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MM 362

Ceramics and Glasses


Spring Semester 2020, FMCE, GIKI

Lecture 16 - 21

Instructor:
Muzammil Irshad
Lecturer

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Ceramic Shaping and Forming
Shaping and Forming

 Binder is a component that is added to hold the powder together while


we shape the body (vinyl alcohol, ethylene glycol, Borax).
 Binder provides the plasticity necessary for forming and green strength.

 Slurry is a suspension of ceramic particles in a liquid (As the amount of


water is decreased it becomes more solid.)

Plasticizer is the component of a binder that keeps it soft or pliable; it


improves the rheological properties (Glycerine, Ethylene glycol).

 Green is a ceramic before it is fired. Brown, white, or gray potter’s


clays are well known green ceramics.
 A transition state between the loose powder and the high-density
sintered product (bonds between the grains are not strong).

 Slip is the liquid-like coating used to form the glaze when fired.

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Ceramic Shaping and Forming

Shaping and Forming: Various additives

 Suspending agents required to prevent solids from settling within the slurry. (e.g. Methyl
cellulose)

 Deflocculating agents aid in the formation of slurries by preventing the agglomeration of


fine particles (e.g. Monoethylamine).

 Some slurries have a tendency to foam during mixing. Antifoaming agents or defoamers
may be used to control this action.

 Chemical activators also may be used as additives to aid in subsequent sintering or


processing of powders.

What is the difference between suspension and colloid ?

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Ceramic Shaping and Forming
Shaping and Forming

 Many shaping methods are used for ceramic products and these can
be grouped into three basic categories:

1) Powder compaction: dry pressing, hot pressing, cold isostatic


pressing, etc. (Powder compaction is simply the pressing of a free
flowing powder).

2) Casting: using a mold with the ceramic as, or containing, a liquid or


slurry poured into a porous mold.

3) Plastic forming: extrusion, injection molding, etc. using pressure to


shape the green ceramic

 Plastic forming consists of mixing the ceramic powder with a large


volume fraction of a liquid to produce a mass that is deformable
(plastic) under pressure.
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Ceramic Shaping and Forming
Shaping and Forming: Dry Pressing.

 Dry pressing is ideally suited to the formation of simple solid shapes and consists of three basic
steps: filling the die, compacting the contents, and ejecting the pressed solid.

 Low capital equipment costs it is the most widely used high-volume forming process for ceramics.

 Formation of simple solid shapes.


Three basic steps

 Filling the die

 Compacting the contents


 Small flat parts such as insulators, chip carriers, or cutting tools can be
produced at rates up to several thousand per minute.  Ejecting the pressed solid

 The pressure used in dry pressing as high as 300 MPa.


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Ceramic Shaping and Forming
Shaping and Forming: Hot Pressing

 In hot pressing the die assembly is contained within a high


temperature furnace.

 During hot pressing the ceramic powders may sinter


together to form a high-density component (We can densify
materials without binders)

 Dies for use at high temperatures are expensive and do not


generally last long.

 Hot pressing is limited to simple solid shapes, such as flat


plates, blocks, and cylinders.

 We can densify at temperatures lower than those needed for


conventional pressureless sintering.

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Ceramic Shaping and Forming (Hot Pressing)

Properties Of Graphite Die

 Graphite is the most widely used die material and can be used at
temperatures up to 2200°C and pressures between 10 and 30 MPa.

 It is easy to machine (but the dust is toxic if inhaled—like coal dust).

 It is inexpensive.

 Its strength increases with increasing temperature.

 It has good creep resistance.

 It has excellent thermal conductivity.

 It has a relatively low coefficient of thermal expansion.

Why metallic die has a little use above 1000C?

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Ceramic Shaping and Forming
Shaping and Forming: Hot Pressing

 Inductive heating is generated via application of a high frequency electromagnetic field using an induction coil
The Heating rate has to be controlled since:
 An extremely slow cooling rate will result grain growth

 Extremely fast cooling rates will generate thermal stresses and can damage the mold itself.

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Ceramic Shaping and Forming: Hot pressing
Indirect Resistance Heating:
 The mold containing the ceramic is placed in a chamber
 The chamber is resistive heated via a separate heating element present in the chamber itself
 The I2R effect allows heating of the heating element and convective heating heats up the mold
 Ceramic in the mold is heated indirectly from the heating element then to the mold, this type of heating is called
IRH (generally takes longer time)
 First the chamber attains the targeted temperature and then only the mold surface attains the required temperature

Direct heating:

 Mold is connected to the power supply and is heated directly via resistive heating by passing current through it.

 The direct contact allows rapid heating of the mold and enhances power activity in achieving sintering in short
durations and at lower temperatures.

