Composites: Part A 32 !

2001) 9971006
www.elsevier.com/locate/compositesa

Use of electrophoretic deposition in the processing of bre reinforced

ceramic and glass matrix composites: a review
A.R. Boccaccini a,*, C. Kaya b, K.K. Chawla c
a

Fachgebiet Werkstofftechnik, Technische Universitat Ilmenau, PF 100565, D-98684 Ilmenau, Germany

Interdisciplinary Research Centre !IRC) for High Performance Applications & School of Metallurgy and Materials, The University of Birmingham,
Edgbaston, Birmingham B15 2TT, UK
c
Department of Materials and Mechanical Engineering, University of Alabama at Birmingham, Birmingham, AL 35294, USA

Abstract
Electrophoretic deposition !EPD) is a simple and cost-effective method for fabricating high-quality `green' composite bodies which, after
a suitable high-temperature treatment, can be densied to a composite with improved properties. In this contribution, we describe the use of
EPD technique in the fabrication of bre reinforced composites, with an emphasis on composites with glass and ceramic matrices containing
metallic or ceramic bre fabric reinforcement. EPD has been used to inltrate preforms with tight bre weave architectures using different
nanosized ceramic particles, including silica and boehmite sols, as well as dual-component sols of mullite composition. The principles of the
EPD technique are briey explained and the different factors affecting the EPD behaviour of ceramic sols and their optimisation to obtain
high inltration of the bre preforms are considered. In particular, the EPD fabrication of a model alumina matrix composite reinforced by
Ni-coated carbon bres is presented. The pH of the solution and the applied voltage and deposition time are shown to have a strong inuence
on the quality of the inltration. Good particle packing and a high solids-loading were achieved in most cases, producing a rm ceramic
deposit which adhered to the bres. Overall, the analysis of the published data and our own results demonstrate that EPD, being simple and
inexpensive, provides an attractive alternative for ceramic inltration and coating of bre fabrics, even if they exhibit tight bre weave
architectures. The high-quality inltrated bre mats are suitable prepregs for the fabrication of advanced glass and ceramic matrix composites for use in heat-resistant, structural components. q 2001 Elsevier Science Ltd. All rights reserved.
Keywords: A. Ceramicmatrix composites !CMCs); E. Prepreg; Electrophoretic deposition

1. Introduction
The development of bre reinforced ceramic and glass
matrix composites is a promising means of achieving lightweight, structural materials combining high-temperature
strength with improved fracture toughness, damage tolerance and thermal shock resistance [1]. Considerable
research effort is being expended in the optimisation of
ceramic composite systems, with particular emphasis
being placed on the establishment of reliable and costeffective fabrication procedures. In this context, while the
initial efforts were in the fabrication of unidirectional
composites, they are increasingly shifting towards the
more isotropic composite materials reinforced by twodimensional !2D) and three-dimensional !3D) bre architectures. The majority of the research undertaken so far on the
2D reinforcement of ceramics has been conducted using
* Corresponding author. Present address: Department of Materials,
Imperial College, London SW7 2BP, UK.
E-mail address: a.boccaccini@ic.ac.uk !A.R. Boccaccini).

ceramic fabrics, including SiC-based !e.g. Nicalon w,

Nippon Carbon Co., Japan), alumina and aluminosilicate
woven bre mats [25]. Metallic fabrics are commercially
available also [6] and are made from a variety of metals
including stainless steel and special alloys !e.g. Hastelloy
X). These fabrics provide interesting reinforcing elements
for the fabrication of ductile phase reinforced brittle matrix
composites, including glass matrix composites.
Ceramic and glass composites incorporating 2D or 3D
bre reinforcements are particularly prone to exhibiting
uncontrolled microstructures and residual porosity. This is
because it is extremely difcult to achieve complete inltration of the matrix material into the bre tows !where the
intra-tow openings may be down to the order of #100 nm).
Traditional processing routes for 2D or 3D bre reinforced
ceramic matrix composites have disadvantages. In particular, simple slurry inltration is unable to penetrate tight bre
weaves, while chemical vapour inltration !CVI) is an
expensive technology due to the numerous re-inltration
steps required and the high-cost equipment involved [4].
Electrophoretic deposition !EPD) has been developed in

1359-835X/01/$ - see front matter q 2001 Elsevier Science Ltd. All rights reserved.
PII: S 1359-835 X!00)00 168-8

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A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

preforms has been studied theoretically and experimentally

[1315].
In the present work, a complete literature review focusing
on the particular use of EPD to inltrate ceramic and
metallic bre preforms with the ultimate goal of fabricating
composite materials is presented. Typical EPD experimental procedures and the results achieved are described in
detail, taking as example a model alumina matrix composite
reinforced by Ni-coated carbon bres.

