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METALURGIA DE POLVOS

PROCESAMIENTO DE
CERAMICAS Y CERMETS

ME477 Lecture 08 1
METALURGIA DE POLVOS
• CARACTERISTICAS
• PRODUCCION DE LOS POLVOS
• PRESION Y SINTERIZADO
• ALTERNATIVAS DE PRENSADO Y ZINTERIZADO
• MATERIALES MAS USADOS
• CONSIDERACIONES DE DISEÑO

ME477 Lecture 08 2
METALURGIA DE POLVOS

Metodo para producir piezas metalicas a partir de la mezcla de


polvos metalicos y no metalicos
1. Los productos obtenidos mediante este proceso no requieren
de acabado
2. Se pueden obtener piezas solidas y tambien porosas
3. Los materiales que requieren altas temperaturas se producen
facilmente con este proceso (filamentos de tungsteno)
4. Se obtien productos de alta precision.
5. Es factible automatizar los procesos

ME477 Lecture 08 3
LIMITACIONES Y DESVENTAJAS
• Alto costo del equipo y herramientas
• Alto costo de los polvos metalicos
• Dificultades en el almacenamiento
• Peligros de incendios
• Degradacion
• Variaciones de la densidad
• Se puede fabricar productos grandes 20 a 30 kilos, pero la
mayoria de los productos estan alrededor de los 3 kilos

ME477 Lecture 08 4
CARACTERISTICAS DE LOS
POLVOS
La forma de los polvos se puede definir mediante los
siguientes atributos:
1. Tamaño de las particulas y su distribucion
2. Forma y estructura interna interna de las
particulas
3. Area superficial

ME477 Lecture 08 5
MEDIDAS DE LAS PARTICULAS

• Si la forma de la particula es esferica, una sola


medida es adecuada
• Para otras formas se requiere de dos o mas
dimensiones
• Se utiliza mallas para tener las medidas de las
particulas
• Una malla 200 significa que se tiene 200 aberturas
por pulgada lineal
• Entonces en una pulgada cuadrada se tiene
200x200 = 40000
ME477 Lecture 08 6
Figura 16.2 - Malla de criba para seleccionar tamaños de particulas

ME477 Lecture 08 7
Figura 16.3 - varias formas posibles de particulas

ME477 Lecture 08 8
FRICCION ENTRE PARTICULAS Y
CARACTERISTICAS DE FLUJO
• La friccion entre particulas afecta la disposicion a fluir
y a compactarse, el angulo de reposo es un buen
indicador, los angulos grandes indican alta friccion,
las particulas de menor tamaño tienen mayor friccion
y generan grandes angulos

Figura 16.4 friccion interparticular,


a mayor angulo mayor
friccion

ME477 Lecture 08 9
DENSIDAD DE LAS PARTICULAS
• Densidad real: Densidad del volumen verdadero del material
• Densidad volumetrica: es la densidad de los polvos en el
estado suelto despues de vaciado, esto incluye los poros
• Factor de empaquetamiento: Es la relacion entre la densidad
volumetrica entre la densidad real
• POROSIDAD + FACTOR DE EMPAQUETAMIENTO = 1

ME477 Lecture 08 10
Production of Metallic Powders
• In general, producers of metallic powders are not the
same companies as those that make PM parts
• Virtually any metal can be made into powder form
• Three principal methods by which metallic powders
are commercially produced
1. Atomization
2. Chemical
3. Electrolytic
• In addition, mechanical methods are occasionally
used to reduce powder sizes

ME477 Lecture 08 11
Gas Atomization Method
High velocity gas stream flows through an expansion
nozzle, siphoning molten metal from below and
spraying it into a container
• Droplets solidify into powder form

Figure 16.5 (a) gas


atomization method

ME477 Lecture 08 12
Conventional Press and Sinter

• After the metallic powders have been produced, the


conventional PM sequence consists of three steps:
1. Blending and mixing of the powders
2. Compaction - pressing into desired part shape
3. Sintering - heating to a temperature below the melting point to
cause solid-state bonding of particles and strengthening of part
• In addition, secondary operations are sometimes
performed to improve dimensional accuracy, increase
density, and for other reasons

