Materials Processing (Casting, Forming and Welding)

Swarup Bag
Department of Mechanical Engineering
Indian Institute of Technology Guwahati

Materials Processing
 Module 6

Solid state deformation

✓ Friction, ultrasonic, diffusion and explosive welding
✓ Mechano-Chemical Ball Milling
✓ Friction Consolidation
✓ Case studies

Materials Processing (Casting, Forming and Welding) 2

 Introduction
➢ Coalescence between the surfaces of fabricated parts are achieved by:
➢ Only pressure or both heat and pressure
➢ On the application of both heat and pressure, developed heat is not enough to melt the surfaces
➢ Feedstock material (Filler wire) is not utilized
❑ Need of solid state Welding process
➢ Joining of dissimilar metals and alloys
➢ Joining of difficult to weld metals like Aluminum and super alloys
➢ To develop stronger and Intermetallic free welds
❑ Solid state welding Techniques
✓ Friction welding
✓ Ultrasonic welding
✓ Diffusion welding
✓ Explosive welding

Materials Processing (Casting, Forming and Welding) 3

 Introduction
❑ Bonding Mechanism of solid state welding process
✓ Localized Melting
✓ Diffusion
✓ Recrystallization
✓ Adhesion
✓ Interfacial Reaction
✓ Interfacial morphology
▪ Localized Melting
➢ Frictional heating while joining are responsible for localized melting, observed mainly in Explosive, Friction and
Ultrasonic welding
➢ Melting facilitates the formation of inter-metallic compounds that lowers the bonding strength
▪ Diffusion
✓ It is a thermally activated phenomena pertaining to the material properties and transient temperature

Materials Processing (Casting, Forming and Welding) 4

 Introduction
▪ Recrystallization
✓ Migration of grain boundaries occurs while developing the intimate contact between surfaces

▪ Adhesion
➢ Bonding between the surfaces developed due to atomic attraction
➢ Adhesion forces reaches to its maximum at interatomic distance of 10-10 m and it’s having inverse relation with square of
atomic distance
▪ Interfacial reaction
➢ Reaction of oxide films with weld metals
✓ Solubility of oxide at interface is required
➢ Reaction between two weld metals
✓ Formation of intermetallic compounds
➢ Phase transformation occurs while solidification of molten material

Materials Processing (Casting, Forming and Welding) 5

 Friction welding

Five (5) five types of friction welding: Linear, Rotary, Stir, Radial and Orbital

The types of friction welding differs by types of relative motion

✓ Friction Welding (FRW) - solid state welding process

✓ Work piece rotates at high rotational speed
✓ Compressive force at the contact of work pieces is applied
✓ Heat is produced due to the friction
✓ Material displaces plastically at the faying surfaces

One piece is held stationary while the other is rotated at high speed

Materials Processing (Casting, Forming and Welding) 6

 Linear friction welding
Advantages
✓ Avoids cracking and porosity
✓ Process is fast and repeatable
✓ Easy to automate
✓ Energy efficient
✓ No shielding gas is required

Applications: Mostly for

joining aero-engine compressor
blades to compressor disks
Materials: Titanium alloys and
Phases: (a) initial phase, (b) transition phase
nickel based superalloys
(c) equilibrium phase (d) deceleration and forge phase

Materials Processing (Casting, Forming and Welding) 7

 Rotary friction welding
Delivering the energy to the weld
interface:

Direct drive - the rotating part is

continuously driven by the equipment
spindle motor
Inertia - the rotating part is connected
to a flywheel

Only symmetric parts can be welded

8
 Rotary friction welding

Applications

Turbine shafts
Piston rods
Copper-aluminium electrical connections
Cutting tools
Tubular transition joints combining dissimilar metals (Aluminium-Titanium and
Aluminium-Stainless steel)

Advantages

✓ Similar to linear friction welding

✓ Reduces intermetallic formation and allowing for a range of dissimilar materials to be
joined 9
 Inertia friction welding

✓ Uses kinetic energy to perform welding

✓ Flywheel stores the kinetic energy
✓ Once the flywheels are up to speed, the
motor driving the flywheels is
disengaged
✓ Flywheels release the kinetic energy at
the interface
✓ It brings uniformity in energy supply to
the welding system

Materials Processing (Casting, Forming and Welding) 10

 Friction welding
Application of Friction welding

✓ Critical aircraft engine components

✓ Automotive parts like engine valve
✓ Hydraulic piston rod and track roller in agricultural equipment
✓ Friction welded are often replaced by expensive casting and forging

