Introduction to Powder Metallurgy and

Powder Manufacturing
Powder Technology-MM6521

Debasis Chaira

Department of Metallurgical & Materials Engineering

1
National Institute of Technology Rourkela
Why Powder Metallurgy ?

• Higher raw material utilization

• Low energy requirement
• Near net shape (no machining cost)
• Low temperature processing

2
Powder: A finely divided solid, smaller than 1 mm in its maximum
dimension.
Characteristics of powder:
• High surface area to volume ratio
• The particles exhibit behavior that is intermediate between that of a solid
and a liquid.
• Powders will flow under gravity to fill containers or cavity (behave like a
liquid).
• Powders are compressible like a gas. But the compression of a metal
powder is irreversible, like the plastic deformation of a metal.
Powder metallurgy: it is the study of the processing of a metal powders,
including the fabrication, characterization, and conversion of a metal
powders into useful engineering components. 3
• Fabrication of difficult to process materials.
• Synthesis of non-equilibrium materials such as amorphous, micro-crystalline or
metastable alloys
• Processing of complex parts.
• Economic production of specialty alloys, typically composites containing mixed
phases.

4
• High volume production of precise, high quality structural parts from ferrous alloy. 5
This is a modern way of producing metal
part to exact sizes by blending elements or
metal powders together.

The powders are then compacted in a die

(like a mould) and heated in a sintering
furnace to bond the particles.

The process of powder metallurgy includes

blending, mixing, pressing and sintering.

6
There are many advantages:
• It can be used to make parts that are very
difficult to machine like gears very
accurately
• The surface finish after Powder Metallurgy
is complete is very smooth and shiny and
so doesn’t need work to file or smooth the
parts
• It requires relatively low processing
temperatures.
• It produces a uniform microstructure.
• There is no waste, so materials are used
efficiently.
• Components of refractory or high
melting point materials can be easily
7
manufactured without melting.
Powder metallurgy processing

8
Basic steps in powder metallurgy

9
Processing Steps of Powder Metallurgy

10
 Applications of Powder Metallurgy
• The modern era of powder metallurgy is Tungsten lamp filaments
traced to Coolidge who used tungsten Armor piercing projectiles
powder to develop a durable lamp filament Electrical contacts
for Edison (1910) Jet engine components
Tungsten Light bulb Filament: Cutting tools
500 hrs at 2500C Heating elements

1 kg of tungsten powder produces

1,50,000 filaments for 40W bulbs
15 mm

• Cemented carbides, porous bronze bearings,

and copper-graphite electrical contacts (1930’s)
• Fabrication of new tungsten alloys and
refractory metals (1940’s) Anti-armor projectile
Powder Metallurgy in Automobile

12
Automobile parts manufactured by PM: a) oil pump parts, b) transmission parts

Automotive connecting rod

manufactured by hot forging.
Composition: Fe-2Cu-0.8C, UTS:
825 MPa, YS: 550 MPa

Connecting rod 13
 The brake pad manufactured by PM:
Parts manufactured by PM: a) distribution pulleys, b) photo image
fuel pump parts
• The material is a mixture of Fe,
graphite, Cu, Zn and Sn
(60Fe20Cu5Sn15C). MoS2 is also
added to improve lubricating
property. The mixture is sintered
at the temperature range of 700-
1000 C (LPS). The sintered
structures have a lower wear rate.
• Sintered PM brake pads have
Brake disk: a) Brake disk (weight: 8.44 kg), manufactured from gray lower wear rate, higher thermal
cast iron used in the sedan automobile, b) brake disc made of Al-SiC
composite material (weight: 3.32 kg) specially designed for the same
stability and insensitive to
automobile humidity changes as compared to
organic brakes.
14
Defense Applications: Tungsten Heavy Alloys (WHA)
High density tungsten heavy alloys (WHA) are
used for radiation absorption, kinetic energy
penetrators and aircraft wing weights.

• Composition of W based high density alloy:

85-98 % W- (2-7)%Ni-(7-8)%Fe and also
Kinetic energy penetrator (KEP)
Mo (4-16)% is added.
• Sintering temperature: 1465-1525 C (LPS)

• Long rod kinetic energy penetrator (KEP)

manufactured by LPS WHA alloy to defeat
armor.

