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Sintering of slip cast composite Al2O3-ZrO2 ceramics

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October 2018
ResearchGate
Conference: 9th International Scientific and Expert Conference TEAM 2018 · At: Novi Sad,
Serbia
Project: Monolithic and composite advanced ceramics for wear and corrosion protection -
WECOR

Authors:

Ivana Sever Lidija Ćurković Irena Zmak

University of Zagreb University of Zagreb University of Zagreb

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Abstract and Figures

Slip casting method can be used for forming monolithic and composite ceramics, in which
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a stable aqueous suspension of ceramic particles is poured into a plaster mould. Zirconia-
research
toughened alumina composite ceramics possess many attractive properties such as high-
temperature mechanical strength, wear resistance, low thermal conductivity and good
20+ million
thermal shock resistance. Compared to monolithic alumina ceramics, composite Al2O3-
members
ZrO2 ceramics have enhanced fracture toughness and flexural strength due to the
embedded zirconia grains in the alumina matrix. In this paper, water-based suspensions 135+ million
with a total of 70 wt. % solid phase content (monolithic Al2O3 and composite Al2O3-ZrO2 publications
ceramic suspensions) were prepared. The solid phase of composite ceramic suspensions 700k+ research
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consisted of either 1 or 10 dry weight base (dwb) % addition of zirconia (ZrO2) powder, projects
and the rest was alumina powder. The used zirconia (ZrO2) powder was partially
stabilized with the 3 mol % yttria (Y2O3). A dispersant (Dolapix CE 64) and a binder
(polyvinyl alcohol-PVA) were added for the stabilization of water-based suspensions. The
stability of 70 wt. % monolithic (Al2O3) and composite (Al2O3-ZrO2) ceramic suspensions
was evaluated by rheological measurements and sedimentation tests. Suspensions were
homogenized in a planetary ball mill and green bodies were prepared by slip casting of
stable suspensions in a plaster mould. After the sintering, the density of the sintered
monolithic and composite ceramic samples was measured and compared.

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Sintering of slip cast composite Al2O3-

ZrO2 ceramics
I. Sever, L. Ćurković, I. Žmak

Faculty of mechanical engineering and naval architecture, 10000 Zagreb, Croatia,

ivana.sever@fsb.hr

Abstract
Slip casting method can be used for forming monolithic and composite ceramics, in which a
stable aqueous suspension of ceramic particles is poured into a plaster mould. Zirconia-toughened
alumina composite ceramics possess many attractive properties such as high-temperature mechanical
strength, wear resistance, low thermal conductivity and good thermal shock resistance. Compared to
monolithic alumina ceramics, composite Al2O3-ZrO2 ceramics have enhanced fracture toughness and
flexural strength due to the embedded zirconia grains in the alumina matrix.
In this paper, water-based suspensions with a total of 70 wt. % solid phase content (monolithic Al2O3
and composite Al2O3-ZrO2 ceramic suspensions) were prepared. The solid phase of composite
ceramic suspensions consisted of either 1 or 10 dry weight base (dwb) % addition of zirconia (ZrO2)
powder, and the rest was alumina powder . The used zirconia (ZrO2) powder was partially stabilized
with the 3 mol % yttria (Y2O3). A dispersant (Dolapix CE 64) and a binder (polyvinyl alcohol - PVA)
were added for the stabilization of water-based suspensions. The stability of 70 wt. % monolithic
(Al2O3) and composite (Al2O3-ZrO2) ceramic suspensions was evaluated by rheological
measurements and sedimentation tests. Suspensions were homogenized in a planetary ball mill and
green bodies were prepared by slip casting of stable suspensions in a plaster mould. After the
sintering, the density of the sintered monolithic and composite ceramic samples was measured and
compared.

Keywords: alumina - zirconia composite ceramics, slip casting, stability, rheology

1. INTRODUCTION alumina, ZTA ceramics are characterized with

high fracture toughness due to zirconia's
The demand for new and improved ceramic
transformation of the tetragonal phase to
materials is constantly growing, especially over
monoclinic phase [3]. These improved
the last few decades. Although monolithic
properties such as high mechanical strength,
ceramics have a wide application scope, some
wear resistance, high flexural strength and
features such as brittleness and a low damage
fracture toughness extend the application scope
tolerance make them inadequate for some
of ZTA ceramics [4]. It has been used for
applications. Better features can be achieved by
different cutting tools, biomedical implants,
embedding ceramic fibres or grains in a ceramic
dental ceramics, structural ceramic parts and
matrix to obtain a ceramic composite with
lately armour materials [5,6].
improved properties [1].
The transformation of the tetragonal phase to
The addition of zirconia grains (ZrO2) to
monoclinic phase in stabilized zirconia acts as a
alumina matrix forms zirconia-toughened-
dissipative mechanism for fracture energy. This
alumina (ZTA) ceramic. Engineering
dissipative fracture energy is due to volume
applications of zirconia were made possible by
expansion during the tetragonal to monoclinic
the discovery of the stabilization of the
phase transformation [7]. When a crack appears
tetragonal phase using either magnesium oxide
in the material, the grains next to the crack
(MgO) or yttrium oxide (Y2O3) [2]. In addition

