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Determination and Control of Metallic Impurities

in Alumina Deposits Obtained by Aqueous
Electrophoretic Deposition
ARTICLE in JOURNAL OF THE AMERICAN CERAMIC SOCIETY MARCH 2001
Impact Factor: 2.61 DOI: 10.1111/j.1151-2916.2001.tb00734.x

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J. Am. Ceram. Soc., 84 [4] 73339 (2001)

journal

Determination and Control of Metallic Impurities in Alumina Deposits

Obtained by Aqueous Electrophoretic Deposition
Begona Ferrari, Juan Carlos Farinas, and Rodrigo Moreno*
Instituto de Ceramica y Vidrio, CSIC, 28500 Arganda del Rey, Madrid, Spain
Electrophoretic deposition (EPD) is a suitable manufacturing
method for depositing thin and thick films onto conducting
materials. Usually, EPD is performed in organic vehicles,
where handling difficulties and health hazards are important
problems. These difficulties can be solved using aqueous
suspensions; however, the high voltages that develop during
EPD increase the rate of hydrolysis and galvanic reactions. As
a result, pores or metallic contamination can be retained in the
ceramic deposit. The deposition of Al2O3 onto zinc electrodes
in water is described in this work. The formation and characteristics of Al2O3 deposits and the effect of Zn2 contamination have been studied as a function of the processing conditions (current density and deposition time) and the slurry
properties (dispersing state and solids content). A neodymium:yttrium aluminum garnet (Nd:YAG) laser, coupled to an
inductively coupled plasma spectrometer, has been used to
determine the contamination profile in the ceramic coatings.
By controlling the intensity of the electric field applied to
the slurry, as well as the slurry conductivity and solids content,
the contaminating effect of the electrode can be reduced
significantly.

I.

on advanced ceramics has been performed for nonaqueous solvents,2 8,28 33 thus, their commercial use has been limited, because of health, environmental, and economical considerations. In
addition, the use of water implies important benefits, such as better
temperature control and faster kinetics. For these reasons, the use
of water as a suspending liquid is receiving increased interest.34
Different authors have studied the EPD kinetics in water,17,35 as
well as the effect of colloidal properties on the electrical parameters.36 38 These studies are focused on obtaining uniform, dense
deposits with a controlled microstructure, either as monolithic
materials10,36,38 or laminates.37,39 42 Unfortunately, secondary
phenomena, such as water electrolysis or oxidation reactions, can
reduce the efficiency of the process and may lead to the formation
of bubbles and contamination by metallic ions that originate from
the electrode.26,37,38,43,44
The large potentials that are developed during EPD promote
electrochemical corrosion of the metallic electrodes. Most EPD
applications involve the coating of metals, such as silver, nickel, or
steels, to increase their resistance to corrosion or wear. However,
the possible contamination of the metallic substrate during coating
previously has not been studied. In this work, zinc has been
selected as the metal electrode, because it is an inexpensive
material that often is used to describe the electrochemical phenomena in electrolytic cells. Zinc can be easily oxidized but can be
used as a case material, because the other metals also oxidize.
During EPD, the corrosion potential of the most-common metals is
largely surpassed. The coating contamination that is produced
because of zinc corrosion also can be observed in the formation of
coatings onto stainless steels or in the shaping of nickel/zirconia
(Ni/ZrO2) multilayers for solid oxide fuel cells (SOFCs).
The evaluation of the contamination effect that originates from
metallic components requires more attention in water systems.
This work is an attempt to establish a rapid, reliable technique to
determine the contamination profile under different EPD conditions. For this purpose, inductively coupled plasmaatomic emission spectroscopy (ICPAES), through laser ablation, has been
used for direct chemical analysis of the green deposits.
The purpose of this work is to study the processing parameters
that are involved in the EPD of alumina (Al2O3) in water, using
zinc electrodes, and to establish a methodology for determining the
contamination profile along the deposit. A further objective is to
control the different processing variables to reduce such contamination, which would result in improved deposit properties and
ensure the reliability of the process.

