[ LOW TEMPERATURE BALL MILLING MACHINE ] 2013

1. INTRODUCTION
1.1 BACKGROUND THEORY
A ball mill, a type of grinder, is a cylindrical device used in grinding (or mixing) materials like ores, chemicals, ceramic raw materials and paints. Ball mills rotate around a horizontal axis, partially filled with the material to be ground plus the grinding medium. Different materials are used as media, including ceramic balls, flint pebbles and stainless steel balls. An internal cascading effect reduces the material to a fine powder. Industrial ball mills can operate continuously, fed at one end and discharged at the other end. Large to mediumsized ball mills are mechanically rotated on their axis, but small ones normally consist of a cylindrical capped container that sits on two drive shafts (pulleys and belts are used to transmit rotary motion). A rock tumbler functions on the same principle. Ball mills are also used in pyrotechnics and the manufacture of black powder, but cannot be used in the preparation of some pyrotechnic mixtures such as flash powder because of their sensitivity to impact. Highquality ball mills are potentially expensive and can grind mixture particles to as small as 5 nm, enormously increasing surface area and reaction rates. The grinding works on the principle of critical speed. The critical speed can be understood as that speed after which the steel balls (which are responsible for the grinding of particles) start rotating along the direction of the cylindrical device; thus causing no further grinding.Ball mills are used extensively in the mechanical alloyingproces in which they are not only used for grinding but for cold welding as well, with the purpose of producing alloys from powders. High energy ball milling of powder particles as a method for materials synthesis has been developed as an industrial process to successfully produce new alloys and phase mixtures in 1970s. This powder metallurgical process allows the preparation of alloys and composites, which cannot be synthesized via conventional routes. In nanomaterials research, this top down techniques well used to fine-tune the grain sizes of the materials in nanoscales. A variety of milling devices has been developed for different purposes including tumbler mills, attrition mills, shaker mills, vibratory mills, planetary mills etc. In this work, Fritsch planetary micro mill, pulverisette 7 was used for milling. (Here grinding bowls rotates 1|Page

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on their own axis while simultaneously rotating through an arc around the central axis. The grinding balls and the material in the grinding bowl are thus acted upon by the centrifugal forces, which constantly change in direction and intensity resulting in efficient, fast grinding process. The grinding bowl and the supporting disc rotate in opposite directions, so that the centrifugal forces alternatively act in the same and opposite directions. This results in, as a frictional effect, the grinding balls running along the inner wall of the grinding bowl, and impact effect, the balls impacting against the opposite wall of the grinding bowl. The energy thus created by impact is many times higher than for traditional mills. This results in excellent grinding performance and considerably shorter grinding times. Atmospheric contamination can be minimized by sealing the vial with flexible O ring after the powder has been loaded. If a milling medium-a fluid (usually an organic fluid) is used, contamination by the milling tools can be prevented and also it minimizes the wear. A few parameters exists in high energy ball milling which on changing, we can produce a wide range of fine particles with different sizes and consequently with different physical properties. These parameters are (1) Type of mill, (2) Milling atmosphere, (3) Milling media, (4) Intensity of milling, (5) Ball to powder weight ratio (BPR), (6) Milling time and (7) Milling temperature. There are mainly two kinds of ball mill, grate type and overfall type due to different ways of discharging material. There are many types of grinding media suitable for use in a ball mill, each material having its own specific properties and advantages. Key properties of grinding media are size, density, hardness, and composition.

Size: The smaller the media particles, the smaller the particle size of the final product. At the same time, the grinding media particles should be substantially larger than the largest pieces of material to be ground.

Density: The media should be denser than the material being ground. It becomes a problem if the grinding media floats on top of the material to be ground.

Hardness: The grinding media needs to be durable enough to grind the material, but where possible should not be so tough that it also wears down the tumbler at a fast pace.

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Composition: Various grinding applications have special requirements. Some of these requirements are based on the fact that some of the grinding media will be in the finished product. Others are based in how the media will react with the material being ground.
o

Where the color of the finished product is important, the color and material of the grinding media must be considered.

Where low contamination is important, the grinding media may be selected for ease of separation from the finished product (i.e.: steel dust produced from stainless steel media can be magnetically separated from non-ferrous products). An alternative to separation is to use media of the same material as the product being ground.

Flammable products have a tendency to become explosive in powder form. Steel media may spark, becoming an ignition source for these products. Either wetgrinding, or non-sparking media such as ceramic or lead must be selected.

Some media, such as iron, may react with corrosive materials. For this reason, stainless steel, ceramic, and flint grinding media may each be used when corrosive substances are present during grinding.

The grinding chamber can also be filled with an inert shield gas that does not react with the material being ground, to prevent oxidation or explosive reactions that could occur with ambient air inside the mill. Similarly, liquid nitrogen can be used to brittle the sample and the above purpose also. Aside from common ball mills there is a second type of ball mill called planetary ball mill. Planetary ball mills are smaller than common ball mills and mainly used in laboratories for grinding sample material down to very small sizes. A planetary ball mill consists of at least one grinding jar which is arranged eccentrically on a so-called sun wheel. The direction of movement of the sun wheel is opposite to that of the grinding jars (ratio: 1:-2 or 1:-1 or else). The grinding balls in the grinding jars are subjected to superimposed rotational movements, the so-called Coriolis forces. The difference in speeds between the balls and grinding jars produces an interaction between frictional and impact forces, which releases high dynamic energies. The

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interplay between these forces produces the high and very effective degree of size reduction of the planetary ball mill.