ME477 Lecture 08 13
Figure 16.7 - Conventional powder metallurgy production sequence: (1) blending, (2)
compacting, and (3) sintering; (a) shows the condition of the particles while (b)
shows the operation and/or workpart during the sequence

ME477 Lecture 08 14
Blending and Mixing of Powders

• For successful results in compaction and sintering, the


starting powders must be homogenized
• Blending - powders of the same chemistry but possibly
different particle sizes are intermingled
– Different particle sizes are often blended to reduce porosity
• Mixing - powders of different chemistries are combined
– PM technology allows mixing various metals into alloys that would
be difficult or impossible to produce by other means

ME477 Lecture 08 15
Compaction
Application of high pressure to the powders to form them into
the required shape
• The conventional compaction method is pressing, in which
opposing punches squeeze the powders contained in a die
• The workpart after pressing is called a green compact, the
word green meaning not yet fully processed
• The green strength of the part when pressed is adequate for
handling but far less than after sintering

ME477 Lecture 08 16
Figure 16.9 - Pressing in PM: (1) filling die cavity with powder by
automatic feeder; (2) initial and (3) final positions of upper and
lower punches during pressing, and (4) ejection of part

ME477 Lecture 08 17
Sintering
Heat treatment to bond the metallic particles, thereby
increasing strength and hardness
• Usually carried out at between 70% and 90% of the metal's
melting point (absolute scale)
• Generally agreed among researchers that the primary
driving force for sintering is reduction of surface energy
• Part shrinkage occurs during sintering due to pore size
reduction

ME477 Lecture 08 18
Figure 16.12 - Sintering on a microscopic scale: (1) particle
bonding is initiated at contact points; (2) contact points grow into
"necks"; (3) the pores between particles are reduced in size; and
(4) grain boundaries develop between particles in place of the
necked regions

ME477 Lecture 08 19
Densification and Sizing
Secondary operations are performed to increase density,
improve accuracy, or accomplish additional shaping of the
sintered part
• Repressing - pressing the sintered part in a closed die to
increase density and improve properties
• Sizing - pressing a sintered part to improve dimensional
accuracy
• Coining - pressworking operation on a sintered part to press
details into its surface
• Machining - creates geometric features that cannot be
achieved by pressing, such as threads, side holes, and other
details

ME477 Lecture 08 20
Impregnation and Infiltration
• Porosity is a unique and inherent characteristic of PM
technology
• It can be exploited to create special products by filling the
available pore space with oils, polymers, or metals
• Two categories:
1. Impregnation
2. Infiltration

ME477 Lecture 08 21
Impregnation
The term used when oil or other fluid is permeated into
the pores of a sintered PM part
• Common products are oil-impregnated bearings,
gears, and similar components
• An alternative application is when parts are
impregnated with polymer resins that seep into the
pore spaces in liquid form and then solidify to create
a pressure tight part

ME477 Lecture 08 22
Infiltration
An operation in which the pores of the PM part are filled
with a molten metal
• The melting point of the filler metal must be below
that of the PM part
• Involves heating the filler metal in contact with the
sintered component so capillary action draws the filler
into the pores
• The resulting structure is relatively nonporous, and
the infiltrated part has a more uniform density, as well
as improved toughness and strength

ME477 Lecture 08 23
Materials and Products for PM
• Raw materials for PM are more expensive than for
other metalworking because of the additional energy
required to reduce the metal to powder form
• Accordingly, PM is competitive only in a certain range
of applications
• What are the materials and products that seem most
suited to powder metallurgy?