Disadvantages
✓ Process is restricted to joining symmetrical objects (round bars or tubes of
same diameter)
✓ One of the materials must be ductile
✓ Alignment of the work piece for uniform rubbing and heating is difficult
Materials Processing (Casting, Forming and Welding) 11
 Friction Stir Welding (FSW)
➢ Solid State Welding process in which coalescence is achieved by
frictional heat combined with pressure
➢ The objectives of the FSW tool is to
▪ Generate heat at the work piece
▪ Move the material to form weld joint
➢ Frictional and deformational effects results in plasticizing of the
materials

➢ Advancing Side : The side which has similar sense of tool rotation
and traverse/translation direction is termed as advancing side Figure: FSW process

➢ Retreating Side : The side which has opposite sense of tool rotation
and traverse/translation direction is termed as retreating side

Materials Processing
Solidification
(Casting,
Processing
Forming and Welding) 12
 Friction Stir Welding (FSW)

Materials Processing (Casting, Forming and Welding) 13

 Attributes for monitoring FSW joints
➢ Tool Rotation Rate (rpm)
▪ Clockwise or counter-clockwise direction
▪ Tool rotation results in stirring and mixing of material around the pin.
▪ Higher tool rotation rate generates higher temperature due to frictional heating resulting in intense mixing & stirring.
➢ Tool Traverse Speed (mm/min)
▪ Effects in flow of stirred material from the front to the back of the pin.
➢ Tool Rotation Rate (degree)
▪ Suitable tilt angle ensures effective holding of material by the shoulder while moving the material from the front to the
back of the pin.
➢ Plunge Depth/ Pin Insertion Depth
▪ Important for producing sound/smooth weld surface.
▪ Shallow plunge depth: Shoulder doesn’t touch contact the work piece surface, thus cannot move the material from the
front to back of the pin producing welds with surface groove or tunnel/inner channel.

Materials Processing (Casting, Forming and Welding) 14

 Tools in FSW process

(a) Straight cylindrical pin tool

(b) Straight cylindrical square thread pin tool
(c) Straight cylindrical V-thread pin tool
(d) Taper cylindrical pin tool
(e) Taper cylindrical square thread pin tool
(f) Taper cylindrical V-thread pin tool

➢ Higher compressive yield strength at elevated temperature

➢ Dimensional stability and creep resistance
➢ Thermal fatigue strength to resist repeated heating and cooling cycles Good fracture toughness
➢ Low coefficient of thermal expansion

Materials Processing (Casting, Forming and Welding) 15

 Hybrid Friction Stir Welding (HFSW)
❑ Thermal energy assisted FSW
✓ Electricity, induction, laser, plasma, arc, hot gas stream, gas torch
✓ Electricity and induction are used for resistance heating of the workpieces
✓ Laser, gas and arc/plasma are applied for direct preheating
❑ Mechanical energy assisted FSW
✓ Ultrasonic energy is the only mechanical energy employed for this purpose
✓ Ultrasonic vibrations directly soften the material without much variation in the process temperature

Materials Processing (Casting, Forming and Welding) 16

 HFSW of dissimilar materials
✓ Plasma assisted FSW process utilized to join Al and CU
✓ Preheat is beneficial for to enhance the temperature of
harder workpiece in front of tool pin while dissimilar
welding
✓ Due to difference in flow stress value, Tool wear reduces
✓ Weld zone increases in size with time – plunging period
✓ weld zone size remains almost constant

Figure: Depiction of dissimilar welding of Al and Cu (Yaduanshi et al. 2016, Materials and Design).

Materials Processing (Casting, Forming and Welding) 17

 Defects in FSW process
✓ Inappropriate material flow and heat generation
✓ Tool rotational rate
✓ Tool traverse speed
✓ Improper tool geometry selection
✓ Insufficient plunge depth
✓ Unequal thickness of joining materials
✓ Gap between plates

❑ Tunnel defect
✓ One of the most common defect in FSW process
✓ Occurs below the workpiece surface
✓ While welding, improper selection of parameters lead to insufficient
heat generation and thus reduce material plasticization at the stir zone

Materials Processing (Casting, Forming and Welding) 18

 Ultrasonic Welding

➢ Coalescence is produced at the faying surfaces by the application of high frequency vibratory energy

- while the workpieces are held together under moderately low static pressure

➢ Produces a weld by oscillating shear forces at the interface between the two metals being joined

