Nickel Alloys: Thermal Treatment and Thermomechanical Processing$

JH Weber, Special Metals Corporation, Huntington, WV, USA

Y Khalfalla, University College Dublin, Dublin, Ireland
KY Benyounis, Dublin City University, Dublin, Ireland
r 2016 Elsevier Inc. All rights reserved.

1 Introduction 1
2 Primary Melting 1
3 Remelting 3
4 Hot Working 3
5 Cold Working 3
6 Heat Treatment and Finishing 4
References 4
Further Reading 4

1 Introduction

The availability of useful product forms is the primary goal of the production and thermomechanical processing of nickel alloys.
Many product shapes are manufactured, including flat products such as plate, strip and sheet, solid sections such as rounds,
octagons, and squares, and hollow sections such as seamless tubing. These shapes are useful only if the application requirements
including dimensional specifications and physical and mechanical properties are met. The chemistry and microstructure of the
alloys control these properties.
Production of nickel alloys involves a sequence of manufacturing processes that convert raw material into the several product
forms. A schematic diagram showing the overall material flow and production steps is portrayed in Figure 1. Manufacturing starts
with primary melting of raw materials and scrap. This may be followed by a remelting process to produce improved ingots for the
start of the mechanical working processes. The ingots are then hot-worked to yield intermediate products more suitable to
subsequent working. Secondary hot-working or cold-working is used to shape the alloys into their final form. Heat treatments and
finishing operations, such as straightening and surface conditioning, complete the production cycle.

2 Primary Melting

The primary melting and casting operations produce ingots of the required chemical composition and alloy microstructure.
Chemistry control is paramount, not only for the major alloying elements, but also for active elements such as aluminum,
titanium, and contaminants such as lead, bismuth, arsenic, and sulfur. The ingot structure should be uniform and clean.
Unfortunately, segregation of alloying elements due to gravity and solidification parameters can occur on both macro and micro
scales. Casting practices aim to minimize the presence of inclusions, internal stress, and ingot cracking.
Three melting and refining methods are used in primary melting: (1) the combination of electric furnace (EF) melting followed
by argon–oxygen–decarburization (AOD) refining; (2) air induction melting (AIM), and (3) vacuum induction melting (VIM).
The EF–AOD method has several advantages for alloy melting. The electric furnace provides a molten bath of an approximate
alloy composition in preparation for further chemistry refining and tailoring in the AOD process. Because the two operations are
performed in sequence and the electric furnace can achieve very rapid melting, the EF–AOD combination can produce large
batches of alloy efficiently. The presence of a slag cover and the injection of gases such as oxygen allow significant refining of
the melt bath to occur during AOD. Thus, large amounts of scrap material can be used as input to the process. Another result of
the refining action is that the EF–AOD process is not well suited to producing alloys containing large amounts of active elements
such as aluminum and titanium. These elements tend to be lost to the slag during the refining action. Nickel–chromium–iron
alloys are typically melted using the EF–AOD combination.
The AIM process can produce relatively high-purity alloys. This is a melting rather than a refining process and it requires cleaner
raw material input than for the EF–AOD. Therefore, scrap use is limited. Melting is performed open to air and there is essentially
no slag present. Composition adjustments must be made by raw material additions to the charge as only minimal change is

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Change History: July 2015. Y. Khalfalla and K.Y. Benyouniss added an Abstract, added a list of keywords, expanded the text with review of additional articles,
and extended the list of references accordingly.

Reference Module in Materials Science and Materials Engineering doi:10.1016/B978-0-12-803581-8.03382-8 1

2 Nickel Alloys: Thermal Treatment and Thermomechanical Processing

Figure 1 General process flow for manufacture of nickel alloy product forms.

possible using this technique. Nickel–copper alloys are typically produced by AIM. Alloys containing active or volatile elements
can be made by AIM if these elements are added at the end of the process just prior to casting. This minimizes the time for
oxidation and/or volatilization loss.
The primary advantage of VIM is that the process is carried out in a vacuum chamber. The batch size is limited to about 20–25
tons because the entire operation must be carried out in the chamber. Major chemistry adjustments are achieved by additions to
the charge. Due to the vacuum environment, degassing, and removal of volatile contaminants occurs. High-purity alloys
 Nickel Alloys: Thermal Treatment and Thermomechanical Processing 3

containing large levels of active elements are produced using this technique. Nickel–chromium alloys and nickel-based superalloys
use VIM as the primary melting process.