Introduction

(EPD) already is recognized as a

powerful method for depositing thin and thick films onto
conductive substrates.1 8 In comparison with other emerging
technologies that are focused on the manufacturing of active or
protective coatings onto metals, such as chemical vapor deposition
(CVD), physical vapor deposition (PVD), and plasma sputtering,
EPD has some important advantages, which primarily are related
to the coating thickness that can be attained and the low processing
costs.9 13
EPD consists of the preparation of a stable, homogeneous slurry
or a solution to which a dc electric field is applied. As a
consequence of this external field, particles migrate to the oppositely charged electrode via electrophoresis. In the vicinity of the
electrode, a second process occursparticle deposition via a
complex mechanismwhich has not been described completely
yet. There is a loss of particle stability, because of deformation of
the double layers during migration (which promotes thickening of
the diffuse double layer in the direction opposite to motion, as a
consequence of retardation effects), the local increase of the solids
concentration, and the increased ionic strength.14 18
This technique has been known for a long time19 27 but only
recently has received its due attention. However, most of the work
LECTROPHORETIC DEPOSITION

II.

Experimental Procedure

Zinc disks 30 mm in diameter and 0.4 mm thick were used as

substrates, without previous surface treatment. The possible surface oxidation should have no effect on either the electrode
conduction or the analytical data. A commercial Al2O3 powder
with a purity of 99.4%, a specific surface area of 8 m2/g, and a
mean particle size of 0.5 m (Product A16SG, Alcoa, Pittsburgh,
PA) was used as the ceramic material. Al2O3 slurries were
prepared in deionized water via strong mechanical agitation for 3
min using a high-shear mixer (Model L2R, Silverson, Waterside,
Chesham Bucks, U.K.).

S.-I. Hiranocontributing editor

Manuscript No. 189947. Received August 23, 1999; approved February 11, 2000.
This work was supported by CICYT (Spain), under Project MAT97-0676.
*Member, American Ceramic Society.

733

734

Journal of the American Ceramic SocietyFerrari et al.

A solids content of 5 wt% was used, although the effect of the

solids loading also was considered by studying slurries with a
solids content of 20 wt%. A commercial polyelectrolyte that was
based on an ammonium salt of poly(acrylic acid) (Dolapix CE64,
ZschimmerSchwarz, Lahnstein/Rhein, Germany) was selected as
a dispersant. Slips with different deflocculant (referenced as the
solids) concentrations (0 1 wt%) were prepared to study the
optimum stability conditions, by measuring the zeta potential
(Mass Transport Analyzer, Micrometrics Instrument Corp.,
Norcross, GA) and conductivity (WTW, Ft. Myers, FL). Measurement of the zeta potential was conducted on slips that were
prepared with a solids content of 20 wt%, as a function of the
polyelectrolyte concentration; hence, no supporting electrolyte was
necessary.
The experiments were performed using a power supply (Model
433-3250, Labconco, Kansas City, MO) that was capable of
operating under conditions of either constant current intensity (up
to 400 mA) or constant voltage (up to 1000 V). In this work, all the
tests were performed at a constant current density (i.e., intensity).
The electrophoretic cell consisted of a glass beaker that contained
electrodes attached to a micrometric screw, which ensured the
parallelism of both surfaces and maintained at a constant distance
of 2 cm. Platinum was used as a counter electrode, to avoid
contamination.
Deposition experiments were performed using the most-stable
Al2O3 slip, by applying different current densities (1.4, 2.8, and
4.2 mA/cm2) for deposition times up to 30 min. The slips were
maintained under agitation, using a magnetic stirrer to avoid
sedimentation. The evolution of voltage during the EPD experiments was registered in all cases. The deposits were dried under
room conditions for 48 h and then characterized by measuring the
weight and the thickness. A digital indicator (Mitutoyo, Kanagawa, Japan) was used to determine the thickness.
Chemical analyses of the green deposits were made via direct
solid sample analysis, using the technique of inductively coupled
plasmaatomic emission spectrometry with laser ablation (LA
ICPAES). This technique is based on irradiation by a laser of a
solid sample that is introduced into an ablation chamber, which
promotes the fusionvaporizationatomizationionization of the
sample. This vapor is carried by an argon current and solidifies as
micrometer- and submicrometer-sized particles, which then are
analyzed by the plasma spectrometer. Prolonged irradiation results
in deeper penetration, and, therefore, a more-thorough sample
analysis. The spectrum profiles were obtained by considering the
facts that (i) one pulse corresponded to the analysis of a sample
depth of 10 m and (ii) the packing density was constant within
the deposit. A frequency-quadrupled neodymium:yttrium aluminum garnet (Nd:YAG) laser (Model LSX-100, Cetac Technologies, Omaha, NE) operating at 266 nm, coupled with an ICPAES
instrument (Model Optima 3000DV, PerkinElmer, Eden Prairie,
MN), was used. The detection of zinc, via plasma spectrometry,
was performed using the emission line located at 213.856 nm. The
in-depth contamination profiles were determined by irradiating the
deposits that were detached from the electrode, starting from the
face that was in contact with the electrode and also from the
opposite face. The number of applied pulses was high enough to
completely cross the samples. The effect of the current density, the
deposition time, the solids content, and the slurry conductivity on
the resulting contamination profile was studied.
Al2O3 deposits were sintered at 1550C for 2 h. Microstructural
observations were made on polished and thermally etched surfaces, in the edge and in the bulk of the sintered deposits, to detect
possible heterogeneities in the microstructure.

