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Sinterin

g
treatment of a

The thermal
powder or compact at a
temperature below the melting point of the main constituent,
for the purpose of increasing its strength by bonding together
of the particles

What Happens During Sintering?


1. Atomic diffusion takes place and the welded areas formed during
compaction grow until eventually they may be lost completely.
2. Recrystallisation and grain growth may follow, and the pores tend to
become rounded and the total porosity, as a percentage of the whole
volume tends to decrease.

Sintering Atmospheres

The operation is almost invariably carried out under a protective


atmosphere, because of the large surface areas involved, and at
temperatures between 60 and 90% of the melting-point of the particular
metal or alloys.

Advantages of Powder
Technology

Particular advantages of the powder technology include:


1.Very high levels of purity and uniformity in starting materials
2.Preservation of purity, due to the simpler subsequent fabrication process
(fewer steps) that it makes possible
3.Stabilization of the details of repetitive operations, by control of grain
size during the input stages
4.Absence of binding contact between segregated powder particles or
"inclusions" (called stringering) as often occurs in melt processes
5.No deformation needed to produce directional elongation of grains
6.Capability to produce materials of controlled, uniform porosity.
7.Capability to produce near net shape objects.
8.Capability to produce materials which cannot be produced by any other
technology.
9.Capability to fabricate high strength material like turbines

Types of Sintering
1. Solid state sintering
Only solid phases are present at
the sinter temperature
2. Liquid phase sintering
Small amounts of liquid phase are
present during sintering
3. Reactive sintering
Particles react with each other to
new product phases

Important Parameters in
Sintering
We can divide these parameters into
four broad categories
Powder preparation:
-- Particle size
-- Shape
-- Size distribution

Driving Force for Sintering


As with all processes, sintering is
accompanied by an increase in the free
energy of the system. The sources that give
rise to the amount of free energy are
commonly referred to as the driving forces for
sintering. The main possible driving forces are
The curvature of the particle
surfaces
An externally applied pressure
A chemical reaction

Driving Force for Sintering


Schematically it can be shown as

Stages of Sintering
Three stages are distinguished in
sintering

First Stage
After burn out of any organic
additives, two things happen to
the powder particles when the
mobility of the surface atoms
has become high enough;
initially rough surface of the

Stages of Sintering

Second Stage
Densification and pore shrinkage. If
grain boundaries are formed after the
first stage, these are new source of
atoms for filling up the concave areas
which diminishes the outer surface of
the particle

Third Stage
Grain growth takes place, the pores
break up and form closed spherical

Stages of Sintering
The three stages in the dry sintering can be
shown as

Sintering
Mechanism:
Sintering
occurs by diffusion of atoms through the microstructure. This
diffusion is caused by a gradient of chemical potential atoms move from an
area of higher chemical potential to an area of lower chemical potential. The
different paths the atoms take to get from one spot to another are the
sintering mechanisms. The six common mechanisms are:
Surface diffusion Diffusion of atoms along the surface of a particle
Vapor transport Evaporation of atoms which condense on a different surface
Lattice diffusion from surface atoms from surface diffuse through lattice
Grain boundary diffusion atoms diffuse along grain boundary
Plastic deformation dislocation motion causes flow of matter
Lattice diffusion from grain boundary atom from grain boundary diffuses
through lattice

Mechanisms of Sintering

Liquid Phase Sintering


The pores in the compact are
largely surrounded by the liquid
phase and the driving force for
sintering is liquid surface energy
With high liquid fractions, full
density can be achieved almost
entirely by rearrangement

Liquid Phase Sintering


The pores in the compact are
largely surrounded by the liquid
phase and the driving force for
sintering is liquid surface energy
With high liquid fractions, full
density can be achieved almost
entirely by rearrangement

Liquid Phase Sintering


Grain boundary wetting breaks the
polycrystalline particle into single crystal
particles in the initial stages of liquid
phase sintering. These single crystal
particles then spheroidize and coarsen
Polycrystalline
particle

