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Ceramic Slurry
Related terms:
Casting manufacture
John Campbell OBE FREng DEng PhD MMet MA, in Complete Casting Handbook,
2011
Casting
John Campbell, in Complete Casting Handbook (Second Edition), 2015
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economics (Ball, 1991, 1998)Ball, 1991Ball, 1998. There is no record that
the process has ever used a good design of pouring basin, but with very small
castings, particularly if poured rather slowly, require such narrow sprues that a
conical basin may be acceptable, because surface tension will assist to keep air out
of the sprue. Finally, the casting is relatively easily extracted by separating the
mould halves after solidification.
Casting processes
K.G. Swift, J.D. Booker, in Process Selection (Second Edition), 2003
Process description
• A precision pattern generates the mold which is coated with a ceramic slurry.
The mold is dried and baked. The molten metal is then poured into the mold
and allowed to solidify. The mold is broken to remove the part (see 1.7F).
Materials
• All metals, but to a lesser degree, aluminum, magnesium, zinc, tin and copper
alloys.
Process variations
• Variations on the composition of the ceramic slurry and curing mechanism.
• Plaster, wood, metal or rubber are used for patterns.
Economic considerations
• Production rates of up to 10/h typical.
• Lead times can be several days.
• Material utilization high.
• Low scrap losses.
• Best suited to metals having high melting temperatures and/or that are
difficult to machine.
• Can be combined with investment casting to produce parts with increased
complexity with reduced cost.
• Suitable for small batches and medium-volume production.
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• Can be used for one-offs.
• Tooling costs moderate.
• Equipment costs moderate to high.
• Direct labor costs moderate to high.
• Finishing costs low. Usually no machining is required.
Typical applications
• All types of dies and molds for other casting and forming processes
• Cutting tool blanks
• Components for food handling machines
• Pump impellers
• Aerospace and atomic reactor components
Design aspects
• High complexity possible – almost any shape possible.
• Use of cores increases complexity obtainable.
• Inserts, bosses and undercuts possible.
• Placing of parting line important, i.e. avoid placement across critical
dimensions.
• Cored holes greater than Ø0.5 mm.
• Where machining required, allowances of up to 0.6 mm should be observed.
• Draft angle usually zero, but 0.1–1° preferred.
• Minimum section ranging 0.6–1.2 mm, depending on material used.
• Sizes ranging 100 g–3 t in weight, but less than 50 kg better.
Quality issues
• Low porosity.
• Mechanical properties are good.
• Good surface detail possible.
• Surface roughness ranging 0.8–6.3 μm Ra.
• A process capability chart showing the achievable dimensional tolerances is
provided (see 1.7CC). An allowance of ±0.25 mm should be added for
dimensions across the parting line.
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Parting lines sometimes pronounced on finished casting.
•
Casting Processes
K.G. Swift, J.D. Booker, in Manufacturing Process Selection Handbook, 2013
Materials
All metals, but to a lesser degree aluminium, magnesium, zinc, tin and copper
alloys.
Process Variations
• Variations on the composition of the ceramic slurry and curing mechanism.
• Plaster, wood, metal or rubber are used for patterns.
Economic Considerations
• Production rates of up to 10/h typical.
• Lead times can be several days.
• Material utilisation is high.
• Low scrap losses.
• Best suited to metals having high melting temperatures and/or that are
difficult to machine.
• Can be combined with investment casting to produce parts with increased
complexity with reduced cost.
• Suitable for small batches and medium-volume production.
• Can be used for one-offs.
• Tooling costs are moderate.
• Equipment costs are moderate to high.
• Direct labour costs are moderate to high.
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• Finishing costs are low. Usually no machining is required.
Typical Applications
• All types of dies and moulds for other casting and forming processes.
• Cutting tool blanks.
• Components for food handling machining.
• Pump impellers.
• Aerospace and atomic reactor components.
Design Aspects
• High complexity possible – almost any shape possible.
• Use of cores increase complexity obtainable.
• Inserts, bosses and undercuts are possible.
• Placing of parting line important, i.e. avoid placement across critical
dimensions.
• Cored holes greater than 0.5 mm diameter.
• Where machining is required, allowances of up to 0.6 mm should be observed.
• Draft angle usually zero, but 0.1–1° preferred.
• Minimum section ranges from 0.6 to 1.2 mm, depending on material used.
• Sizes range from 100 g to 3 t in weight, but less than 50 kg better.
Quality Issues
• Low porosity.
• Mechanical properties are good.
• Good surface detail possible.
• Surface roughness is in the range 0.8–6.3 μm Ra.
• A process capability chart showing the achievable dimensional tolerances is
provided (Figure 3.7(b)). An allowance of ±0.25 mm should be added for
dimensions across the parting line.