1.2 ENGINEERING DESIGN

The various components of the low-temperature ball mill are: (i) Double wall steel vacuum container, (ii) RPM Controlled motor, (iii) Coupling and interfacing, (iv) balls, and mounting stand. (i) Double wall steel vacuum container: A stainless steel double wall container about volume 150 cc was designed to hold the cryogenic liquid (liquid nitrogen) for longer time during rotation. The inside vacuum of the double wall container in the range of high vacuum. The container is mainly used for the grinding of materials. (ii) RPM controlled Motor: An electrical motor having provision to control the RPM by both mechanical clutch and via electronic mean. A variac of 0.5 KW is fitted with the motor to control the voltage/current by manual mean. (iii) Coupling and interfacing: The container and the controlled motor was attached with a coupling made up of hard-rubber to minimize vibration. (iv) Balls: Stainless steel ball of requisite diameter was used for the synthesis of nanomaterial. (v) Mounting stand: Mounting made up off MS and SS materials and is design to hold the motor, container in an angular orientation Angular- Variable Speed Cryo-Ball Mill overall specification 1. Cryo-sample Cell capacity: 350 ml. (double wall steel vacuum cell)-hold 2hrs in a single fill; after 2 hr fill again (directly fill provision, without stopping / stop and fill, then start),Holds for 4 hrs while not working . 2. RPM of Ball Mill: variable RPM( 0-100rpm) 3. Critical RPM: near about 75 (angle dependent) 4|Page (v)

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4. Angle of cell axis w.r.t vertical direction: 45 deg.( suitable) , can be adjusted 5. Ball diameter: Steel ball (preferred) of 12 mm (radius of curvature of the cell lower edge), 22mm, 4-5mm 6. Sample: Ball ratio:: 1: 10x (x = 1, 2, up to 10 as reported by various author, one can select this parameter as per requirement. 7. Sample (heavier then LN2) grinded in LN2 medium as slurry (one can use any organic solvent with this).

Fig 1.1 : LOW TEMPERATURE BALL MILLING MACHINE

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2. WORKING PRINCIPLE
2.1. REQUIRED PARAMETERS FOR MILLING :
In principle, the reduction in grain size is accomplished by the kinetic energy transfer from balls to powder. Since the kinetic energy of the balls is a function of their mass and velocity, dense materials are preferred like steel or tungsten carbide. Other materials used as balls are agate, sintered corundum, zirconium dioxide, Teflon, chrome nickel, silicon nitride etc. In order to prevent excessive abrasion, the hardness of the grinding bowl used and of the grinding balls must be higher than that of the materials used. Normally grinding bowls and grinding balls of the same material should be chosen. In the initial stage of milling, a fast decrease of grain size occurs which slows down after extended milling. Once the minimum steady state grain size is reached, further refinement ceases. Initially the kinetic energy transfer leads to the production of an array of dislocations. This is accompanied by atomic level strains. At a certain strain level, these dislocations annihilate and recombine to form small angle grain boundaries separating the individual grains. Thus sub grains are formed with reduced grain size. During further milling, this process extends throughout the entire sample. To maintain this reduction in size, the material must experience very high stresses. But extended milling could not able to maintain the high stresses and hence reduction of grain size is limited in extended milling. The two other parameters which also causes this limit to grain size reduction are the local temperature developed due to ball collisions and the overall temperature in the vial. Temperature rise arises from balls to balls, balls to powder and balls to wall collisions.

The impact speed and the impulsive load of the grinding balls are the two key parameters, which determine the kinetic energy transfer. The impulsive load of grinding balls is given by

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mv t

(1)

where m is the ball mass, v is the ball velocity andt the ball-vial contact time. When the mill is rotated, the ball are picked up by the mill wall and carried nearly to the top, where they break contact with wall and with each other during the upward movement. While in contact with the wall, the balls do some grinding by slipping and rolling over each other, but most of the grinding occurs at the zone of impact, where the free falling balls strike the bottom of the mill. If the speed is too high, however, the balls are carried over and the mill is said to be centrifuging. The speed at which centrifuging occurs is called the critical speed. Little or no grinding is done when a mill is centrifuging, and operating speeds must be less than the critical. The critical speed of the ball mill is given as:
1 2 g Rr

nc

(2)

Where R is the radius of the ball mill, r is the radius of the ball, n c is the critical speed of the ball mill and g is the acceleration due to gravity.

2.2 MILLING MECHANISM :

Again the actual milling mechanism depends on two phenomena sequentially 1. Brittle fracture due to high impact force acted between balls and wall surface . 2. Rolling the fractured grain and making its sharp edges to finished surface . In the cryogenic jar there are more than one ball with different sizes are used .

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Different sized balls are used for different purpose and serves for different purpose In first phase the bigger balls with high impact force crack or fracture the bigger grain and converts in to smaller grain . Then the smaller balls with low KE only rolls the fractured balls and finishes its surfaces .Using different sized balls have another purpose .i.e there are some corners or places where bigger balls can rich . At that condition smaller ball can approach to that portion and easily mill at that place .The grains are milled as it get crushed between balls and ball-jar surfaces . The collision between ball or ball and jar surfaces are of very high impact and KE which leads to fracture of grain .

Fig 2.1 : MECHANISM OF MILLING

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3. MANUFACTURING OF THE MACHINE AND ITS SUBCOMPONENTS

DIFFERENT SUB COMPONENTS REQUIRED
1. Double walled SS Cryogenic Jar 2. SS Ball of different sizes 3. Vacuum providing provision 4. Coupling driving unit 5. Motor (Prime mover) 6. Variac(Speed control unit) 7. Machine base: a. Motor, with jar mounting b. Base support c. Angle providing provision 8. Liquid medium

3.1. DOUBLE WALLED CRYOGENIC JAR

This is the most important part of the entire setup, where our all machining process is carried out.The output procedureof the machine, or efficiency of the machine, totally depend upon this jar. So, designingand manufacturing of this is very much important. So, it should be carefully done. Generally, it is consist of double walled type(inner wall and outer wall).There is gap, maintained between both wall.The gap between the both wall is, maintained vacuum. The vacuum is maintained to reduce, the heat conduction from outer atmosphere, into the inner jar or the machining portion of the machine. By maintaining vacuum we withdraw allmedium from the gap portion of double wall. So, heat from outside atmosphere, does not get any medium, to come inside the machining portion of inner wall. Hence thelow temperature is maintained for long time. 9|Page

