Full Density Powder Processing Techniques

Technology of full density powder
materials and products

Professor Jakob Kbarsepp
Institute of Materials Engineering
Tallinn University of Technology
1.
2.
3.
4.
5.
6.
7.
Introduction: full density processing

Hot pressing
Hot isostatic pressing
Sinter HIP
Powder extrusion
Powder forging
Alternative hot consolidation processes
1. Introduction: full density processing

Powder metallurgy (P/M) is
the most diverse
manufacturing approach
among various metalworking
technologies.
There are three main
reasons (see Fig.) for using
powder metallurgy - the art
and science of producing
powders and of utilizing
powders for the production
of massive materials and
shaped products
Introduction: full density processing (cntd. 1)
Influence of porosity
(density) on impact
strength and tensile
strength of P/M materials.

The effect of porosity on fatique strength

Permissible porosity depends on application
field
Higher loads call for higher density
Conventional P/M technology (press- and -sinter
technology) in most cases doesn`t enable to
achieve full density.
Hot consolidation processes (hot pressing, HIP,
extrusion etc) enable to produce full-density or
near full-density or near full-density powder
materials/products

High performance applications
require higher densities
The symbols are:
P/M = press and sinter
reP = press, sinter and repress
P/S+F = press, sinter and forge
CIP+S= cold isostatically press and sinter

HIP = hot isostatically press
HIP+F = hot isostatically press and forge
Three variables influencing P/M processing methods component size, density and performance (as a percentage of wrought

Challenge of P/M technology production of net-shape
(with final dimensions) and full density
materials/products
Utilizing full density processing the performance levels
can exceed (see Fig.) those associated with wrought
materials (if control is gained over defects, impurities,
microstructure and product homogeneity)
The density effect on the strength and ductility of a forged 4640 steel

Liquid phase sintering (LPS) is widely employed to obtain full density products
without application of simultaneus pressure during sintering.
Applications of LPS: W-Ni-Fe heavy alloys, WC-Co cemented carbides, TiC-Fe
cermets, Co5Sm-base magnets etc.
Infiltration other technique for obtaining full density (see section 7.9).
Phase diagram of an ideal

system for liquid-phase sintering
Typical microstructure of a liquid-phase sintering

and infiltration system

The traditional P/M cycle involves the sequential application of
pressure (to compact powder) and temperature (to sinter the
powder). Many full density processes involve simultaneous
heating and pressurization.
The simultaneous heating and pressurization add cost and
complexity that are best justified by increased performance.

The four concerns discussing hot consolidation of powders are:
1) Temperature: full density processing is normally effective at
T>0.5Ts (Ts melting temp.)
2) Stress: only full density does the effective stress at the
interparticle contacts equal to applied stress (because pores
act as stress concentrators)
3) Strain: large shear strains disrupt surface films on the
particles, but contribute to tool wear.
4) Strain rate:
high strain rate reduces ductility (fracture is more likely)
low strain rate gives more plastic deformation with a higher
final density

Three mechanisms of pore
elimination:
1)Plastic yielding occurs when the
effective stress exceeds the material
yield strength
2)Power law creep occurs when
both the stress and temperature are
high and rate of densification
depends on the diffusion rate for
dislocation climb
Initial and intermediate stages of densification for

spherical powders
3)Lattice and grain boundary

diffusion occurs when the
diffusivity is highly sensitive to
temperature and the temperature
has the most important influence on
the densification rate

Application fields of full density or near-full density powder
materials
Structural ceramics
High-temperature composites
Metal-bonded diamond tools
P/M high speed steel tools
Products from refractory metals
Products from Ni-base superalloys and corrosion
resistant alloys
Products from low-alloy steels etc.
2. Hot pressing
2.1 Process
Uniaxial hot pressing =
pressing on sintering
temperature
Uniaxial pressing in
graphite die at
pressures up to 50
MPa and temperatures
up to 2200C in
controlled atmosphere
(Ar, N2, vacuum)
Hot pressing (cntd. 1)

Hot pressing is the simplest
hot consolition technique:
Temperature:
up to 2200oC
Time: 13 hours
Pressure:
up to 50 MPa
Die material:
graphite, refractory
metals, ceramics

Mechanism of pore elimination
(compaction):
particle rearrangement and plastic
yielding/plastic flow (at point contacts)
grain boundary and lattice diffusion (as
densification progresses)

Hot pressing can be used for consolidation of different material
combinations:
single powders or powder mix
alternating layers of powders (for production of laminated
composites)
mix of powder and whiskers
powders + thin sheets of metal/ceramics
sheets of continous fibers with powders (plasma sprayed on
fibers)
powder cloth + fiber mats etc.
Depending on the material the lay-up sequence will vary
significantly.

