Colloidal processing of ceramics and

composites
R. Moreno*
Colloidal processing has demonstrated its suitability to produce complex shaped ceramics and ceramic
metal composites with tailored microstructure. By combining different shaping methods, it is possible to
produce complex three-dimensional bodies as well as single or multilayer coatings, self-sustaining films
and laminates. This work summarises the main features of colloidal processing, including colloidal stability
and stabilising mechanisms focusing the importance of the rheological behaviour in the shaping step. The
most common shaping methods and consolidation mechanisms based on suspensions are presented as
well as their capabilities for producing composites with complex shapes and microstructures.
Keywords: Suspensions, Rheology, Composites, Processing

This paper is part of a special issue on Novel Advanced Ceramic and Coating Processing

Introduction
Engineered materials with enhanced properties are
needed to meet the increasing exigencies of everyday
applications. When searching a new material two aspects
must be considered: on the one hand, the profile of
properties it must satisfy, and on the other hand, the
capability to produce a component with the desired
geometry, size and microstructure. That is, the choice
of a processing route strongly depends on the type
of material to be produced and its final shape, and
processing (in particular the shaping step) determines
the final properties of the material.1,2
A common classification of engineering materials
differentiates three broad families: metals, polymers
and ceramics, which can combine themselves to produce
a fourth category, that of hybrids or composites. Metals
are usually stiff and tough, but they are also soft and
deform easily. The main limitations of metals are their
reactivity and the low resistance to corrosion. Ceramics
are non-metallic, inorganic solids, which harden after a
thermal treatment that provides high resistance to
corrosion and chemicals, high refractoriness, hardness,
etc. However, a major limitation of ceramic materials is
their inherent brittleness. Ceramics are usually formed
from powders so that typical shaping processes of metals
such as deformation methods cannot be used in
ceramics. Polymers are organic solids built up from the
association of unit chains of carbon atoms, the so called
monomers. Polymers are light and floppy, and the
properties strongly depend on temperature. They are
easy to shape into complicated parts by melting and
pouring or injection into a mould cavity. One typical
shaping process for polymers is injection moulding
where the part can be simply obtained either by melting
a thermoplastic polymer before injection into a cold

Institute of Ceramics and Glass (CSIC), Kelsen 5, 28049 Madrid, Spain

*Corresponding author, email rmoreno@icv.csic.es

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cavity of a mould or by injection of a thermosetting

polymer into a mould cavity that is further heated.
Metals and ceramics have several commons, as mining
and powder processing, and the needing of a thermal
treatment to get the final microstructure when using
such a powder processing approach. As a consequence,
ceramics and metalceramic composites have many
similarities and can be processed using the same powder
metallurgy approach. Although this is not possible for
polymers derivatives and composites, since any thermal
treatment would destroy the polymer structure, polymers are often used in ceramic processing as additives
for many important purposes,3 such as deflocculants to
provide stability to the suspension, binders to provide
consistency, or monomers that polymerise to form a
chemical gel in some shaping processes, including
gelcasting or injection moulding, the last being a
characteristic shaping technique for polymers, but also
for the processing of ceramic and/or metal powders.
The manufacture of ceramics and ceramic based
composites is based on powder processing techniques,
which are difficult to control since the starting powders
are transformed into a complex shaped part through
several processing steps, each one being a possible
source of defects. The defects introduced at any stage
will persist in the subsequent stages. If the starting
powders have defects they could not be removed during
consolidation, so that the purity and control of the
starting powders is a first key parameter to obtain defect
free materials. This explains the great development of
the synthesis routes and their implications in ceramics.4,5
However, this also requires a careful control of all
parameters at every step to avoid new defects.