- while they are held together under pressure

❑ Interfacial Interaction
➢Localized temperature rises resulting from interfacial slip and plastic deformation.
➢Temperature is also influenced by power, clamping force, and thermal properties of the material.
➢Localized Plastic Deformation
➢Metallurgical phenomena such as recrystallizing, phase transformation, etc..... can occur
❑ Types of Ultrasonic Welding
➢Wedge Reed System
➢Lateral Drive System

Materials Processing (Casting, Forming and Welding) 19

 Ultrasonic Welding
❑ Wedge Reed System Clamping force

➢ Accurate control on the parameter is not possible due to its bending mode through Mass
which mechanical vibrations transfer to the work piece.
➢ The anvil sometimes act as a vibrating part and resonates out of phase to the reed. wedge Transducer

➢ That is why the wedge reed system is more useful for the joining of sheets with large
Sonotrode
thickness. tip

Weldment
❑ Lateral Drive System Vibration

➢ Lateral drive system is simple and Anvil

allows the welding parameters to be Force

measured via transducer Fig. Wedge Reed

➢ It gives good results for thin

specimens due to its lower rigidity Fig. Lateral drive

Materials Processing (Casting, Forming and Welding) 20

 Power Generation in Ultrasonic Welding

✓ Frequency is transformed to vibration energy through the transducer

✓ Energy requirement established through the following empirical relationship

– E = k(HV t)3/2
Frequency
– E = electrical energy Electrical energy
converter
– HV = Vickers hardness number

– t = thickness of the sheet

Vibratory
✓ The constant “k” is a complex function that appears to involve transducer
primarily the electromechanical conversion efficiency of the
transducer, the impedance match into the weld, and other
characteristics of the welding system. Different types of
transducer systems have substantially different k values

Materials Processing (Casting, Forming and Welding) 21

 Diffusion bonding
• A solid-state welding process that produces coalescence of the faying Force Work pieces

surfaces by the application of pressure at elevated temperature.

A
• The process does not involve macroscopic deformation, or relative B
motion of the workpieces.

• A solid filler metal may or may not be inserted between the faying Fig. Schematic illustration of diffusion welding
surfaces. 1st stage deformation and
interfacial boundary formation
Asperities come into contact

❑ Stages of Bond Formation

• 1st stage
– deformation forming interfacial boundary.
• 2nd stage
– Grain boundary migration and pore elimination.
• 3rd stage 2nd stage boundary migration and 3rd stage volume diffusion
– Volume diffusion and pore elimination. Pore elimination pore elimination

Materials Processing (Casting, Forming and Welding) 22

 Factors Influencing Diffusion bonding
❑ Relation between Temperature and Diffusion Coefficient

Temperature Time
D = D0 e -Q/KT X = C (Dt)1/2 = Diffusion Length
– X = Diffusion length
– D = Diffusion coefficient – C = A constant
– D0 = Diffusion constant – D = Diffusion coefficient
– t = Time
– Q = Activation energy

– T = Absolute temperature

– K = Boltzmann's constant

Materials Processing (Casting, Forming and Welding) 23

 Explosive Welding
➢ Types of solid state welding that utilizes explosive force to create metallurgical bond between two metal components.
➢ Due to short time duration of impact, there is adiabatic heat rise
➢ Application: Cladding carbon steel plate with a thin layer of corrosion resistant material
Explosion
➢ Process Geometry Chemical explosives
▪ Parallel plate bonding is used for larger
plates.
Flyer (cladding)
▪ Flyer plate velocity ranges from 250-500
m/s. Deformed zone
Substrate
▪ Collision point velocity ranges from 1500-
3000 m/s. Figure : Explosive welding
▪ Collision angle is 5-200 . The major process variables:
(i) Impact velocity
The impact must be sufficiently high to cause the colliding metal surfaces (ii) Stand-off distance
to flow hydro dynamically when they intimately contact each other. (iii) Angle of approach

Materials Processing (Casting, Forming and Welding) 24

 Explosive Welding
• Shock wave propagation should exceed
the sonic velocity.
• Most metals have sonic velocity from
2000 to 6000 m/s.
• Explosive velocity greater than 120% of
sonic velocity of the material should not
be used because of deleterious effect of
shock rarefaction.
𝐸
• Sonic velocity of material: Vs =
ρ
• Vs : Sonic Velocity; E: Elastic Modulus;
ρ: Material Density
25
 Explosive Welding
• Detonation Velocity: It is characteristic of type of
explosive and has been shown to be directly
proportional to the explosive density.

• For nitroguanidine explosive it ranges from 2000 -

5000 m/s for explosive densities 0.14 to 0.9 g/cm3.