Liquid

Liquid Phase Sintering


Wetting is a very important
phenomena which is happening
during LPS
Figure represents the surface
tensions of a multi-phase junction as
lv
vectors drawn parallel
to the
sv

respective surfaces
sl

Liquid Phase Sintering


The surface energies for different interfaces
is given by
sl = solid/liquid
sv = solid/vapor
lv = liquid/vapor
The vectors representing these surface
energies must balance at the three phase
triple junction. This equation representing
this balance
issvknown
Youngs
sl ascos(
)lv equation

Liquid Phase Sintering


lv
sv

sl

sv

lv

Large sv, wetting


small
sl

Large sl, non-wetting


Large

Liquid Phase Sintering

Grain boundary
wetting during LPS
occurs when A
and B approach
zero

AB BL cos(B ) AL cos(A)

Grain B

BL

AB
Grain A

Liquid

AL

Examples of LPS
Powder Metallurgy parts
-- Copper/Tin alloys
-- Iron/Copper structural parts
--Tungsten Carbide/Cobalt cemented
carbides
Ceramics
-- Silicon Nitride with a glassy liquid phase
(2wt% alumina + 6wt% yttria)
-- SiC with Silicon liquid phase

Disadvantages of LPS
Compact slumping (shape distortion)
which occurs when too much liquid is
formed during sintering
The same parameters which control
the sintered microstructure often
control the final properties
Useful application temperature of the
material is sometimes limited by the
presence of too much low melting
point material

Reactive Sintering
Two or more constituents in a compact
react during sintering to form a new phase
or phases
The reaction is normally exothermic and
can contribute to an enhancement of
sintering
In some cases the reaction is so
exothermic that it can generate sufficient
heat to cause self-sintering without
external heating except that required for
initiating the reaction

Reactive Sintering
This is the basis of combustion
synthesis which if properly
controlled can produce a relatively
dense compact of the synthesized
reaction product
Example of reaction sintering is
3TiO2 + 4AlN 2Al2O3 + 2TiN + N2

Sintering Procedure
Ancient sintering techniques for the
making of pottery and ceramic art
objects remain in wide use to this
day but research has also led to
more advanced techniques which
work for a wider array of ceramics

Sintering Procedure
In a typical sintering procedure
-- Most ceramic materials have a
lower
affinity for water and a lower
plasticity index than clay,
requiring
organic additives in
the stages before
sintering
-- A mixture of binder, water and
ceramic powder is pressed into a
mold to form a green body (unsintered
item)

Sintering Procedure
-- The green compact is placed on a
mesh belt and moved slowly
through
the sintering furnace
-- In the preheat zone, the lubricant
volatilizes, leaves the part as a
vapor,
and is carried away by the
dynamic
atmosphere flow

Sintering Procedure
-- The temperature within the
furnace
rises slowly in the
preheat zone until
reaching the
actual sintering
temperature
-- It remains essentially constant
during
the time at that
temperature, and
proceeds
into the cooling zone where
the
drop in part temperature is

Sintering Procedure
Schematica
lly

Sintering Procedure
As the parts travel through the
furnace, the temperature cycle
results in changes in composition
and microstructure
In the hot zone metallurgical
bonds develop between particles
and solid state alloying takes
place
The microstructure developed
during sintering determines the

Sintering Atmospheres
The operation is almost invariably
carried out under a protective
atmosphere, because of the large
surface areas involved, and at
temperatures between 60 and
90% of the melting-point
These are essential for almost all
sintering processes, to prevent
oxidation and to promote the

Sintering Atmospheres
In practice dry hydrogen, cracked
ammonia, and partially combusted
hydrocarbons are mainly used
Although the first named is often
precluded because of cost. It is
however, used for sintering
carbides and magnetic materials
of the Alnico type

Sintering Atmospheres
It can replace pure hydrogen for
many applications at approximately
one-third the cost, with the obvious
exceptions where reaction with
nitrogen cannot be tolerated
It is particularly useful for sintering
iron, steel, stainless steel, and
copper-base components