Ceramic matrix composites

The increasing demands of engineering devices cannot
be achieved by a single material. For example, aircrafts
engines need structural materials with low densiy and
high strength and stiffness and good resistance to
2012 Institute of Materials, Minerals and Mining
Published by Maney on behalf of the Institute
Received 15 July 2011; accepted 12 December 2011
DOI 10.1179/1743676111Y.0000000075

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1 Schematic classication of ceramic based composites

abrasion, impact and corrosion. In the case of functional

materials the main concern is to design the adequate
material for the specific function it has to do (e.g.
biomedical, optical, electronic, etc.) while maintaining
a minimum range of mechanical properties to allow
handling and integration into a device or structure.
There are no single materials able to provide a broad list
of excellent properties, so that many times it would be
necessary the combination of several materials in order
to obtain such unique combination of properties. A
composite can be defined as a multiphase material that
maintains at least partially, the properties of the
different constituents such that a better combination of
properties is obtained.
There are many composites naturally occurring in
nature, such as moluscs shells, wood and bones, among
others. A strong effort has been devoted in the last two
decades to imitate these naturally existing microarchitectures, which are the origin of biomimetics.6 In
general, they consist on laminar structures combining
ceramic and polymeric layers. Callister2 makes a simple
classification of composites according to three main
divisions: particle reinforced, fibre reinforced and structural composites. The flow diagram of Fig. 1 summarises the classification of composites including some
special cases not considered by Callister, such as
platelets, or coatings and functionally graded materials
(FGMs) as particular examples of structural composites. In the first case, particles are equiaxed (e.g.
spherical) or have a low shape factor when particles are
non-spherical.

Introduction to ceramic processing

The final material is produced from a powder that is
subjected to different processing stages. Many of the
detrimental heterogeneities arise from the powder itself,
such as agglomerates and contamination. Other defects
are introduced during powder preparation and beneficiation, on the one hand, and during shaping and
consolidation, on the other hand. In order to produce
better materials, it will be necessary to develop methods
for the synthesis of pure, controlled powders with lower
number and size of defects and to avoid the introduction
of new defects in the processing steps.7
Ceramics are mainly produced by powder processing
techniques, according to the following steps:
(i) powder synthesis and/or beneficiation before
consolidation
(ii) forming to produce a component of the desired
shape and size
(iii) drying and burn out of organics
(iv) sintering at high temperature to reach the final
microstructure and properties
(v) final machining and shaping.
One of the most important steps of the processing
cycle is forming, where powders consolidate into a selfsupported shaped body, the so called green body.
Forming defects can hardly be removed in the subsequent processes (drying, debinding and sintering) and
they become fracture origins which reduce the properties
of the product or lead to a high rejection rate. Table 1
summarises the feed materials, moulds and shapes of

Table 1 Feed materials, moulds and shapes of green bodies produced by common forming processes
Type of process

Feed material

Mould

Shape

Dry or semidry pressing

- Axial pressing
- Isostatic pressing
Plastic moulding
- Jiggering
- Extrusion
- Injection molding
Suspension forming
- Slip casting
- Tape casting
- Gel casting
- Coagulation casting
- Electrophoresis

Powders
- Powder or flowing granules
- Powder or fragile granules
Plastic paste
- Plastic paste with binders
- Plastic paste with binders
- Blend of granules and polymers
Dispersed suspension
- Free flowing suspension
- Suspension with binders
- Suspension with gel-formers
- Suspension with coagulants
- Low solids content suspensions

Metallic non-porous
- Steels, WC, Resins
- Elastomers
Nozzles
- Tools for calibrating
- Ceramic or metallic nozzle
- Metallic mould (cooled or heated)
Complex shaped moulds
- Plaster, porous moulds
- Mylar, glass substrates
- Metallic, non-porous moulds
- Metallic, non-porous moulds
- Working electrode
(metal, graphite, fabrics)

- Simple, planar
- Complex, central axis
- Recipients, bowls
- Elongated axial symmetry
- Intrincated, small
Complex shapes and tailored
microstructures, monoliths,
coatings, laminates and FGMs

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green bodies produced by common forming processes.

In general, ceramic forming techniques can be classified
according to three categories, depending on the relative
content of liquid characteristic of the process:
(i) dry pressing methods, where the liquid content is
typically ,7%
(ii) plastic forming, with typical liquid contents of
1520 for extrusion or up to 3040% in the case
of injection molding
(iii) colloidal shaping methods that make use of
suspensions, where the content of liquid is
generally .50%.