• Detonation velocity: 𝑉𝑑 = 1440 + 4020 𝜌𝑒

β
• Flyer Plate Velocity: 𝑉𝑝 = 2𝑉𝑑 sin ( )
2

• Explosive Pressure: P ∝ 𝑉𝑑 2 𝜌𝑒

𝜌𝑒 ∶ Explosive Density; β: Dynamic Bend Angle

26
 Explosive Welding

Explosive welding is mainly used for

lap joints in difficult to weld metals

✓ Aluminium to stainless steel

✓ Aluminium to nickel alloys
✓ Stainless steel to nickel
✓ Aluminium to brass
✓ Titanium to steel,
✓ Zirconium to stainless steel,
✓ Zirconium to nickel base alloys
✓ Copper to aluminium

27
 Case study on dissimilar welding of EN AW 6082 and EN AW5083
❑ Objective
➢ To analyze the effect of keeping constant tool rotational speed (TRS) to welding speed (WS) ratio (r) on microstructural
mechanical properties
❖ Tool Description
✓ Tool made up of DIN EN 1.7131 steel having pentagonal and triangular shapes were utilized
❑ Inferences withdrawn from the analysis:
✓ Three distinct zones were characterized in the extracted samples influenced from
FSW parameters and pin shape namely Nugget zone (NZ), thermodynamically
affected zone (TMAZ) and fusion zone (FZ) (Figure 2).
✓ Onion type rings produced by pentagonal shaped pin (higher circumference) is
more distinctive and wider NZ on contrast with the triangular shaped (Figure 3).
Figure 1 : Pentagonal and triangular
✓ Tunnel and cavity types of defect were present in the joint fabricated by shapes tool (Kasman et al. 2017,
metals MDPI)
triangular shaped pin due to insufficient heat input results in inadequate material
flow at TRS of 400 and 500 rpm and WS of 40 and 50 mm.min-1 (Figure 4).

Materials Processing (Casting, Forming and Welding) 28

 Case study on dissimilar welding of EN AW 6082 and EN AW5083
✓ Ultimate tensile strength (UTS) of
triangular shaped pin enhanced with
increasing the tool rotational speed.
However, this behavior was not
analyzed for pentagonal shaped pin.
✓ Efficiency for joint strength varies from
Figure 3: Nugget zone consisting of onion rings (Kasman
55% to 68%. These variations depend et al. 2017).
on the defects in welded joint and
strength of base material.
✓ Hence, by increasing or decreasing
TRS and WS while making “r”
constant, profile, structure and UTS Figure 2: Cross-section
of welded joint
value changes significantly. Figure 4: Defective welded joint samples (Kasman et al. 2017).

Materials ProcessingSolidification
(Casting, Forming and Welding)
Processing 29
29
Thank you
for your kind attention

30
Materials Processing (Casting, Forming and Welding)

Swarup Bag
Department of Mechanical Engineering
Indian Institute of Technology Guwahati

Materials Processing
 Module 6

Solid state deformation

✓ Friction, ultrasonic, diffusion and explosive welding
✓ Mechano-Chemical Ball Milling
✓ Friction Consolidation
✓ Case studies

Materials Processing (Casting, Forming and Welding) 2

 Introduction
❑ Ball Milling
✓ It is a type of grinding technique that primarily employs balls as the grinding medium, achieving bulk material
pulverization through impact, compression, and friction into extremely fine powders.
✓ It initiates solid-state chemical reactions at room temperature via mechanical energy.
✓ High-energy ball mill facilitates the plastic deformation required for cold welding.
❑ Mechanical alloying
✓ It is a powder processing technique developed started to fabricate nickel-based dispersion strengthened (ODS)
superalloys for gas turbine applications.
✓ Mechanical alloying process begins with blending of powders in required proportion and loading the mixtures to the mill
with grinding medium (commonly steel balls are utilized).
✓ Processing of powder consists of cold welding, fracturing and rewelding of powder particles in cyclic manner in high
energy ball mill led to the formation of new alloy.
✓ This methodology is having capability of synthesizing wide range of equilibrium and non-equilibrium alloy phases.