2. Literature review

Fig. 1. Schematic diagram of the EPD cell for obtaining ceramic deposits on
conductive bre mats. The bre mat acts as the positive electrode when the
particles in the suspension are negatively charged !e.g. silica particles at
pH 9 [4]).

recent years as a novel, simple and inexpensive method for

achieving complete inltration of tightly woven bre
preforms [4,7]. The technique is based on using nanoscale
ceramic particles in a stable non-agglomerated form !such
as in a sol or colloidal suspension) and exploiting their net
surface electrostatic charge characteristics while in suspension. On application of an electric eld the particles will
migrate towards and deposit on an electrode. If the deposition electrode is replaced by a conducting bre preform, the
suspended particles will be attracted into and deposited
within it, providing an appropriate means of effectively
inltrating densely packed bre bundles. A schematic
diagram of the basic EPD cell is shown in Fig. 1.
The movement of ceramic sol particles in an aqueous
suspension within an electric eld is governed by the eld
strength, and the pH, ionic strength and viscosity of the
solution [4]. The electrophoretic mobility !EM) of the
charged particles in suspension is given by [8]:
EM

U
1z

;
E
4ph

where U is the velocity, E the eld strength, 1 the dielectric

constant, z the zeta potential and h the viscosity. Accordingly, a suitable suspension for EPD should have highparticle surface charge, high dielectric constant of the liquid
phase and low viscosity. Moreover, low conductivity of the
suspending medium to minimise solvent transport is
required.
The phenomenon of electrophoresis has been known
since the beginning of the last century [9] and has found
extended application in ceramic technology. In available
comprehensive review articles, complete descriptions of
the basics of the EPD technique and its applications in
ceramics have been presented [8,1012]. Moreover, the
deep electrophoretic penetration of porous substrates,
which is related to the EPD inltration of tight bre

Table 1 presents an overview of the published work dealing with the application of the EPD technique for the fabrication of bre reinforced ceramic and glass matrix
composites. Other types of ceramic composite systems,
such as whisker reinforced composites [16,17], laminated
composites [1820], composite coatings [21], composites
with porous layers [22] and functionally graded materials
[2224] have been fabricated by the EPD technique. Moreover, the use of electrodeposition to coat ceramic bres with
metals with the aim to fabricate metal matrix composites has
also been investigated [25,26]. However, research on these
areas will not be reviewed here, this paper being restricted to
the use of EPD for the fabrication of bre reinforced
ceramic and glass matrix composites.
The feasibility of inltrating ceramic woven bre
preforms by EPD has been demonstrated for a variety of
single and mixed component ceramic sols, as summarised in
Table 1. Mainly graphite [22,2732], SiC-based
[4,7,22,3340], alumina [35,4143] and aluminosilicate
!mullite) [37,44,45] woven bre mats have been employed.
The matrices investigated have been silica, alumina,
mullite, SiC, Si3N4 and borosilicate glass. Both aqueous
and non-aqueous suspensions have been used, although
aqueous colloidal suspensions or sols are preferred due to
environmental and cost advantages [46]. The experiments
have been invariably carried out in laboratory scale, using
EPD cells of small dimensions, i.e. the gap between the
electrodes was between 1 and 5 cm in most studies, and
the area of the bre preforms inltrated was smaller than
100 cm 2. When EPD is used as a ceramic forming technique, it is possible to use either constant current or constant
voltage conditions. An analysis of the literature showed,
however, that all investigations have been conducted by
using constant voltage conditions, the reason being most
probably that this is the simplest mode of operation.
In the case of non-conductive bres, such as aluminosilicate !mullite) bres of the type Nextel w 720 !3M Co., MN,
USA) or alumina bres !e.g. Almax w, Mitsui Mining Co.,
Japan), a modication of the basic EPD cell must be
conducted. This has been called electrophoretic ltration
deposition !EFD) and it is a modication of a method
used previously by Clasen [47]. Here, both electrodes are
made from stainless steel and a lter metallic membrane is

