Why Powder Metallurgy is Important?

• PM parts can be mass produced to net shape or near net shape, eliminating or
reducing the need for subsequent machining

• PM process wastes very little material - about 95% of the starting powders
are converted to product

• PM parts can be made with a specified level of porosity, to produce porous

metal parts − Examples: filters; oil-impregnated bearings and gears

• Certain metals that are difficult to fabricate by other methods can be shaped
by powder metallurgy − Example: Tungsten filaments for incandescent lamp
bulbs are made by PM

• Certain alloy combinations and cermets made by PM cannot be produced in

other ways

• PM compares favorably to most casting processes in dimensional control

• PM production methods can be automated for economical production

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
 Basic steps of the Powder Metallurgy Process
Powder size: 0.1 to 1000 μm
METAL POWDER PRODUCTION
The significant manufacturing methods may be classed as:

1. Physical methods

2. Chemical methods

3. Mechanical methods
METAL POWDER PRODUCTION ……contd.

1. Physical methods
Atomization
Gas atomization
Water atomization
Liquid gas atomization
Centrifugal atomization
Vacuum atomization

Electrolytic Method
METAL POWDER PRODUCTION ……contd.

2. Chemical methods
Chemical Reduction
from the solid state
from the gaseous state
from the aqueous solution

Chemical Decomposition of Compounds

Decomposition of metal hydrides
Decomposition of metal carbonyls
METAL POWDER PRODUCTION ……contd.

3. Mechanical methods
Crushing

Milling in a ball/rod/attritor mill

Mechanical Alloying
 CERAMIC POWDER PRODUCTION
Solid phase Liquid phase Gas phase Miscellaneous
reactant reactant reactant synthesis
Solid state reactant Precipitation Evaporative Solvent removal
•Solution heating or condensation •Spray drying
cooling •Freeze drying
•Evaporative •Spray roasting
salting out
•Chemical reaction
with insoluble
product
Thermal Hydrothermal Gas phase reaction Sol-gel synthesis
decompositions of a synthesis with solid product
solid •Forced insolubility •Thermal
Oxidation or •Dissolution decomposition Melt solidification
reduction of a solid reprecipitation •Oxidation or
reduction
•Combination
reactions with a
solid product
 Atomization
Atomization refers to the process of breaking up bulk
liquids into droplets

Atomization: process of breaking up liquids into droplets

Spray: collection a variety of sizes of fluid droplets moving in a
controlled fashion
Atomization: mechanisms of Particle disintegration
WATER GAS

(a) Stable sheet;

(b) Growth of sinus waves sheet
(c) Ligament formation
(d) Ligament breakdown
 Atomization
Water Atomization Gas Atomization

316L steel powder

GA –LC atroalloy
Microstructure after sintering of 316L powder
Water Atomization Gas Atomization
 Atomization: factors influencing
Fine particle sizes are favoured by:
(a) Low metal viscosity
(b) Low metal surface tension
(c) Superheated metal
(d) Small nozzle diameter, i.e.
low metal feed rate.
(e) High atomizing pressure
(f) High atomizing agent volume
(g) High atomizing agent velocity
(h) High atomizing agent viscosity
(i) Short metal stream (F)
(j) Short jet length (E)
(k) Optimum apex angle ()
 Atomization: factors influencing

Sphericity of a metal powder is favoured by:

(a) High metal surface tension
(b) Narrow melting range
(c) High pouring temperature
(d) Gas atomization, especially inert gas
(e) Low jet velocity
(f) Long apex angles in water atomization
(g) Long flight paths.
 Centrifugal Atomization

Ultrasonic Atomization

Electrostatic Atomization
 Advantages of atomization
1. Freedom to alloy
2. All particles have the same uniform composition
3. Control of particle shape, size and structure
4. Higher purity
5. Lower capital cost.
 Electrolytic Method
It is used extensively in the preparation of copper, beryllium, iron and nickel powders.
Adjustment of the chemical and physical conditions during electrodeposition makes it
possible to cause the metal to deposit loosely on the cathode of the cell either as a light
cake or in flake form. Both are readily crushed to a powder. The method yields a high
purity metal with excellent properties for conventional powder metallurgy processing.

The following are the factors promoting

An electrolytic cell for the deposition of metal
powder.
powdery deposits:
(a) high current densities;
(b) weak metal concentrations;
(c) additions of colloids and acids;
(d) low temperature;
(e) high viscosities;
(f) avoidance of agitation;
(g) suppression of convection.

Thickening of the electrolyte lowers the rate of ionic diffusion. As a result, the supply of
metal ions to the cathode is hampered and as a consequence, the powder begins to form at
high current densities (predominant factor).
 Electrolytic Method: Cu production

The electrolytic process for copper powder is similar to that in copper refinery.
However, instead of using impure cast copper anodes, electrolytically refined
copper anodes are used. The cathode is generally cast antimonial lead. The
electrolyte concentration is 50 g/l of CuSO4· 5 H2O (in contrast to 150 g/l for
refining) while the current density is 535 A/m2 (in contrast to 107–215 A/m2 for
refining). CD cathode: 600-4000 A/m2
Bath voltage ~ 1-2 V; H2SO4 150-250 g/l
Typical properties of electrolytic powders, as
influenced by the conditions of electrolysis

Electrolyte composition:
 Copper ions concentration: 5 g/l
 Sulphuric acid concentration: 160 g/l
 Cathodic current density: 0.3 A/cm2;
 Electrolyte flow rate: 0.17 l/min;
 Time of powder removal (deposition time
after which the powder is removed by brush or
by tapping): 60 min;
 Temperature: (50±2)C
 Chemical Methods
Chemical Reduction
-from the solid state: The production of iron, copper,
tungsten, and molybdenum powders from their respective
oxides are well-established commercial processes.