Ball Milling and Friction Consolidation 3

 Working principle of Ball Milling
❖ Ball milling works on the principle of impact and abrasion.
✓ Impact: Occurs due to Collison between the surface of moving balls and material
✓ Abrasion: Occurs due to Collison between both powder particles and ball with surface of mill
❖ Sequential steps involved while processing of material:
✓ Initial state: Powders particles are flattened by Collison of ball
✓ Intermediate step: Significant changes occurs in the particle shape (a) and (b): Movement of ball mill
(c): Critical speed shown by yellow arrow
✓ Final step: Extremely deformed metastable structure is obtained
(a) (b) (c)

Low speed with sliding High speed with centrifuging Critical speed with cascading

Ball Milling and Friction Consolidation 4

 Working principle of Ball Milling
✓ A ball mill basically consists of hollow Horizontal section
Rotating direction of mill
cylinder shell rotating about axis
✓ To get the optimum efficiency of ball mill,
critical speed must be achieved given by:

1 g
nc = 2π R−r

where, R = radius of hollow cylinder Materials

r = average radius of ball Grinding medium

g = gravitational force
Grinding efficiency = [(A-B)/A]*100 Movement of supporting disc
A = amount of material sieve before grinding
B = amount of material in sieve after grinding
Figure : Powder processing mechanism
through ball mill

Ball Milling and Friction Consolidation 5

 Process Variables in Milling
❑ Feed rate
✓ With enhancing the feed rate, reduction in size of part occurs as in this case material is in contact for shorter time
❑ Weight of balls
✓ On discharging the ball with heavy weight, fine product is achieved. This occurs due to increase in charge weight
either by utilizing ball materials of high density or by increasing the number of balls.
✓ Hardened steel, tool steel, tempered steel and bearing steel are commonly utilized material for ball mill
❑ Milling Energy or speed
1
✓ Kinetic energy of grinding medium (𝐸 = 2 𝑚𝑣 2 ), where ‘𝑚’ is mass and “𝑣” is velocity of grinding medium

✓ By increasing the speed of rotation of mill will enhance the movement of balls led to the formation of fine product
✓ On augmenting the speed above critical (nc ) balls pinned to the inner wall and not move downward to apply any
impact force
✓ Hence, the maximal speed must be less than “nc ” such that balls falls from maximum height to create maximum
Collison.

Ball Milling and Friction Consolidation 6

 Process Variables in Milling
❑ TYPE OF MILL
✓ Selection of mill depends on type of powder, amount of powder to be milled, and final composition of required
product.
❑ BALL TO POWDER WEIGHT RATIO
✓ Ratio of weight of the ball to the powder ratio (BPR) referred as charge ratio.
✓ Higher charge ratio results in quick refinement of crystallite size with reduction in amount of powder synthesization
✓ For SPEX mill, BPR values vary from 4:1 to 30:1
✓ For an attritor, BPR values vary from 50:1 to 100:1
❑ PROCESS CONTROL AGENTS
✓ These agents are adsorbed on the surface of powder particles to minimize cold welding and lower the surface tension
to reduce larger plastic deformation.
✓ Energy required for this physical phenomena is 𝑬 = 𝜸∆𝑺, where 𝛾 is specific surface energy and ∆𝑆 increase in
surface area

Ball Milling and Friction Consolidation 7

 Selection of Grinding medium for Milling Process
❖ To do efficient milling of powder particles, proper choice of nature, size and distribution of grinding medium is required
➢ Specific gravity
✓ Commonly, grinding medium with high density led to the fine product as the higher kinetic energy of balls impart
more amount of energy to the powder
➢ Initial feed size
✓ Grinding medium must larger than powder particle size, it is required to utilize grinding balls of different size
instead of one type to improve the efficiency.
➢ Hardness
✓ Harder the grinding medium, lesser will be powder contamination, and consequently media will last longer
➢ pH value
✓ Strong acid or basic slurries react with some metallic media
➢ Discoloration
✓ Some of the grinding medium results in development of color while functioning, hence it is not recommended for
coating in white color.
Ball Milling and Friction Consolidation 8
 Contamination during Milling
❖ During the milling process continuously, fresh atomic surfaces are created, hence contamination by O2 and N2 are real
problem
✓ Argon commonly utilized to create inert environment.
❖ On performing Milling with liquid surface agent can reduce particles surface energy facilitates smaller particle sizes to
form. Consequently, some of the particles observed in sample as contaminant.
❖ Contaminations occurs from steel balls
✓ Less foreign particles are introduced if milling media of dissimilar materials are utilized
✓ While milling their will be a chance of welding of powder on pot and diffusion takes place on milling surfaces
❑ Necessary steps for minimizing Contamination
✓ Pots must be designed in accordance with material required to mill
✓ Milling with sand: Processing with high purity sand (quartz) to remove stuck on material
✓ Utilizing Acetone while Milling