2.2 Applications
1.
2.
3.
4.
5.
6.
Large parts/products from WC-Co hardmetals

Products from Be alloys in nuclear reactors, missile
and aerospace applications
Diamond-metal composite cutting tools (e.g
diamond+Co)
Micro Infiltrated Macro Laminated Composites
MIMLC
Fiber-reinforced materials
Sputtering targets for deposition of thin films etc.

Ceramic materials are characterized by extremely low fracture
toughness. Efforts to improve the toughness include:
Incorporation of particulates
Incorporation of whiskers or fibers
Cermet (ceramic/metal composite) technology in which the tough

metallic component absorbs energy
Inclusion of a phase which undergoes tranformation due to the

stress field associated with a crack (transformation toughening).
Transformation leads to volume expansion producing compressive
stress on the crack tip
Utilization of the concept of compositional gradient MIMLC-type

materials

Improved toughness of ceramic materials and composites
can be attributed to:
crack branching and crack deflection
crack bridging (e.g in cermets where metal matrix
ligaments effectively bridge the macroscopic crack plane)
fiber of whiscers matrix decohesion and pullout
(e.g in fiber/whiscers reinforced ceramic matrix

composites)
plastic deformation = one of the best mathods of improving
fracture toughess of a material
(e.g in MIMLCtype materials)

Conceptual MIMLC structure
Soft, ductile, low modulus

high toughness phase
Hard, brittle, high
modulus
low toughness phase
Schematic view of a conceptual MIMLC structure

MIMLC gradient material:
On a macro scale is laminated with alternating
layers of hard and brittle ceramic-like material
and ductile and tough metal-like layer
On a micro scale the ceramic-like material is
inter-penetrated with the ductile and tough metal
like material.

Improved toughness of MIMLC: can be attributed to:
Increased resistance (higher than that of

ceramic-metal composites) to fracture due to
energy absorbtion via plastic deformation
Crack bridging in plastic zone of a composite

Example of MIMLC:W-Ni-Fe grandient material
MIMLC: Al2O3-Ni grandient material

One of the prime uses
is material against:
ballistic penetration
hyper-velocity impacts

Hot pressing of Al2O3-Ni gradient material
MIMLC composite
lay up assembly
(for production of Al2O3-Ni
gradient material)

Schematic processing sequence for producing the fiber reinforced
glass and glass-ceramic matrix composite by hot pressing
1000oC, 300 bar

A typical stress-strain curve for fiber reinforced glass matrix composite

Hot pressing of composites by utilizing
displacement reaction synthesis:
Examples of in-situ synthesized
temperature) composites:
1)Mo2C + 5Si = 2MoSi2+SiC
in-situ
(high-
(MoSi2 based composite reinforced by SiC particles)

2) 4.5NiAl + 3NiO = 2.5Ni3Al + Al2O3, or
12NiAl + 3NiO = 7.5NiAl + 2.5Ni3Al + Al2O3
(Al2O3 reinforced Ni-Al composite)
3. Hot isostatic pressing (HIP)

3.1 Process
HIP = high-temperature
pressing (hot
consolidation) of
encapsulated powders or
sintered high-density
(density >92% of
theoretical) compacts.
Pressure: 100...300 MPa
Time: 2...6 hours
HIP-low strain rate
process because stress
rise in slow
Hot isostatic pressing (HIP) (cntd. 1)

Preparative steps of HIP:
1.
Encapsulation:
container production
leak testing
filling
2. Degassing (evacuation of absorbed
gases and moisture) and crimping of
the can

Typical HIP cycles:
I HIP in unit with internal heating zone
II HIP of externally heated encapsulated part

A cross section view of the HIP vessel

Recent developments of HIP equipment:
1. Increased Cooling HIP systems (providing

productivity and decrease in cost)
2. Ultra High Pressure and Temperature Systems
pressures up to 1000 MPa
Temperatures up to 3000C
3. Duplex systems for HIP, WIP, CIP (hot isostatic
pressing, warm isostatic pressing, cold isostatic
pressing)

Advantages of HIP:
1. Materials/products of higher performance

2. Cost savings because of
lower lifecycle cost (of higher performance
materials)
the HIP near-net shape process
lower unit costs of large parts and
production volumes of small-weight parts