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Figure 4.22. Examples of unfired ceramic bodies by direct inkjet printing from the
30 vol.% Al2O3 wax-based slurries [83] and piezoelectric ceramic structures formed
by robocasting a concentrated lead zirconate titanate ink [82].
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Combustible or volatile pore-forming agents, like some organics or carbon
powders, are added to ceramic slurry (one kind of suspension); the agents will be
burned out or volatilized during sintering and then many pores are left to form
porous ceramic. For example, porous mullite with air permeability can be prepared
by using the mullite and iron powders as the raw materials, ethyl silicate as the
binder, and using the pore-forming agent by molding it with slurry and sintering it
in an oxidative atmosphere [3,31]. The ethyl silicate binder will release ethanol and
water through polyreaction during sintering, and a large number of pores will be
left behind after volatilization of the ethanol and water. The porosity of the final
product could reach 35%–40%, and it can be adjusted by the content of ethyl
silicate and increase with the relative content of mullite when the binder content is
fixed. Ceramics with porosity of 50%–56%, pore size of 20–450 μm, and bending
strength of higher than 20 MPa were prepared by using alumina as the aggregate
and 20% carbon powder as the pore-forming agent, sintering at 1,120–1,170°C of
the mold from the slurry [32].
Recently, the environmentally friendly preparation of porous ceramics with starch
as the pore-forming agent was investigated. The aqueous slurry of ceramic
powders and starch was prepared and then poured into a mold without infiltration
and heated to 50°C–70°C [33]. At this temperature, the starch powders react with
water, which leads to the expansion of the powders and the absorption of water.
Finally, the liquid slurry converts to a hard body shaped like the mold. In the end,
the product is obtained by demolding, drying, and sintering to remove the starch.
The pores left after the burnout of the starch keep the shape and distribution of the
original starch powders. Therefore, the porosity and pore size are determined by
the original starch powder size and content. This process has the advantages of
easy operation, controllable porosity, and low cost, which makes it attractive for the
preparation of porous ceramics. The rice, corn, and potato powders, or a mixture of
them, can be used as the binder and pore-forming agent. Porosity has a close
relationship with the volume ratio of the starch and with the expansion in the solid-
hardening process. In addition, the concentration of fine starch powders, which are
removable during sintering, influences the porosity of the product.
The alumina slurry was prepared by mixing 75%–80 wt% α-Al2O3 powders of
submicrometers (averaging 0.7 μm) and 5%–30 vol % starch [34]. The final
product, with porosity of 36%–37% (with open-cell foams < 30%) and pore size of
60 μm, was obtained by demolding, drying at 105°C, and sintering at 1,570°C.
The commercial starch powders come from grains (e.g., corn, wheat, and rice) or
other crops (potato) [35]. The important features for the wide application of starch
are densification, gel, binding, and membrane formation. The starch powders are
white at room temperature, dense, and insoluble in water, and are 2–170 μm in
size. They are insoluble in water below 50°C, which means that the powders can be
processed without affecting the structure. However, the molecular bond will be
destroyed at temperatures of 55–80°C (depending on the starch type and
concentration), and the starch powders will expand many times with the absorption
of water. The slurry with mixed ceramic powders and starch was poured into the
mold and then heated to 60°C–80°C. After that, the starch expands with the
absorption of water and binds the ceramic particles to form solid green product for
the next sintering. In addition, the starch can increase the strength of the solid
body as the binder to ensure that demolding occurs before the full drying. After
sintering, the pores in the ceramics correspond to the content, shapes, and sizes of
the original starch powders. Different kinds of ceramic products, like thermal
insulation parts, infiltration parts, gas combustors, and biological ceramics, can be
prepared by this process. Figure 5.5 shows several products with various shapes.
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Figure 5.5. Porous alumina products made by molding starch with solid bonds
[35]. (The height of the owl and the thumb are 45 and 60 mm, respectively).
Antiwear engineering ceramics (like silicon nitride) are hard to machine after
sintering, while porous ceramics do not have this problem [36]. Different processes
were applied to preparing porous Si3N4, including partly sintering at 1,500°C–
1,550°C for 2 hours and complete densification at 1,800°C for 10 minutes. A
further step is the introduction of volatile, decomposable, and combustible starch
particles, in which the selected starch comes from rice, potato, and corn, into the
Si3N4 mixture to develop regularly arranged, large pores. The starch in the green
product first is burned out in a muffle furnace at 500°C–600°C, and then the green
product is moved to the alumina crucible in a graphite furnace for sintering
without pressure. The obtained pores’ sizes and shapes in the sintered Si3N4 are
quite close to the starch. When the starch content reaches 30 vol%, closed-cell
pores are found; at above 30 vol%, the number of open-cell pores increases.