Ball Milling and Friction Consolidation 9

 Mechanical Alloying
❑ Sequential steps involved in Mechanical alloying
✓ Initially powders are mixed in required proportion and loaded to the mill with grinding medium
✓ Process control agent (PCA) is feed to reduce excessive cold welding of powder particles
✓ Consequently, milled powder consolidated into bulk shape and subsequently heat treated to obtained desired
properties
❑ Raw materials for Mechanical alloying
✓ Raw materials utilized for this process consist of commercially available pure powders of metals, alloys and
refractory compounds.
✓ Powder particle size must be lesser than grinding ball size as its particle sizes reduces exponentially with milling
time.
✓ Addition of oxides, carbides, and nitrides to the alloy referred as Dispersion-strengthened materials
✓ Sometime cryogenic medium liquid nitrogen is used to reduce the temperature of milling referred as wet milling
✓ Wet grinding of particles are more suitable than dry to fabricate fine products as the molecules of solvent observed on
newly milled surface and subsequently lower their surface energy.

Ball Milling and Friction Consolidation 10

 Mechanical Alloying

Water cooled stationary tank

Gas seal
Metal A
Heat treatment
Heated container
Steel can
v
Metal B
Machining

v v v
Intermetallic Mechanically alloyed Extrusion
powder process
Ball mill
Die assembly Hot rolling
Final product
Oxide
Figure : Schematic illustration of sequential steps in fabricating product from powders
using mechanical alloying routes

Ball Milling and Friction Consolidation 11

 Mechanism of Mechanical Alloying
❑ BALL-POWDER COLLISIONS
❖ Initial stage of processing
✓ It consists of loading blended powders with grinding medium and further subjected for heavy deformation
✓ While this process, particles of powder are flattened, cold welded, fractured and rewelded in repeated manner
✓ At initial state, due to collision of the grinding ball ductile material flatten and work hardened
✓ Due to severe plastic deformation, surface to volume ratio of powder particles increases and simultaneously ruptures
surface films of present contaminants (Figure 1).
✓ Apart from the cold welding of powders, some of the particles may also coated on grinding medium or inner walls led
to the development of thin layer that protect the grinding medium from wear and tear.

Initial stage

Figure: Ball-powder-ball collision of powder mixture while mechanical alloying

Ball Milling and Friction Consolidation 12

 Mechanism of Mechanical Alloying
❖ Intermediate stage of alloying processing
✓ In this stage, due to increase amount of cold working, number of crystal defects are present such as dislocations, grain
boundaries and vacancies. Finally, the particle converted into convoluted lamellae (Figure a).
❖ Final stage of alloying processing
✓ During this step, lamellae converted to finer and convoluted structure and the final composition of part almost like
starting of blend. This is referred as steady state.
✓ At this step, microhardness of the alloy achieves saturation level due to presence of higher strain energy.
Concentration of
Metal A Metal B
Interdiffusion

Meta stable phase

Dispersoids
Dispersoids Precipitate
phase Concentration of
Metal B Metal A
Intermediate stage Final stage

Ball Milling and Friction Consolidation 13

 Mechanism of Mechanical Alloying
❑ Evolution of particle size
✓ Newly created surfaces of particles from milling allow to weld together in weld condition led to increase in particle
size
✓ At the initial stage of milling, powder particles are soft on utilizing ductile to ductile or ductile to brittle material
combination
✓ Further continuing the deformation, particles are work hardened and fatigue fracture occurs
✓ Due to continuous impact of grinding ball, structure of particle get refined, but particle size remain same
✓ On milling for certain duration, steady-state equilibrium is achieved (balance between rate of cold welding) that
tends to increase average particle size.
✓ Due to presence of defects like vacancies, dislocations, stacking faults and increased number of grain boundaries
increase the probability of diffusivity of solute element into matrix.
✓ However time required to form a particular structure in any mechanical alloying system depends on initial particle
size and type of milling

Ball Milling and Friction Consolidation 14

 Mechanism of Mechanical Alloying
❑ Mechanical alloying during milling occurs utilizing three different
combination of metals and alloys:
Milling energy
Ball to Powder weight ratio ✓ Ductile to ductile products
Size

Lower temperature
✓ Ductile to brittle products
✓ Brittle to brittle products

Milling time (h)

Figure: Refinement of particle size with milling time.

Rate of refinement enhanced with increasing milling
energy, ball to powder weight ratio and lower
temperatures.