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Specification & Material details of Jar 1. Inner wall a. Specification i. Inner dia 52.50 mm ii. Outer dia 60.00 mm iii. Length 104.00 mm 3.70 mm iv. Thickness b. Materials details i. Stainless steel 1. .15% to .27% C 2. 13% to 26% Cr

Fig 3.1 :design of inner jar

2. Outer wall a. Specification i. Inner dia 80.00 mm ii. Outer dia 87.00 mm iii. Length 110.00 mm 3.50 mm 10 | P a g e iv. Thickness

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b. Materials details i. Stainless steel 1. .15% to .27% C 2. 13% to 27% Cr

Fig 3.2 : DESIGN OF OUTER JAR 3. Base plate a. Specification i. Inner wall dia 57.00 mm 4.20 mm 85.00 mm 4.20 mm ii. Inner wall thickness iii. Outer wall dia 4. Gap distance 10 iv. Outer wall thickness

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Fig 3.3 : DESIGNING OF CRYOGENIC JAR

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Manufacturing Process For manufacturing of the double walledjar, two numbers of SS Pipes of dia: 1. Outer 62mm, Inner 50mm 2. Outer 88mm, Inner 78mm arebroughtfrom the market. Then, theseare brought for Lathe Operation.

Sequence of Operation

1. Cutting to the required size 2. Turning of inner and outer surfaces 3. Facing ofboth pieces 4. Making the base plate, black smithy 5. A ring of wideness, equal to the gap distance(10mm), is cut from the flat plate, using black smithy. 6. Both pieces are welled and joined to the both pipes accordingly. 7. The ring is welded at its inner portion, with the outer top of the inner pipe & its outer portion, with theinner top edge of outer pipe. So that, the inner pipe will be remain suspended, with the help of ring, from the outer pipe. 8. Thenagain, the excess welded metal is again cut by means of Lathe Operation. 9. The inner face of the inner pipe &outer surface of theouter pipe is polished, with the Lathe Operation. Now the double walled container or jar is ready.

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Fig 3.4 : SEQUENCE WISE CRYOGENIC JAR MANUFACTURING

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The machining process used are: I. Lathe operation a. Turning b. Facing c. Finishing II. Black smithy a. Cutting b. Flattening III. Welding a. Joining

Precaution shouldbe taken

I.

All the joint(welding) are made in such a manner that, there should not be any leakage or blowhole.

II.

The inner surface of inner wall, should be polished, as the fineness of grain, depending on thepolishnes of the inner surface of inner wall.

III.

The inner jar, outer jar, base plates& ring must be concentric, so that no unbalanced mass should be present, during rotation.

3.2STAINLESS STEEL BALL

The stainless steel balls is used as the main or primary cuttingtool, in this machine. It continuously roll on the inner surface of the inner wall. It is said as multi cutting tool. As each and every point on the spherical surface of the ball, work as a machine tool. In this machine, more than one, that is simultaneously 3 to 5 balls, of different sizes is taken, during machining. While the jar is rotatingall balls simultaneously roll, inside the jar. There will a time come, when one ball climbs over another, and drops again on the jar surface. During falling, it has high impact force. So, when it falls on the specimen material, it crushed thespecimeninto the small sizes.

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The specimen material is grinded two techniques such as : By rolling of ball on jar surface. By falling of one ball on the specimen metal, with high impact force. The balls in this machine, performs two operations: Crushing Rolling

By crushing first, the balls makes the specimen material into small grains and by rolling, then it finishes the grain surface. During rolling, the sharp edges of the grains

are polished and fine grains are found. Here, more than one ball of different size are taken. This is done so because different size ball perform different operation: Big sized ball crushed into small grains. Small ball is used to roll and polishes the grain. It also prevent the grain fracture, caused due to Low temperature High impact forces

Of bisg sized balls.

Specification Dia of 2mm to 4mm size

Material Stainless steel with Hadness .15 to .27 %C

13 to 26 %Cr

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Manufacturing Readily available in market.

Fig 3.5 :

SS balls

3.3. COUPLING
Coupling is a part of driving unit, which transfer the power from the Motor to the Jar. Generally here, the coupling used is one type of flexible coupling. coupling is flexible type to absorb sudden jerk, produced by, starting of motor. The sock absorbing provision is taken care by filler metal, used in coupling. The filler metal is hard plastic or hard rubber, that has high compressive strength. So, when during starting of the Motor, it rotates with the high torque. Soit may give a jerk to the Metal Jar. So, during that Jerking, filler metal is get compressed and absorb the sock. 18 | P a g e The

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Hence failure due to impact loading is avoided. One end of coupling is directly connected to the Motor Shaft, and other end is connected to the Coupling Rod of Jar. The Motor shaft portion is joined to the coupling, by means of screw fastening mechanism and coupling rod is also joined to the coupling by fastening a screw. Specification Inner dia 12mm Material Used Coupling material o Cast Iron %C %Fe

o Hard Rubber Filler material o Cast Iron %C %Fe

o Hard Rubber

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Fig 3.6 : DESIGN OF COUPLING

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Manufacturing The suitable size of coupling is bought from market. Then the inner dia of coupling is turned to exact required size and outer dia is turned to reduce unwanted mass of coupling. On the mounting plate, there is a single hole at the top and several holes are present on a common arc. These holes are made at a perpendicular measured angle as 45, 60, 75 from horizontal. The top hole is fixed one. By shifting the bottom base of Motor and fixing with the holes with respective angular position. We can get desired angular position of our rotating jar from horizontal. This angle providing provision is provided to, make the concentration of specimen material, at a point. It also gather the specimen material and balls at a concentrated position so that, the machinability of the machine and machining time will be decreased. It is also used for proper mixing of the compound powder and of homogeneous grain size.