Colloidal processing
Interparticle forces and colloidal stability
Most ceramic operations include the dispersion of
powders in liquids, either for direct consolidation from
the suspension (as in casting processes, gel forming, etc.)
or as an intermediate step for further processing
operations, as in the case of milling and mixing, spray
drying, filter pressing, etc. The great advances in the
fundamentals of colloid science have allowed the
improvement of conventional ceramic processing and
the development of new forming techniques.810
A colloidal dispersion is a multiphase system in which
one phase (or more) is dispersed in a continuous one
or medium. At least one dimension lies within the
nanometre (1029 m) to micrometre (l026 m) range, so
that colloidal dispersions are mainly systems containing large molecules and/or small particles. The interface between the dispersed phase and the dispersing
medium plays an essential role in the surface properties, including adsorption, surface charge, electrical
double layer, etc. In colloidal suspensions, there are
particles immersed in a surrounding medium. The total
interaction is the result of particleparticle interactions, as well as mediummedium and particlemedium
interactions.1113
One of the most important features of a colloidal
dispersion is the strong tendency of particles to
aggregate. Encounters between particles dispersed in
liquid media occur frequently and the stability of
dispersion is determined by the interaction among the
particles during these encounters. The principal cause of
aggregation is the existence of van der Waals attractive
forces among the particles, which are long range forces.
To counteract these and promote stability, equally long
range repulsive forces are required. This can be achieved
by different ways which can be generalised in two
general mechanisms: the electrostatic mechanism, resulting from the interactions between charged particles in a
medium, and the polymeric mechanism, where stabilisation arises from the effect of polymers in the medium.14
Van der Waals forces arise from three different
phenomena:
(i) the interaction between a permanent dipole with
other permanent dipole (Keesom interaction)
(ii) the interaction between a permanent dipole with
a polarisable atom that produces an induced
dipole (Debye interaction)
(iii) when no permanent dipoles are present, instantaneous dipoles are formed due to fluctuations in
the distribution of electronic charge (London
dispersion interaction).

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If there are no permanent dipoles the first two

contributions do not occur but the last is always present
and plays a key role in the stability of colloidal
suspensions. All these forces vary with separation
distance as D26.
The attractive potential energy VA is directly proportional to a particle radius a, a material constant, the
Hamaker constant A, and is inversely proportional to
distance of separation D
Aa
(1)
12D
Most substances develop an electric surface charge when
brought into a polar liquid. Typical charging mechanisms are ionisation, ion adsorption and ion dissolution.
This surface charge influences the distribution of nearby
ions. Ions of opposite charge (counterions) are attracted
towards the surface and ions of like charge (co-ions)
are repelled away from the surface. This leads to the
formation of an electric double layer made up of the
charged surface and a neutralising excess of counterions
over co-ions distributed in a diffuse manner in the polar
medium.
The Stern model considers that the double layer is
divided into two parts separated by a plane (the Stern
plane) located at about a hydrated ion radius from the
surface, and also considered the possibility of specific
ion adsorption. Specifically adsorbed ions are attached
to the surface by electrostatic and/or van der Waals
forces strongly enough to overcome thermal agitation.
The centres of specifically adsorbed ions are located in
the Stern layer, i.e. between the surface and the Stern
plane. Ions with centres located beyond the Stern plane
form the diffuse part of the double layer.
Acidic species such as MOH2z are formed at acidic
conditions, whereas species MO2 are formed at basic
conditions. There is a pH value at which the activities of
the positive and the negative species at the particle
surface are equal and the net charge density is zero. This
pH defines the point of zero charge (PZC). The
parameter used to measure the stability of a suspension
is the zeta potential, which is the potential existing at the
shear plane between the rigid and the diffuse layers. In
order to assure the stability of a suspension, it is
necessary to have high values of zeta potential, so that
working pH will be far away from the PZC. The pH
where the zeta potential is zero is referred to as
isoelectric point. In the absence of specific adsorption
the PZC coincides with the isoelectric point.
The linear addition of the electrostatic and dispersion
potentials is the basis of the DLVO theory for colloids
stability. When the attractive potential is added to the
repulsive electrostatic potential, there is the typical curve
for charge stabilised colloidal particles: the repulsive
potential VR between two planar surfaces can be
calculated by


64pkTar? c2
Aa
exp ({kD){
VT ~VR zVA ~
(2)
12D
k2
VA ~{

where r is the total ionic concentration in the bulk of

the suspension, k is the Boltzmann constant, T is the
absolute temperature, k is the inverse of the Debye
length that gives the thickness of the double layer and c
is given by

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stabilisation may be achieved by three different mechanisms, as illustrated in Fig. 3:

(i) depletion stabilisation, in which the macromolecules are free in suspension
(ii) steric stabilisation, where the macromolecules
are attached to the particle surface
(iii) electrosteric stabilisation, when adsorbed polymers are charged (referred to as polyelectrolytes),
which combines both electrostatic repulsion
provided by the charges and steric hindrance of
the anchored polymer to the total interaction
pair potential.