ME477 Lecture 08 24
PM Materials – Elemental Powders

A pure metal in particulate form


• Used in applications where high purity is important
• Common elemental powders:
– Iron
– Aluminum
– Copper
• Elemental powders are also mixed with other metal
powders to produce special alloys that are difficult to
formulate by conventional methods
– Example: tool steels

ME477 Lecture 08 25
PM Materials – Pre-Alloyed Powders
Each particle is an alloy comprised of the desired
chemical composition
• Used for alloys that cannot be formulated by mixing
elemental powders
• Common pre-alloyed powders:
– Stainless steels
– Certain copper alloys
– High speed steel

ME477 Lecture 08 26
PM Products

• Gears, bearings, sprockets, fasteners, electrical contacts,


cutting tools, and various machinery parts
• Advantage of PM: parts can be made to near net shape or
net shape
– They require little or no additional shaping after PM processing
• When produced in large quantities, gears and bearings are
ideal for PM because:
– The geometry is defined in two dimensions
– There is a need for porosity in the part to serve as a reservoir for
lubricant

ME477 Lecture 08 27
PM Parts Classification System
• The Metal Powder Industries Federation (MPIF)
defines four classes of powder metallurgy part
designs, by level of difficulty in conventional pressing
• Useful because it indicates some of the limitations on
shape that can be achieved with conventional PM
processing

ME477 Lecture 08 28
Figure 16.16 - Four classes of PM parts (side view shown;
cross-section is circular): (a) Class I - simple thin shapes,
pressed from one direction; (b) Class II - simple but thicker
shapes require pressing from two directions; (c) Class III - two
levels of thickness, pressed from two directions; and (d) Class
IV - multiple levels of thickness, pressed from two directions,
with separate controls for each level

ME477 Lecture 08 29
PROCESSING OF CERAMICS
AND CERMETS
• Processing of Traditional Ceramics
• Processing of New Ceramics
• Processing of Cermets
• Product Design Considerations

ME477 Lecture 08 30
Types of Ceramics and Their
Processing
• Ceramic materials divide into three categories:
1. Traditional ceramics – particulate processing
2. New ceramics – particulate processing
3. Glasses – solidification processing

ME477 Lecture 08 31
Overview of Ceramics Particulate
Processing
• Traditional ceramics are made from minerals
occurring in nature
– Products include pottery, porcelain, bricks, and cement
• New ceramics are made from synthetically produced
raw materials
– Products include cutting tools, artificial bones, nuclear fuels,
and substrates for electronic circuits
• The starting material for all of these items is powder

ME477 Lecture 08 32
Overview of Ceramics Particulate
Processing - continued
• For traditional ceramics, the powders are usually mixed
with water to temporarily bind the particles together and
achieve the proper consistency for shaping
• For new ceramics, substances other than water are
used as binders during shaping
• After shaping, the green parts are fired (sintered),
whose function is the same as in powder metallurgy:
– To effect a solid state reaction which bonds the material into a
hard solid mass

ME477 Lecture 08 33
Figure 17.1 - Usual steps in traditional ceramics processing: (1)
preparation of raw materials, (2) shaping, (3) drying, and (4) firing
Part (a) shows the workpart during the sequence, while (b) shows the
condition of the powders

ME477 Lecture 08 34
Preparation of the Raw Material
for Traditional Ceramics
• Shaping processes for traditional ceramics require the
starting material to be a plastic paste
– This paste is comprised of fine ceramic powders mixed with water
• The raw ceramic material usually occurs in nature as rocky
lumps, and reduction to powder is the purpose of the
preparation step in ceramics processing

ME477 Lecture 08 35
Comminution

Reducing particle size in ceramics processing by use of


mechanical energy in various forms such as impact,
compression, and attrition
• Comminution techniques are most effective on brittle
materials such as cement, metallic ores, and brittle
metals
• Two general types of comminution operations:
1. Crushing
2. Grinding

ME477 Lecture 08 36
Jaw Crusher
Large jaw toggles back and forth to crush lumps against
a hard, rigid surface