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Fig 3.7 : COUPLING MANUFACTURING

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3.4. MOTOR
In this machine motor is the prime mover. It takes the electric power from the source and supply rotation to the jar . Here the motor used is of special type. This motor is of two phase reversible type. That means the shaft rotation can be made both clock wise and anti clockwise manner . The both rotation is provided to the machine to properly mix and distribute the specimen material , to produce homogeneous compound powder and to avoid the non stickiness

of specimen material on the machining jar surface . A special provision of clutch arrangement is also there in this motor . Thats why it is also called clutch motor . It is used to sudden disengagement of motor and machining jar . There is a hand rotating motor shaft from the lever by the help of which we can dis engage the other driven unit ( cryogenic jar ) . This thing will

happen when we want to stop the machining or milling process suddenly . Here by the help of clutch arrangement it mechanically controlled . It is also controlled electrically . For this provision variac is provided .By the help of variac we can control the speed and vary the speed as per requirement . Generally for our machining purpose we need the speed more than the critical speed calculated which is about 70 to75 rpm. So by adjusting the variac we can get our desired rpm .

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Fig 3.8 : MOTOR ASSEMBLYING

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OTHER DETAILS :

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3.5. VARIAC
It is previously studied that it is used for speed control of our prime mover or motor. By adjusting the resistance and the voltage dropped across it we can adjust or vary the speed of motion. It is connected in series with the motor or load in the electrical circuit.

The connection guide circuit map is shown below.

Fig 3.9 : VARIAC AND ITS CONNECTION GUIDE CKT

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3.6. MACHINE BASE & SUPPORT:The base & support of entire set up is divided in to 3 parts as1. Vertical mounting 2. Angle providing mechanism 3. Base

3.6.1. VERTICAL MOUNTING

It is made up of a mild steel metalplate of suitable size & thickness. It iswelded vertically on the base. The motor also with the metal jar is mounted vertically on the surface . The motor base is fastened with nut & bolt on the vertical moving plate. As the motor & the jar eccentrically loaded on the vertical plate. The plate thickness should be enough so that it will not bend bend due to the eccentric load .

SPECIFICATION : Length : 16 Breadth : 13 Thickness : 6 MATERIAL : Mild Steel: ( 0.3 to 0.6 %C )

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DESIGN :

Fig 3.10 : DESIGN OF VERTICAL MOUNTING

MANUFACTURING : 1. Froma big 6mm metal sheet , required sized and shaped plate is cut by the help of gas cutting . 2. Prepare the edge by the help of bench grind .

3. Polish the surface by the help of hand grind .

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Fig 3.11 : VERTICAL MOUNTING PLATE MANUFACTURING

3.6.2 ANGLE PROVIDING ARANGEMENT :

For giving different angle to the metal jar with respect to the cryogenic jar with respect to the ground or horizontal a special arrangement is made on the

mounting plate .The design of ansle providing provision is discussed below

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DESIGN :

Fig 3.12 : DESIGN OF ANGLE PROVIDING ARRANGEMENT

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Manufacturing : 1. First prepare the plate and design it arrangement on it . 2. Find out the position of platform holes for the motor base according to recurred angles . 3. Punch the points with the punch tool . 4. Drill the holes by Drilling Machine with 10 mm Drill bit . 5. Weld it on the base with a accurate vertical angle with proper leveling .

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Fig 3.13 : MANUFACTURING OF ANGLE PROVIDING ARRANGEMECT

3.6.3. BASE
It is the main support on which all the subcomponents are mounted . The mounting plate is fixed vertically by welding . The variac and the power switch is also fixed on it . A special arrangement is done for proper leveling of the entire setup . For this 4 nuts are welded at the four corner of the base . Then the bolts are inserted from bottom of the base by fastening . So by fastening the bolts for a fixed length the level can be adjusted . Where no level adjustment is recurred simply remove the bolts from the nut and just keep it on floor . The base is made up of mild steel and the mounting plate, leveling nuts are joined by welded joint and the variac, power switch are fixed by screw fastening . The mass of the base should be sufficient so that it can support the eccentric load of 32 | P a g e

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the motor and cryogenic jar .Also the fastening and other joints should be tightly made so that sound and noise will be created during milling process . As the entire setup is made up of metal body a earthling arrangement should be done for

safety operation .

Fig 3.14 : BASE AND MOUNTING PLATE

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Fig 3.15 : MACHINE WITH ALL ARRANGEMENTS 34 | P a g e

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4.

TESTS AND RESULTS

4.1. TEST
Engineering designingof a cryogenic ball mill is a challenging task and very much interesting for engineers and technologists. The importance and useful of a Cryogenic (low temperature) ball mill is very high for material research, particularly for the synthesis of nanomaterials. Most important thing is that by the help of this device one can get fine particle/ nonoparticle of polymers or fiberious materials, which is not possible any other technique.

