Module 3

POLYMERS & POWDER METALLURGY

Introduction to Polymers used for additive manufacturing

A polymer is a large molecule made up of chains of repeating basic molecular units called
monomers. Many polymers are named by their basic monomer unit with the prefix poly.
Polyvinyl chloride (PVC) is the polymer of vinyl chloride.

Polyamide (Nylon 6)
Polyamide is a plastic material used to print 3D objects. Printed from polyamide powder, this
material is also known as nylon.

Polyamide material's structure comes from a polymer containing amide functions.

Polyamide is used in 3D printing in a variety of formats. Polyamide in powder form is used

in SLS (Selective Laser Sintering). Printers made by 3D Systems and EOS GmbH use this
method to melt polyamide plastic with laser energy.
Nylon
Polyamide (Nylon 6)
In wire form in FDM (or fused deposition modelling),the polyamide material is heated until in a
liquid state, then extrudes from a nozzle that applies it layer by layer in order to create the
desired object. Stratasys and 3D Systems, the two industry leaders, distribute 3D printers for
polyamide.

Polyamide parts have excellent long-term stability and are resistant against most chemicals.
They can be made watertight by impregnation.

Phenol formaldehyde resins

Phenol formaldehyde resins are synthetic polymers obtained by the reaction of phenol or
substituted phenol with formaldehyde.

They have been widely used for the production of moulded products including billiard balls,
laboratory countertops, and as coatings and adhesives.

Phenol- formaldehyde resins having low degree of polymerization are soft.

Phenol formaldehyde resins
They possess excellent adhesive properties and are usually used as bonding glue for laminated
wooden planks and in varnishes

Phenol- formaldehyde resins having high degree of polymerization are hard, rigid, scratch-
resistant and infusible.

They can withstand very high temperatures. They act as excellent electrical insulators also.

USES
They are used for making moulded articles such as radio and TV parts, combs, fountain pen
barrels, phonograph records etc.

They are used for making electrical goods such as switches, plugs etc.

They are used for impregnating fabrics wood and paper.

They are used as bonding glue for laminated wooden planks and in varnishes.
PLA (PolyLactic Acid)

PolyLactic Acid most commonly known as PLA, is a polymer made from renewable resources.
Contrary to other thermoplastics which are petroleum-based, some of the raw materials used
for PLA’s production include corn starch and sugarcane.

PLA is a low cost commodity material. Now a days this is widely used 3D printing material due
to its good properties.
• There is no fancy features needed to print this material, its of great low cost filament with a
lot of colours in the market.

• Visually its glossy and can be painted very easily.

• It is well suited for non mechanical applications to do as low toughness and low heat
resistance.

• It is fantastic for general printing applications or prototyping.

ABS (Acrylonitrile butadiene styrene )

ABS is an impact-resistant engineering thermoplastic & amorphous polymer. ABS is made up

of three monomers: acrylonitrile, butadiene and styrene.

Acrylonitrile: It is a synthetic monomer produced from propylene and ammonia. This

component contributes to ABS chemical resistance & heat stability.

Butadiene: It is produced as a by-product of ethylene production from steam crackers. This

component delivers toughness & impact strength to ABS polymer.

Styrene: It is manufactured by dehydrogenation of ethyl benzene. It provides rigidity &

processability to ABS plastic
ABS has been around 3D printing since the inception of the fused deposition
modelling machine.

• ABS is not significantly stronger when compared to PLA, however, it is

tougher so it will flux more before it fractures and performs better under
impact. These traits make ABS an excellent choice for functional prototypes.

• ABS exhibits some nice benefits but to reliably print this material there are
some processing challenges. It tends to wrap when its not evenly heated. So
enclosed chamber is strongly encouraged. Not all printers can print at this
higher temperature as well.
Polyesters
Polyester is a category of polymers which contains the ester functional group in their main
chain.

Polyester is currently defined as:

“Long chain polymers chemically composed of at least 85% by weight of an ester and a dihydric
alcohol and terephthalic acid”.

The name “polyester” refers to the linkage of several monomers (esters) within the fiber.

Properties polyester.
Effects of moisture: Polyester absorbs only a very small amount of moisture and the tenacity
and elongation are unaffected by moisture.

Effects of bleaches: Not affected by oxidizing and reducing bleaches.

Effects of organic solvents: Resistant to all dry cleaning solvents.