III.

Vol. 84, No. 4

current that passed between the electrodes. The reference solutions

consisted of deionized water with different concentrations of
deflocculant without ceramic powder. Figure 1(a) shows the
resulting polarization curves that were obtained in water. The same
experiment was performed using similar solutions that used
ethanol instead of water as the medium. The curves that were
obtained are plotted in Fig. 1(b). The cell geometry was the same
in both cases, and the distance between the electrodes also was
constant during the test.
A comparison of both plots clearly shows that, regardless of the
deflocculant concentration, the current density for aqueous solutions must be 10 times greater than that for the ethanol-based
solutions to maintain the same electrical field. This is the reason
why the aqueous EPD kinetics, as well as corrosion of the
electrode, are faster. Consequently, the contamination effects also
are more significant.
Figure 2 shows the variation of the zeta potential of Al2O3, as
a function of the polyelectrolyte concentration. For a polyelectrolyte concentration of 0.2 wt%, at which point the slurry is not
stable, the zeta potential has a value of zero. The maximum zeta
potential is obtained for a dispersant concentration of 0.4 wt%,
which has been assumed to be the optimum content for further
EPD tests. The pH of the slurries without dispersant was 9.2.
Dispersant additions of up to 1 wt% cause the pH decrease slightly,
down to 8.9. At this pH value, the polyelectrolyte is expected to be
fully dissociated and strongly anchored to the surface. This
condition provides the steric hindrance that is required to avoid
coagulation in a primary minimum; hence, no further pH control is
necessary.
An aqueous slurry with an Al2O3 content of 5 wt%, and 0.4
wt% deflocculant, was selected for further tests. Consecutive EPD
tests (increasing in deposition time, from 1 min to 30 min) were
performed using a fresh slurry for each current density applied

Results and Discussion

Polarization curves of the zinc electrode in the range of voltages

used in this study (up to 100 V) were constructed, to determine the
response of the material to the application of an external field in
various media. These polarizations were determined by applying
different voltages to a reference solution and registering the

Fig. 1. Polarization curves of reference deflocculant solutions prepared at

various concentrations in (a) water and (b) ethanol.

April 2001

Determination and Control of Metallic Impurities in Alumina Deposits Obtained by Aqueous EPD

Fig. 2. Zeta potential of Al2O3, as a function of the deflocculant

concentration.

(1.4, 2.8, and 4.2 mA/cm2). Figure 3 shows a plot of the evolution,
with time, of the weight/area and thickness of the green dried
deposits for the three selected electrical conditions. The evolution
of both parameters, relative to deposition time, do not follow the
expected linear kinetics that have been proposed by Hamaker;19
instead, the evolution follows an S-shaped curve. However, the
weight/thickness ratios are constant up to the 30 min tests for 1.4
and 2.8 mA/cm2, so the deposits retain their densities under the
described electrical conditions. The S-shaped behavior that is
observed in both measurements could be due to the presence of
impurities that originated from the corrosion of the metallic
electrode, in addition to the continuous change of the slurries
properties after each deposition test.
No voltage variation was detected during the formation of
coatings 500 750 m thick. This observation suggests that the
deposits behave as conductive coatings below a certain thickness.
The voltage increased only for long deposition times and high
current densities, which indicated that some barrier to conduction
existed. The conduction path could be associated with the presence
of water or metallic contamination in the deposit.
At this point, an accurate analysis of the contamination profile
along the deposit is necessary to understand the causes of the
evolution of voltage. Direct chemical analysis on the green
deposits was made using LAICPAES, through ablation of both
faces of the deposits. This technique determines the elements that
are present but not their oxidation state, because the sample has
been vaporized by the plasma. The analysis can be discussed by

Fig. 3. Evolution of thickness (open symbols) and weight/area (solid

symbols), relative to deposition time, for various current densities, using
slurries with a solids content of 5 wt%.