Ball Milling and Friction Consolidation 15

 Mechanism of Mechanical Alloying
❑ DUCTILE- DUCTILE PRODUCTS
✓ For the fabrication of product through this condition at least 15% of ductility need to achieve for alloying.
✓ Mechanism of alloying through this mode, involves two ductile components
✓ At initial state, ductile parts get flattened to platelet shape by micro forging of ball mills
✓ Flattened particles get cold welded and transform to composite lamellar structure
✓ On enhancing milling timing, composite powder work hardened and thus hardness and brittleness enhances
✓ With further milling, elemental lamellae of welded layer both coarse and fine particles convoluted due to random
cold welding of equiaxed particles
✓ Alloy formation occurs at this stage due to combination of reduced diffused distances (interlamellar spacing),
enhanced lattice defect density and heating effect arises from milling operation
✓ When hardness and particle size reach to steady state (hardness and particle size to saturation stage), on further
milling true alloying at the atomic level results in transformation of solid solutions, amorphous and intermetallic
phase.

Ball Milling and Friction Consolidation 16

 Mechanism of Mechanical Alloying
❑ DUCTILE TO BRITTLE PRODUCTS
✓ Conventional oxide dispersion strengthened (ODS) process lie in this category as the oxide particles (brittle in nature)
are dispersed in ductility matrix.
✓ At the initial step, ductile particles of powder get flattened due to ball-powder-ball collisions whereas, brittle oxide get
fragmented
✓ With progress of milling these particles occluded by ductile constituents and trapped in these particles
✓ On further milling, ductile powder get work hardened and transformation of lamellae to refine structure
✓ Continuing milling, lamellae further got refined, interlamellar spacing reduces and brittle particle uniformly dispersed

Oxide

Lamellae

Ball Milling and Friction Consolidation 17

 Mechanism of Mechanical Alloying
❑ BRITTLE TO BRITTLE PRODUCTS
✓ At the first step brittle-brittle parts get fragmented while milling and particle size reduced sequentially
✓ At very small size further reduction is not possible, hence powder particle behave in ductile nature referred as limit
of comminution i.e. the reduction of solid material particle size by fracture via grinding
✓ On achieving the proper mixture of two components, further milling facilitates the alloying by diffusional process.
✓ Mechanism that contribute to transfer of material during processing of brittle parts include deformation of material
plastically due to :
❖ Hydrostatic stress state in powder facilitates by ball mill
❖ Micro-deformation in defect free volumes
❖ Surface deformation
❖ Local rise in temperature

Ball Milling and Friction Consolidation 18

 Mechanochemical Ball Milling
❖ Mechanochemical processing (MCP) or mechanochemical synthesis term implemented for powder processing in which
chemical reactions and transformation of phase occurs on the application of mechanical energy.
✓ MCP has been usually performed in high-energy mills (SPEX mills) and rarely in low energy mill
❖ Thermodynamic Aspects
✓ Mechanosynthesis analysis takes place according to the governing reaction
MO + R M + RO (MO = metal oxide, R = reductant)
✓ These solid-state reactions consists of the formation of product phase at the interface of component phase
✓ Hence in above reactions, formation of metal M takes place at the interface of MO and R (Figure 1)
✓ Subsequently, enhancement of product phase consists diffusion of atoms of reactant phase that primarily control the
reaction rates.
✓ Mechanical alloying substantially enhance the reaction kinetics as the repeated cold welding and fracture of powder
particles increases the contact area by continuously bringing new surface

Ball Milling and Friction Consolidation 19

 Mechanochemical Ball Milling
❖ Depending on conditions of milling, two entirely different kinetics are possible:
✓ Reaction may approach to very small while each collision led to gradual transformation
✓ If the enthalpy of reaction is very high, self-propagating high temperature synthesis (SHS) (referred as combustion
reaction) can take place.
▪ In ductile-brittle components, microstructural morphology consists of dispersion of brittle oxide particles in
ductile matrix. Hence, intimate contact develops. Consequently, if both oxides and reductant are hard and brittle
then agglomerates of reactant does not develop and hence combustion will not initiate.
▪ During mechanical alloying of mechano-chemical process, powder is in close contact with the milling tools, hence
generated heat is lost partially to the ball and environment. Hence, the preheating of part is required to initiate the
combustion reaction.
▪ Finally, the removal of unwanted parts from product is difficult owing to the high reactivity of metallic phase
associated with nanocrystalline grains.
▪ Hence the by-product phase can be separated by leaching in dilute acid or hot water.