Polyesters
Properties polyester.
Effects of acids: Polyester fibres are highly resistant to mineral and organic acids. Weak acid
can not effect on them even on boiling. Strong mineral acid such as H2SO4 can only hydrolyze
them on boiling for hours together.

Dye ability: Disperse dye and some pigments can be used for coloration.

Uses of Polyester
As apparel: Men’s wear, women’s wear, children’s wear
As blended fabrics: Polyesters are widely used in blends with cotton, wool, acrylic, nylon etc
fibres for making quality fabrics.
As home furnishings: Carpets, curtains, draperies, sheets, pillow covers, wall coverings,
upholstery etc are made of polyester fibres.
As industrial use: Polyester fibres are used in manufacturing of tire cord, power belt, ropes,
tarpaulin, nets, hoses, conveyor belt etc.
Classification Of Polymers
By Origin
By Monomer
By Thermal Response
By Mode Of Formation
By Structure
By Application & Physical Properties

By Origin
1. Natural Polymers- Polymers which are isolated from natural materials are called as natural
polymers. E.g. Silk, Wool, Natural rubber, Cellulose, Starch, Proteins etc.

2. Synthetic Polymers- Polymers synthesized in laboratory from low molecular weight

compounds, are called as, synthetic polymers.
Ex- Terylene, Polyethylene, Polystyrene, Synthetic rubber, Nylon, PVC, Bakelite, Teflon etc.
Classification Of Polymers
By Monomer
1. Homo Polymers- A polymer consist of identical monomers is called homo polymer. E.g.
Polyethylene, PVC, Polypropylene, Nylon 6

2. Co Polymers- A polymer consist of monomers of different chemical structure are called

copolymers. E.g. Nylon 6,6

By Thermal Response
1. Thermoplastic Polymers
• They are easily moulded in desired shapes by heating and subsequent cooling at room
temperature.
• They are soft in hot and hard on cooling
• They my be linear or branched chain polymers. E.g. PE, PVC, PS, PP
Classification Of Polymers
By Thermal Response
2. Thermosetting Polymers
• This polymer is hard and infusible on heating
• These are not soft on heating under pressure and they are not remolded.
• These are cross linked polymers and are not reused.
Ex- Phenol formaldehyde, epoxy, polyester.

By Mode Of Formation
1. Addition Polymers- The polymers formed by the addition of monomers repeatedly without
removal of by products are called addition polymers.
Ex-Teflon, Polyethylene, Polypropylene, PVC.

2. Condensation Polymers- They are formed by the combination of two monomers by removal
of small molecules like H2O, Alcohol or NH3
E.g. Polyamides(Nylons), Polyesters.
Classification Of Polymers
By Structure
1. Linear Polymers- In these polymers monomers are linked with each other and form a long
straight chain.
E.g. HDPE, Nylons

2. Cross-linked Polymer- In these monomeric units are linked together to constitute a 3D

network.
• The links involved are called cross links.
• They are hard, rigid .and brittle due to their network structure.
Ex-Bakelite, Formaldehyde resins, Vulcanized rubber

By Applications & Physical Properties

1. Fibers
2. Plastics
3. Resins
Concept of functionality
what functionality means,
The ability to perform a task or function; that set of functions that something is able or
equipped to perform.

Functionality in polymer chemistry

The functionality of a monomer is defined as the number of bonds that a monomer's
repeating unit forms in a polymer with other monomers.

Polydispersity
what polydispersity means. The state of being polydisperse. A measure of the degree to which
a colloid is polydisperse.

PDI or Poly dispersity index is very important index in Polymer chemistry.

For wide molecular weight distribution ie, if the polymer chain lengths are not uniform in size
then PDI will not be close to unity and PDI will be close to unity of the chain lengths are
uniform
Polymer Processing: Methods of spinning for additive manufacturing
Wet spinning
Polymer Processing: Methods of spinning for additive manufacturing
Wet spinning

This is the oldest, most complex and also the most expensive method of man-made yarn
manufacture. This type of spinning is applied to polymers which do not melt and dissolve only
in non-volatile or thermal unstable solvents.

Spinning process
• In wet spinning, a non-volatile solvent is used to convert the raw material into a solution.
• The solvent is extruded through the spinneret either by simply washing it out or by a
chemical reaction between the polymer solution and a reagent in the spinning bath.
• After extrusion, the solvent is removed in a liquid coagulation medium.
• Finally the filament yarn either is immediately wound onto bobbins or is further treated for
certain desired characteristics or end use.
The wet-spinning process is capable of spinning a large number of fibers
simultaneously since several spinnerets can be placed in a coagulation bath. In
this process, a polymer is dissolved in an appropriate solvent, which is then
drawn into a nonsolvent (coagulation bath) by submerging spinnerets in the
coagulation bath.