Egg whites can be substituted for the starch and play the same role [37]. A 12.5-
wt% water solution was obtained by adding egg whites/water with a ratio of 1:7,
and it is close to natural fresh egg whites (11%–13%). The dissolution of egg
whites should be conducted below 40°C. Alumina powders are added at room
temperature, and then aqueous ceramic slurry of 10%–25 vol% is obtained. After
that, air is introduced to the formation of foam and then to hardening. After
molding the material in a polymer mold, it is dried at 95°C for 2 hours, heated to
400°C at a rate of 1°C/min, then heated to 1,600°C at a rate of 5°C/min and
maintained at this temperature for 2 hours, and finally cooled in the furnace. The
two-step heating process is designed to prevent cracking from thermal stress. The
main problem is the shrinkage cracking, which is partly due to the low content of
organics, and it can be improved with organic additives that have no influence on
the foam’s stability.
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Figure 6. SEM images of alumina powders of different powder sizes (a) 400 nm, (b)
12.0 μm.
Ceramic slurry is obtained by mixing ceramic powder, carrying vehicle, binder, and
dispersant to produce uniformly dispersed ceramic slurry. It is important to
optimize the slurry composition in order to obtain high green density, low green
shrinkage, and sufficient green strength to produce defect-free demolding.
Dispersant is used to separate the agglomerated particles in a slurry by controlling
the interparticle forces affecting the colloidal stability of the system. Dispersion of
ceramic powder processing is very important to obtain a high reliability sintered
structure. Any inhomogeneity is a potential flaw in the sintered parts. Hence, the
agglomerates, which exist in most commercially supplied powders, either have to
be broken down or removed [22]. The dispersion condition of slurry has a direct
impact to the green density. Well-dispersed slurry is required to produce green
bodies with high packing densities and uniform micro-structures. Therefore,
density and shrinkage measurements of the green parts are typically carried out for
the optimization of dispersant concentration. Green density indicates how tightly
the ceramic particles are packed in the green part. In addition, it is the key for
achieving low sintered shrinkage, high dimensional resolution, and less distortion
on resultant sintered part. Therefore, it is considered as a dominant parameter in
forming ceramic micro-components.
Ceramic binder is a substance that is used to bind ceramic particles into the
desired shape in the mold. In addition, it enhances green strength and improves
flexibility of the ceramic parts. Polymers and waxes are the two major ingredients
that are mainly present equally in a typical ceramic binder [23–25]. In most of slurry
systems, binders play a crucial part in preparing optimum ceramic slurry. The more
binder added, the stronger the green body is expected. Additionally, binders must
be taken off from green parts before sintering. The more added binder, the more
difficult the debinding process will be. Because of large amount of binder, more
gas will be formed during the binder burnout step, which causes internal stresses,
possible part damage, and geometry distortion.
Water-, preceramic polymer-, and wax-based slurries are employed and their
process parameters are optimized for the fabrication of ceramic micro-components
using soft lithography [24]. Water-based slurry process has been employed
extensively in many forming techniques, such as tape casting and slip casting. The
use of water as a dispersing liquid is attractive because of cost, environmental, and
health benefits. Aqueous binders such as Duramax B-1000 (Rohm and Haas, USA)
and Duramax B-1007 (Rohm and Haas, USA) were used together in the
experiments. They are commercially available low-foaming binders. In addition,
their high dispersion in water enables an effective adsorption on the powder in
water, reducing possible cracks on the green body during drying. The high solid
loading of the binders increases the particle binding in the green body, which
improves its flexibility. During the drying of the slurry, the polymer particles bind
the particles together and increase the green strength. On the other hand,
Duramax D-3005 (Rohm and Haas, USA) was used as a dispersant. D-3005 is an
ammonium salt of a polyelectrolyte, commercially available for dispersing different
ceramic powders in aqueous suspensions. D-3005 has a low molecular weight,
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which makes it effective at low use levels. The dispersant is supplied as a 35%
solution in water. It was found that the minimum binder concentration used in the
slurry without damaging the resultant green parts during both drying and
demolding processes was about 20:25 mg/g powder for different powder sizes.
Less binder concentration increases the possibility to damage the green parts.
Using the optimum binder concentration resulted in complete and crack-free
green parts as shown in Figure 7.
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Figure 8. SEM images of defected green parts fabricated using solvent-based slurry
(a) Moisture content resultant voids, (b) Broken green parts by insufficient
preceramic coatings resin (PCR), (c) Broken green parts by strong adhesion to
poly(dimethylsiloxane) (PDMS) mold.
Figure 9. (a) Optical and (b) SEM images of ceramic green micro-pistons fabricated
using solvent-based slurry.
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Paraffin wax is a mixture of alkane hydrocarbons having CnHn+2 formula where
20 ≤ n ≤ 40. They are solid in room temperature and start to melt in temperature
starting from 37 °C. Paraffin wax is a very popular binder in low-pressure injection
molding for its low cost and versatile working temperatures. In addition, the
resultant high-strength green parts make it effective binder for complex shape
ceramics [28]. Paraffin wax (Sigma–Aldrich, UK) has the melting point of 53–57 °C.