735

considering two possible contamination mechanisms that occur

simultaneously during the EPD test: migration and diffusion. The
rate of diffusion is dependent on the concentration gradient of the
ions in the deposit. The second mechanism is the migration of ions
due to the electric-field gradient, which, in this case, can increase
with decreasing slurry conductivity and/or increasing applied
current density.
Figure 4 shows the in-depth emission intensity profiles of zinc,
as determined from the face that is in contact with the electrode
(Fig. 4(a)) and from the opposite face (Fig. 4(b)), for deposits that
were obtained after 20 min at various current densities. The greater
the applied current, the stronger the emission signal near the
electrode. However, the in-depth behavior differs, depending on
the total deposit thickness.
The thicknesses of the deposits obtained by applying a current
density of 1.4, 2.8, and 4.2 mA/cm2 for 20 min are 500, 1200,
and 1800 m, respectively. The 500-m-thick sample shows a
very low emission intensity but is constant along the sample. The
emission peak is stronger at the contact distance as the applied
current density increases; however, the intensities of all the
emission peaks decrease and attain the same intensity level at a
depth of 500 m. In the first sample, 500 m corresponds to the
total deposit thickness, which suggests that the zinc contamination
is passing through the deposit, which becomes conductive. In the
other cases, Zn ions cannot cross the deposit, because of the
electric field is not high enough. When analysis is performed from
the opposite side, planar low intensity signals are recorded; that is,
the contamination is negligible. This observation is in good
agreement with the previously mentioned evolution of voltage,
which starts to increase only when the deposit attains a thickness
of 500 m. Conductivity also could decrease when the deposit
dries, as a consequence of electro-osmotic phenomenon. However,
the processing time, as well as the deposit thickness and packing
density, necessary for these phenomena to occur are greater than
those obtained in this work.44 Consequently, one can conclude that
the diffusion of metallic ions increases as the applied current
increases and that the ions do not migrate beyond a certain
thickness.
A similar analysis was made by comparing two Al2O3 deposits
that were obtained after two different deposition times. Figure 5
shows the emission intensity profile of the green deposit that was
obtained at a current density of 2.8 mA/cm2 after a deposition time
of 10 min (the total thickness was 500 m), in comparison with the
deposit that was obtained after 20 min under the same conditions
(a total thickness of 1800 m). Once again, the thinnest deposit
shows a lower Zn emission near the face that was in contact with
the electrode (Fig. 5(a)), whereas the signal for both samples are
similar at the face that is in contact with the slurry (Fig. 5(b)).
Hence, although the oxidation rate is the same in both cases, the
ionic concentration gradient increases as time increases and, after
20 min, the contamination increases by diffusion in the area close
to the electrode. In the opposite face, the signals are inverted, so
that the emission intensity is stronger for the shortest deposition
time. This finding confirms the previously reported results.
Generally, the electrode oxidation and particle deposition are
faster than the migration of ions through the deposit; hence,
stronger EPD conditions only produce much-higher contamination
in the vicinity of the electrode. The processing conditions may be
adjusted to obtain uniform deposits with controlled and reduced
contamination.
Another possible way to control deposit uniformity is to modify
the slurry properties. Two different approaches were proven: (i)
changing the solids content of the slurry and (ii) changing the
deflocculant concentration.
The effect of the solids content was studied by comparing the
characteristics of slurries with solids content of 5 and 20 wt%, each
prepared with 0.4 wt% dispersant. The conductivity increases from
150 S/cm to 500 S/cm when the solids content is increased.
Consequently, the electrical conditions at the slurry change. Figure
6 shows the voltage increments measured in the consecutive tests
that were performed by applying a current density of 2.8 mA/cm2
for times up to 30 min for both solids contents. For the slurries

736

Journal of the American Ceramic SocietyFerrari et al.