When the fibers come out of the bath, they precipitate and solidify. These
solidified fibers are then stretched on a rotating drum.

This process is used to make rayon, acrylic, modacrylic, and spandex fibers.
It is a liquid bath providing the precipitation of an extruded or cast polymer
solution with the resulting formation of a solid membrane matrix.

Coagulation medium is responsible for the phase inversion process, and most of
the time, it is represented by water. Some organic solvents (such as ethanol or
isopropanol) can be also used to induce polymer precipitation, and even vapors
and supercritical fluids can be considered as coagulation media for the phase
inversion process.
Polymer Processing: Methods of spinning for additive manufacturing
Wet spinning

Example: Wet spinning is used in the production of aramid, Lyocell, PVC, viscose rayon,
spandex, acrylic and modacrylic fibers.

Advantages:
►Large tows can be handled

Disadvantages:
►Slow (70-150 yds/min)
►Washing to remove impurities
►Solvent and chemical recovery
Polymer Processing: Methods of spinning for additive manufacturing
Dry spinning
Polymer Processing: Methods of spinning for additive manufacturing
Dry spinning
Dry spinning is used for polymers that need to be dissolved in a solvent. Solvent spinning (dry
spinning and wet spinning) are used by 30% of the fibers.

Spinning process:
• In dry spinning, a volatile solvent is used to dissolve the raw materials and form a solution.
• Then the solution is purified by filter.
• The solution is extruded through a spinneret into a warm air chamber where the solvent
evaporates, solidifying the fine filaments.
• Finally the filament yarn either is immediately wound onto bobbins or is further treated for
certain desired characteristics or end use.

Example: Dry spinning is used in the production of acetate, triacetate, and some acrylic,
modacrylic, spandex, and vinyon (PVC,PVA) fibers.
Advantages:
►Yarn does not require purification Disadvantages: ►Flammable solvent hazards
►Solvent recovery
Biopolymers
It is a polymer that is developed from living beings. It is a biodegradable chemical compound
that is regarded as the most organic compound in the ecosphere.

The name “Biopolymer” indicates that it is a biodegradable polymer.

Example of Biopolymers
Some Biopolymer examples are
Proteins
Carbohydrates
DNA
RNA
Lipids Nucleic acids
Peptides

The most common biopolymer is Cellulose. It is also the most abundant organic compound on
this planet. It comprises of 33% of all plant component on Earth.
Biopolymer Classification
1. Sugar based Biopolymers
Starch or Sucrose is used as input for manufacturing Polyhydroxibutyrate.

Sugar based polymers can be produced by blowing, injection, vacuum forming and extrusion.

Lactic acid polymers (Polylactides) are created from milk sugar (lactose) that is extracted from
potatoes, maize, wheat and sugar beet.

2. Biopolymers based on Synthetic material

Synthetic compounds that are obtained from petroleum can also be used for making
biodegradable polymers such as aliphatic aromatic copolyesters.

Though these polymers are manufactured from synthetic components, they are completely
compostable and bio- degradable.
Biopolymer Classification
3. Cellulose based Biopolymers
• These are used for packing cigarettes and confectionary.
• This polymer is composed of glucose and is the primary constituent of plant cellular walls.
• It is obtained from natural resources like cotton, wood, wheat and corn.
• The production of biopolymer may be done either from animal products or agricultural
plants.

• Biopolymer Uses
• These polymers play an essential role in nature. They are extremely useful in performing
functions like storage of energy, preservation and transmittance of genetic information and
cellular construction.
• Starch based biopolymers can be used for creating conventional plastic by extruding and
injection molding.
• Biopolymers based on synthetic are used to manufacture substrate mats.
• Cellulose based Biopolymers, such as cellophane, are used as a packaging material.
Moulding and casting of polymers
Plastic moulding is the process of shaping plastic using a rigid frame or mould.

This technique allows for the creation of objects of all shapes and sizes with huge design
flexibility for both simple and highly complex designs.