SiC !Nicalon w) woven bre mat/

mullite
SiC !Nicalon w) woven bre mat/
Si3N4
SiC !Nicalon w) woven bre mat/
SiC
Aluminosilicate !Nextel-610)
woven bre cloth/Be
C-bre and woven bre mat/
Si3N4 and Al2O3
Alumina !Almax w) woven bre
mat/alumina
C-bre !or cloth)/SiC

1995

SiC !Nicalon w) woven bre mat/

mullite

316L stainless steel bre

preform/soda-lime glass !with
silica interface)
SiC !Nicalon w) bre cloth/SiC

C-cloth/YSZ,SiC !Nicalon w)
bre cloth/alumina,stainless
steel wire mesh/alumina
316L stainless steel bre
preforms/alumina
316L stainless steel bre
preform/borosilicate glass !with
silica interface)
SiC !Nicalon w) woven bre mat/
yttrium disilicate
C-bre and bre cloth/alumina,
zirconia, lead zirconate titanate
Alumina multilayer blanket
!Safl w)/mullite

1997

1997

1997

1998

1998

1998

1998

1998

1997

Alumina !Almax w) woven bre

mat/mullite

1996

1996

1995

1995

1995

1995

1995

Not-specied

Aqueous suspension

Mixed !diphasic) aqueous sol of

mullite composition, pH 4

Yttrium disilicate aqueous sol,

pH 7
Suspensions in isopropyl alcohol

Silica sol, pH 46

Recycled glass powder

Nanosized yttrium disilicate

powder
Submicron alumina, zirconia
and PZT powders
Silica nanopowder, silica sol,
boehmite sol

Boehmite sol, pH 4

Suspension in acetone, addition

of surfactants
Non-specied

Silica sol, pH 9, particle size

20 nm

Boehmite sol

Non-specied

SiC powder

Fumed silica/alumina liquid

dispersion, nanosized dalumina powder
Soda-lime glass powder

Mixed !diphasic) aqueous sol

!mullite composition) and
polymeric sol
Aqueous mixed sol, pH 3.1

60

Boehmite sol, particle size

50 nm
a-SiC powder !11 wt% Al2O3
powder)
Fumed silica and boehmite
sol,and polymeric mullite sol

10

50200

Not-specied

400

60

200

Suspension in ethanol, use of

different surfactants
Aqueous sol, pH 4

Si3N4 powder Al2O3 powder

320

320

320

100

Constant voltage !V)

EPD parameters

Suspension in acetone

Suspension in acetone

Polymeric sol, pH 4,
concentration 6 g/l
Suspension in acetone

Aqueous mixed sol, pH 4.4

Aqueous sol, pH 10

Suspension conditions

Be particles

C and Si powders

Si3N4 and Y2O3 powders

Silica sol, particle size 20 nm

!12 wt% boehmite sol)
Fumed silica
nanoparticles,boehmite sol in
mullite composition
Polymeric mullite sol

SiC !Nicalon w) woven bre mat/

silica
SiC !Nicalon w) woven bre mat/
mullite

1991 1993 1994

1995

Matrix precursors

System: bre/matrix

Year

Table 1
Overview of previous research on using EPD for the fabrication of bre reinforced ceramic and glass matrix composites

28 min

10 s5 min

1 min

8 min

1 min

Not-specied

1 min

1 min

1 min

Not-specied

5 min

1015 min

20 min

1015 min

1 min

1 min

15 min

Deposition time

[43]

[29]

[40]

[54]

[50]

[22]

[39]

[53]

[38]

[42]

[28]

[35,41]

[27]

[37]

[37]

[37]

[36]

[34,35]

[4,7,33]

Reference

A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

999

C-bres and felts/hydroxyapatite

C-bres/alumina316L stainless
steel bres/titania
Aluminosilicate !mullite) bre
weaves !Nextel 720)/mullite

2000

2000

2000

2000

Aluminosilicate !mullite) bre

weaves !Nextel 720)/mullite
Ni-coated C-bres/borosilicate

316L stainless steel bre

preform/silica

1999

2000

System: bre/matrix

Year

Table 1 !continued)