Sintering Atmospheres

The most widely used


atmospheres primarily because of
their lower cost, are produced by
partial combustion of hydrocarbons

Post Sintering Operations

1)Re-Pressing
Even with the best control that is
feasible in practice, there will
inevitably be some variation in the
dimensions of parts produced
from a given material in a given
die set

Post Sintering Operations

Typically, it is possible for parts


'as-sintered' to be accurate to a
tolerance of -0.0508mm per mm,
in the direction at right angles to
the pressing -direction, and
0.1016mm per mm parallel to the
pressing direction

Post Sintering Operations

Dimensional accuracy can be


greatly improved by re-pressing
the part after sintering. This
operation is called sizing

Post Sintering Operations

2) Hot Re-Press
Hot Repressing will give even
greater densification, with
consequent greater improvement
in the mechanical properties, but
less accurate control of the final
dimensions is to be expected

Post Sintering Operations

3) Hot Isostatic Pressing


HIP is used as a post-sintering
operation to eliminate flaws and
micro-porosity in cemented
carbides

Post Sintering Operations


4) Forging
Forging is a comparatively recent
technique in which a blank is hot
re-pressed in a closed die which
significantly changes the shape of
the part, and at the same time
can give almost complete density
and hence mechanical properties
approaching or even surpassing
those of traditional wrought parts

Post Sintering Operations


5) Infiltration
An alternative method of
improving the strength of
inherently porous sintered parts is
to fill the surface connected pores
with a liquid metal having a lower
melting point. Pressure is not
required, capillary action is
sufficient

Post Sintering Operations

6) Impregnation
This term is used for a process
analogous to infiltration except
that the pores are filled with an
organic as opposed to a metallic
material

Post Sintering Operations


7) Heat Treatment
Although many, perhaps the bulk
of sintered structural parts are
used in the as-sintered or sintered
and sized condition, large
quantities of iron-based parts, are
supplied in the hardened and
tempered conditions. Heating
should be in a gas atmosphere
followed by oil-quenching

Post Sintering Operations

8)

Surface-Hardening

Carburizing and carbonitriding of


PM parts is extensively used, and
again gaseous media are
indicated

Post Sintering Operations


9)

Steam Treatment

A process peculiar to PM parts is


steam-treatment which involves
exposing the part at a
temperature around 500C to high
pressure steam. This leads to the
formation of a layer of magnetite

Post Sintering Operations


10) Blueing
Heating in air at a lower
temperature (200-250C) can also
be used to provide a thin
magnetite layer that gives some
increase in corrosion resistance,
but it is much less effective than
steam treatment

Post Sintering Operations

11) Plating
Sintered parts may be plated in
much the same way as wrought or
cast metals, and copper, nickel,
cadmium, zinc, and chromium
plating are all used

Post Sintering Operations

12) Coatings
A large percentage of hard metal
cutting tool inserts are now coated
using chemical vapor deposition
(CVD) or physical vapor deposition
(PVD)

Post Sintering Operations


13) Mechanical Treatments
Although a major attraction of PM
parts is that they can be produced
accurately to the required
dimensions, there are limitations
to the geometry that can be
pressed in rigid dies, and
subsequent machining, for
example of transverse holes or reentrants at an angle to the

Post Sintering Operations


14) De-burring
De-burring is done with sintered
parts, and is used to remove any
'rag' on edges, resulting from the
compacting operation or a
machining step

Advantages of Sintering
Particular advantages of this
powder technology include:
1. the possibility of very high purity
for the starting materials and their
great uniformity
2. preservation of purity due to the
restricted nature of subsequent
fabrication steps

Advantages of Sintering
3. stabilization of the details of
repetitive operations by control of
grain size in the input stages
4. absence of stringering of
segregated particles and
inclusions (as often occurs in melt
processes)
5. no requirement for deformation
to produce directional elongation
of grains

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