model was generated: X25= + 2.50e+1z41 + 2.10e+2z42 + 7.45e+2 z41= + 1.00e+0z31 z31= + 1.00e+0z21 z21= + 1.00e+0z11 z11= + 9.19e-1X14 - 1.12e-1 z42= - 1.59e-1z31 + 9.96e-1z32 z31= + 1.00e+0z21 z21= + 1.00e+0z11 z11= + 1.84e+0X2 - 1.25e+0 z32= + 2.14e-1z21 + 1.02e+0z22 z21= + 1.00e+0z11 z11= + 1.99e-1X7 - 2.18e+0 z22= - 4.51e-1z11 + 1.37e+0z12 z11= + 1.46e-5X27 - 3.68e+0 z12= - 1.01e-1X16 - 2.68e-2X24 + 3.29e+0 Mean Absolute Percentage Error: Approximation Error Variance: OUTPUT VARIABLE: X25 - avg layer RELEVANT INPUT VARIABLES: X14 - V X2 - Mn X7 - Cr X27 - solid rate X16 - NI-EQ X24 - powder
Chapter 8. 4 Leverage of This Knowledge

9.40 % 0.1993

147

Appendix

CHOSEN HEURISTICS: Data Length: 9 Number of Input Variables: 22 Max. Lagged Time: 0 Model Type: input-output-model / exclusively linear / static The embraced linear model is: X25 = 2003.830933 + 22.995251X14 -61.247478X2 + 8.895004X7 -0.001405X27 -29.596924X16 -7.855000X24

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148

Appendix

Chapter A. 6 New Chromium Equivalence Denition

For the chosen data basis the following best model was generated: X17= + 3.11e-1z21 + 6.19e+0z22 + 1.72e+1 z21= + 1.00e+0z11 z11= + 1.86e+0X14 - 3.61e-1 z22= + 2.76e-1z11 + 9.99e-1z12 z11= + 3.15e+0X4 - 1.36e+0 z12= + 3.32e-1X5 + 1.31e-1X15 - 2.29e+0 Mean Absolute Percentage Error: Approximation Error Variance: OUTPUT VARIABLE: X17 - new Cr RELEVANT INPUT VARIABLES: X14 - V X4 - Si X5 - W X15 - Cr-Eq CHOSEN HEURISTICS: Data Length: 16 Number of Input Variables: 15 Max. Lagged Time: 0 Model Type: input-output-model / exclusively linear / static The embraced linear model is: X17 = 0.666030 + 0.578787X14 + 5.386530X4 + 2.048034X5 + 0.811128X15 6.57 % 0.0512

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149

Appendix

Chapter A. 7 New Nickel Equivalence Denition


For the chosen data basis the following best model was generated: X18= - 5.35e-1z21 + 4.52e+0z22 + 1.14e+1 z21= + 1.00e+0z11 z11= + 6.89e-1X5 - 2.58e-1 z22= + 3.37e-1z11 + 7.53e-1z12 z11= + 1.05e+0X9 - 5.97e-1 z12= + 1.70e-1X8 - 7.72e-2X15 + 3.93e-1 Mean Absolute Percentage Error: Approximation Error Variance: OUTPUT VARIABLE: X18 - new NI RELEVANT INPUT VARIABLES: X5 - W X9 - Mo X8 - Ni X15 - Cr-Eq CHOSEN HEURISTICS: Data Length: 16 Number of Input Variables: 17 Max. Lagged Time: 0 Model Type: input-output-model / exclusively linear / static The embraced linear model is: X18 = 11.977810 -0.368111X5 + 1.598563X9 + 0.579666X8 -0.262729X15 19.96 % 0.3663

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150

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