Rheology of concentrated suspensions

2 Potential energy of interaction as function of separation distance according to DLVO theory



zey0
exp (zeyo =2kT){1
~
c~tanh
exp (zeyo =2kT)z1
4kT

(3)

The shape of the curve, plotted in Fig. 2, is the

consequence of the addition of the exponential decay
of the repulsive term and the more steeply decaying oneover-distance relationship of the attractive term. It has
three characteristic features:
(i) a maximum that creates an effective activation
energy for aggregation. The larger the barrier,
the longer the system will remain stable
(ii) a primary minimum where particle surfaces enter
into contact leading to coagulation, where
particles can be hardly redispersed
(iii) a secondary minimum, where particles do not
touch each other thus leading to flocculated
particles that can be easily redispersed.
Addition of suitable polymeric dispersants is commonly
used to create stable colloidal suspensions. Polymeric

3 Polymeric stabilising mechanisms: a depletion; b steric;

c electrosteric

Most ceramic processes make use of concentrated

suspensions, in which particle interactions are very
frequent leading to overlapping among double layers.
Then, DLVO theory has important restrictions and zeta
potential measurements do not provide accurate information. For the characterisation of concentrated suspensions, the best tool is the rheology, since it is very
sensitive to any variations in the stability conditions (i.e.
deflocculant type and concentration, pH, presence of
other electrolytes and additives, etc.), mixing conditions,
particle size distribution and shape, solids loading, etc.
Knowledge of rheological behaviour is essential in
processing operations that involve slurries or pastes,
including beneficiation, shape forming, and coating/
deposition.15,16
Rheology is the science of deformation and flow of
matter. When a stress s is applied to a solid it deforms
elastically according to Hookes law
(4)

s~Gc

where G is the elastic modulus (Youngs modulus) and c

is the strain. When the strain falls to zero the sample
recovers its original shape. If the shear is large, then the
structure of the sample can break and hence it not only
deforms but starts to flow. In the simplest case the
response follows Newtons law


(5)

s~g c


where c is the velocity gradient (also known as the shear

rate) and g is the viscosity. The unit of viscosity is Pa s.
By definition Newtonian behaviour is when the viscosity
is independent of shear rate and does not depend on the
shear history. Most simple liquids such as water, acetone
or oils are Newtonian. Liquids showing any variation
from this behaviour are referred to as non-Newtonian.
Figure 4 illustrates plots of shear stress versus shear rate
(the so called flow curves). Most common colloidal
suspensions are shear thinning (also referred to as
pseudoplasticity) because the viscosity decreases as the
shear rate increases. Shear thickening (dilatancy) occurs
when viscosity increases with shear rate, as in the case of
clay based slips at high shear conditions (.1000 s21),
which are typical of mixing, pumping, spraying, brushing and injection processes. Clay based slips and
concentrated suspensions usually cannot flow until a
minimum yield stress sy is exceeded. The simplest case
corresponds to Bingham plastic flow which means that
the linear flow curve is independent of the shear rate
above sy. When there is a yield stress and the behaviour
on shearing is shear thinning, the sample is said to be
plastic.

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4 Flow curves of different types of rheological behaviour

In addition to the shear rate dependence, the rheological behaviour of suspensions is often time dependent; the viscosity changes with the time of shearing.
Pseudoplastic slurries which show time dependent
viscosities are referred to as thixotropic whereas time
dependent dilatancy is antithixotropy or rheopexy.