Consider a case of crystal of sodium chloride NaCl as a simple and convenient model of a brittle aterial. Such a crystal is composed of a lattice of positively charged sodium ions and negatively charged chloride ions arranged such that each ion is surrounded by six ions of the opposite sign. Between the oppositely charged ions there is an attractive force whose magnitude is inversely proportional to the square of the separation of the ions. There is also a repulsive force between the negatively charged electron clouds of these ions which becomes important at very small interatomic distances. Therefore two oppositely charged ions have an equilibrium separation such that the attractive and repulsive forces between them are equal and opposite. It can be appreciated that if the separation of the ions is increased or decreased by a small amount from the equilibrium separation, there will be a resultant net force restoring the ions to the equilibrium position. The ions in the sodium chloride crystal lattice are held in equilibrium positions governed by the balance between attractive and repulsive forces. Over a small range of interatomic distances the relationship between applied tensile or compressive force and resulting change in ion separation is linear. That is, in this region (AB) Hookes law applies: strain is directly proportional to applied stress. The Youngs modulus of the material (stress/strain) describes this proportionality. In this Hookes law range the deformation of the crystal is elastic; i.e. the original shape of the crystal is recovered upon removal of the stress .In order to break the crystal it is necessary to separate adjacent layers of ions in the crystal and this involves increasing the separation of the adjacent ions beyond the region where Hookes law applies i.e. beyond point B in Fig. into the plastic deformation range. The applied stress 35 | P a g e

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required to induce this plastic behavior

is known as the elastic limit or yield stress, and is

sometimes defined as the materials strength .

Fig 4.1 .Forces versus distance on an atomic scale

A body under stress stores energy-strain energy. This strain energy is not uniformly distributed throughout the solid but is concentrated around holes, corners and cracks. The theory of crack formation and propagation has been well demonstrated in literature. It was postulated that for along the intersection of glide planesfracture to occur the propagation of cracks has to be promoted, and the condition that should lead to a fracture is that a certain minimum length of the micro cracks (defect sites) should be formed . This concept was later modified in works of Cottrell who stated that such cracks can also be created by the coalescence of dislocations in solids. According to this model micro cracks can develop and dislocations can coalesce at the interfaces of crystals, or at the intersection of two dislocations, or in the case of mosaic structure, at the boundaries of the blocks .Fracture is a problem of energetic. The propagation of the initially-formed cracks requires that the energy of elastic deformation should be at least as high as the interfacial energy of the system]. It was pointed out that fracture energy was much higher than surface free energy .Thus, the specific surface energy of solids is about 0.05 0.5 36 | P a g e

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Jm2, whereas the specific fracture energy for brittle solids is 5 Jm2, for plastic solids it is 10 Jm2, and for metals is approximately 500 Jm2.

4.2. SEM ( Scanning Electron Microscopic ) OBSURVATION OF NaCl MILLING :

We shall now discuss the microstructural evolution of the ball-milled powder using SEM. The process of mechanical milling of powder normally involves repeated welding, fracturing, and rewelding of powder particles. This process leads to the reduction of crystallite size caused by plastic deformation. fg shows SEM micrographs of NaCl samples, revealing the information about the nature of particles when cryomilled for 2, 4, and 8 hours. Figure is the micrograph of the starting powder showing large (50 to 100 lm) cuboidal-shaped NaCl crystallites bounded by {100} facets. As compared with the starting microstructure, several important characteristics can be observed in cryomilled powder. Figure shows a SEM micrograph of a sample

cryomilled for 2 hours. Most NaCl crystallites have undergone fracturing (marked by white arrows) leading to the formation of fragmented crystallites. The cuboidal shape of the starting crystallite is still retained. Cryomilling leads to a decrease of crystallite size (1 2 lm) as shown in the inset of Figure revealing small crystallites. Figure reveals the representative micrograph of 4 hours cryo-milled sample. The crystallites have further been fractured and fragmented pieces can be clearly observed. However, some facets of the crystallite are still retained (marked bywhite arrows). The formation of finer scale cuboidalshapedNaCl crystallites can also be observed onsurface of the fractured crystallites as indicated by dotted black arrows. The inset shows higher magnification micrograph of these particles with facets. SEM micrograph of the 8-hour cryomilled sample is shown in Figure 2(d). The original cuboidal-shaped NaClcrystallitesare not observed in the microstructure. The larger crystallites (as observed in the 4-hours milledsample) are completely fragmented leading to the formation of smaller crystallites, which are marked by dotted white arrows. The inset shows the formation of finerscale crystallites (~1 lm). Further cryomillingdoes not lead to a change in the microstructure as well as in the crystallite sizes. 37 | P a g e

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Fig 4.2 : sample aftercryomilling

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We shall now discuss SEM observation of the cryomilled samples which are subsequently RT milledfor different time scale. We shall present some representative SEM micrographs. Figure is the SEM micrograph of sample cryomilled for 2 hours and subsequently RT milled for 5 hours. The micrograph illustrates the bimodal distribution of the crystallites. The crystallites have a typical cuboidal morphology (marked by white arrow). The inset shows the finer scale crystallites along with the bigger faceted NaCl crystallites. Some of these bigger crystallites have well-developed facets. The SEM micrograph of sample cryomilled for 2 hours and RT milled for 10 hours is shown in Figure . The microstructure again shows a bimodal distribution of the NaCl crystallite with bigger crystallites showing pronounced faceting. It is clear that longer RT milling leads to further reduction of crystallites. However, the crystallite undergoes a morphological change from a cuboidal to a cuboctahedron shape. The SEM microstructure of a sample cryomilled for 4 hours and RT milled for 10 hours is shown in Figure . The size of the crystallites has indeed been reduced as compared to the earlier two cases. The shapes of the crystallites have been changed to cuboctahedral-shaped crystallites (marked by a black arrow). Figure shows a SEM micrograph of the samplecryomilled for 8 hours and subsequently RT milled for 10 hours. The crystallite size has been reduced much finer scale and the shape of the crystallites has been changed. Some crystallites have a near spherical shape. The inset of Figure shows a high magnification micrograph of a crystallite with a near spherical shape.