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Ceramic Shaping and Forming: Hot pressing (Types of products)

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Ceramic Shaping and Forming
Shaping and Forming: Isostatic pressing
 Isostatic pressing involves the application of hydrostatic pressure to a powder in a flexible container (pressure
applied through a liquid or gaseous medium surrounding the compacted part).

Advantage of applying the isostatic pressure?


The advantage of applying pressure in all directions is that there is more uniform compaction of the powder and
more complex shapes can be produced than with uniaxial pressing.

 95% of theoretical density


can be achieved for ceramics.

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Shaping and Forming (Cold Isostatic Pressing)
CIP

A flexible (polyurethane) mold


immersed in a pressurized liquid medium
(commonly water) is used in the cold
isostatic pressing method.

 There are two types of cold isostatic


pressing: wet bag and dry bag.

 In the wet bag method the mold is


removed and refilled after each pressure
cycle.

 In the dry bag method the mold is an


integral part of the vessel.

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Shaping and Forming (Cold Isostatic Pressing)
Wet-bag CIP
 Powder is weighed into a rubber bag and a metal mandrel is inserted that makes a seal with the mouth of the
rubber bag.
 The sealed bag is placed inside a high-pressure chamber
 Fluid (soluble oil/water mixture)
 Pressure 20-1000 MPa
 After pressing, pressure is released, remove mold then component.
 Used to produce laboratory samples and low-volume production parts

Dry-bag CIP
 The main distinction is that the rubber mold is now an integral part of the press.
 High-pressure fluid is applied through channels in the mold.
 After pressing, the pressed part is removed without disturbing the mold.
 Production rates 1 part per second; industrially.
 For example production of spark plugs are.
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Wet-bag CIP

Dry-bag CIP

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Shaping and Forming (Cold Isostatic Pressing)

 Manufacturing of Spark plugs:

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Shaping and Forming
Hot isostatic pressing (HIP)
 The hot isostatic press (HIP) uses the simultaneous application of heat and
Isostatic pressure (Used for tool bits, ball bearing, pump components Biomedical
implants etc.) piezoelectric ceramics such as BaTiO3, SrTiO3, and lead zirconate
titanate (PZT)

 As a pressure medium a gas (Nitrogen or Argon) is used.

 The work pressures 100 MPa to 300 Mpa.

There are two variants of HIPing:


 Encapsulated: using a deformable container
 Not encapsulated: it is shaped and sintered first, then HIPed

What is the draw back of uniaxial pressing?


Drawback of uniaxial pressing is that top and bottom surfaces get compressed more
compared to the core and sides of the ceramic sample

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Shaping and Forming
Hot isostatic pressing (HIP)

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Ceramic Shaping and Forming
Shaping and Forming: Slip Casting:
 Low cost process used for mass-production of pottery.
 Mold are made of plaster, which pulls water out of clay.
 Slip consists of fine (<10 μm) ceramic powder particles that
are suspended in a fluid (water).
 Liquid clay body is poured into plaster moulds.
 Layer is formed on the inside cavity of the mould.
 The cast piece is removed from the mould and allowed to dry
(green-ware piece).
 Then furnace fired, with or without decoration and glaze.  Ceramic powders are mixed
with a viscous liquid such as
 Production of complex shapes, sanitary-ware, basins and polyvinyl alcohol or
methylcellulose and water to
alumina crucibles, gas turbine-rotors. produce a plastically deformable
mass.

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Ceramic Shaping and Forming
Shaping and Forming: Slip Casting:
The process of transforming your clay into a slip is called the
slaking (disintegrate) process. Slip Casting
 Different clays have different slaking times, so It’s important
to use the same types of clay so it can be successfully fired at
the same temperature.
How to pour out the casting Slip?
Carefully pour your slip into the cavity of the mold and the
plaster of Paris mold will start to absorb water from the clay
and the drying process of the clay will begin. Once the clay has
started to dry to a suitable thickness (the timing will depend on
the size of the mold, but for a medium/small mold, 10 minutes  Deflocculation is to "disperse the particles
should do), then you can pour out the excess clay slip. in a slip so that less water is required to make
the slip fluid." A few drops of sodium silicate
 Molds are made from plaster of Paris (CaSO4.2H2O) as can be used to achieve this.
they’re highly absorbent.

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Ceramic Shaping and Forming
Shaping and Forming: Extrusion:
 Extrusion is a process where a ceramic billet is
pushed through a die

 Extrusion involves forcing a deformable mass


through a die orifice

 The process is widely used to produce ceramic


components having a uniform cross section and a large
length-to-diameter ratio such as Ceramic tubes and
rods bars.