Ball Milling and Friction Consolidation 20

 Mechanochemical Ball Milling

MO

M(+RO)

Figure 1: Schematic illustration of chemical reaction takes place between two parts – metal oxide (MO) and reductant
(R) in mechanochemical reactions. Product phases (M and RO) form at interface between reactants and prevent further
reaction takes place, since reactants are not in contact.

Ball Milling and Friction Consolidation 21

 Mechanochemical Ball Milling
❑ Effect of attributes on Mechanochemical processing
❖ Process parameters of milling process play a significant role on nature and kinetics of product phase obtained from
displacement reactions. Optimum conditions must be achieved for initiation of chemical reaction using following attributes:
➢ Milling temperature
✓ If both reactants are in solid state, enhanced diffusivity at higher level of temperature, increases the kinetics of
reaction and subsequently shorter time required for completion of reaction.
➢ Ball to powder weight ratio
✓ Time required for reaction to complete reduced with enhancing the BPR as the ignition time (tig) decreases with
increasing average frequency collisions.
➢ Process control agent (PCA)
✓ Utilization of PCA as an additive restricts interparticle cold welding while collision led to reduce the reaction rate
➢ Grinding ball diameter
✓ Ignition time (tig) for combustion reaction reduced with increasing ball diameter

Ball Milling and Friction Consolidation 22

 Friction Consolidation
❑ Consolidation
✓ It is a process of enhancing the mechanical strength of material obtained from particle-to-particle interactions
❖ Different process of consolidation
➢ Cold welding
✓ When particles of the two surfaces are close enough so that their free surface energies led to strong attractive
forces referred as cold welding.
➢ Fusion bonding
✓ Multiple point of contacts created on application of point load produces heat that led to fusion or melting. On
removal of load, solidification takes place and finally mechanical strength enhances.
❖ Consolidation mechanism
➢ Mechanical theory
✓ It takes place between irregular shape of particle. As the particle undergo deformation, particle
boundaries at the edge of the boundary bond formation takes place.

Ball Milling and Friction Consolidation 23

 Friction Consolidation
❑ Frictional consolidation (FC)
▪ In first stage alloy powder is manufactured by mechanical alloying using dry, high-energy and milling process in an attritor.
▪ Second stage is to consolidate mechanically alloyed powder by friction consolidation or by hot isostatic pressing.
❑ Different component of frictional forces while consolidation:
➢ Interparticulate friction
✓ Occurs at particle/particle contacts and expressed in term of coefficient of interparticulate friction (𝜇𝑖 )
✓ More significant at lower applied loads
✓ Materials utilized for reducing these effects are known as glidants e.g. colloidal silica
➢ Die wall friction
✓ Obtained from material being pressed against die wall and moved down it
✓ This component of force dominant on application of higher amount of external load and expressed in terms of 𝜇𝑤
✓ Lubricants (Magnesium and stearate) designed for reducing component of forces in such a way that it has low
shear strength and strong cohesiveness.

Ball Milling and Friction Consolidation 24

 Case Studies on Friction Consolidation of INCOLOY alloy Powder
➢ In this study INCOLOY alloy (iron-chromium-aluminum alloy) ODS powders have consolidated through friction
consolidation and its impact is analyzed and compared with conventional material
✓ While consolidation process, sample obtained from ball milling subjected to tortional straining under hydrostatic
loading
✓ Key components for frictional consolidation consist of stationary billet chamber and rotating die. Chamber fabricated
material: Inconel 720 super alloy and rotating die made up of Tungsten-Rhenium. Compressive force

✓ Heat generated due to friction and plastic deformation of material led to Torque
Die
softening of material.
✓ Because of undergoing rotation and compression, gap between the particles are
reduced and finally the soften particles are cold welded and consolidated
✓ Refined grained structure with low porosity have been achieved to fabricate
ODS material. Backing plate
Figure: Schematic of friction consolidation

Ball Milling and Friction Consolidation 25

 Case Studies on Friction Consolidation of MA956 Powder

✓ Wider range of grain sizes present at different location within friction consolidated sample as compared to the conventional
material
✓ Perception of Y-Al-O (Yttrium aluminum garnet) was achieved (helpful for enhancing mechanical strength) by frictional
consolidation that was absent in conventional material.

Figure : Micrograph and EDS spectra of Y-Al-O elements in frictional consolidated and congenitally
consolidated (Catalini et al. 2013, Journal of nuclear material).

Ball Milling and Friction Consolidation 26

Thank you
for your kind attention

Ball Milling and Friction Consolidation 27