Boehmite sol and fumed silica

nano-powder
Nanosized borosilicate glass
powder

Silica sol, particle size 15 nm

!12.5 wt% B2O3, 2 wt%
boehmite sol)
Submicron hydroxyapatite
powder
Nanosized d-alumina and
titania powders
a-alumina and silica powders

Matrix precursors

Mixed suspension in ethanol;

addition of surfactants
containing carboxylic acid and
amine
Mixed aqueous sol stable at pH
4.5
Aqueous colloidal sol, pH 8.5

Suspensions in ethanol

Suspension in isopropyl alcohol

Aqueous sol, pH 9

Suspension conditions

12

100

60

50

Constant voltage !V)

EPD parameters

4.5 min

4 min

7 min

1 min

10 s5 min

2 min

Deposition time

[32]

[45]

[44]

[31]

[30]

[52]

Reference

1000
A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

Fig. 2. SEM micrograph of EPD-inltrated Nicalon w bre mat using a

mixed sol of mullite composition. Details of the EPD technique used are
given in the original work [38]. A high level of matrix inltration is seen. It
was also shown that the deposited material fairly kept the original mullite
stoichiometric composition [38].

placed between the deposition electrode and the nonconducting bre preform [35,41,42]. On applying a relatively high voltage !e.g. 60 V for alumina sol [35]), the
alumina particles migrate and deposit on to the membrane
from one direction only, through the bre preform, until a
sufcient matrix thickness which envelopes the preform is
achieved. The high voltage causes hydrogen evolution at the
anode but the gas is prevented from becoming part of the
compact by the presence of the lter membrane. In this way
aluminaalumina [35] and mullitemullite [45] woven bre
reinforced ceramic matrix composites could be fabricated.
An analysis of the published work shows that the quality
of the inltration also depended strongly on the architecture
of the bre preform employed but, in general, EPD was able
to inltrate even the very tight woven bre mats used. The
parameters of the EPD inltration process, i.e. voltage
applied and deposition time, were optimised in the different
studies to obtain a high solids-loading in the intra-tow
regions and rm, adherent, ceramic deposits. When using

Fig. 3. Macrograph showing the development of microcracking in SiC

Nicalon w bre mats EPD-inltrated with mullite composition mixed sol
upon drying. Extensive microcracking is developed in thick deposits !left).
This is minimised by depositing thin lms of 12 mm thickness !right) [34].

1001

diphasic !or mixed) sols !e.g. silicaalumina dual sols of

mullite composition), the process becomes more complicated than with the single species !e.g. single silica or
alumina sols). This is because it is necessary to control
the mobility and zeta potential of both species in order for
both of them to migrate to the same electrode and co-deposit
without segregation under EPD conditions. In particular, for
the fabrication of mullite matrices, it is necessary to maintain the initial silicaalumina proportion in the deposit
material to warrant stoichiometric mullite composition.
Several authors have shown ways to engineer the surface
charge of the particles by the addition of surfactants [44] or
to control short range particleparticle interactions and
rheological characteristics of the colloidal suspensions by
careful variation of the particle size, solids-loading and pH
[48,49]. In the case of diphasic !mixed) sols of mullite
composition, the pH is chosen so that both species are oppositely charged, i.e. the alumina and silica particles are positively and negatively charged, respectively. Thus,
heterocoagulated particle clusters are formed, which move
as single, composite particles [38,43]. An example of a
Nicalon w bre mat inltrated by a mixed sol of mullite
composition using EPD is shown in Fig. 2 [38]. A high
level of matrix inltration is seen. It was shown in this
work that the deposited material fairly kept the original
mullite stoichiometric composition.
One of the most critical processing steps that must be
optimised, as emphasised by most authors, is the drying of
the inltrated bre preforms. This is because extensive
microcracking of the gelled ceramic matrix can occur on
drying, as usually occurs in solgel processing. Cracking
frequently develops due to the differential shrinkage of the
gel network generating tensile stresses at the surface, which
may lead to the catastrophic growth of microscopic aws
[50]. However, thin lms !,12 mm) can be dried without
cracking because the tensile stresses developed when they
shrink are insufcient to cause the growth of cracks [50].
Thus, a careful control of the thickness of the matrix materials deposited by EPD is required, as highlighted in the
literature [4,35]. Fig. 3 shows the different cracking development upon drying in two Nicalon w bre mats which have
been EPD-inltrated with mullite composition sol [34]. The
sample with thicker deposit exhibits extensive microcracking, while the optimisation of deposit thickness leads to a
minimisation of microcracking.
The analysis of the literature reveals that when the EPD
and drying conditions were optimised, the inltrated bre
fabrics were of sufcient quality !high inltration, no
macroporosity and minimal microcrack development) to
be used as preforms for the fabrication of ceramic or glass
matrix composites.
The EPD process has also been successfully applied to
inltrate metallic bre fabrics. Boehmite, silica and titania
nanoparticles have been used as precursors for the ceramic
matrices [22,31,51,52]. In borosilicate and soda-lime glass
matrix composites, EPD inltration of the metallic bre