Plastic Moulding Techniques

1) Injection Moulding
2) Thermo forming
3) Compression Moulding
4) Blow Moulding
Injection Moulding
Injection Moulding Process is a manufacturing process used for producing parts or components
by injecting molten material into the mould cavity. Injection molding can be performed with
only one of these materials like glass, plastics, etc. and most commonly, thermoplastic
polymers are used.

Injection Moulding machine consists of following parts

a. Hopper
b. reciprocating screw
c. Heater
d. Nozzle
e. Fixed pattern
f. Movable pattern
• The reciprocating screw rotates by means of a motor and its reciprocating motion is provided
by the hydraulic system.
• The Plastic granules are to be poured into the hopper and they will be pass through the
chamber due to the rotation of the screw.
• The Heater heats the granules to its critical temperature.
• The thermoplastic molten liquid is pressurized (by the hydraulic system) outside the Assembly
and allowed to travel through a nozzle of small diameter(Dn)[injector] with high velocity and
low pressure into the space between the molds.
• The liquid will fill the mold with uniform compaction among the atoms and thereby density is
uniform.
• After filling the liquid in the mold, by the cooling process, it will be solidified.
Thermoforming

Thermoforming is the process where thermoplastic polymer sheet is heated & deformed into
desired shape. The process is widely used in packaging of consumer products and to fabricate
large items such as bathtubs, contoured skylights, and internal door liners for refrigerators.

Thermoforming consists of two main steps: heating and forming. Heating is usually accomplished
by radiant electric heaters, located on one or both sides of the starting plastic sheet at a distance
of roughly 125 mm (5 in.).

Duration of the heating cycle needed to sufficiently soften the sheet depends on the polymer, its
thickness and color.
Mechanical Thermoforming

Mechanical thermoforming, uses matching positive and negative molds that are brought
together against the heated plastic sheet, forcing it to assume their shape. In the pure
mechanical forming method, air pressure (positive or negative) is not used at all. The formed part
cools in the tooling and is subsequently demolded. Due to cooling down, the orientations of the
molecule chains keep their stretched positions.

Advantages
• Heavy parts can be produced (up to 125 kg)
• Large parts can be manufactured (up to 4 m2 )
• Flexible wall thickness (0.05 – 16 mm)
• Cost - effectiveness for small batches (tooling costs)
• Low costs for modifications and for color change
• Homogeneous multilayer applications are possible
Mechanical Thermoforming

Disadvantages
• Less scope for design (undercuts)
• No uniform distribution of wall thickness
• Temperature control is difficult
• For a given semifinished product, the manufacturer has no influence over the
formulation of the film, if dealing with purchased film.

Applications.
Thermoforming is a secondary shaping process, the primary process being that which produces
the sheet or film. Only thermoplastics can be thermoformed, since extruded sheets of
thermosetting or elastomeric polymers have already been cross-linked and cannot be softened
by reheating. Common thermoforming plastics are polystyrene, cellulose acetate and cellulose
acetate butyrate, ABS, PVC, acrylic (polymethylmethacrylate), polyethylene, and polypropylene.
Compression Moulding

• The compression molding process is used for temperature activated

thermosetting polymers.

• Compression Molding is a molding method in which the molding material

(especially Thermoplastics or Thermoset plastics) is generally preheated and is
placed in a mold cavity. The heating or cooling given to the cavity depends upon
the type of plastic used.

• Compression molding basically involves the pressing of a deformable material

charge between the two halves of a heated mold, and its transformation into a
solid product under the effect of the elevated mold temperature.

• Compression molding temperatures are often in the range 140-200 0C; mold
pressures can vary from 35 atm to 700 atm.
Compression Moulding
Compression moulding process takes place in following steps:
Step-1. Heating the mould.
The mould is heated to a certain temperature as per the plastic raw material requirement.
General temperature range is 165° - 182°C.

Step-2. Preheating the plastic

The material can be Sheet Moulding Compound (SMC), Bulk Moulding Compound (BMC), Thick
Moulding Compound (TMC) or the material can either be granulated powder or a preform tablet.
Preheating is done in a small convection heater.

Step-3. Placing the plastic in the cavity and mould closing

The preheated plastic is then placed into the mould cavity followed by closing the mould halves
together. After closing the mould, breathe cycle is introduced to remove any air bubbles trapped
inside. The pressure and temperature is then held for some period of time.
Step-4. Curing reaction
Curing is a chemical process employed in polymer chemistry and process engineering that
produces the toughening or hardening of a polymer material by cross-linking of polymer chains.
Compression Moulding
Compression moulding process takes place in following steps:
Step-4. Curing reaction
Curing is a chemical process employed in polymer chemistry and process engineering that
produces the toughening or hardening of a polymer material by cross-linking of polymer chains.