Disadvantages of HIP:
little shear on the particle surfaces (because of

consolidation by hydrostatic stress). Therefore:
1)it is necessary (in some applications) to subject
HIP-compact to post-consolidation deformation
or
2)the microstructural defects can be minimized by
use of powders atomized with rapid solidification
rate and clean handling in inert gas

3.2 Mechanism of consolidation
Full density is
achieved more
easily under the
conditions of higher
packing density
Packing density of
commercial
spherical powders
vary from
0.62...0.72
Mostly pre-alloyed
powders are used

Two models of the HIP process
1. Microscopic model: calculates density as a function of the
process variables: time, pressure, temperature, initial packing
density, material properties. Model predicts density.
2. Macroscopic model: shape change under pressure is
analyzed utilizing plastic theory of porous metals.
Macroscopic models are tools to predict the size and shape
change (important in production of net-shape parts).

Microscopic model: three stages of consolidation process
0) stage of packing
density
1) stage of
connected
porosity
2) stage of closed
porosity

Microscopic model:
HIP maps (density vs
temperature maps) at
constant pressure and
initial packing density
Two mechanisms of
HIP densification:
(1)Plastic yielding
(2)Power-law creep (the
dominant mechanism
of densification)

Macroscopic model:
A comparison of the
predicted shape change for
axisymmetric product to the
actual shape change after
HIP

3.3 Application fields:
1. P/M tool steels:
high speed steels
cold work tool steels (0.83.9% C)
wear and corrosion resistant steels (1.73.7% C)
HIP/clad products (see section 7.10)
2. Ni-base superalloys
3. Corrosion resistant Ni- and Fe-based alloys
4. Titanium and titanium aluminide
5. Metal matrix composites MMC
6. Hardmetals and cermets etc.

Characterization of P/M tool steels:
Microstructure is characterized by fine and
evenly distributed carbides which improve
toughness, wear resistance, grindability,
workability
High-carbon (up to 3.9%) and high-carbidevolume (up to 45 vol%) steels
The largest tonnage application at about 12 000
tons worldwide
All of the P/M tool and high speed steels have:

fine and evenly distributed carbides
improved toughness and wear resistance
improved technological properties such as hot
workability, machineability (in annealed condition), more
uniform heat treatment response in large section,
predictable size change after heat treatment
Primary carbides in heat treated P/M T15 (left) and conventional T15 (right) high-speed
steels

HIP fabrication of metal matrix composites Ti/SiC
4. Sinter HIP
Disadvantages of HIP:
1)Encapsulation prior HIP-ing is as
expensive and time consuming step
2)Canning in most cases precludes the
fabrication of compex shapes
Sinter HIP techniques (Sinter+HIP,
Sinter/HIP or Sinter-HIP etc.) enable to
produce complex and net shape full
density products
Sinter HIP (cntd. 1)

4.1 Sinter + HIP
Both Sinter + HIP
and Sinter/HIP =
containerless
pressure-assisted
consolidation
technique of
sintered parts (with
porosity below 8%)

Different technological schemes of Sinter+HIP:
1.
2.
3.
4.
Sinter + HIP in different cycles

Sinter + HIP in the same cycle eliminating extra
sintering and cooling step
CHIP = CIP/Sinter + HIP
PIM/Sinter + HIP
where:
CIP cold isostatic pressing
PIM powder injection molding

Sinter + HIP of Ti-alloys
The main advantages of Sinter+HIP technology are:

possibility to produce complex and near net shape
products
possibility to achieve full density
The most widely used process for consolidation of complex
in shape products are :
1.
2.
CHIP = CIP + Sinter + HIP

PIM/Sinter + HIP = PIM + Sinter + HIP
The first stage of

PIM/Sinter + HIP
process, where:
PIM powder injection
molding

4.2 Sinter/HIP or Sinter-HIP
1.
Sinter / HIP = pressure

assisted
sintering/overpressure
sintering
2.
The main difference

betweenSinter+HIP in the
same cycle and
Sinter/HIP:
use of substainally
lower (almost an order
of magnitude) gas
pressure
the requierments of the
equipment are less
demanding

Advantages of Sinter/HIP (Sinter-HIP) as against
conventional HIP:
1)Elimination of both containerization and
separate sintering cycle
2)Pressure (5-15 MPa) is generally an order of
magnitude lower
3)The requirements of the equipment are less
demanding and therefore the cost of lowpressure equipment is lower

Sinter/HIP process is preferable for production of low-cobalt alloys of
medium grain size (2m)