Figure 17.2 -
Crushing operations: (a)
jaw crusher

ME477 Lecture 08 37
Roll Crusher
Ceramic lumps are squeezed between rotating rolls

Figure 17.2 - Crushing operations: (c) roll crusher

ME477 Lecture 08 38
Grinding

In the context of comminution, grinding refers to the


operation of reducing the small pieces after crushing
to a fine powder
• Accomplished by abrasion, impact, and compaction
by hard media such as balls or rolls
• Examples of grinding include:
– Ball mill
– Roller mill
– Impact grinding

ME477 Lecture 08 39
Ball Mill
Hard spheres mixed with stock are rotated inside a
large cylindrical container; the mixture is carried up
the container wall as it rotates, and then pulled back
down by gravity for grinding action

Figure 17.3 - Mechanical methods of


producing ceramic powders: (a) ball mill

ME477 Lecture 08 40
Roller Mill
Stock is compressed against a flat horizontal grinding
table by rollers riding over the table surface

Figure 17.3 -
Mechanical methods of
producing ceramic powders:
(b) roller mill

ME477 Lecture 08 41
Ingredients of Ceramic Paste for
Shaping

1. Clay (hydrous aluminum silicates) - usually the main


ingredient because of ideal forming characteristics
when mixed with water
2. Water – creates clay-water mixture with suitable
plasticity for shaping
3. Non-plastic raw materials, such as alumina and silica
- reduce shrinkage in drying and firing but also
reduce plasticity of the mixture during forming
4. Other ingredients, such as fluxes that melt (vitrify)
during firing and promote sintering, and wetting
agents to improve mixing of ingredients
ME477 Lecture 08 42
Shaping Processes
• Slip casting
– The clay-water mixture is a slurry
• Plastic forming methods
– The clay is plastic
• Semi-dry pressing
– The clay is moist but has low plasticity
• Dry pressing
– The clay is basically dry (less than 5% water) and has no
plasticity

ME477 Lecture 08 43
Slip Casting

A suspension of ceramic powders in water, called a slip, is


poured into a porous plaster of paris mold so that water from
the mix is absorbed into the plaster to form a firm layer of
clay at the mold surface
• The slip composition is 25% to 40% water
• Two principal variations:
– Drain casting - the mold is inverted to drain excess slip after a
semi-solid layer has been formed, thus producing a hollow product
– Solid casting - to produce solid products, adequate time is allowed
for entire body to become firm

ME477 Lecture 08 44
Figure 17.5 - Sequence of steps in drain casting, a form of slip
casting: (1) slip is poured into mold cavity, (2) water is absorbed
into plaster mold to form a firm layer, (3) excess slip is poured
out, and (4) part is removed from mold and trimmed

ME477 Lecture 08 45
Overview of Plastic Forming
• The starting mixture must have a plastic consistency,
with 15% to 25% water
• Variety of manual and mechanized methods
– Manual methods use clay with more water because it is
more easily formed
• More water means greater shrinkage in drying
– Mechanized methods generally use a mixture with less water
so starting clay is stiffer
• Plastic Forming Methods:
– Hand modeling (manual method)
– Jiggering (mechanized method)
– Plastic pressing (mechanized method)
– Extrusion (mechanized method)

ME477 Lecture 08 46
Hand Modeling

Creation of the ceramic product by manipulating the


mass of plastic clay into the desired geometry
• Hand molding - similar only a mold or form is used to
define portions of the part geometry
• Hand throwing on a potter's wheel is another
refinement of handcraft methods
– Potter's wheel = a round table that rotates on a vertical
spindle, powered either by motor or foot-operated treadle
– Products of circular cross-section can be formed by throwing
and shaping the clay, sometimes using a mold to provide the
internal shape

ME477 Lecture 08 47
Jiggering
Similar to potter's wheel methods, but hand throwing is
replaced by mechanized techniques

Figure 17.6 - Sequence in jiggering: (1) wet clay slug is placed on a convex mold;
(2) batting; and (3) a jigger tool imparts the final product shape