t f i t li i h Th h i
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Conference Paper to Sintering
high hardness
of slip cast and chemical
composite stability
Al2O3-ZrO2
ceramics
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volume and in shape of the crystal cells take
place on account of the elastic stresses during
the propagation of the crack. All these processes
lead to an increase in toughness of the ceramic
material [2].
Different technologies, such as dry-pressing,
tape casting, pressure casting, slip casting or
spraying can be used to produce composite
ceramics. All of these forming methods start
with a suspension of ceramic powder, water and
additives [8]. Slip casting is a colloidal
technique used for the consolidation of the
ceramic powder from an aqueous suspension.
The slip, i.e. the suspension, is poured into a
porous mould which withdraws water from the
slip producing a green body ready for sintering.
Slip casting is a widely used inexpensive
process suitable for producing both monolithic
and composite ceramics even for complex
geometries. However simple this technique may
be, it requires adequate understanding of colloid
suspensions and their behaviour [9,10]. In order
to obtain a material with high green density and
microstructural homogeneity, different casting
parameters must be properly adjusted such as
suspension viscosity and stability, as well as the
suspension composition. To achieve low
suspension viscosity, but also high green and
sintered density, various additives are added to
the suspensions, such as the dispersants and
binders [11]. The addition of dispersants
eliminates the powder’s tendency to
agglomerate due to the attractive intra-particle
van der Waals forces. The obtained slip has low
viscosity with high solid loading to ensure high
green density and homogeneous microstructure
[12].
In this paper, water-based suspensions with a
total of 70 wt. % solid phase pure Al2O3 as well
as mixture of Al2O3 and ZrO2 powder were
studied. Two composite ceramics were prepared
with 1 and 10 dwb % of the 3 mol % yttria-
partially stabilized zirconia (ZrO2) powder. A
dispersant (Dolapix CE 64) and a binder (PVA)
were added for the stabilization of water-based
suspensions. The stability of 70 wt. %
monolithic Al2O3 and composite Al 2O3 - ZrO2
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transform into monoclinic phase. The changes in
of
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ceramic suspensions was evaluated by
rheological measurements and sedimentation
tests. Suspensions were homogenized in a
planetary ball mill and green bodies were
prepared by slip casting of stable suspensions in
a plaster mould. After the sintering at 1600 °C,
the density of the sintered monolithic and
composite ceramic samples was measured and
compared.
2. MATERIALS AND METHODS
USED FOR RESEARCH
2.1. Preparation of monolithic
alumina and composite alumina -
zirconia ceramic suspensions
Monolithic alumina suspensions were
prepared with a total of 70 wt. % solid phase,
and composite alumina - zirconia suspensions
with 1 and 10 dwb % addition of the 3 mol %
yttria-partially stabilized zirconia (ZrO2) powder
(SkySpring Nanomaterials, Inc., USA). High-
purity Al2O3 powder was used, with the average
particle size 300-400 nm (Alcan Chemicals,
USA). A commercial carbonic acid based
polyelectrolyte dispersant Dolapix CE 64
(Zschimmer & Schwarz Chemie GmbH,
Germany) and binder PVA (polyvinyl alcohol,
Sigma Aldrich, USA) were used to stabilize
highly concentrated alumina and alumina -
zirconia suspensions. The optimal amounts of
the dispersant (Table 1) were determined in
preliminary experiments.
The binder (PVA) was dissolved in deionised
water at a temperature of 60 °C. The optimal
amounts of the dispersant (Table 1) were added
to the solution of the binder and water and added
into the grinding jar of the planetary ball mill.
After that, 70 wt. % of dry ceramic powder was
added into the grinding jar. Ten alumina balls
were used for the mixture homogenization,
which lasted for 90 minutes at a speed of 300
rpm. Alumina balls were separated from the
suspension after the homogenization using a
sieve. The suspension underwent an ultrasonic
treatment for 15 min in an ultrasonic bath –
Bransonic 220 (Branson Ultrasonics Corp.,
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USA) to remove the air bubbles and achieve
better homogeneity.
2.2. Rheological analysis of ceramic
suspensions
Rheological properties of ceramic
(monolithic and composite) suspensions were
determined using a rotational viscometer DV-III
Ultra (Brookfield Engineering Laboratories,
Inc., USA) in a small sample chamber with
spindle SC4-18. Pre-shearing lasted for 2 min at
a shear rate of 100 s-1. The shear rate was
gradually increased from 0.1 to 180 s-1, and then
reduced back to 0.1 s-1. The shear rate
increase/decrease interval was divided in 50
equal time frames, which lasted for 3 seconds
each. Rheological measurements were
conducted just before each shear rate change.
2.3. Sedimentation tests
Aqueous ceramic suspensions (monolithic
and composite) with 20 wt. % of dry solid phase
were prepared with the corresponding amounts
of the dispersant and the binder (Table 1). The
pH value was adjusted using 0.1 M HCl, 0.1 M
NaOH and the pH-meter FE20/EL20 (Mettler
Toledo GmbH, Switzerland). 14 ml of
suspensions, each with a different pH value
(from 2 to 12) were poured into test tubes and
set aside on a stand. The ceramic powder will
remain dispersed in a stable suspension, while in
an unstable suspension the ceramic powder will
settle on the bottom of the test tube. Sediment
volume was recorded after 1 h, 24 h, 72 h and 7
days for each suspension.