Ceramic slurry based on paraffin wax could be improved with the addition of
dispersants, which improves ceramic particle dispersion and enhances wetting of
the binder on the ceramic particles [28]. Stearic acid (C18H36O2) supplied by
Sigma–Aldrich, UK with a melting point of 69–71 °C was used as a dispersant in
the paraffin wax-based slurry. Paraffin wax played the role of both the binder and
the carrying medium. In the mixing step, the minimum amount of binder, which
provides the necessary convenient molding process, was decided as the
optimization criterion. For binder concentration less than 50 mg/g powder, it was
found that it is difficult to mix the ceramic slurry using mechanical stirrer. By
increasing the binder concentration to about 200 mg/g and 100 mg/g, it was easier
to get homogeneous slurry using mechanical stirring. However, the slurry freezes
faster before completing the filling, especially in thin micro-features, due to its
high viscosity. As a result, incomplete micro-parts were obtained. Further
increasing the binder content to about 260 mg/g, the filling process was improved
and a complete filling was achieved, as shown in Figure 10.
Based on the assessments of the given slurries, water-based slurry proved to offer
the greatest potential to realize suitable ceramic micro-components fabrication
approach.
Sedimentation behavior of aqueous ceramic suspensions with different particle
sizes and dispersant concentrations was studied to find the conditions for the
maximum dispersion [29,30]. Suspensions stability is closely related to particle size
and the amount of dispersant concentration as shown in Figure 11. All particles
have a natural tendency to settle, generating higher sedimentation heights when
no dispersant is added. The sedimentation height of the suspension with the
smallest particle size is the highest when compared to the other suspensions. On
the other hand, the stability is improved with the addition of the dispersant. It is
notable that as the powder particle size is increased, the required amount of the
dispersant to affect suspension stability is reduced. This is because a higher specific
surface area requires more dispersant. With further increase of the dispersant, the
settled height of all suspensions remained almost constant.
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Figure 44. Photographs of the lost foam process: (a) expanded polystyrene patterns;
(b) patterns being dipped in ceramic coating; (c) mold box with loose sand around
pouring cup; and (d) finished castings.
Manufacture of the patterns can be highly automated, using blowing and steam-
expansion processes. However, after being removed from the die the patterns are
usually dimensionally unstable and, to obtain stability, have to be conditioned in a
temperature-controlled room for a number of days (Vatankhah and Littleton,
2001). Pouring can be manual or completely automated. Complex shapes can be
produced, without the use of cores, by gluing (often hot melt) smaller bits of
polystyrene together. The coating permeability is a significant factor in the process,
and therefore a knowledge of the properties of the coating is essential for
controlling and understanding it.
Recent work at the University of Birmingham has shown that, under certain
circumstances, a highly unstable interface can be created between the liquid metal
front and the retreating polystyrene, as the gaseous products attempt to escape
(Figure 45). Other results indicate that in thick sections the variation of density in
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the polystyrene can significantly change the way in which the liquid metal flows.
Other problems arise from the hot-melt glue lines. These materials have different
combustion characteristics. The glue bead also gives rise to additional metal, in the
area of the join, that can affect the feeding characteristics of a section.
Figure 45. Real-time X-ray images of lost foam casting showing progression of
front from left to right (frame speed is 1/25 s). Using this technique it is possible to
see how unstable the front is as a result of out-gassing. In the second frame some
of the front has gone behind the line of the front in the first frame, which is
delineated by the black line.
Despite these inherent problems, the process gives some economical advantages
and has been used in a number of plants around the world for long series casting
runs. An example is in the GM Saturn engine plant in Tennessee, where the
process is used for aluminum heads and blocks, and ductile cast-iron differential
cases and crankshafts.
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The SP process uses a liquid-to-solid inkjet plotter that deposits the polymer on a
movable Z-platform (Fig. 3). Two molten polymers, i.e., a thermoplastic building
wax (used to make the mold) and a supporting wax (used to support overhangs and
cavities in the mold), are fed to heated movable inkjet print heads capable of
motion in the x–y plane. The piezoelectric-driven inkjet heads deposit the build and
support materials as very fine droplets (⩽75 μm) at a high rate of 6000 drops/min.
The molten droplets ejected from the inkjets solidify upon impact with the cooler
mold surface. Any spacing between build polymer walls in a layer is filled with a
support wax to provide support to the mold walls and to avoid the filling of the
voids with build material during the milling operation. After the deposition of each
layer, the cutter mills the mold surface to make it smooth and horizontal for the
deposition of a next build layer. After the mold is built, the support polymer is
dissolved using an organic solvent that does not attack the build polymer. The
mold is then infiltrated using ceramic slurries to fabricate green ceramic
components.
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