ME477 Lecture 08 48
Plastic Pressing

Forming process in which a plastic clay slug is pressed


between upper and lower molds contained in metal rings
• Molds are made of porous material such as gypsum, so
when a vacuum is drawn on the backs of the mold halves,
moisture is removed from the clay
• The mold sections are then opened, using positive air
pressure to prevent sticking of the part in the mold
• Advantages: higher production rate than jiggering and not
limited to radially symmetric parts

ME477 Lecture 08 49
Extrusion

Compression of clay through a die orifice to produce


long sections of uniform cross-section, which are
then cut to required piece length
• Equipment utilizes a screw-type action to assist in
mixing the clay and pushing it through die opening
• Products: hollow bricks, shaped tiles, drain pipes,
tubes, and insulators
• Also used to make the starting clay slugs for other
ceramics processing methods such as jiggering and
plastic pressing

ME477 Lecture 08 50
Semi-dry Pressing
Uses high pressure to overcome the clay’s low plasticity
and force it into a die cavity

Figure 17.7 - Semi-dry pressing: (1) depositing moist powder into die cavity,
(2) pressing, and (3) opening the die sections and ejection

ME477 Lecture 08 51
Dry Pressing
Process sequence is similar to semi-dry pressing - the main
distinction is that the water content of the starting mix is
typically below 5%
• Dies must be made of hardened tool steel or cemented
carbide to reduce wear since dry clay is very abrasive
• No drying shrinkage occurs, so drying time is eliminated
and good dimensional accuracy is achieved in the final
product
• Typical products: bathroom tile, electrical insulators,
refractory brick, and other simple geometries

ME477 Lecture 08 52
Clay Volume vs. Water Content
• Water plays an important role in most of the
traditional ceramics shaping processes
• Thereafter, it has no purpose and must be removed
from the clay piece before firing
• Shrinkage is a problem during drying because water
contributes volume to the piece, and the volume is
reduced when it is removed

ME477 Lecture 08 53
Drying

The drying process occurs in two stages:


• Stage 1 - drying rate is rapid and constant as water
evaporates from the surface into the surrounding air and
water from the interior migrates by capillary action to the
surface to replace it
– This is when shrinkage occurs, with the risk of warping and cracking
• Stage 2 - the moisture content has been reduced to where
the ceramic grains are in contact
– Little or no further shrinkage occurs

ME477 Lecture 08 54
Firing of Traditional Ceramics

Heat treatment process that sinters the ceramic material


• Performed in a furnace called a kiln
• Bonds are developed between the ceramic grains, and this
is accompanied by densification and reduction of porosity
• Therefore, additional shrinkage occurs in the
polycrystalline material in addition to that which has
already occurred in drying
• In the firing of traditional ceramics, a glassy phase forms
among the crystals which acts as a binder

ME477 Lecture 08 55
Glazing
Application of a ceramic surface coating to make the piece
more impervious to water and enhance its appearance
• The usual processing sequence with glazed ware is:
1. Fire the piece once before glazing to harden the body of the piece
2. Apply the glaze
3. Fire the piece a second time to harden the glaze

ME477 Lecture 08 56
Processing of New Ceramics
• The manufacturing sequence for the new ceramics can be
summarized in the following steps:
1. Preparation of starting materials
2. Shaping
3. Sintering
4. Finishing
• While the sequence is nearly the same as for the
traditional ceramics, the details are often quite different

ME477 Lecture 08 57
Preparation of Starting Materials
• Strength requirements are usually much greater for
new ceramics than for traditional ceramics
• Therefore, the starting powders must be smaller and
more uniform in size and composition, since the
strength of the resulting ceramic product is inversely
related to grain size
• Greater control of the starting powders is required
• Powder preparation includes mechanical and
chemical methods