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Fig 4.3 :Samples after both room temperature and cryomilling

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4.3. PROCESS VARIABES

Material of Milling Media

The material used for the milling media (milling chamber, vial, balls) is important due to impact of the milling balls on the inner walls of the milling chamber. Some specific materials are used for specialized purposes. Commonly materials include various steels (stainless, tool, hardened chromium, tempered, bearing steel and tungsten carbide lined), tungsten carbide, zirconia, agate, alumina and silicon nitride. The specific gravity plays an important role. In general, high-density and larger balls give better results because of high impact forces on the powders. The balls should be more dense than the material to be milled. Even though most of the investigators generally use only one size of the milling medium, there have been instances where different size balls have been used in the same investigation. It has been predicted that the highest collision energy can be obtained if balls with different diameters are used . Use of milling balls of the same size has been shown to produce tracks. Consequently, the balls roll along a well-defined trajectory instead of hitting the end surfaces randomly. Therefore, it is necessary to use several balls, generally a combination of smaller and larger balls to randomize the motion of the balls . The properties of materials used as milling media are given as Material Main composition Density (g cm3) Abrasion resistance Agate SiO2 2.65 Good Corundum Al2O3 >3.8 Fairly good Zirconium oxide ZrO2 5.7 Very good Stainless steel Fe, Cr, Ni 7.8 Fairly good Tempered steel Fe, Cr 7.9 Good Tungsten carbide WC, Co 14.714.9 Very good

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Ball-to-Powder Ratio

The ball to powder ratio (BPR) or charge ratio is another milling parameter and represents the weight ratio of the milling balls to the powder charge. A wide range of BPR have been used in a variety of investigations from values as low 1:1 to as high 220:1.

Extent of Filling of the Milling Chamber

It is necessary that there is enough space for the balls and the powder particlesto move around freely in the milling chamber. The filling depends on type of mill.Generally about 50% of the space is left empty but in attritorsthis value is 2030%.

Milling Atmosphere

The milling atmosphere can contaminate the powder and as a results milling is frequently carried out in evacuated, argon, or helium charged milling. Other atmospheres can be used if particular effects are desired. Nitrogen and ammonia have been used to produce nitrides and hydrogen atmospheres to produce hydrides. The intention application of hydrogen in milling chamber was a real breakthrough in hydrogen storage technology for synthesis of nanocrystalline hydrides. The presence of air in the milling chamber can result in the formation of oxides, oxisulphates or sulphates .Contamination can be avoided by milling the powders with a milling media made up of the same material as that of the powders being milled.

Milling Speed

The milling speed can have an important influence but this varies with the type of mill. Above a certain critical speed, the balls will be pinned to the walls of the milling chamber and not exert any impact force on the powder. Below this critical speed, however, the higher the milling

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speed, the higher the milling intensity will be. For the higher speeds the temperature of the milling chamber may reach a high value.

Milling Time

According to many researchers the milling time is the most important milling parameter. However, the level of contamination will increase with milling time and some undesirable phases may form if a powder is milled too long. Substantial reduction in particle size usually occurs with milling time and typically takes the form of exponential decay.

4.4. EFFECTS AND SIDE EFFECTS DURING BALL MILLING :

Temperature Effects

Since diffusion processes are involved in the formation of a nanostructure, it is expected that the temperature of milling will have a significant effect. Two kinds of temperature effects during milling are usually taken into account: local temperature pulses due to ball collisions and the overall temperature in a vial. During the milling process part of the milled powder is attached to the vial walls and, other part is attached to the balls. The remaining part is in a free state moving in the volume of the milling chamber. All these parts have different temperatures. The temperature of the powder influences the diffusivity and defect concentration in the powder thus influencing the phase transformations induced by milling. The results of measurement and calculation of the milling temperatures show that there is only a moderate temperature rise during milling and that local melting can be ruled out. Bi powder was milled and the temperature of milling was calculated. The value was below its melting point 271C. The temperature increase of the milling balls in two laboratory mills was studied recently. The ball temperature remains below 100C in a SPEX mixer mill and it is cooler when flat-ended rather than round-ended vial is used. Temperatures over 200C are typical in a planetary mill operating at similar milling intensities. The results presented in Fig. 43 | P a g e

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were obtained using a Fritsch P-5 mill with two vial sizes and rotational speeds. The final temperatures are indeed much higher than the temperatures obtained with the SPEX 800 mill. The temperature could be increased further via increasing the speed of the mill. In fact, the highest temperature obtained with the smaller bowl was 327C at 318 rpm. A decrease of the temperature is expected at very high speeds, as the balls stay attached to the container wall for too long, reducing both heating and efficiency of milling. It is suggested that the higher ball temperatures result from more oblique collisions and friction, while the lower temperature but higher intensity of the mixer mill with flat-ended vial is due to the larger portion of frontal impacts. Ball temperature-milling time curves obtained using a Fritsch P-5 planetary mill.

Contamination

The serious problem which is usually cited in mechanochemical research is contamination. The small size of milled particles, availability of large surface area, and formation of new surfaces during milling all contribute the contamination of the powder. . As mentioned above, the milling atmosphere can be one source. However, if steel balls and milling chambers are used iron contamination can contribute as a further factor. It is most serious for the high-energy mills. Lowenergy mills result in much less, often negligible Fe contamination. Other milling media, such as tungsten carbide or ceramics, can be used but contamination from such media is also possible. Surfactants (process control agents) may also be used to minimize contamination. Using a seasoned milling chamber i.e. media coated with the product powder-resulted in very low values for Fe contamination. Application of shortest milling times and self-coating of the balls with milled material can be also helpful.

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Amorphization

During high-energy milling, the size of crystals decreases to some critical values. Further energy supply to these crystals of limiting size causes further deformation of crystals, energy accumulation in the volume or at the surface of crystals, and subsequently amorphization.The occurrence of an amorphous phase is generally interferred by observing the presence of broad peaks in the X-ray diffraction patterns. It is not possible to distinguish among solids which are truly amorphous, extremely fine grained or a solid in which very small crystals are embedded in an amorphous matrix. Hence, it has been the practice to recognize such observations as X -ray amorphous, suggesting that the identification was done only by X-ray diffraction methods. It is desirable that the X-ray diffraction observations are confirmed by other techniques as well .