 Clay with a suitable rheology for the extrusion


process (essentially a paste) can be made by
controlling the amount of water.

 one end of die is kept open (which is the required


cross section). A ram to push it through the die
opening.
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Ceramic Shaping and Forming

Shaping and Forming: Extrusion:


Direct extrusion
The direction of material flow and ram pushing are in the same direction
Indirect Extrusion:
The direction of material flow and ram pushing are opposite to each other

Disadvantage of Direct extrusion:


 Higher frictional forces experienced on the entire surface of the billet
 Those must be overcome in forcing the billet through the opening of the die
on the opposite end
 Very high pressures are required

Advantage of Indirect Extrusion:


 only the frictional forces of the material coming out need to be overcome.
 This allows extrusion of bigger cross sections, enhancing extrusion speeds,
and with less heating due to the reduced friction.
 The life of the die is enhanced as well

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Shaping and Forming: Extrusion:

compositions of extrusion bodies

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Ceramic Shaping and Forming

Shaping and Forming: Extrusion:

Limitations of Extrusion process:


 Limitation on the length of the extruded material dictated by the
maximum length of the ram push-rod.
 The surface impurities of the initial billet may affect the surface of the
extruded material and spoil its aesthetics

Advantage of Extrusion process:


 Complex cross-sectional geometry can be attained

Applications in modern ceramics:


 Alumina shells for sodium vapor lamps
 Manufacturing of the honeycomb-shaped catalyst supports for
automotive emission-control devices (i.e. catalytic convertor, DPF)

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Catalytic convertor
Ceramic Shaping and Forming
Shaping and Forming: Extrusion:
Honeycomb-shaped catalytic convertor in cars

Cordierite (Mg2Al4Si5O18 )
Cordierite (a magnesium aluminosilicate), is used as a substrate
and support for catalysts in catalytic converters.
 Silicon carbide (SiC) is also used as a DPF material.
Why it is chosen ?
It benefits from a higher melting point than cordierite
It is lightweight, have low thermal expansion, can operate at very
high temperatures without melting, and conducts heat poorly
(helping to retain exhaust heat for improved catalytic efficiency).
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Ceramic Shaping and Forming

 Ceramic parts (Automotive) offer the distinct advantages of lower


fuel consumption (due to their higher operating temperatures, higher
thermal efficiency, and lighter weight) and reduced exhaust emissions
(because of the more complete combustion of fuel at higher operating
temperatures). The outstanding wear resistance of ceramics is also
advantageous.
Acicular Mullite

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Ceramic Shaping and Forming

Shaping and Forming: Hot Rolling (e.g Al2O3 in Al Matrix)

 Hot rolling is the process of passing the slab or billet through rolls
(at high temperatures) for achieving reduced cross section or required
shape.

 Two or more horizontal rolling cylinders rotate in opposite


directions

 Billet to pass through a cross section that is reduced from the


original cross section of the billet

 Ceramic billet experiences compressive forces perpendicular to


the rolling direction.

 The material is pushed forward owing to compressive stresses,


and frictional forces induce shear and help in refining the grains.

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Ceramic Shaping and Forming

Shaping and Forming: Injection Molding

 Injection molding is another technique that is widely used in


shaping thermoplastic polymers.

 For forming and shaping ceramic components can also be


applied and if the ceramic powder is added to a thermoplastic
polymer

 The polymer is usually referred to as the binder (called the


material a ceramic-loaded polymer)

 The ceramic powder is added to the binder

 Usually mixed with several other organic materials to


provide a mass that has the desired rheological properties

 The major limitation is that the initial tooling costs of the


mold can be quite high.
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Ceramic Shaping and Forming
Shaping and Forming: Injection Molding
 The plastic mass is first heated, at which point the thermoplastic polymer Turbine Blades
becomes soft, then forced into a mold cavity

 The mixture is allowed to cool in the mold during which time the thermoplastic
polymer hardens

 Injection molding is used to fabricate ceramic components with complex


shapes

 Cycle times can be rapid (10 sec), injection molding can be a high-volume
process.

 Because of the large volume fraction of organic material there is a high degree
of shrinkage

 Shrinkage of 15–20% is typical, so precise control of component dimensions is


difficult.
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Ceramic Shaping and Forming
Shaping and Forming: Injection Molding
 The additives that have been used to form SiC shapes by injection molding.
 The organic part of the mix accounts for about 40 vol%

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Ceramic Shaping and Forming
Ceramic Tape Casting:

 Tape casting is a casting process used in


the manufacture of ceramic tapes from
ceramic slurry.

 The Tape Casting process involves the


casting the slurry onto a flat moving carrier
surface.

 The slurry usually consists of a ceramic


powder with the appropriate additions of
solvents plasticisers and binders.