Table 1. Composition of prepared ceramic suspensions

Suspension Dry powder Composition of ceramic Dispersant Binder content,

content, wt.% powder content, wt.% wt.%

1 70 100 % Al2O3 0.2 0.5

2 70 99 % Al2O3 + 1 % ZrO2 0.3 0.5
3 70 90 % Al2O3 + 10 % ZrO2 1 0.5

2.4. Preparation and sintering of hour; then 3 °C min-1 to 1600 °C. To complete
ceramic green bodies the sintering process, samples were held for 2
Production of ceramics by slip casting hours at a temperature of 1600 °C after which
method involves pouring of highly concentrated they were furnace cooled to room temperature.
water-based slip (suspension) into a plaster Monolithic alumina ceramics and composite
mould. To produce ceramic green bodies, water alumina – zirconia ceramics prepared by above
is absorbed by the mould through capillary described process are shown in Figure 1.
action. This way, dense cast form is obtained
which minimizes shrinkage in the final sintering
process.
After 24 hours, green bodies were removed from
plaster moulds and dried at 100 °C for 1 hour.
Finally, dried green bodies were grinded and
polished to form the desirable shape. Shaped
green bodies were then sintered at 1600 °C in an
electric furnace (Nabertherm P310, Germany).
Sintering process was carried out as follows: Fig. 1. Sintered ceramic samples: (A) 100%
Al2O3, (B) 99% Al2O3 + 1% ZrO2, (C) 90% Al2O3 +
1 °C min-1 to 600 °C, with holding time of 1
10% ZrO2

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2.5. Density measurements suspensions, which also confirms the previous

statement. The addition of zirconia powder
The density of the sintered samples was
increases the viscosity and the shear stress.
measured using a laboratory scale with Density
Kit MS-DNY-43 (Mettler Toledo GmbH,
Switzerland). Sintered samples were weighed,
first in the air and then in a liquid (distilled
water) of known temperature. The density is
calculated by a computer program according to
the ASTM C373-88 (Standard Test Method for
Water Absorption, Bulk Density, Apparent
Porosity, and Apparent Specific Gravity of Fired
Whiteware Products, Ceramic Tiles, and Glass
Tiles). The density is defined according to the
standard by the equation:

(1)
where:
V – sample volume, cm3,
α – correction factor (α =0.99985),
A – sample mass in air, g,
B – sample mass in liquid, g,
ρ0 – liquid density, g cm-3, Fig.2. Flow curves: (A) viscosity (η) vs. shear
rate (γ), and (B) shear stress (τ) vs. shear rate (γ)
ρL – air density, g cm (ρL=0.0012 g cm ).
-3 -3

3.2. Sedimentation tests results

3. RESULTS AND
ACHIEVEMENTS
3.1. Rheological flow curves
Rheological flow curves show the
dependence of shear stress (τ) on viscosity (η) as
well as on shear rate ( γ), and can be used for
predicting the nature of interactions among
particles in the suspension. The alumina and
alumina - zirconia suspensions flow curves are
shown in Figure 2.
The obtained results show that the
suspension viscosity decreases with increasing
shear rate (Figure 2A), that is, all suspensions
show typical pseudoplastic behaviour,
characteristic for non-Newtonian fluids [13].
Figure 2B shows that the shear stress increases
with the increasing shear rate for all
Values of sediment volumes at different pH
after 1 h, 24 h, 72 h and 7 days of sedimentation
are shown in Figure 3A for the alumina
suspensions without the addition of zirconia
powder. It is visible that the alumina
suspensions are stable in acidic (2-5) and
alkaline (8-12) pH region during the first hour.
After 7 days phase separation is visible
throughout the studied pH values.
Values of sediment volumes at different pH
after 1 h, 24 h, 72 h and 7 days of sedimentation
for the alumina suspensions with the addition of
1 dwb % of zirconia powder are shown in Figure
3B. During the first few hours, alumina -
zirconia suspension is stable in the acidic (pH
2-4) and alkaline (pH 7-12) region. The pH
region of stability is shifted to the left with the