15
 Biomedical Applications: Orthodontic Bracket
• The bracket is made of austenitic SS and is affixed to the tooth
surface using biocompatible adhesive and is used to align teeth by
applying constant stress. This component is made by powder
injection molding of SS powder which is subsequently sintered to
nearly full density.
• Gas atomized austenitic SS powder is mixed with thermoplastic
binder and injection molded into the oversized shape. Sintering is
Stainless steel orthodontic performed at 1325 C for 1-4 hours in vacuum or H2. The final
bracket made by powder
injection molding density is over 98 %, UTS-550 MPa, 25 % elongation with good
corrosion resistance.

• Ti-6Al-4V alloy, Ti, Co-Cr alloys, stainless steel

• Biocompatibility
• Good corrosion resistance

Porous platinum heart pacemaker

electrode (left), metallographic cross-
16
section (right)
 Limitations and Disadvantages
with PM Processing
• High tooling and equipment costs
• Metallic powders are expensive
• Problems in storing and handling metal powders
Examples: degradation over time, fire hazards with certain metals
• Limitations on part geometry because metal
powders do not readily flow laterally in the die
during pressing
• Variations in density throughout part may be a problem,
especially for complex geometries
 Methods of Powder Production
• The formation of a powder involves the delivery of energy to the material to create new
surface area.
• Important characteristics are process efficiency, energy content, type of feedstock and
possible source of contamination.
• The selection of one method over another method depends on understanding the process, its
economics, the resulting powder characteristics and how those characteristics match with
the intended application.

• Atomization- (i) Gas atomization (ii) Water atomization (iii) Centrifugal atomization
• Mechanical comminution- (i) Machining (ii) Milling (iii) Mechanical alloying
• Electrolytic fabrication technique
• Chemical fabrication technique:
(i) decomposition of a solid by gas
(ii) Thermal decomposition

18
 Methods of Powder Production
• The microstructure, bulk and surface properties, chemical purity, porosity, shape,
and size distribution of the particles depend on the method used.
• Such characteristics significantly affect the flow and permeability during
compaction and in subsequent sintering operations.
• Particle sizes produced range from 0.1 to 1000 μm.

Particle shapes in metal powders, and the processes by which they are produced. Iron powders
are produced by many of these processes. 19
 Atomization
• Commercial atomization units operates as high as 400 kg/min.
• Atomization provides the majority of metal powders.
• Both elemental and pre-alloyed powders are formed by such processes.
• It is attractive because of the applicability to several alloys and easy process control.

 Atomization produces a liquid-metal stream by injection molten metal

through a small orifice.

 The stream is broken by jets of inert gas or air  gas atomization or
water atomization.

 The size and shape of the particles formed depends on the temperature of
the molten metal, rate of flow, nozzle size, and jet characteristics.

 Gas atomization usually results in more spherical particles.

 The liquid metal stream is disintegrated by rapid gas expansion out of a

nozzle. 20
 Gas atomization
• The high velocity gas emerging from the nozzle
creates a siphon, pulling molten metal into the gas
expansion zone.
• A high gas velocity aids breakup of the mold,
giving a fine spray of molten droplets. During
flight through the collection chamber, the droplets
lose heat and solidify.
• For high temperature metals, a closed, inert gas-
Horizontal gas atomization
filled chamber is used to prevent oxidation.
• Gas atomization is capable of • In horizontal gas atomizer, large filter area retains
production rates as high as 100 the powder while allowing gas to escape.
Kg/min.
• Atomization technique is applied to
produce powder of Al, Ni, Mg, Co,
Pd, Cu, Fe, Au, Sn, Zn and Be.
21
 Vertical gas atomization

The formation of a metal powder by gas atomization involves

the break-up of the liquid stream by rapidly expanding gas.
Because of suction pressure in the gas expansion zone, the
stream first forms into thin hollow sheet, and subsequently
forms ligaments, ellipsoids and spheres.

• It is important to exhaust the gas to avoid a back pressure.

• In vertical gas atomization, cyclone separator is incorporated for gas exit (possibly
recycling) while leaving behind the fine particles.
• The particle shape is spherical with a fairly wide size distribution.
22
 Salient features of gas atomization
• Gas atomization can be performed under
totally inert atmosphere, maintaining the
integrity of high alloy feedstock.
• The particle shape is spherical with a fairly
wide size distribution.
• Atomization process has large number of
process variables:
 Gas type
 Alloy type
 Residual atmosphere
 Melt temperature
 Gas pressure
 Gas velocity
 Gas feed rate
 Gas temperature
 Nozzle temperature 23
The liquid melt stream breaks into a sheet Ligament diameter =
and eventually droplets. The final particle
size will depend on the ligament diameter.