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A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

3. A case in point: Ni-coated carbon bre reinforced

alumina matrix composite
3.1. Description of the EPD experimental procedure

Fig. 4. SEM micrograph of a metallic bre mat which has been fully
inltrated by silica sol using EPD. The working voltage was 4 V and
deposition time 2 min [52].

preforms was conducted by using silica nanoparticles in

colloidal suspensions [53,54]. In these composites, the
EPD porous silica deposit was used to provide adequate
matrix/bre interfacial bonding and to avoid possible
reactions between the silicate glass matrices and the
metallic bres.
Using EPD, the inltrated metallic fabrics were sufciently inltrated with matrix material so as to be used as
preforms for the fabrication of metal bre reinforced ceramic or glass matrix composites. An example of a metallic
bre mat, fully inltrated by silica sol using EPD, is shown
in Fig. 4 [52]. The working voltage was 4 V and deposition
time 2 min.
It must be pointed out that the reinforcement of ceramic
matrices by continuous ductile elements has not been as
much investigated as their ceramicceramic counterparts,
despite the advantages they may offer. These include an
increased resistance to damage during composite processing
due to the intrinsic ductility of metallic bres and the possibility of exploiting their plastic deformation for composite
toughness enhancement [55].
Overall, it appears that EPD is a very versatile and costeffective technique to inltrate complex bre architectures,
paving the way for the development of ceramic and glass
matrix composites with 2D and 3D reinforcement. Moreover, due to the high matrix homogeneity and high relative
density achieved in the green bodies by EPD, several
authors showed that the required subsequent densication
stage can be carried out by pressureless sintering
[32,35,40,42,44,51,52,53], avoiding, therefore, the costintensive traditional hot-pressing route. Specic experimental information about the EPD fabrication of Ni-coated
carbon bre reinforced alumina matrix composites, a system
being developed currently by the authors, is given below.
The objective is to describe the processing steps and to show
the way for optimisation of the EPD parameters.

The feasibility of fabricating Ni-coated carbon bre reinforced alumina matrix composites via a single-inltration
EPD process is considered here, as a typical example of the
application of EPD technique in the fabrication of ceramic
composites.
A commercially available boehmite !g-AlOOH) sol
!Remet corp, USA, Remal A20) having 40 nm average
particle size was used as alumina source. The sol contains
20 wt% solids-loading and the boehmite particles are in the
lath shape. The as-received boehmite sol was seeded with
nanosize !13 nm) d-alumina powder !Aluminium Oxide C,
Degussa AG, Germany) containing 0.5 wt% a-alumina
!BDH Chemicals, UK). The seeding powder was rst
dispersed in distilled water, then the dispersion was added
to the boehmite sol while this was stirred magnetically.
Finally, the seeded boehmite sol was ball-mixed for 12 h
using high purity TZP balls in a plastic container.
Ni-coated carbon bres !Inco spp, Incobere, 12K50,
UK) were used as reinforcement. These bres were in the
form of continuous tows of Ni-coated single carbon bres,
with 12,000 tows coated to 50% by weight with nickel. The
nickel coating provided excellent conductivity which is
essential for EPD, as well as ease of bre handling and
adequate wettability. The tows were unidirectionaly aligned
in a grooved perspex frame. EPD experiments were carried
out under vacuum. Ni-coated carbon bres held in the frame
were used as the deposition electrode !cathode). Two stainless steel plates on either side of the cathode served as the
positive !anode) electrodes. After the bre preform was
placed in the sol, the system was vacuum degassed to
remove any entrapped air, and then the cell electrodes
were connected to a 060 V dc power supply. EPD was
performed subsequently under constant voltage conditions
!5, 10, 15 and 20 V) using varying deposition times !from 50
to 500 s). An electrode separation distance of 15 mm was
used in all the experiments. Under the applied electric eld,
the very ne boehmite particles possessing a net positive
surface charge, as determined from the EM data, migrated
towards the negative electrode, i.e. the Ni-coated carbon
bre tows. The particles inltrated the bre tows and deposited until a sufcient matrix thickness, which enveloped the
bre tows, was achieved. The bre preform acting as
electrode was connected to a balance linked to a computer.
The apparatus is able to record the weight gain per millisecond during the deposition process, i.e. in real time. The
dimensions of the cathode !25 25 mm 2) were half the
anode's dimensions !50 50 mm 2) in order to eliminate
the `edge effect' which may give an inhomogeneous
thickness from the centre to the edges of the cathode. The
EPD-prepared green body specimens containing about 25
30 vol% bre loading were dried under humidity controlled