Vol. 84, No. 4

Fig. 4. In-depth Zn profiles corresponding to laser irradiation on (a) the surface in contact with the electrode and (b) the opposite surface of green deposits
prepared at various current densities (for slurries with a solids content of 5 wt%).

Fig. 5. In-depth Zn profiles corresponding to laser irradiation on (a) the surface in contact with the electrode and (b) the opposite surface of green deposits
prepared by applying a current density of 2.8 mA/cm2 for 10 and 20 min (for slurries with a solids content of 5 wt%).

Fig. 6.

Voltage increment during deposition for slurries with solids contents of 5 and 20 wt%.

with a solids content of 20 wt%, a voltage increment is registered

for times of 5 min, whereas for slurries with a solids content of
5 wt%, a voltage increment occurs for depositions of 15 min.
The evolution of thickness and weight/area of the deposits
obtained from both slurries, relative to deposition time, is plotted
in Fig. 7. For slurries with a solids content of 5 wt%, the evolution
of both parameters is similar. For slurries with a solids content of
20 wt%, the weight/area curve deviates, with respect to the curve
of thickness, after only 5 min of deposition. This phenomenon
could be related to a decrease in the powder concentration in the
slurry, because the deposits are thicker. However, it has been
proven that the total variation of the particle concentration after

completion of the experiment is only 11% of the initial powder

mass in the case of slurries with a solids content of 20 wt%,
whereas for slurries with a solids content of 5 wt%, the total
variation of the particle concentration is 32%. Then, the deviation is not produced by a decrease in the powder concentration;
instead, it must be related to the electrical properties of the system.
In fact, the conductivity of the slurry with a solids content of 20
wt% is 3 times larger than that of the slurry with a solids content
of 5 wt%; thus, the electric field between the electrodes is 3 times
lower and, hence, the rate of electrophoresis also is lower.
Therefore, nonconductive, uniform deposits 500 m thick can
be obtained from slurries with a solids content of 20 wt% after 5

April 2001

Determination and Control of Metallic Impurities in Alumina Deposits Obtained by Aqueous EPD

737

Fig. 7. Evolution of thickness (open symbols) and weight/area (solid symbols), as a function of deposition time, for slurries with solids contents of 5 and
20 wt%.

min of deposition. For longer times, the difference in the evolution

of thickness and weight/area suggests that the packing density
decreases.
The green deposits obtained from slurries with a solids content
of 20 wt% at a current density of 2.8 mA/cm2 after 20 min of EPD
also were analyzed via LAICPAES, as shown in Fig. 8; this
figure also shows analysis of the sample with a solids content of 5
wt%. This plot shows that, under the same electrical conditions
and even when the same amount of particles were deposited for
both slurries (350 mg/cm2; see Fig. 7), an increased solids
loading has a noticeable effect on the contamination profile. The
signal intensity is almost constant and very low. This phenomenon

is related to the low oxidation rate of the electrode in the

concentrated slurry and the limited motion of ionic impurities
when the quantity of big particles moving in the opposite sense
increases. The deposition growth kinetics during the first minutes
are double (15 mg/cm2min for a slurry with a solids content of
5 wt% and 30 mg/cm2min for a slurry with a solids content of 20
wt%); therefore, migration of impurities is obstacled before.
Literature about EPD has widely contended that the solids
content does not have a direct influence on the characteristics of a
deposit; such research considers the solids content to affect only
the deposit mass per unit area. Therefore, the deposited mass
should increase linearly as the solid concentration increases,

Fig. 8. In-depth Zn profiles corresponding to laser irradiation on (a) the surface in contact with the electrode and (b) the opposite surface of green deposits
prepared by applying a current density of 2.8 mA/cm2 for 20 min (for slurries with solids content of 5 and 20 wt%).

Fig. 9. In-depth Zn profiles corresponding to laser irradiation on (a) the surface in contact with the electrode and (b) the opposite surface of green deposits
prepared by applying a current density of 2.8 mA/cm2 for 20 min on slurries with a solids content of 5 wt% and deflocculant (Dolapix) concentrations of
0.4 and 0.6 wt%.