Where m is the melt density

 is the surface energy
W is sheet thickness
V is gas velocity

Effect of particle size on atomization

24
pressure and melt temperatures. (Ignoring the end effects)
Poor control
Gas Atomization
Splats, agglomerates and Controlled flow conditions
satellites (free of satellites)

• The turbulence and

mixing near the nozzle
will cause fine particles
to re-enter the gas
expansion zone.
• The solidified small
particles are carried
into the flight path of
the molten large
droplets, resulting in
agglomeration and
satellites.
• The elimination of
satellites is important
for good packing and
flow attributes.
25
 Centrifugal atomization • Centrifugal atomization is essentially used to
prepare powder of controlled shape and size
from reactive metals.
• Used for reactive metals and alloys like Zr, Ni
and Ti superalloys.
• A consumable electrode is rotated rapidly
(about 50,000 rev/min) in a helium-filled
chamber. The centrifugal force breaks up the
molten tip of the electrode into metal
particles.
• The centrifugal force throws off the moten
metal as a fine spray which solidifies into a
powder.

26
Spherical steel powder produced by centrifugal atomization
Effect of parameters in centrifugal atomization

• Smaller particles are generated with faster rotation rates, larger rotational diameter and
lower surface energy liquid.
• During flight, the ligaments pinch into droplets and eventually form spheres.
• If there is insufficient superheating, solidification will form ligamental particles before
spheroidization.
• Generally, the particle shape is spherical and an average particle size of 250 µm is 27
common.
 Water atomization
• High pressure water jets are directed against
the melt stream, forcing disintegration and
rapid solidification.
• The water can be directed by a single jet or
multiple jets.
• The powder shape is irregular, rough with
some oxidation due to rapid cooling.
• Typical mass flow rates are about 5 kg of
water for every kg of metal powder.
• Chemical segregation within an alloy particle
is limited since the particles solidify rapidly.
Schematic diagram of water atomization• Synthetic oils or other nonreactive liquids can
be used instead of water to gain better control
• Water has a much lower
of particle shape and oxidation.
compressibility and higher density • Pressure is the main process control variable
than gas, hence distance between in water atomization.
water exit from the nozzle and • The nozzle-to-melt distance is less of an
impact with the melt stream is a influence in water atomization than gas
secondary factor atomization. 28
Various mechanisms of powder production by
water atomization
A high pressure or high water velocity, causes a
decrease in the mean particle size (D).
 is a constant which
incorporates both material and
atomizer design effects.
P is the atomization pressure
V is water velocity
 Is the angle between the melt
stream and the water nozzle
K, n are constant

29
 Comparison of atomization techniques

Process Size range, µm Particle shape Size distribution Cost

Gas atomization 15-300 Rounded, moderate moderate
spherical
Water 5-800 Irregular, nodular wide low
atomization
Centrifugal 200-600 spherical bimodal high
atomization

30
Methods of Powder Production-
Reduction

31
 Metal powder production by
reduction
• If the partial pressure ratio is
above the equilibrium line, then
pure iron is stable and oxide
reduction will occur.
• If the partial pressure ratio falls
below the equilibrium line, then
oxide is stable; below 560 C the
stable oxide is Fe3O4, while above
the temperature the stable oxide is
FeO.

Thermodynamics:
32
Partial reduction of an oxide
particle to form metal powder

The dependence of 50 %
reduction time of NiO by H2 33
with temperature
 Methods of Powder Production-
Electrolytic deposition
– Utilizes either aqueous solution or fused salts.
– The powders produced are among the purest
available.

34
 Electrolytic fabrication technique
• Metal powders of high purity can be
prepared by this technique.
• Example: Pd, Cu, Fe, Zn, Mn and Ag.
• Only elemental powders are practical.
• Contaminants can hinder the formation and
deposition of powders at the cathode.

• An electrolytic cell operation of powder.