Colloidal forming methods

Colloidal processing has demonstrated to be very
efficient for producing near-net shaped bodies with
tailored microstructures by maintaining the homogeneous structure of the suspension during the formation
of the green body, i.e. the consolidation step.1720
During the last two decades, an increasing number of
novel near-net shaping forming techniques have been
developed. The physical or chemical processes responsible for the formation of a green body may vary and
also the experimental techniques and devices to facilitate
consolidation, but in all cases well dispersed suspensions
with high solids loadings are needed to fill the moulds or
to retain the structure of the suspensions by fast drying
without shape deformation. There are several classifications of the consolidation mechanisms. Lewis18 classifies
the consolidation techniques into three categories:

(i) consolidation via fluid removal occurring in

shaping techniques such as slip casting, pressure
casting, osmotic consolidation, tape casting and
robocasting
(ii) consolidation via particle flow, as in sedimentation, centrifugation and electrophoretic deposition (EPD)
(iii) consolidation via gelation, which includes shaping techniques such as aqueous injection moulding, direct coagulation casting and gelcasting.
Sigmund et al.19 divide the direct casting methods in two
groups:
(i) processes that manipulate interparticle potentials
and create physical gels via a percolating network
of particles
(ii) percolating networks formed by additives using
physical or chemical processes.
Table 2 summarises the most frequent consolidation
mechanisms and forming techniques used in colloidal
processing of ceramics in the light of existing literature.
In general, filtration, flocculation, coagulation and
injection are used for manufacturing 3D parts, while
evaporation methods are used for large surfaces exposed
to air, i.e. coatings (obtained by dipping, spin coating or
EPD) and thin substrates (as in tape casting). However,
those processes suitable for the preparation of thin
substrates and/or coatings can be successfully used to
process multifunctional coatings, laminated composites
or FGMs. This is possible if the stability of the
suspensions and their rheology, on one hand, and the
growing kinetics of deposited particles, on the other
hand, is controlled. Some processes, such as filtration or
EPD, have well known mathematical laws to predict the
formation kinetics of the growing cake or wall, and the
process time is a fundamental parameter of the process.
Other processes are not time dependent, this being the
case of constant volume forming processes, based in the
consolidation inside a non-permeable mould, such as
flocculation, coagulation and gelation. Consolidation
processes based on evaporation are also time independent, the kinetics depending in much more scale on the
rate of the process itself (withdrawal rate in dipping and

Table 2 Consolidation mechanisms and forming techniques used in colloidal processing of ceramics
Route

Mechanism

Forming technique

Features

Fluid removal

Filtration

Slip casting
pressure
vaccuum
centrfugal
microwaves
Screen printing
Tape casting
Electrophoresis
Dipping
Spin coating
Spraying
Short range forces
Temperature induced
Coagulation casting
Direct solidification
Thermogelation
Protein casting
Starch consolidation
Freeze casting
Injection moulding
Gelcasting

Complex, three-dimensional (3D)

Evaporation

Flocculationcoagulation

Gelation

Flocculation
(Weak agglomerates)
Coagulation
(Hard agglomerates)
Thermal gelation

Chemical gelation

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Substrates and coatings, two-dimensional

Complex, 3D
Complex, 3D
Complex, 3D
Complex, 3D; porous

Complex, 3D

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5 Schematic view of sequential slip casting process to

produce layered materials (right, up) or FGMs (right,
down)

gyration speed in spin coating) and other physical

parameters such as nozzle diameter in spraying, blades
height in tape casting, etc. However, the viscosity at the
characteristic shear rate of the process is a key factor in
all cases.
Another factor to be considered for the classification
of colloidal forming methods is the mould. In filtration
methods a well dispersed suspension with moderate to
high solids content (3040 vol.-%) is prepared and then
poured into the cavity of a permeable mould that
absorbs the water of the suspension by capillarity while
the particles attach to the mould forming a cake. The
cake continues to loose water until it dries and slightly
shrinks allowing easy removal. The wall thickness L
formation follows a parabolic growth with casting time t

Colloidal processing of ceramics and composites

7 Microstructure of green nanocomposite formed by

micrometre sized iron particles coated with ceramic
nanoparticles

L2c ~

2kdp=dxt
gL wC =wS {1

(6)

where wc and ws are the volume fractions of solids in the

cast and in the suspension, gL is the liquid viscosity, k is
the permeability and dp/dx is the gradient pressure
across the compact. According to this parabolic law,
there is a maximum thickness that it is possible to reach
by slip casting, usually of a few millimetres. This means
that when green bodies thicker than 58 mm are prepared by slip casting, there is probably an evaporation
layer at the top that contributes to the total thickness.
This can lead to a density gradient in the body. However, it is possible to build up laminates and complex
structures by sequential slip casting, if the casting rate of
individual suspensions is first determined. This allows
manufacturing a variety of tailored materials, including