A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

1003

Fig. 5. EPD of boehmite sols on to Ni-coated carbon bre mats. Graphs of the !a) electrophoretic deposit weight and !b) electrophoretic deposit thickness, as a
function of deposition time for different applied voltages.

atmosphere for one day and left in normal air for another
day before being pressureless sintered at 12508C for 2 h
under nitrogen atmosphere.
To prepare green and sintered bre reinforced ceramic
matrix composite !CMC) samples for cross-sectional scanning electron microscopy !SEM), the specimens were
placed in a vacuum chamber and vacuum-impregnated
with Epox resin. Impregnated green and sintered CMC
samples were left to harden overnight and then cut into
slices using a diamond saw. A high resolution scanning
electron microscope !Field Emission Gun, FEG SEM,
Hitachi S-4000, Japan) was employed to characterise the
various microstructural features of the inltrated and
sintered composite bodies, including grain shape and size,
porosity distribution and location, ductile interface, deposit
thickness and inltration of the matrix into the bre architecture in both green and sintered samples.
3.2. Evaluation of EPD experiments
The boehmite sol used was kinetically stable and well
dispersed, as there were no big heteroocculated

agglomerates within the suspension. EPD experiments

were carried out under vacuum in order to eliminate
the undesirable formation and entrapment of bubbles
within the deposit due to the electrolysis !evolution of
gases) of the aqueous sol dispersion medium. Under
vacuum, very ne boehmite particles can penetrate
deep into the inter/intra-bre tows, lling all the
voids, resulting in the formation of high-quality, dense
green !and sintered) composites.
The graphs in Fig. 5!a) and !b) show the results of
electrophoretic deposit weight and thickness, respectively, as a function of deposition time for different
applied voltages. EPD experiments were performed for
up to 500 s, as this gave a deposit thickness of about
660 mm which was enough to produce a composite with
an acceptable green density. The deposit thickness
increased with increasing deposition time. When
aqueous-based sols are used in EPD experiments, one
associated problem is the electrolysis of the water.
Higher voltages resulted in rapid deposit formation,
but also in the undesirable formation and entrapment
of bubbles within the deposit due to the electrolysis

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A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

Fig. 6. SEM micrographs of EPD-inltrated unsintered Ni-coated carbon

bre reinforced alumina matrix composite containing 30 vol% bre loading. The bre preform was inltrated using an applied voltage of 15 V for
400 s. Both !a) high and !b) low magnication micrographs show that the
Ni-coated carbon bre preform was fully inltrated with the boehmite sol.
Even regions where the Ni-coated bres were nearly touching each other
have been fully impregnated by the nanosize boehmite particles, leading to
high-quality green bodies.

of the aqueous sol dispersion medium, while low

voltages reduced the electrolysis, but they also needed
higher deposition times. Thus, a compromise had to be
found and voltage and deposition time were optimised.
Voltages higher than 20 V were not used. The thickness
of selected electrophoretic deposits, measured from the
bre surface, is plotted against the deposition time for
different voltages in Fig. 5!b). The formation of the
deposit was very rapid in the rst 150 s and then
increased steadily.
In situ !real time) deposit weight measurements
provided very reliable data to determine accurately the
deposition rate. The rate of deposition was very high at
the beginning !up to 150 s), and then it started to
decrease with increasing deposition time. The decrease
in deposition rate was attributed to the increase in the
resistance of the deposit, as the current diminishes due
to the increase in deposit thickness and the removal of
charged boehmite particles from the sol. As a result of
the decrease in the potential drop across the suspension,