Sinter + HIP process is preferable for low-cobalt alloys of fine grain size (<1m)

Industrial Sinter/HIP cycle

Applications of Sinter/HIP:
1. Hardmetals (cemented carbides)
2. Composites (MoSi2+Al2O3)
3. P/M tool steels
4. P/M stainless steels
5. Si3N4 based structural ceramics
6. Complex shapes utilizing
CIP+Sinter/HIP and PIM+Sinter/HIP

4.3 Pulsed Sinter/HIP
Time-temperaturepressure profile of the
Pulsed Sinter/HIP:
1. Thermal Spike HIP
2. Pressure Spike HIP
5. Powder extrusion
Powder extrusion mechanics
Powder extrusion: high-temperature consolidation at high
strain rates and high stresses.
Three main groups of
processes:
1 loose powder
extrusion
2 extrusion of presintered powder
compacts
3 extrusion of
encapsulated powders
Powder extrusion (cntd. 1)

Conventional processes of extrusion are:
- extrusion of pre-compacted and pre-sintered compacts
(e.g Fe-based materials high speed steels)
- extrusion of encapsulated powders (refractory and
reactive powders)
Specific feature of extrusion: powder partides are
subjected to high shear and deformation helping braking
up oxide skin and promting nascent particle-particle
contact (the major adventage over HIP)
Extrusion pressure (for wrought

and particulate material):
P K ln R
where
K extrusion constant for the

material (combines flow
stress, friction, temperature,
material properties etc into
one parameter) decreases
with increasing temperature
Si
Sf
- extrusion ratio
(reduction ratio)
must exceed 10
for adequate
densification

Special processes of powder extrusion:
duplex extrusion (co-extrusion)
multi-temperature extrusion
extrusion of composites in semi-solid (mushy) state
extrusion with changing direction of powder flow
extrusion using low extrusion ratios

Special process of extrusion duplex extrusion (co-extrusion) is a process which
results on one material forming a layer on another over the entire length of the
final product (e.g tube on rod).
Special process of extrusion multi-temperature extrusion for good proportional
co-reduction.
Examples are:
co-extrusion of Cr (1300C) and steel (1050C)
co-extrusion of UO2 (2000 C) and steel (700C)
Multi-temperature
co-extrusion
of chromium and steel

Special process of powder extrusion:
extrusion of composites in the semi-solid
state (mushy state extrusion).
Pecularity: liquid phase fraction 1030 vol %
decrases extrusion pressure (flow stress)
markedly.
Example: metal matrix composites (MMC-s)

Special process of powder extrusion: extrusion with
changing direction of powder flow
1 conventional extrusion
2 single shear extrusion
3 double shear extrusion

Extrusion with changing direction of powder flow aims to eliminate the problem
of in homogeneous shear in the conventional extrusion
The total shear deformation in the double shear extrusion process can be
expressed (see Fig.)
Ttotal = V2/V1 + V3/V2 = S1/S2 + S2/S3

where S1/S2 and S2/S3 represent the extrusion ratio for zone 1 and zone 2,
respectively
Schematic of the deformation in double

shear extrusion

Special process of powder extrusion:
extrusion using low extrusion ratios

Applications:
1. Intermetallic compounds (Ti3Al, Ni3Al etc.)
2.
3.
4.
5.
6.
Cu-based alloys
Ni-based alloys
W-based alloys
P/M high speed steels
Oxide dispersion hardened (strengthened)
alloys etc.
6. Powder forging
The role of final density of pure iron on the mechanical properties (tensile
strength, elongation, impact resistance).
Powder forging offers a process for producing parts with very high densities.
Powder forging (cntd. 1)

Different hot powder forging techniques:
1. Powder forging
(powder upsetting)
2. Powder repressing
3. Superplastic
forming of powders
The powder forging is very similar to conventional hot forging.

The major difference preform is particulate material.

Differentiation between two schemes:
Powder forging:
high strains
better structure, good
mechanical properties
high die wear
Powder repressing:
low strains
more defects, not
optimal mechanical
properties
low die wear, more
complex shapes
The main mechanism of pore elimination (compaction) plastic yielding

(plastic flow)
There take place changes during powder forging in:
density (porosity)
rate of work hardening (increasing with the porosity (see Fig.))
Poisson`s ratio (0.30.5)
Compressive deformation of
porous iron with various initial
porosities

The pore collapse in forging is significantly different from
that encountered under the hydrostatic conditions (HIP)
The difference in pore collapse contributes to more shear
and bonding in powder forging (as against HIP)
Pore collapse in powder hot forging and hot isostatic pressing (HIP)