Mechanochemical Equilibrium

The objective of high-energy milling is the preparation of a milled material having the fines suitable for further application. However, this particle size reduction is, in many cases, complicated by particle size enlargement where smaller particles are put together to form larger entities in which the original particles can still be identified. Experience shows that after achievement of a certain degree of dispersion further comminuting is reduced, or there may even be an increase of particle size, due to the interaction of particles. In a typical experiment, copper was milled in a mill loaded with steel balls for 110 hours followed by separation of milled material in a 60 m sieve. Both the coarse and the fine fractions were milled for another 48 hours and a product of approximately the same sieve analysis was obtained because of the comminuting of the coarse fraction and aggregation of the fines. Huttig called the particle size distribution and he demonstrated the same phenomenon with other brittle materials. On the basis of these experiments Huttig postulated the existence of an equilibrium state of comminution. Tanaka suggested the following equation for characterizing the kinetics of milling

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Where Wzis the energy input, S the specific surface at equilibrium and k a constant . Later the process of new surface area formation was described by equation

whereSis specific surface after time t and Smis maximum specific surface . Constant k2 implies the significance of rate constant of new surface formation. Equation describes also processes in which the formation of new surface is limited by milling equilibrium after a certain time of milling. Jimbo described the phenomenon characterized by the increase of the size, the decrease of the specific surface area and the specific total pore volume with the increase of milling time as the negative grinding phenomenon .This phenomenon is in a very close relation to the aggregation and agglomeration effects discussed in the next paragraph.

Agglomeration and Aggregation

In the course of the milling process a gradual deterioration of affectivity is to be observed. The energy input proportional surface increase gets impossible to obtain first explanation in mechanochemistry was given in the year 1937: with decrease of particle size, the number of defect locations runs out hence the increase of milling resistance, at extreme disparity is approached. These Equations can be applied for the mathematical description of such process. As it is well known in mechanochemistry, attaining a certain value, the surface area begins to diminish .Thorough investigation of this process on several solids has shown that three stages can be clearlydistinguished:

Surfactants

There are several expressions used in literature for substances which preferentially adsorb onto the interfaces, prevent aggregation and stabilize the separated nanoparticles. The terms such as surfactants, surface active agents, process control agentsandlubricantsare most frequently 46 | P a g e

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applied. In principle, stabilization can be accomplished by electrostatic (charge, or inorganic) stabilization or steric (organic) stabilization .Steric stabilization is achieved by surrounding particles with a layer of substances which are sterically bulky such as polymers. These large adsorbates provide a steric barrier that prevents close contact of the fine particles. The coil dimensions of surfactants are usually larger than the range over which the attraction forces between nanoparticles areactive. The water molecule plays here a special role. If a surfactant is added to water, its hydrocarbon chain tend to self-associate to minimize contact with water molecules. If the water is able to solubilize the polar head and the alkyl chains equally, no aggregates are formed. The shape of the surfactant plays an important role in forming the assembly . If the surfactant molecules have a very large polar head and a small chain forming a cone shape, the chains tend to self-associate to form a spherical aggregate called a normal micelle If the surfactant has a shape of a champagne cork spherical reverse micelles are formed . This is termed a water-in-oil droplet. In surfactant systems containing large amounts of both oil and water, the shape and dimension of the aggregates changes. Adding more water induces a new phase transition, with the surfactant molecules reorganizing as a planar or lamellar film. The other types of surfactant shapes are also possible as an onion shape on Electrostatic stabilization occurs by the adsorption of ions to the electrophilic surface . Electrostatic stabilization involves the creation of an electrical double layer arising from ions adsorbed on the surface and associated counterious which surrounds the particle . Surfactant chemicals as a group have some unusual chemical and physical properties. In addition to the tendency for their adsorption at phase interfaces, they also demonstrate several other important properties. One of these properties is selfassociation between surfactant molecules of exactly the same structure leading to the formation of micelles . In high-energy milling, surfactants have been used at a level of about 15 wt.% of the total powder charge into the mill . The nature and quantity of surfactants used and the type of powder milled would determine the final size, shape, and purity of the powder particles. Use of a larger quantity of surfactants normally reduces the particle size by 23 orders by magnitude. For example, it was reported that milling aluminium for 5 hours produced a particle size of about 500 m when 1% stearic acid was used as a surfactant. However, when 3% of stearic acid was used, the particle size was only 10 m . The choice of polymer surfactants varies from case to case. They must be mobile enough to provide access for the addition of monomer units, while stabile enough to 47 | P a g e

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prevent the aggregation ofnanocrystals. By using surfactants (or mixtures of surfactants) that bind differently to the different crystallographic faces, we can control the shape of the nanocrystals [Puntes et al. 2001]. However, it should be realized that there is no universal surfactant. There have been several reports in literature that milling can be influenced by the addition of surfactants into the mill . The most of the results have been interpreted in terms of two major mechanisms. The first mechanism is called Rebinder effect. According to this concept, the adsorption of surfactants results in a decrease of the surface energy of solids where by their strength and resistance to mechanical effects decrease . The classical explanation of the chemomechanical effect is based on the Griffiths theory of fracture of solids weakened by a priori cracks. Molecules and ions of the surfactant intrude into the microcracks. The concept of Rebinder effect comprises the whole complex of phenomena promoting deformation and fracture. The essential feature is that, because of the reversible interaction of the solid with the surfactant, less work is required for the generation of new surface. After Juhasz and Opoczky, Rebinder concept about the reduction of surface energy and the consequent decrease of fracture energy is untenable, since it is known that fracture energy is primarily determined by plastic deformation at the crack front and that stresses arising on fracture surfaces can only marginally, if at all, influence the propagation of cracks.