Step-5. Mould opening and Ejection

After the plastic is cured, the part can be removed from the mould. To remove the part, ejection
system is employed. The mould has ejector pins and ejector plates assembled on both halves
below the cavity and punch back plates. The plates push the ejector pins which remove the part
from cavity.
Compression Moulding
Compression moulding process takes place in following steps:
Step-4. Curing reaction
Curing is a chemical process employed in polymer chemistry and process engineering that
produces the toughening or hardening of a polymer material by cross-linking of polymer chains.

Step-5. Mould opening and Ejection

After the plastic is cured, the part can be removed from the mould. To remove the part, ejection
system is employed. The mould has ejector pins and ejector plates assembled on both halves
below the cavity and punch back plates. The plates push the ejector pins which remove the part
from cavity.
Advantages of Compression Moulding
1. Low running cost.
2. Good dimensional stability.
3. Density of part is uniform.
4. Shrinkage of part is uniform throughout.
5. No degradation of fibers during flow of plastic.
6. Great impact strength of part.
7. Uniform flow of plastic in entire cavity.
8. Warping and internal stresses are minimal.
9. Shorter lead time
Disadvantages
1. Initial cost is high.
2. Uneven parting lines are available.
3. Flash (scrap) produced cannot be recycled.
4. High cycle time as curing time is more.
5. Not suitable for complex parts as material may not flow in intricate gaps.

APPLICATIONS
1. Dinnerware like plates, bowls are made of melamine by compression moulding process.
2. Handles of utensils like cookers, pans are made using CM process.
3. In earlier times, door knobs were made with this process.
4. Television, telephone housings.
5. Radio housings.
6. Electrical parts like switches, switch boards, insulators.
7. Body and interior panels of cars, vans, etc.
Blow Moulding

• The basic principle of the blow molding process is to inflate a softened

thermoplastic hollow preform against the cooled surface of a closed mold,
where the material solidifies into a hollow product.

• Packing is the major area of application of small to medium-size disposable

blow molded products.

• Blow molded containers are also used for cosmetics, toiletries, pharmaceutical
and medical packaging and a variety of household products.
POWDER METALLURGY

PM is Metal processing technology in which parts are produced from metallic powders.

Powder metallurgy is the name given to the process by which fine powdered materials are
blended, pressed into a desired shape, and then heated to bond surfaces

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 ~ 97% of 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 PM
Basic Steps In Powder Metallurgy (P/M)

• Powder Production

• Blending or Mixing

• Compaction

• Sintering

• Finishing
Powder production:
Raw materials => Powder; Powders can be pure elements, pre-alloyed powders

Compaction: compaction is performed using dies machined to close tolerances. Dies are made of cemented carbide,
die/tool steel; pressed using hydraulic or mechanical presses.

The basic purpose of compaction is to obtain a green compact with sufficient strength to withstand further handling
operations.

Sintering: Performed at controlled atmosphere to bond atoms metallurgically; Bonding occurs by diffusion of atoms;
done at 70% of abs. melting point of materials.

It serves to consolidate the mechanically bonded powders into a coherent body having desired on service behavior
Densification occurs during the process and improvement in physical and mechanical properties are seen.
Furnaces – mesh belt furnaces (up to 1200C), pusher type furnace, batch type furnaces are also used.

Secondary operations: Operations include repressing, grinding, plating can be done; They are used to ensure close
dimensional tolerances, good surface finish, increase density, corrosion resistance etc.
Powder Production Techniques

Mechanical methods of powder production:

• Chopping or Cutting
• Abrasion methods
• Machining methods
• Milling

Chemical methods of powder production:

• Reduction of oxides
• Precipitation from solutions
• Thermal decomposition of compounds
• Hydride decomposition
• Thermit reaction
• Electro- chemical methods

Physical methods of powder production:

• Water atomization
• Gas atomization
Powder Production Techniques

Mechanical methods of powder production:

cheapest of the powder production methods; These methods involve using mechanical forces such as compressive
forces, shear or impact to facilitate particle size reduction of bulk materials.

Chopping or Cutting
In this process, strands of hard steel wire, in diameter as small as 0.0313 inches are cut up into small pieces by
means of a milling cutter

This technique is actually employed in the manufacturing of cut wire shots which are used for peening or shot
cleaning.