 The ceramic tape produced can be used


for a variety of purposes, including the
manufacture of electronic components such
as ceramic capacitors, piezoelectrics.
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Ceramic Shaping and Forming
Shaping and Forming: Rapid prototyping

Rapid prototyping (RP) or solid freeform fabrication (SFF) is


used to form ceramic Components
These are based on a common principle:
 Computer directly controls the shaping process by accessing
computer-aided design (CAD) files.

 RP can be use to form 3D component without the use of a


die or a mold.

 It is used for the fabrication of parts from polymers for


design verification and form-and fit applications.

 These techniques have more recently been applied to


forming parts out of ceramics
1. Stereolithography (SLA)
2. Fused deposition modeling (FDM)
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Ceramic Shaping and Forming

Stereolithography
In SLA the component is formed from an epoxy resin
This machine has four important parts:
1. A tank filled with several gallons of liquid photopolymer. The
photopolymer is a clear, liquid plastic.
2. A perforated platform immersed in the tank. The platform can
move up and down in the tank as the printing process proceeds.
3. An ultraviolet laser
4. A computer that drives the laser and the platform

To form ceramic components by SLA the polymer must be loaded


with ceramic powders e.g. Si3N4, SiO2 and Al2O3 powders
 One of the advantages of stereolithography is its speed Prototypes
 A photopolymer or light-activated resin is a
and designs made with stereolithography are strong enough to polymer that changes its properties when exposed to
be machined and can also be used to make master patterns light e.g. styrene, and acrylates.
for injection molding.
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Ceramic Shaping and Forming: Stereolithography

 The action of the laser is to harden (cure) the


photosensitive polymer where the beam strikes
the liquid, forming a solid layer of plastic and
adhere to the platform. When the initial layer is
completed, the platform is lowered by a distance
equal to the layer thickness and a second layer is
formed on top of the first by the laser and so on.

 This process is repeated again and again until


the entire object has been formed and is fully
submerged in the tank.

The platform is then raised to expose a three-


dimensional object.

After it is rinsed with a liquid solvent to free it


of excess resin, the object is baked in an
ultraviolet oven to further cure the plastic.

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Ceramic Shaping and Forming
Fused deposition Modeling (FDM):

 FDM 3D printer technique use a thermoplastic filament, which is


heated to its melting point and then extruded, layer by layer, to create a
three dimensional object.

 The source material is a thermoplastic polymer filament that is


heated and extruded to form the product.

 The computer controls the x–y position of the filament and the
deposition rate

 The filament can be loaded with up to 60 vol % ceramic powders;


once the part is completed the binder is removed and the part is
sintered.

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Ceramic Shaping and Forming
Shaping and Forming:
Fused deposition of ceramics (FDC)
 It is a modified FDM process where ceramic powder loaded
thermoplastic filaments are extruded through the FDM.

 During fused deposition of ceramics, thermoplastic polymers


melt carry the ceramic powders along with it.

 The green ceramic parts are similar to injection-molded parts


having 40-45 volume % binder in it.

 Post operations in the FDC process could include trimming


(parts while in the green state before binder removal and Sintering).

 The parts are then subjected to a binder removal and sintering


cycle for densification.

 Binder system development is a major key to a successful FDC


process. (also powder size and distribution)
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Ceramic Shaping and Forming

Fused deposition of ceramics (FDC)

What is binder system and its significance ?


 The binder system could be viewed as a parent that nurtures a child until the child is able to live on
his/her own.

 A binder system with low viscosity, high strength, high strain, high modulus and easy binder burnout
would enable the green filament to be easily fabricated in the FDC (Fused deposition of ceramics)
process into green structures and the green structures to survive the post processing.

Why the properties of ceramic powder are important ?

 The most important parameters one needs to consider when choosing ceramic powders are surface
area, chemical composition, particle size and their distribution. For example, fine grained, wide-size
distribution ceramic powders lower the overall viscosity of the FDC mixture during compounding.

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Ceramic Machining:
Machining

Powder processing process produces near net shape products.

In many cases some machining of the ceramic compact is necessary to

1. Meet dimensional tolerances

2. Improve the surface finish

3. Remove surface flaws

Types of machining

Green machining

Final machining (after sintering/firing machining)

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Ceramic Machining:
Machining:
Green machining
 Machine a ceramic compact before sintering.
 Green machining have many advantages over sintered product
machining.
 Reduction in machining time i.e. 10X
 Reduction in machining cost i.e. 20X
Final machining
 Tool costs are high because ceramics are hard and brittle,
Diamond tools.
 Long machining time.
 Grinding, lapping, sand-blasting and water jet machining are used
for machining.

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