Height strains >50% ensure:
pore elimination
good interparticle bonding (due to disintegration of oxide films during
shear)
The preform and forged height to diameter ratio (H/D) showing the region of high
densification without fracture

All mechanical characteristics except ductility (hardness, yield strength,
dynamic properties) of powder forged materials are often superior to
wrought products
Inclusions seriosusly degrade properties in spite of full density (see Fig.)
The effect of oxigen inclusions on the impact toughness of full-density 4340

steel processed by powder forging

Features of powder forging:
a) powder forging in trap die
(to net shape) tight
control of preform mass is
important
a)
b)
b) conventional forging in
an impression die with
flash large variations of
the mass of preform is
permitted

Stages of powder forging process:
(a) powder fill
(b) pressing
(c) ejection of preform
(d) preheating (in
controlled
atmosphere)
(e) powder hot forging (in
controlled
atmosphere)

Superplastic forming:
Superplasticity ability of particular

material under certain conditions to
undergo extraordinary high tensile
elongations. This phenomenon occurs in:
metals/alloys
intermetallic compounds
glass ceramics
ceramics

Powder superplastic forging (superplastic forming)
One of preconditions of superplastic forming

structural superplasticity (relies on microstructure)
Requirements of structural superplasticity:
1. Ultra fine (stable during the process) grain size
(metals < 10m, ceramics < 1 m)
2. Deformation temperature T > 0,5 TS
3. Low strain rates (102...10-6); high strain rate
sensitivity

Superplastic forming:
Important factor for superplastic
forming strain rate sensitivity (=
resistance to necking):
Flow stress:
=Km
where
m strain rate sensitivity exponent
(in superplastic condition m>0.3)
Strain rate sensitivity exponent m vs
temperature for the superplastic
forming of ultra high carbon steel
(UHC)
strain rate
K material and structure constant

Changes on grain structure before and after superplastic
forming and conventional powder forging:
Dominating mechanisms of
deformation of metals and
intermetallic compounds:
grain boundary sliding
diffusion
intergranular
dislocation slip

Difference between a conventional and isothermal die forging (nearly
identical to superplastic forming)

Another precondition of superplastic forming transformation
superplasticity (internal stress superplasticity)
Requirements: for superplastic forming (of ceramics):
1. Ultra fine (sub-micron) grain size (<1m)
2. Stress-induced transformation toughening internal stresses generation by
phase transformations
Example: Yttria-stabilized tetragonal zirconia (ZrO 2+5,2 wt%Y2O3), elongation to failure
up to 800% at 1550C
NB! The finer grain size makes superplastic ceramics prone to concurrent grain
growth

Advantages of powder forging over conventional
forging:
1)near-net shape capability
2)full-density products/materials
3)high degree of material utilization and energy savings
4)enhanced mechanical, particularly dynamic
properties (fatique strength, fracture toughness)

Applications of powder forging:
Components for automotive transmission (Fe-based

alloys)
Applications of powder superplastic forming:
1. Ultra high carbon steels
(UHC steels)
2. Mechanically alloyed materials
( e.g TiAl Ti3Al intermetallic compounds)
3.
Superplastic ceramics
(e.g ZrO2-Y2O3, Al2O3+ZrO2-Y2O3) etc.

Powder forged automotive transmission components:
Powder forged
connecting rods
Powder forged internal ring gear
7. Alternative hot consolidation processes

7.1 Combustion synthesis (self-propagating high
temperature synthesis; SHS; SPS; reactive/ reaction
synthesis)
Combustion synthesis (SHS, SPS) = formation of
chemical compounds (usually refractory compounds)
involving self-propagating exothermic reactions between
the reactants.
Preconditions:
exothermic reaction
proper granulometry of powders
external source of heat for initiation
Combustion synthesis (cntd 1)

Combustion synthesis reaction is as follows:
aiX + bjYj = Z + Q
where:
X V, Mo, W, Hf, Ti etc metals
Y C, B, N, Si, O, S non-metals or metals (production of intermetallic
compounds)
Z chemical compound
Q exothermic release of energy
Variations of combustion synthesis:
Propagation of combustion wave (SHS)
Simultaneus combustion (SC)

Three different reaction methods:
- solid phase system
- solid-liquid system
- solid-gas system
Advantages of combustion synthesis (in comparison with
conventional P/M technology)
1) Exothermic process
2) Short processing time
3) A wide variety of different materials can be produced
4) Production of chemical compounds as well as composites
5) High purity of the end product