ME477 Lecture 08 58
Shaping of New Ceramics
• Many of the shaping processes for new ceramics are
borrowed from powder metallurgy (PM) and
traditional ceramics
– PM press and sinter methods have been adapted to the new
ceramic materials
• And some of the traditional ceramics forming
techniques are used to shape the new ceramics,
such as: slip casting, extrusion, and dry pressing
• The processes described here are not normally
associated with the forming of traditional ceramics,
although several are associated with PM

ME477 Lecture 08 59
Hot Pressing
Similar to dry pressing except it is carried out at
elevated temperatures so sintering of the product is
accomplished simultaneously with pressing
• This eliminates the need for a separate firing step
• Higher densities and finer grain size are obtained, but
die life is reduced by the hot abrasive particles
against the die surfaces

ME477 Lecture 08 60
Isostatic Pressing
Uses hydrostatic pressure to compact the ceramic
powders from all directions
• Avoids the problem of nonuniform density in the final
product that is often observed in conventional
uniaxial pressing
• Same process used in powder metallurgy

ME477 Lecture 08 61
Powder Injection Molding (PIM)
Ceramic particles are mixed with a thermoplastic
polymer, then heated and injected into a mold cavity
• The polymer acts as a carrier and provides flow
characteristics for molding
• Upon cooling which hardens the polymer, the mold is
opened and the part is removed
• Because temperatures needed to plasticize the
carrier are much lower than those required for
sintering the ceramic, the piece is green after molding
• The plastic binder is removed and the remaining
ceramic part is sintered

ME477 Lecture 08 62
Sintering of New Ceramics
• Since the plasticity needed to shape the new
ceramics is not normally based on water, the drying
step required for traditional green ceramics can be
omitted for most new ceramic products
• The sintering step is still very much required
• Functions of sintering are the same as before:
1. Bond individual grains into a solid mass
2. Increase density
3. Reduce or eliminate porosity

ME477 Lecture 08 63
Finishing Operations for New
Ceramics
• Parts made of new ceramics sometimes require finishing,
which has one or more of the following purposes:
1. Increase dimensional accuracy
2. Improve surface finish
3. Make minor changes in part geometry
• Finishing usually involves abrasive processes
– Diamond abrasives must be used to cut the hardened ceramic
materials

ME477 Lecture 08 64
Design Guidelines for PM Parts - I
• Economics usually require large quantities to justify
cost of equipment and special tooling
– Minimum quantities of 10,000 units are suggested
• PM is unique in its capability to fabricate parts with a
controlled level of porosity
– Porosities up to 50% are possible
• PM can be used to make parts out of unusual metals
and alloys - materials that would be difficult if not
impossible to produce by other means

ME477 Lecture 08 65
Design Guidelines for PM Parts - II
• The part geometry must permit ejection from die after
pressing
– This generally means that part must have vertical or
near-vertical sides, although steps are allowed
– Design features such as undercuts and holes on the part
sides must be avoided
– Vertical undercuts and holes are permissible because they
do not interfere with ejection
– Vertical holes can be of cross-sectional shapes other than
round without significant difficulty

ME477 Lecture 08 66
Figure 16.17 - Part features to be avoided in PM: side holes and (b)
side undercuts since part ejection is impossible

ME477 Lecture 08 67
Design Guidelines for PM Parts - III
• Screw threads cannot be fabricated by PM; if required,
they must be machined into the part
• Chamfers and corner radii are possible by PM pressing,
but problems arise in punch rigidity when angles are too
acute
• Wall thickness should be a minimum of 1.5 mm (0.060 in)
between holes or a hole and outside wall
• Minimum recommended hole diameter is 1.5 mm (0.060 in)

ME477 Lecture 08 68
Figure 16.19 - Chamfers and corner radii are accomplished but
certain rules should be observed: (a) avoid acute angles; (b) larger
angles preferred for punch rigidity; (c) inside radius is desirable;
(d) avoid full outside corner radius because punch is fragile at
edge; (e) problem solved by combining radius and chamfer

ME477 Lecture 08 69

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