The raw material is dissolved at the
anode and deposited at the cathode. The
external voltage drives the deposition
process.
• After deposition, the cathode deposit is
SEM micrographs of electrolytic copper
washed, dried, ground, screened, and powders show typical sponge and dendritic
annealed to form a powder. shapes. 35
 Methods of Powder Production-
Carbonyls
– Metal carbonyls, such as iron carbonyl [Fe(CO)5] and
nickel carbonyl [Ni(CO)4], are formed by letting iron or
nickel react with carbon monoxide.
– The reaction products are then decomposed to iron
and nickel, and they turn into small, dense, uniformly
spherical particles of high purity.
– Metals like Cu, Cr, Pt, Rh, Au and Co are produced by
carbonyl processing.
– The high energy requirements and health hazards of
carbonyl molecules discourage extensive application
to metals beyond Ni and Fe. 36
Methods of Powder Production- Comminution
– Mechanical comminution (pulverization) involves
crushing, milling in a ball mill, or grinding of brittle or
less ductile metals into small particles.
– A ball mill is a machine with a rotating hollow
cylinder partly filled with steel or white cast-iron balls.
– For brittle materials, the powder particles produced
have angular shapes.
– For ductile materials, particles are flaky and not
suitable for P/M applications.
– There are four fundamental mechanical comminution
processes: impaction, attritioning, shearing and
compression.
37
Various grinding equipment used for powder
production

Dual drive planetary mill

Planetary mill

• Planetary mill is used for preparation of fine powder

• Mixing two/more powder particles
• Used for preparation of nanoparticles
• Used for mechanical alloying to produce alloy in solid state 38
 Attritor mill Laboratory scale ball mill

• There are four fundamental mechanical comminution process: Impaction, attritioning,

compression and impaction
• These four forces are often combined to form metal powder

39
 Problems
1. Cast iron machining chips of 300 m initial particle size are ball
milled to produce a powder with 110 m after 8 h. Calculate the
additional time required to bring the particles to a size of 75 m.

2. The total work needed to mill a brittle material is proportional to the

inverse square root of the particle size. What is the relative difference
in required energy to form a 10 m and a 1 m powder?

40
 Mechanical alloying
• Mechanical alloying (MA) is a powder
processing technique that allows
production of homogeneous materials
starting from elemental blended powder
mixtures.
• MA was introduced in 1960 by INCO to
produce Ni base super alloys for gas
turbine applications.
• Such alloys have high temperature strength
where fine oxides are dispersed.

Process variables
• Mill type Ball-powder-ball collision of powder
• Mill speed mixture during mechanical alloying
• Milling time
• Ball to powder weight ratio (BPR)
• Grinding media
• Vial filling
• Process control agent

41
 Mechanism of mechanical alloying
Ductile-ductile components • Ideal combination of materials for mechanical
alloying.
• It is necessary to have at least 15 % ductile
component for alloying.
• True alloying occurs by the action of repeated
cold welding and fracturing of powder
particles. Cold welding will not occur if ductile
component is absent.

SEM micrograph of convoluted

lamellar structure obtained during
milling of ductile-ductile
components (Ag-Cu) 42
 Ductile-brittle component

Microstructural evolution during milling of a ductile-brittle combination of powders.

This is typical of an oxide dispersion strengthened case (ODS alloy).
• Ductile component is flattened initially by ball-powder-ball collisions.
• Brittle oxide particles are fragmented and then trapped in ductile powder.

43
 Brittle-brittle component
• Comparatively less chance of alloying for such systems.
• Brittle particles are fragmented by milling
• During milling of brittle-brittle systems, the harder (more brittle)
component get fragmented and gets embedded into softer (less brittle)
component. Example: Si-Ge, Mn-Bi systems.

SEM micrograph of Si-Ge

mixture.
Harder Si particles are
embedded into softer Ge
particles.

44
 Machining
• Coarse powder with an irregular shape powders are
produced by machining where shear force is predominant.
• The large amount of machining scraps produced in
metalworking operations are abundant source of powder.
• Lack of control over the powder characteristics, like
chemical contaminants, oxygen ,oil and other metals is a
disadvantage.
• Machining is not first choice for powder production,
proves inefficient and slow.
• Further milling is required for refining the powders.

45
Powders produced by various techniques
(a) Tellurium, milled, accicular
(b) Iron alloy, argon atomized, spherical
with agglomerated fines
(c) Tungsten, gas reduced, polygonal
aggregates
(d) Tin, air atomized, rounded and
ligamental
(e) Iron alloy, centrifugal atomization,
spherical
(f) Tin, splat quenched, flake

46
Powder of various morphologies
(g) Stainless steel, water atomized,
rounded and irregular
(h) Palladium, electrolytic, sponge
(i) Nickel, carbonyl decomposition,
porous and cubic
(j) Iron-based metallic glass, crushed
ribbon, angular plates
(k) Titanium, reduced and milled, irregular
(l) Niobium hydride, milled, angular

47
Methods of producing various metal powders

48