Examples of reactions of combustion synthesis:
Ti + C = TiC
(all solid state)
Ni + 3Al = Ni3Al
(disappearing liquid phase)
2Al + N2 = 2AlN
(solid-gas system)
3SiO2 + 6C + 2N2 = Si3N4 + 6CO2
(gas-phase present in both reactant and product)
Exothermic combustion synthesis can be take place during sintering

of multi-component powder materials = reactive sintering.
Reactive sintering sintering process where an exothermic reaction
is initiated in a mixture of dissimilar (elemental) powders. The
reaction produces a compound and the heat from the reaction is
used to simultaneously sinter the product.
7.2 Pressure-assisted combustion synthesis

Pressure assisted combustion synthesis is used in
conditions where conventional process results in porosity
of product.
The porosity could be due to: porosity of reaction mixture,
changes in molar volume, volatile impurities etc.
Pressure can be applied by various means:

1) Uniaxial pressure
2) Isostatic pressure
3) Pseudo-isostatic pressure
4) Shock wave
5) Centrifugal force
Pressure-assisted combustion synthesis (cntd. 1)

Different schemes of pressure-assisted combustion synthesis:
1)
2)
3)
4)
Reactive hot pressing (RHP)

Reactive hot isostatic pressing (RHIP)
Pseudo-HIP (P-HIP)
High pressure-assisted combustion synthesis
(HPCS)

Reactive hot pressing (RHP) (1):
Uniaxial hot pressing

and simultaneus
combustion
synthesis

Time-temperaturepressure profile for a

typical reactive hot
pressing operation:
Pressure: up to 50 MPa
Time: 600 sek
( 10 minutes)

Applications:
Ceramics (TiB2, TiC etc),
intermetallics (NiAl, Ni3Al
etc) and their based
composites
The effect of pressure on the residual

porosity for pressure-assisted combustion
synthesis of Ni3A and NiAl compositions

Reactive hot isostatic pressing (RHIP):
Time-temperature-pressure
profile for a typical reactive
hot isostatic pressing
operation
Pressure: 100200 MPa
Time: 24 hours
Application: intermetallic
compounds (NiAl, FeAl,
Ni3Al, Al3Ta etc) and their
based composites
(Al3Ta Al2O3 fibers,
NiAl Al2O3 fibers,
NiAl TiB2 etc.)

Pseudo-HIP (P-HIP) (1):
Pseudo-HIP is similar to
conventional HIP, but
pressure is applied through
a granular particulate-based
medium instead of gas

Pseudo-HIP (P-HIP) (2):
Technological pecularities:
Ceramical particulate-based medium (e.g SiO2) as the
pressure-transmitting medium
Pressure: 100700 MPa
Time: 0,5 hours
Application: ceramics and ceramic-based composites
(TiAl-TiB2 etc).
NB! Pseudo-HIP is not isostatic pressing
7.3 Ceramic consolidation process

(CERACON-process)
The CERACON-process is
similar to pseudo-HIP, but the
pressure is not isostatic (and
results in unequal deformation
of the preform)
The CERACON-process =
pseudo-isostatic forming
process
Ceramic consolidation process (cntd.)

Preheating of both preform and ceramic granules
Pressure: up to 1500 MPa
Time: 3060 sek
Unequality (0.5%) of deformation of the preform
Application: near-net shape components from:

- metallic alloys (Ti, Ta, Al)
- intermetallic compounds (TiAl, NiAl etc)
- high-temperatures superconductors etc
7.4 Ceramic mold process

Alternatives to produce full density net shapes:
Step 1: production of complex net shapes by:
1) loose powder packing on a complex shaped mold
2) cold isostatic pressing (CIP)
3) powder injection molding (PIM)
Step 2: Densification to full density by utilizing HIP (or
pseudo-HIP)
The ceramic mold process is a variation of conventional
HIP intended to drastically reduce machining
Ceramic mold process (cntd. 1)
Shematic of the
ceramic mold
process: production
of ceramic mold is
similar to that in
investment casting
The ceramic mold process is

also suitable for producing:
1)Deep cavities (see Fig.)
2)Dual-property components by
bonding different materials
together in one cycle

an oversized ceramic mold to compensate for the
shrinkage during HIP
application of pseudo-isostatic pressure through ceramic
particulate medium
Applications:
net-shape / near-net shape products from metallic

alloys (e.g Ti-alloys)
7.5 Rapid omnidirectional compaction

(fluid die process)
similar to hot isostatic

pressing where pressure
transmitting medium is a
fluid die (omnidirectional
nature of applied pressure)
higher productivity in
comparison with
conventional HIP cycle
(rapid HIP)
Rapid omnidirectional compaction (cntd. 1)
Technological pecularities (cntd):

pressure much higher than in
HIP
Time 115 sek
Temperature: lower than in HIP
Applications: WC-Co hardmetals,
intermetallic compounds etc.
Powder filled fluid die (made from low

carbon steels, Cu+10 Ni alloy, etc)
Rapid omnidirectional compaction (cntd. 2)