The second mechanism states that adsorption of surfactants influences the properties of fragments created by milling. This mechanism is based on the empirical observation that surfactants alter the conditions of energy and mass transport by high-energy milling. Considering the above factors a cryogenic (low temperature) ball mill was designed. During testing and calibration simple salts (NaCl) and fiber Jute was grinds and compared. Also, we are planning to carry out some nanoparticle synthesis from technically important materials as our future work. Also, characterize them to study the important properties.

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5. CONCLUSION

5.1.

APPLICATION

This will be useful in following areas : 1. Research in Nanotechnology, material science of Micro metallurgy. 2. Powder metallurgy. 3. Coalwashery 4. Metal sintering 5. Normal grinding 6. Preparation of Nanomaterials 7. Grinding of Fiber Materials 8. Ore grinding 9. Ceramic materials 10. Chemicals

5.2.

ADVANTAGE OF THIS MACHINE

1. It can provide high speed machining process. 2. Ultra-fine grain, ranging from some millimeter to can be produced. 3. Only machine to grind Fiber particles. 4. As machining process can be conducted in liquid medium, it makes the machining area unaffected from outer atmosphere. 5. Helpful for several research field. 6. Multipurpose usage. 7. Low cost. m or nanometeric range

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5.3. DISADVANTAGE OF THIS MACHINE

1. Not use full for extremely hard material. 2. Vacuum maintain is quit costly. 3. Timely change of machine medium.

5.4.

USE GUIDE FOR USING MACHINE

1. Clean the entire setup thoroughly. 2. Adjust the level adjuster. 3. Ensure that, the power is off. 4. Fix the cryogenic jar, with motor at coupling and properly fix it so that, the alignment of Motor Shaft and Jar Shaft will be, coaxial. 5. Pour the specimen material and ball, into the Jar. The specimen material and Ball, should have suitable mass and volume ratio. 6. Pour the Liquid Nitrogen and fill the jar up to 80%. 7. Assume that, the variac is at off position and then power on the switch. 8. On the Variac, and gradually lower its resistance by its regulator switch. 9. As the Motor Will start rotating and the Jar resistance till an optimum speed is obtained. 10. Adjust the angle of Jar, at suitable angle, by the help of Angle providing arrangement. 11. Run the machine for optimum time with optimum speed, to get desired fineness of grain. 12. Stop the machine, after milling and remove the jar from coupling, and collect the finished powder. 13. Again clean the machine thoroughly. also keep on lowering the

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5.5. PRECAUTIONS TO BE TAKEN

1. Before using the machine, ensure that, power is off. 2. Before power supplying, ensure that, the variac is at off condition. 3. An Earthling supply should be there, for safety.

4. Do not use the level adjuster if not required. 5. Do not change the angle of Jar, while rotating. Stop it, before changing the angle. 6. Stop the Motor, before giving it reverse rotation. 7. Clamp the Motor, with the Mounting plate, tightly. 8. Never remove the Jar, from any parts, other than Coupling Position. 9. Always check, and ensure that, all the joints are rigidly and tightly fixed.

10. Always keep the machine clean and dry, before and after using. 11. While stopping the Motor, always the Clutch, to avoid Jerk, due to

sudden stopping of Motor Shaft,

when power is switched off.

5.6 . WHAT DO WE LEARN, AND SKILLED IN THIS PROJECT

1. Use of Lathe, and its different operation. a. Facing b. Turning c. Threading 2. Drilling 3. Edge grinding and surface grinding 4. Outer threading, by using threading dia. 5. Inner threading, by using threading tap. 6. Alignment making, while manufacturing a compound rotating part. 7. Welding 8. Gas cutting 9. Brazing 51 | P a g e

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10. Importance of measurement 11. Use of a. Vernier caliper b. Spirit level c. Meter gauge d. Different files 12. Material property, and its behavior, towards machining mostly of i. Stainless Steel ii. Mild Steel iii. High Speed Steel iv. Cast Iron v. Galvanized Steel

5.7.

CONCLUSION
The designed prototype low-temperature high energy ball mill will be a very good

device for the synthesis of nanomaterials. The present low temperature based high-tech mechanical grinder is a low-cost device as compared to the international scenario. The vacuum container is made up of stainless steel materials. The vacuum of the steel container is around 1x10
-5

mbar. The internal diameter (51 mm) and the ball size are so chosen to get the critical

RPM around 10. The RPM of the ball mill was adjusted below the critical RPM ( < 10 rpm) by means of mechanical gear and electrical variac. The Designed high tech instrument is working fine and need a little effort to commercialize the same. Then, it will be a very low cost as compared to the international market. Using this device, materials can be powdered in to very fine powder form to nano size in a very small time of few hrs. This powder metallurgical process allows for the preparation of alloys and composites, which cannot be synthesized via conventional routes. In nonmaterial research, this top down techniques well used to fine-tune the grain sizes of the materials in nanoscales.

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REFFERENCE 1. www.wikipedia.com 2. www.sincedirect.com 3. www.howstuffworks.com

4. TEXT BOOK ON INTRODUCTION TO PHYSICAL METALLURGY AND MATERIAL SCIENCE BY O.P.KHANNA . 5. TEXT BOOK ON MANUFACTURING TECHNOLOGY BY P.N .RAO 6. JOURNAL ON The Minerals, Metals & Materials Society and ASM

International 2010 .
7. 8. JOURNAL ON CORRILATION BETWEEN THE MINIMUM GRAIN SIZE PRODUCEED BY MILLING AND MATERIAL PARAMETERS MATERIAL SCIENCE AND ENGINEERING A,2003. 9. JOURNAL ON TENSIAL AND CREEP BEHAVIOUR OF CRYO MILLED PRODUCT OCTA MATERIALIA A,2003 . 10. JOURNAL ON FORMATION OF NANOMATERIALS BY A BALL MILL AT CRYOGENIC TEMP MATERIAL SCIENCE AND ENGINEERING A 2004 .

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