Abrasion Methods:
Rubbing of Two Surfaces:
When we rub two surfaces against each other, hard surface removes the material from the surface of soft material.
Powder Production Techniques

Mechanical methods of powder production:

Abrasion Methods:
b) Filing:
Filing as a production method has been frequently employed, especially to alloy powders, when supplies from
conventional sources have been unobtainable. Such methods are also used for manufacture of coarse powders of
dental alloys. Filing can also be used to produce finer powder if its teeth are smaller.

Machining: Mg, Be, Ag, solder, dental alloy are specifically made by machining; Turning and chips thus formed
during machining are subsequently crushed or ground into powders.

On lathe machine by applying small force we get fine chips. A large amount of machining scrap is produced in
machining operations. This scrap in the form of chips and turnings can be further reduced in size by grinding.
Powder Production Techniques
Mechanical methods of powder production:

Milling
During milling, impact, attrition, shear and compression forces are acted upon
particles.

During impact, striking of one powder particle against another occurs.

Attrition refers to the production of wear debris due to the rubbing action between
two particles.

Shear refers to cutting of particles resulting in fracture.

The particles are broken into fine particles by squeezing action in compression force type.
Ball Milling
• This contains cylindrical vessel rotating horizontally
along the axis. Length of the cylinder is more or less equal
to diameter. The vessel is charged with the grinding
media.

The grinding media may be made of hardened steel, or tungsten

carbide, ceramics like porcelain, alumina, zirconia.

During rolling of vessel, the grinding media & powder particles

roll from some height. This process grinds the powder materials
by impact/collision & attrition.

Milling can be dry milling or wet milling. In dry milling, about 25

vol% of powder is added along with about 1 wt% of a lubricant
such as stearic or oleic acid. For wet milling, 30-40 vol% of
powder with 1 wt% of dispersing agent such as water, alcohol or
hexane is employed.
Powder Production Techniques
Physical methods of powder production:
• Water atomization
• Gas atomization

Atomization
This uses high pressure fluid jets to break up a molten metal stream into very fine droplets,
which then solidify into fine particles.

High quality powders of Al, brass, iron, stainless steel, tool steel, superalloys are produced
commercially.
 GAS ATOMIZATION

Here, melted initial material is collapse with the gas within

the chamber. Heat is transferred from the liquid droplets
to the surrounding gas. And liquid solidifies.

Air, nitrogen, argon or helium are used, depending on the

requirements determined by the metal to be atomized.

The particle shape is spherical or close to spherical.

Irregular particle shapes can only be produced in systems
where reactions between the gas and the liquid metal
cause the formation of solid surface layers.

This is the case, for example, in the air atomization of

aluminium.
 WATER ATOMIZATION

In this method, High pressure water jets are used to bring about the
disintegration of molten metal stream. Water jets are used mainly because of
their higher viscosity and quenching ability. This is an inexpensive process
and can be used for small or large scale production. But water should not
chemically react with metals or alloys used.

In water atomization, a high pressure water stream is forced through nozzles

to form a disperse phase of droplets which then impact the metal stream. In
this method, large quantities of energy are required to supply the water at high
pressure

This production method is significant for low and high alloy steels, including
stainless steel. Because of oxide formation, water atomization is not likely to
be used in the atomization of highly reactive metals such as titanium and the
super alloys. In general, water atomized powders are irregular in shape,
with rough oxidized surfaces.
Powder Characterization Techniques:

Particle Size & Shape Distribution

Powder Structure (particle shape)

1-spherical
2- rounded or droplets
3-angular
4-acicular
5-dendritic
6-Flakes
7-porous
8-irregular
CHARACTERISTICS OF METAL POWDERS
1. Particle shape & size distribution
The shape of particles depends mainly on the method of production of powders, spheroidal shaped particles
have excellent sintering property and irregular shaped particles are good for moulding. Mostly 100μ size
powders are used.

2. Density
True density is mass per unit volume of the solid material apparent density is defined as the mass of loose
powder per unit actual volume filled by the powder it depends on particle shape, size distribution powders
with high apparent density require shorter compressive strike to produce a compact of given density and size.

3. Flow Rate
It is defined as the time required for a measured quantity of powder to flow out of a standard orifice flow rate
should be high to obtain high production rate.