6 Types of ceramic based composites: a Al2O3 material reinforced with Ni particles; b platelet shaped CA6 reinforced
alumina; c Al2O3/Y-TZP coated Al2O3; d c sandwich of monoclinic zirconia in Al2O3/Y-TZP matrix; e Al2O3/Y-TZP laminate; f Al2O3/Y-TZP FGM

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8 Porous ceramics produced by replica (left), gelcasting with agar (centre) and freeze casting (right)

laminates and FGMs (as those shown in Fig. 2), as well

as bulk composites and nanocomposites. Figure 5 shows
a scheme of the sequential slip casting process, in which
different suspensions are subsequently cast, each cast
cake acting as a permeable layer for the next layer. It is
possible to obtain structures type A, B, A, B, or A, B,
C, D, by casting alternatively two suspensions or
casting different suspensions with graded composition.
Figure 6 shows the microstructure of several ceramic
composites obtained by different colloidal methods,
from monolithic materials reinforced with particles or
platelets to coatings, laminates and FGMs.21
An important field of application of colloidal processing is in the production of metal ceramic micro- and
nanocomposites.22 Figure 7 shows the microstructure of
a green body formed by micrometre sized iron particles
coated with ceramic nanoparticles produced for melting
metals. The partial oxidation of metal particles in water
can be controlled such that they can be handled as
ceramic powders facilitating wet processing.
The most important limitation of slip casting is the
restricted thickness that can be obtained by filtration.23
The casting kinetics can be increased with the aid of an
external force, such as centrifugation, the use of
microwaves, the application of vacuum, and the most
popular, the application of an external pressure.24
Processes involving the thermal gelation of a suspension, such as protein forming or direct coagulation
methods, are usually employed to obtain highly porous
materials or foams, although dense materials can be also
obtained by thermogelation of polysaccharides that gel
on cooling. In this case a basic requirement is to
maintain the suspension stable at temperatures of 60
70uC, above the gelation temperature of the polysaccharide (normally between 35 and 40uC) in order to
allow a good dispersion with the gelling additive, which
is previously dissolved.25
Freeze casting could be considered as a special case of
gelation in which water is used as a template.26 The
suspension is frozen in liquid nitrogen and then dried
and ice is removed by sublimation. Figure 8 shows the
typical microstructures of some porous ceramics prepared by the replica method with polyurethane sponge,
direct foaming with agar with a surfactant and bubbling,
and aligned pores formed during sublimation of ice in
freeze casting. These simple methods allow us to design
materials with a great variety of microstructures, pore
size distributions and pore volumes.27

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A great advantage of colloidal processing is the broad

number of possibilities to combine forming methods
and consolidation mechanisms to produce a variety of
composites. It is possible to produce a thick film by tape
casting to be used as a substrate to obtain a coated
material or a multilayer. In the case of tape casting the
binder present in the tape gives the consistency for
lamination, but it can be used also a substrate to be used
for dipping or for EPD. After sintering, laminated
materials with very thin layers are obtained by a simple
route able to produce defect free, uniform layers
integrated in complex structures.

Conclusion
The colloidal is a powerful way to produce ceramics and
ceramicmetal composites with better microstructural
uniformity and higher reliability. The manipulation
of the interaction potentials allows one to maintain
particles apart each other during all processing stages,
including consolidation step. There are three basic
approaches to forming from suspensions: fluid removal,
flocculationcoagulation and gelation, although the first
can be divided into two consolidation mechanisms,
filtration and evaporation. A final advantage in colloidal
processing is the possibility to combine different forming techniques or consolidation mechanisms to design
complex materials with tailored micro- or nanostructures,
including monoliths, coatings, and laminates and FGMs,
with ceramic and/or metallic powders with particle size
ranging from micrometre sized to the nanoscale.

Acknowledgement
This work has been supported by Spanish Ministry of
Science and Innovation (MICINN, grant no. MAT200914369-C02-01).

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Advances in Applied Ceramics

2012

VOL

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NO

5&6

253