3 Remelting

Remelting processes are used to improve the quality of ingots cast from primary melting. This benefits alloy chemistry as well as
facilitating the hot-working processes. Since the remelting processes involve only a small molten pool at any given time, chemical
segregation is minimized and the alloy grain size is controlled. Minor changes in chemical composition can also be effected. Nickel
alloys with more complex chemistries are usually remelted.
The most common remelting techniques for nickel alloys are vacuum arc remelting (VAR) and electroslag remelting (ESR). Both
techniques are consumable electrode melting processes in which the heat is generated by an electric arc between the ingot electrode
cast from the primary melting process and some type of base plate located at the bottom of the mold. VAR involves sequential
melting of the electrode and is performed in a vacuum. Exposure of the molten droplets to the reduced pressure decreases the amount
of dissolved gases and volatilizes a portion of the tramp elements in the alloy. ESR also involves sequential melting of the electrode. It
is performed in air, but a conductive slag is present between the melting electrode and the solidifying ingot. The molten droplets are
thus exposed only to the slag. Refining of the composition and minor chemical composition adjustments occur as a result.

4 Hot Working

Thermomechanical processing of nickel alloys is used to change the shape of the cast ingots into the final product form. Such
processing includes hot working, cold working, and various types of thermal and heat treating techniques. Hot working is
deformation performed at temperatures and strain rates where simultaneous recrystallization and deformation occur and strain
hardening is avoided. All ingots are subjected to hot working for the initial deformation after melting and/or remelting. This is
called ingot breakdown. One purpose of this process is to reduce the ingot to a size and section that is appropriate for later hot or
cold working. Breakdown also decreases chemical segregation and refines the alloy microstructure.
Three types of hot working are used for breakdown – rolling, forging, and extrusion. The process selection depends on the
facilities available, alloy chemistry, and the shape of the finished form. Facilities include not only the mechanical working
equipment itself, but also the type and capacity of the furnaces needed to heat the ingots before and intermittently between
working sessions. Alloy chemistry affects the selection by defining the incipient melting temperature, hot-working temperature
range, microstructural stability, and deformation flow stress. Product shape is critical when the form is hollow, such as
tubing. Jiang et al. (2015) have reported that the optimum hot working condition for alloy 617B are in the temperature range
of 1120–1165 1C and strain rate scope of 0.01–0.1 s
1 with the peak power dissipation efficiency of 48%. Another domain of
1170–1210 1C and 0.1–4.5 s
1 can also be chosen as the optimal working condition at large strains (40.8).
Hot rolling reduces the section of the ingot by passing it through driven rotating rolls. Typical intermediate shapes produced by
rolling include blooms, billets, rods, and plates. Breakdown forging reduces the section of the workpiece by compressive force
between dies. This is done by sequential deformation along the length of the workpiece. Because forging requires significant time,
one or more reheats are required to maintain the alloy within the desired temperature range during working. Computer-controlled
mechanical manipulators are commonly used to rotate the material during forging to minimize workpiece chill due to die contact
during working. Extrusion converts the workpiece into an intermediate length with uniform cross section by forcing the alloy
through a die. If a hollow section is desired, a mandrel is used to form the interior hole. Extrusion is usually the preferred process
when the alloy has a limited hot-working temperature range and/or a high resistance to deformation.
Secondary hot working produces some finished product forms. Where hot working is the final deformation process, the
dimensional tolerances of the product are relatively broad, or a subsequent finishing operation such as machining is used to
produce the required dimensions. The most common of these forms are hot-rolled plate and hot-rolled or forged rod. Hot
extrusion is used to produce larger-sized tubing where dimensions are not critical.