4. Compressibility and Compression Ratio

Both depends upon shape size and size distribution of particles compressibility is defined as the ratio of
initial volume of the powder (Un pressed volume) to final volume green strength to powder also known as
mechanical strength of compressed part.
Scanning Electron Microscopy
In scanning electron microscopy, the electron beam scans the
sample in a raster pattern. First, electrons are generated at the
top of the column by the electron source. These are emitted
when their thermal energy overcomes the work function of the
source material. They are then accelerated and attracted by
the positively-charged anode.

The entire electron column needs to be under vacuum. Like all

components of an electron microscope, the electron source is
sealed inside a special chamber to preserve vacuum and
protect it against contamination, vibrations, and noise. Besides
protecting the electron source from being contaminated,
vacuum also allows the user to acquire a high-resolution image.
In the absence of vacuum, other atoms and molecules can be
present in the column. Their interaction with electrons causes
the electron beam to deflect and reduces the image quality.
High vacuum also increases the collection efficiency of
electrons by the detectors that are in the column.

Scanning Electron Microscope

Generally, two types of electromagnetic lenses are used:
The condenser lens is the first lens that electrons meet as they travel
towards the sample. This lens converges the beam before the electron
beam cone opens again and is converged once more by
the objective lens before hitting the sample. The condenser lens defines
the size of the electron beam (which defines the resolution), while the
main role of the objective lens is to focus the beam onto the sample.

The SEM’s lens system also contains scanning coils, which are used
to raster the beam onto the sample. In many cases, apertures are
combined with the lenses to control the size of the beam.
Ex: Image taken using SEM
Interparticle Friction & Flow Characteristics:

Friction between particles affects ability of a

powder to flow readily and pack tightly

A common test of interparticle friction is the

angle of repose, which is the angle formed by a
pile of powders as they are poured from a
narrow funnel

Smaller particle sizes generally

greater friction and steeper angles

Spherical shapes
the lowest interpartical friction Hall Flow Meter

As shape deviates from spherical, friction

between particles tends to increase
Powder Compaction
Powder compaction is the process of compacting powder in a die through the application of high pressures.

The density of the compacted powder increases with the amount of pressure applied.

1. Die compaction
2. Iso static Pressing
3. Injection Moulding
4. Powder Extrusion
5. Slip Casting
6. Tape Casting
1. Die compaction
In this process, loose powder is shaped in
a die using a mechanical or hydraulic
press giving rise to densification. The
mechanisms of densification depend on
the material and structural characteristics
of powder particles.

Die compaction Stages

i) charging the powder mix
ii) applying load using a
punch (uni-) or double punch (bi-) to
compact powders
iii) removal of load by retracting the
punch
iv) ejection of green compact
 Isotactic Pressing
CIP is a compaction process in which isostatic fluid pressure is applied to a powder mass at room
temperature to compact it into desired shape. The powder parts can be compacted up to 80-90 % of
their theoretical densities. Water or oil can be used as pressuring medium.

In this process, pressure is applied simultaneously and equally in all directions using a fluid to
an elastomeric fluid with powder at room temperature.

Sintered CIP component can reach up to 97 % of theoretical density. Steps in this process is
shown in flowchart.

During pressing, high density is achieved at a low pressure, while the green strength of the
compact rises linearly with pressure.

The pressure applied can range from 100- 400 MPa.

• Initially the applied stress
(exactly shear stress) serves to
improve the density of the
compact by particle sliding and
rotation. In the next stage,
deformation of powder
particles occur and particle
characteristics like shape play
vital role in deciding this stage.
Advantages
• Uniform, controlled, reproducible densification of powder;
• long, slender parts can be pressed;
• neat net shape forming;
• short production times;
• economy of operation for
• complex and large parts.

Applications:
• Metallic filters made from bronze, brass, stainless steel, Inconel, Monel, Titanium, high
speed tools, carbide tools.

• Also ceramic parts such as sparks plugs and insulators are made by this method.
Slip casting

The slip is a mixture of ceramic powder, water and additives. The slip is poured into a porous plaster mold

and left standing while water is absorbed into the mold.

Steps in slip casting:
i) Preparing assembled plaster mould,

ii) filling the mould,

iii)absorption of water from the slip into the porous mould,

iv) removal of part from the mould,

v) trimming of finished parts from the mould

• Sometimes mould release agents like oil, graphite can be used.