the velocity and deposition rate of the charged colloidal

boehmite particles also decreased.
EPD parameters were optimised in order to achieve fully
inltrated Ni-coated carbon bre reinforced alumina
composites with the minimum amount of excess material
being present in the outer regions of the preform. The optimum deposition voltage and time were determined as 15 V
and 400 s, respectively, for full inltration. The full inltration resulted in an EPD deposit thickness of .650 mm.
Using these parameters, it was possible to produce fully
inltrated mats with only a thin !100 mm) excess layer.
This was benecial as the bre mats then have a reduced
propensity to form large cracks during the drying stage. This
cracking is due to the differential shrinkage of the gel
network which generates tensile stresses at the surface of
the deposits, as mentioned above !see Fig. 3).
The SEM pictures shown in Fig. 6 represent the green
microstructures of composites produced under optimised
EPD parameters. Fig. 6!a) shows an SEM micrograph of
an EPD-formed green body containing 30 vol% bre loading. High green densities !about 61% of theoretical density)
were achieved at 15 V for 400 s. Green density was
measured by dividing the mass of the sample by its geometrically determined volume. It can also be seen in Fig. 6!b)
that the Ni-coated carbon bre preform was fully inltrated
with the boehmite sol. Even in regions where the Ni-coated
bres were nearly touching each other, full impregnation
was achieved by the nanosize boehmite powders in a very
short time, i.e. 400 s, leading to high-quality green bodies.
The effectiveness of the EPD providing full deposition
between two bres with a separation of 400500 nm is
clearly visible in Fig. 6!b). It must be noted that these
green samples were not polished in order to avoid damaging
the ductile Ni interface. Thus, some cutting effects are
visible on the carbon bres and the matrix, which resulted
from the contact with the diamond saw during the very
slow-speed cutting operation.
The subsequent composite preparation involved pressureless sintering of the green bodies at 12508C for 2 h
under N2 atmosphere. A fully inltrated and dense
sintered microstructure is shown in Fig. 7. Sintered
densities of about 91% of theoretical density were
measured by using the Archimedes technique. This result
conrms that the electrophoretic processing approach is
very convenient in terms of obtaining dense samples at
relatively low sintering temperatures and avoiding the
cost-intensive hot-pressing procedure, which has been
the common practice for the fabrication of bre reinforced ceramic matrix composites so far.

4. Conclusions
A literature review on the application of the EPD technique in the fabrication of bre reinforced ceramic and glass
matrix composites was carried out. Since the rst studies

A.R. Boccaccini et al. / Composites: Part A 32 !2001) 9971006

1005

Fig. 7. SEM micrograph of vacuum EPD-inltrated Ni-coated carbon bre reinforced alumina matrix composite containing 30 vol% bre loading after
sintering at 12508C for 2 h in nitrogen atmosphere. The micrograph shows the full deposition of the boehmite matrix into the bre preform and a dense
composite microstructure after sintering.

published at the beginning of the 1990s, a variety of bre/

matrix composite systems have been fabricated by EPD.
Carbon, SiC !Nicalon w), alumina !Almax w) and aluminosilicate !mullite) !Nextel w) woven bre preforms have been
used, mainly with silica, alumina, mullite, borosilicate glass
and SiC matrices. Overall, the analysis of the published data
demonstrates that EPD, being simple and inexpensive,
provides an attractive alternative for ceramic inltration
and coating of bre fabrics, even if they exhibit tight bre
weave architectures. The high-quality inltrated bre mats
are adequate prepregs for the fabrication of advanced glass
and ceramic matrix composites for use in heat-resistant,
structural components.
The parameters of the EPD inltration process, i.e.
applied voltage and deposition time, can be optimised to
obtain a high solids-loading in the intra-tow regions and a
rm, adherent ceramic deposit. This was shown in this paper
specically for a model Ni-coated carbon bre reinforced
alumina matrix composite.
Acknowledgements
Helpful discussions with colleagues at the University of
Birmingham, UK !Dr P. Trusty, Dr C.B. Ponton), and at
the Technical University of Ilmenau !Mr U. Schindler,
Dr H.G. Kruger, Prof. H. Kern) are appreciated.
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