Drawback of utilizing metallic
fluid die extensive machining
of fluid die
Solution: use of cast composite
fluid die (see Fig.) enabling
mechanical stripping of
consolidated part and
eliminating expensive canning
sequence
ROC process using a cast
composite fluid die
7.6 Plasma activated sintering (PAS)

(field activated sintering technique (FAST),
spark-plasma sintering)
Plasma activated
sintering = pressureassisted sintering
activated by electrical
discharges between
powder partides
Plasma activated sintering (PAS) (cntd. 1)

Time-temperature-pressure
cycle for the PAS-process:
1) application of pressure
2) initiation of pulsed
discharges resulting in
formation of pulse plasma
between particles (to
activate powder surface)
3) resistance heating (for
densification)
4) lowering of pressure and
temperature
Plasma activated sintering (PAS) (cntd. 2)

Technological parameters:
Pressure: 10-65 MPa
Total time: 10 minutes
Pulse on-state duration: 3060 sek
Application:
ceramic materials
metallic materials
ceramic-metallic composites (hardmetals,
cermets) etc.
7.7 Consolidation by atmospheric pressure (CAP)
The CAP-technique utilizes

atmospheric pressure to provide
pressure during the course of
sintering.
The goal: production of full dense
materials in an inexpensive
manner (without HIP)
Consolidation by atmospheric pressure (CAP) (cntd. 1)
Advantages of CAP technique:

1)The ease of production of complex shape glass
molds
2)Assistance of pressure without use of expensive
high-pressure equipment (required for hot
extrusion or HIP)
3)No costly protective atmospheres are required
4)The ease of glass mold stripping
7.8 Thixomolding; (molding of thixotropic

alloys)
Thixotropic state/structure
can be achieved when any
material in the mushy state
is subjected to higher
shearing action (e.g by
stirring).
Result formation of
nearly spheroidal
degenerate dendritic
partides and viscosity
drops markedly
Thixomolding (cntd. 1)
Al-Mg phase diagram with a
Thixomolding alloy composition and
thixomolding temperature range for
Al-9% Mg alloy.
The goal:
production of near-net shape or netshape parts in a single step
Process characteristics (as against conventional die
casting):
1) Lower molding temperatures material is in semi-solid
state
2) The temperature control at the exit end +/-2C
3) Elimination of most foundy operations (handling of
molten metal, use of fluxes, waste management etc.)
4) Production of complex components directly from
particulate material
5) Potential to produce dispersion strengthened/hardened
materials
Application and
advantages:
Schematic of the injection molding

machine used for Thixomolding
Large scale production

of complex products
from low-temperature
alloys (Mg, Al)
Significant increase in
die life (as against die
casting)
Low porosity and

enhanced mechanical
properties of material
7.9 Infiltration
For wetting liquid melt, the capillary pressure:
P = 2cos()/d
where
d- size of pores
- surface energy of the liquid
- contact angle (=wetting angle formed at the intersection of
liquid, solid and vapor phases)
Infiltration sequence where

capillary forces pull a molten
metal into the open pores
Infiltration (cntd. 1)
Infiltration the process of filling the pores of compact
with open porosity with a lower melting temperature
metal/alloy or other material (glass)
During infiltration a liquid metal may fill pores by
capillary-action (capillary infiltration) or by external force
(external pressure infiltration)
1. Capillary infiltration techniques (see also next Fig.)
a) Capillary-dip infiltration
b) Full-dip infiltration
c) Contact infiltritation
Applications:
electrical contacts, ferrous structural components for
automobiles; metal matrix composites (MMC) etc.
2. External pressure infiltration techniques:
a) gravity-feed infiltration
b) centrifugal pressure infiltration
c) vacuum infiltration
d) HIP-infiltration (HIP-impregnation) (see also next Fig.)
Applications:
mainly nonwetting combinations such as: graphite-Cu,
Al-SiC, Mg-SiC
HIP-infiltration full density
consolidation in conditions
when capillary forces are
ineffective because of poor
wetting, unsuitable pore
size distribution or high
viscosity of the liquid
7.10 Bonding by hot consolidation

For bonding/joining of different materials hot consolidation
techniques can be used, e.g.:
Hot isostatic pressing (HIP-diffusion bonding)
Reactive joining (SHS-joining)
Bonding by hot consolidation (cntd. 1)
1) HIP diffusion bonding provides bonding

between:
two full-dense materials
a full-dense and a porous materials
two porous materials
HIP process provides concurrent densification
and bonding of different materials.