Höganäs process: Production of Fe-powder by direct reduction

using C- The Höganäs process uses pure magnetite (Fe3O4) ore
found in northern Sweden, which has an iron content of
approximately 71.5% after beneficiation by grinding and
magnetic separation.
Höganäs process
 Pyron process

Pyron process uses mill scale taken from steel mills that produce
plain carbon steel products, such as sheet, rod, wire, plate, and
pipe. Mill scales containing alloying elements other than manganese
are not used.
 Höganäs process Pyron process

Scanning electron
Crossmicrograph of particles
sectional view of iron powders
of iron powders
 Chemical Reduction -from the solid state

Process Variables:
The most important process variable is the reduction temperature.

Low reduction temperatures result in powders possessing fine

pores, large specific surface areas, and high green strength.

High reduction temperatures (>0.6 Tm) produce large intra-

particle pores and small specific surface area powders that exhibit
high compressibility.

Extremely low reduction temperatures (<0.3 Tm) can readily

produce pyrophoric powder.

High temperatures can cause excessive sintering and

agglomeration, which lead to difficulties with the breakup of the
sinter cake.
 Chemical Reduction -from the solid state
With tungsten and molybdenum, oxide reduction is used partly for
economic reasons, because the melting points of these metals are very
high. Reduction processes, which use hydrogen as the reducing
medium, are similar for both tungsten and molybdenum oxides.

For molybdenum trioxide, however, reduction is performed in two

stages to control particle size. Due to the high vapor presence of
molybdenum trioxide, the first step is carried out at 600 to 700 °C
(1110 to 1290 °F).

The second step, the reduction of molybdenum dioxide to molybdenum

monoxide, is carried out at around 900 to 1100 °C
(1650 to 2000 °F).
Chemical Reduction
-from the gaseous state: reduction of titanium
tetrachloride vapour with molten magnesium – the well-
known Kroll process.

The commercial production of titanium metal involves the

chlorination of natural or synthetically produced rutile, TiO2, in
the presence of carbon. The resulting titanium tetrachloride is
reduced to metallic titanium by the Kroll process using
magnesium or by the Hunter process using sodium. Most of the
remnant chloride is removed by vacuum distillation or by water
leaching. The final sponge fines typically contain 0.12 to 0.15 wt%
Cl. The inherent chloride content of conventional sponge fines can
lead to incomplete densification and limited
fatigue properties.
-from the aqueous solution: Production of metal powders by
hydrometallurgical processing is based on leaching an ore or ore
concentrate, followed by precipitating the metal from the leach
solution.
The most widely used commercial processes based on
hydrometallurgy are copper cementation and the separation and
precipitation of copper, nickel, and cobalt from salt solutions by
reduction with hydrogen (Sheritt Gordon process).

Processing Conditions. For divalent ions, these processes consist

of precipitation from an aqueous source using hydrogen. The
basic concept is that a metallic ion such as nickel, copper, or
cobalt in the solution reacts with gas (hydrogen) by the following
reaction:
M2+ + H2  Mo + 2H+
or if the solution is ammoniacal:
M2+ + 2NH3 + H2  Mo + 2NH4+
Chemical Decomposition of Compounds
Decomposition of metal hydrides
This involves first hydriding the refractory metals like Ti, Zr,
Hf, V, Th or U by heating the metal in the form of sponge, chip
or turnings or even compact metal in hydrogen.

TiH2 is formed from titanium in the temperature range between

300–500oC.

These hydrides are quite brittle and can be readily ball-milled

into powder of the desired fineness. These may be dehydrided
by heating them in a good vacuum at the same temperature at
which the hydride was formed.

Care must be taken to avoid contamination of O2, N2 and C

during hydriding or dehydriding.
Chemical Decomposition of Compounds
-Decomposition of metal carbonyls
Carbonyls are obtained by passing carbon monoxide over
spongy metal at specific temperatures and pressures.
For example, iron carbonyl (Fe(CO)5) is formed at 70–200
atmosphere pressure and a temperature of 200–220oC.
Iron pentacarbonyl, Fe(CO)5, is a liquid at room temperature,
boiling at 103 °C (217 °F). Nickel tetracarbonyl, Ni(CO)4, boils
at 43 °C (109 °F).
When the pressure is reduced to 1 atm and the temperature is
raised correspondingly, both of these carbonyls decompose to re-
form the metal and carbon monoxide. The latter is recycled to
form more carbonyl and to continue the process. These reactions
are expressed as follows:
Fe + 5CO  Fe(CO)5
Ni + 4CO  Ni(CO)4