738

Journal of the American Ceramic SocietyFerrari et al.

according to the Hamaker equation.19 However, the results shown

here demonstrate the strong influence of the solids content and the
disagreement between the experimental results and the theoretical
equation,18 because of changes in other involved parameters
during the test, mainly the slurry conductivity.36,45
The second approach to changing the slurry properties is to
increase the dispersant concentration slightly, while always maintaining slurry stability. In this case, an increase in the suspension
conductivity also can be expected. Figure 9 shows the in-depth
contamination profiles of samples that were obtained at a current
density of 2.8 mA/cm2 after 10 min from slurries with a solids
content of 5 wt% dispersed with deflocculant concentrations of 0.4
and 0.6 wt%. Both deposits have a similar thickness (500 m).
The plot shows that this small increase in the deflocculant
concentration produces a measurable reduction in the contamination emission intensity along the entire sample thickness. The
reduction in contamination confirms the tendency that, even for
slight variations in conductivity (from 150 S/cm for 0.4 wt% of

Vol. 84, No. 4

deflocculant to 180 S/cm for 0.6 wt% of deflocculant), the higher

the slurry conductivity, the lesser the amount of zinc oxidation.
The effect of metallic contamination on the microstructure of
Al2O3 deposits sintered at 1550C for 2 h was observed using
scanning electron microscopy (SEM). Figure 10 shows images of
the cross-sectional microstructures of deposits near the electrode
(Figs. 10(b) and (d)) and the bulk (Figs. 10(a) and (c)), obtained
using a current density of 2.8 mA/cm2 after 20 min of EPD for
both solids contents. For the deposits that were formed from
slurries with a solids content of 5 wt%, the microstructure close to
the electrode is heterogeneous and a large amount of irregular
porosity is clearly detected (see Fig. 10(b)). When moving toward
the bulk, the microstructure exhibits a high degree of densification,
with a remaining closed porosity (Fig. 10(a)). The zinc inclusions
strongly affect the microstructure, leaving a large amount of
residual porosity. In the samples that were obtained from slurries
with a solids content of 20 wt%, the region near the electrode is
much more homogeneous (Fig. 10(d)), relative to the bulk (Fig.

Fig. 10. SEM micrographs showing the cross-sectional microstructure of deposits formed from slurries with solids contents of 5 wt% ((a) bulk and (b) near
the electrode) and 20 wt% ((c) bulk and (d) near the electrode) obtained for a current density of 2.8 mA/cm2 after 20 min of EPD.

April 2001

Determination and Control of Metallic Impurities in Alumina Deposits Obtained by Aqueous EPD

10(c)), which verifies the lower contamination profiles that were

measured via ICP. Only a narrow layer (5 m thick) was slightly
affected by the zinc contamination.
IV.

Conclusions

Al2O3 deposits or coatings can be obtained in water using

electrodes that are composed of metals such as zinc. When thick
samples are desired, the evolution of thickness deviates from the
linear Hamaker behavior for long electrophoretic deposition (EPD)
times and high current densities, which makes control of the
thickness difficult and affects the reliability.
The possibility to chemically analyze the contamination profile
in the green deposits is a powerful tool for controlling their
properties as a function of the applied EPD conditions. The
technique of using inductively coupled plasmaatomic emission
spectroscopy, coupled with laser ablation (LAICPAES), provides a qualitative but useful image of the state of the in-depth
contamination profile simply and rapidly.
The amount of metallic contamination that is caused by electrode corrosion can be reduced drastically by controlling the
imposed electrical conditions (mainly using a lower applied
current density). However, changing the slurry properties is
another important way of affecting the amount of metallic contamination.
Increasing the conductivity of the slurry (by changing the solids
or deflocculant content) results in a less-aggressive medium for the
zinc electrode. Furthermore, greater solids contents also increase
the growth rate of the deposit, by limiting the motion of ionic
impurities.
Generally, the solids content is thought to affect only the
quantity of deposited mass and not affect the processing conditions. However, it has been demonstrated that changes in the
deposit characteristics can be controlled by varying the slurry
concentration and/or conductivity.
In this work, zinc electrodes were selected for use. However, the
results can be extended to other metals that are used as electrodes
for EPD, because their corrosion potentials are much lower than
those applied during EPD.
Acknowledgments
The authors thank Prof. J. M. Mermet (CNRSLyon University, France) and Cetac
Technologies (USA) for analytical work.

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