1) HIP diffusion bonding (for production of HIP/clad
products):
enables production of gradient-structured materials
NB!
large internal stresses maybe built up due to the
thermal expansion and elastic modulus mismatch.
The stresses increase with an increase in the thickness
of joined materials.

Advantages of HIP diffusion
bonding (compared with
conventional diffusion
bonding):
1) Isostatic prssure enables
bonding of shaped surfaces
2) Plastic deformation only at
microscopic scale enables
HIP diffusion bonding at
higher temperatures
HIP diffusion bonding of powder to solid
3) Powder and porous bodies

can be simultaneusly
densified to a substrate

2) Ractive joining (SHS-joining):
uses combustion synthesis to join different materials
is similar to exothermic welding or exothermic brazing
Advantages of SHS joining:
1) minimal heat induced damage to the substrate since
generated heat is localized

Advantages (cntd.)
2) Ability to form
functionally graded
material joints between
dissimilar substrates
thereby overcoming
matching problems.
Schematic set-up of two reactive joining processes
Thank you for attention!

Full Density Powder Processing Techniques

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Full Density Powder Processing Techniques

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Technology of full density powder

materials and products

Introduction: full density processing

1. Introduction: full density processing

Introduction: full density processing (cntd. 1)

Introduction: full density processing (cntd. 2)

Introduction: full density processing (cntd. 3)

Introduction: full density processing (cntd. 4)

CIP+S= cold isostatically press and sinter

Introduction: full density processing (cntd. 5)

Introduction: full density processing (cntd. 6)

Phase diagram of an ideal

Typical microstructure of a liquid-phase sintering

Introduction: full density processing (cntd. 7)

Introduction: full density processing (cntd. 8)

Introduction: full density processing (cntd. 9)

Initial and intermediate stages of densification for

3)Lattice and grain boundary

Introduction: full density processing (cntd. 10)

Hot pressing (cntd. 1)

Hot pressing (cntd. 2)

Hot pressing (cntd. 3)

Hot pressing (cntd. 4)

Large parts/products from WC-Co hardmetals

Hot pressing (cntd. 5)

Incorporation of whiskers or fibers

Cermet (ceramic/metal composite) technology in which the tough

Inclusion of a phase which undergoes tranformation due to the

Utilization of the concept of compositional gradient MIMLC-type

Hot pressing (cntd. 6)

(e.g in fiber/whiscers reinforced ceramic matrix

Hot pressing (cntd. 7)

Soft, ductile, low modulus

Schematic view of a conceptual MIMLC structure

Hot pressing (cntd. 8)

Hot pressing (cntd. 9)

Increased resistance (higher than that of

Hot pressing (cntd. 10)

Hot pressing (cntd. 11)

MIMLC: Al2O3-Ni grandient material

Hot pressing (cntd. 12)

Hot pressing (cntd. 13)

1000oC, 300 bar

Hot pressing (cntd. 14)

Hot pressing (cntd. 15)

(MoSi2 based composite reinforced by SiC particles)

3. Hot isostatic pressing (HIP)

Hot isostatic pressing (HIP) (cntd. 1)

Hot isostatic pressing (HIP) (cntd. 2)

Hot isostatic pressing (HIP) (cntd. 3)

Hot isostatic pressing (HIP) (cntd. 4)

1. Increased Cooling HIP systems (providing

Hot isostatic pressing (HIP) (cntd. 5)

1. Materials/products of higher performance

Hot isostatic pressing (HIP) (cntd. 6)

little shear on the particle surfaces (because of

Hot isostatic pressing (HIP) (cntd. 7)

Hot isostatic pressing (HIP) (cntd. 8)

Hot isostatic pressing (HIP) (cntd. 9)

Hot isostatic pressing (HIP) (cntd. 10)

Hot isostatic pressing (HIP) (cntd. 11)

Hot isostatic pressing (HIP) (cntd. 12)

Hot isostatic pressing (HIP) (cntd. 13)