5 Cold Working

Cold working is deformation in an alloy accompanied by work hardening – that is, increased strength. Cold working is used as the
final working step when tight dimensional tolerances and manipulation of alloy properties are required. Adjusting the amount of
deformation and the rate at which the deformation is performed can control both strength and ductility. Cold working also
produces a good surface finish.
Common cold-working processes used for nickel alloys are rolling, drawing, tube reducing, and forging. Factors affecting the
choice of process include alloy characteristics, equipment availability, and shape of the finished form. Alloy characteristics include
work hardening rate, strain rate sensitivity, and deformation flow stress. Equipment considerations are similar to those for hot
4 Nickel Alloys: Thermal Treatment and Thermomechanical Processing

working with the added concern for lubrication between the equipment and workpiece. Rolling is used to produce flat products
such as sheet and strip. It can also be used to produce rods. Drawing can produce sections, i.e., rounds and hexagons, as well as
hollows. Tube reducing is normally used only for hollow shapes and tubing.

6 Heat Treatment and Finishing

Several types of heat treatments are used to process nickel alloys. These include homogenization, stress relieving, annealing, and
aging. Homogenization is typically used to treat ingots after melting to decrease or eliminate chemical segregation. These high-
temperature heat treatments are often quite long, e.g., greater than 24 h, due to the size of the ingots and the extent of segregation.
Stress relief treatments are used to reduce casting strains or to decrease residual stress resulting from cold work. Annealing
treatments involve elevated temperature exposures to remove the effects of cold work or promote the dissolution of precipitates in
the microstructure to form a solid solution. Alloys are usually softened by the annealing treatments. Sheet and strip are often given
bright anneals as the final process. This annealing is performed in a protective atmosphere to prevent discoloration of the smooth
rolled surface. Aging, also called precipitation-hardening, is used to precipitate beneficial constituents in alloy microstructures.
Aging treatments are usually performed after annealing or cold working to obtain the desired combinations of strength and
ductility in the product.
Special conditioning operations are used to remove surface oxides, achieve a required surface finish, or obtain the final shape
dimensions. Pickling is a chemical process that is used to remove oxides from hot-worked material. When the nickel alloy contains
a significant level of chromium, a fused salt pretreatment must often be used prior to pickling to facilitate the oxide removal.
Surface blasting is also used to remove hot-work oxides. The blast medium for nickel alloys is usually a fine oxide grit or stainless
steel shot. Machining is the operation of choice for obtaining the required final shape dimensions. Machining operations include
turning, grinding, and buffing.
Aboutalebi et al. (2015) have studied impacts of aging and thermomechanical treatments on the martensitic transformation
and superelasticity of a highly Ni-rich Ti-51.5 at.% Ni. Outcomes indicated that solution annealed and aged samples at 700 1C
shows no superelasticity due to high nickel content in the matrix of the alloy. For the aged samples, full superelasticity is detected
by aging at 400 and 500 1C. Applying 20% cold rolling before aging directed to rise aging temperature for perceiving good
superelastic behavior.
The heat treatment affects remarkably the microstructure of the nickel–aluminum bronze alloy and its mechanical properties.
The strength and hardness increase with the increasing content of hard phases in the alloy. Also, the erosion–corrosion resistance
can be improved by generation of hard phases such as b0 and κ phases by heat treatments Wu et al. (2015).

References

Aboutalebi, M.R., Karimzadeh, M., Salehi, M.T., Abbasi, S.M., Morakabati, M., 2015. Influences of aging and thermomechanical treatments on the martensitic transformation
and superelasticity of highly Ni-rich Ti-51.5 at.% Ni shape memory alloy. Thermochimica Acta 616, 14–19.
Jiang, H., Dong, J., Zhang, M., Zheng, L., Yao, Z., 2015. Hot deformation characteristics of Alloy 617B nickel-based superalloy: A study using processing map. Journal of
Alloys and Compounds 647, 338–350.
Wu, Z., Cheng, Y.F., Liu, L., Lv, W., Hu, W., 2015. Effect of heat treatment on microstructure evolution and erosion−corrosion behavior of a nickel−aluminum bronze alloy in
chloride solution. Corrosion Science 98, 260–270.

Further Reading

Betteridge, W., Heslop, J., 1974. The Nimonic Alloys, second ed. New York: Crane, Russak & Co., pp. 115−156.
Mankins, W.R., Lamb, S., 1990. Nickel and Nickel Alloys, Metals Handbook, tenth ed. Metals Park, OH: ASM International, pp. 428−445.
Tundermann, J.H., Tien, J.K., Howson, T.E., 1996. Kirk−Othmer Encyclopedia of Chemical Technology, fourth ed. New York: Wiley, pp. 1−17.