• Hollow and multiple parts can be produced

Slip casting
• Advantages of slip casting:
Products that can not be produced by pressing operation can
be made, no expensive equipment is required, works best with finest powder particles

• Disadvantage:
slow process, limited commercial applications

• Applications: tubes, boats, crucibles, cones, turbine blades, rocket guidance fins; Also
products with excellent surface finish like basins, water closets.
Tape casting
• Tape casting (also called doctor blading and knife coating) is a casting process used in the
manufacture of thin ceramic tapes and sheets from ceramic slurry.

• The ceramic slurry is cast in a thin layer onto a flat surface and then dried and sintered.
Tape casting
• Tape casting (also called doctor blading and knife coating) is a casting process used in the
manufacture of thin ceramic tapes and sheets from ceramic slurry.

• This process involves preparing a dispersion of metal or ceramic powder in a suitable

solvent with the addition of dispersion agent (to improve the dispersion of the particles).
Then a binder is added and fed to a reservoir. Whole mixture is fed on to a moving carrier
film from the bottom of the reservoir.

• This slurry layer is deposited on the film by the shearing action of a blade. The slurry
should be free of air bubbles, otherwise result in porosity. During sintering, the binder is
burnt off first and densification of material occurs.

• The ceramic slurry is cast in a thin layer onto a flat surface and then dried and sintered.
Tape casting
Powder Extrusion
Sintering
In the sintering operation, the pressed-powder compacts are heated in a controlled
atmosphere to right below the melting point.

Three stages of sintering

1. Burn-off (purge)- combusts any air and removes lubricants or binders that would
interfere with good bonding.

2. High-temperature- desired solid-state diffusion and bonding occurs.

3. Cooling period- lowers the temperature of the products in a controlled atmosphere.

• All three stages must be conducted in oxygen-free conditions

Sintering
Types of sintering
a) solid state sintering – This is the commonly occurring
consolidation of metal and alloy powders. In this, densification occurs mainly because
of atomic diffusion in solid state.

b) Liquid phase sintering – The densification in improved by employing a small amount

of liquid phase (1-10% vol). The liquid phase existing within the powders at the
sintering temperature has some solubility for the solid. Sufficient amount of liquid is
formed between the solid particles of the compact sample.
During sintering, the liquid phase crystallizes at the grain boundaries binding the grains.
During this stage, there is a rapid rearrangement of solid particles leading to density
increase. In later stage, solid phase sintering occurs resulting in grain coarsening and
densification rate slows down.
Used for sintering of systems like tungsten-copper and copper-tin. Also covalent
compounds like silicon nitride, silicon carbide can be made, that are difficult to sinter.
Types of sintering
c) Activated sintering – IN this, an alloying element called ‘doping’ is added in small
amount improves the densification by as much as 100 times than undoped compact
samples. Example is the doping of nickel in tungsten compacts.

d) Reaction sintering – IN this process, high temperature materials resulting from chemical
reaction between the individual constituents, giving very good bonding. Reaction sintering
occurs when two or more components reacts chemically during sintering to create final part.
A typical example is the reaction between alumina and titania to form aluminium titanate at
1553 K which then sinters to form a densified product.

Other than mentioned above, rate controlled sintering, microwave sintering, gas plasma
sintering, spark plasma sintering are also developed and practiced.
Types of sintering
c) Activated sintering – IN this, an alloying element called ‘doping’ is added in small
amount improves the densification by as much as 100 times than undoped compact
samples. Example is the doping of nickel in tungsten compacts.

d) Reaction sintering – IN this process, high temperature materials resulting from chemical
reaction between the individual constituents, giving very good bonding. Reaction sintering
occurs when two or more components reacts chemically during sintering to create final part.
A typical example is the reaction between alumina and titania to form aluminium titanate at
1553 K which then sinters to form a densified product.

Other than mentioned above, rate controlled sintering, microwave sintering, gas plasma
sintering, spark plasma sintering are also developed and practiced.
Applications of powder metallurgy

• Production of porous metal filters: Typical filter shapes that can be produced from the
powder include discs, cups, bushings, sheets, tubes. The major advantages of porous
filters include high temperature resistance, good mechanical strength, corrosion, long
service life.

• Self lubricating Bearings

A self-lubricating sintered bearing is a metallic component with high porosity (20-25% in
volume), impregnated in a lubricant oil. The oil contained in the porosity provides a constant
lubrication between bearing and shaft, so the system does not need any additional external
lubricant. Self-lubrication allows this type of sliding bearing to work under hydrodynamic
conditions, resulting in a very low friction coefficient.