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addition of zirconia powder. Phase separation is
also visible after 72 hours.
Values of sediment volumes at different pH
after 1 h, 24 h, 72 h and 7 days of sedimentation
for the alumina suspensions with the addition of
10 dwb % of zirconia powder are shown in
Figure 3C. It is noticeable that the alumina -
zirconia suspension is stable only in the neutral
and alkaline (6-12) pH region. The pH region of
stability is shifted even more to the left with the
increase in amount of the added zirconia
powder.
Fig.3. Values of sediment volume at different pH of
ceramic suspensions after 1 h, 24 h, 72 h and 7 days
of sedimentation: (A) 100% Al2O3, (B) 99% Al2O3 +
1% ZrO2, (C) 90% Al2O3 + 10% ZrO2
3.3. Density measurements results
The results of the density measurements
showed that the density of monolithic Al 2O3
ceramic is 91.4 % of the theoretical alumina
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density (  t = 3.986 g cm-3), Table 2. The
addition of the zirconia powder to alumina
significantly increased the density of the
sintered ceramic samples. The density of the
composite ceramic with 99% Al2O3 and 1%
ZrO2 was 94% of the theoretical density (  t =
3.999 g cm-3), whereas the composite ceramic
with 90% Al2O3 and 10% ZrO2 was only 89.4%
of the theoretical density ( t = 4.172 g cm-3).
Table 2. Density () of the sintered samples
Sample , g cm-3 t, %
100% Al2O3 3.637 91.4
99% Al2O3 + 1% ZrO2 3.759 94
90% Al2O3 + 10% ZrO2 3.729 89.4
4. CONCLUSIONS
In this paper, water-based suspensions with a
total of 70 wt. % solid phase (monolithic Al2O3
and composite Al2O3 - ZrO2 ceramic
suspensions) were prepared. Composite Al2O3-
ZrO2 ceramic suspensions were prepared with 1
and 10 dwb % addition of the 3 mol % yttria-
partially stabilized zirconia (ZrO2) powder to
investigate the effect of zirconia addition on
density of the sintered ceramic samples.
The stability of 70 wt. % monolithic Al2O3
and composite Al2O3-ZrO2 ceramic suspensions
was evaluated by the rheological measurements
and the sedimentation tests. The rheological
measurements showed that the addition of
zirconia powder increases the viscosity and the
shear stress of ceramic suspensions. The pH
region of the stability of the prepared
suspensions is shifted to the lower pH values
with the increasing amount of zirconia powder.
The density of the sintered monolithic and
composite ceramic samples was measured and
compared. The results of the density
measurements showed that the addition of
zirconia powder to alumina increases the density
of the sintered ceramic samples. The density
closest to the theoretical one was observed for
the composition of 99% Al2O3 + 1% ZrO2.
Although the addition of zirconia powder
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increased
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still lower that the theoretical one. Therefore, it
must be considered to add various additives or
to modify the sintering process to further
increase the density.
5. ACKNOWLEDGEMENTS
This work has been fully supported by the
Croatian Science Foundation within the project
IP-2016-06-6000: Monolithic and Composite
Advanced Ceramics for Wear and Corrosion
Protection (WECOR).
6. REFERENCES
[1] S. Pfeifer; P. Demirci; R. Duran; H.
Stolpmann; A. Renfftlen; S. Nemrava; R.
Niewa; B. Clauβ; M.R. Buchmeiser,
Synthesis of zirconia toughened alumina
(ZTA) fibers for high performance
materials. Journal of the European
Ceramic Society 36 (2016), pp.725–731
[2] I.V. Antoniac, Handbook of bioceramics
and biocomposites. Springer
International Publishing Switzerland,
(2016).
[3] P. Maiti; M. Bhattacharya; P.S. Das; P.S.
Devi; A.K. Mukhopadhyay, Indentation
size effect and energy balance issues in
nanomechanical behavior of ZTA
ceramics. Ceramics International 44
(2018), pp.9753–9772
[4] H.L. Calambás Pulgarin; L.B. Garrido;
M.P. Albano, Processing of different
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casting. Ceramics International 39
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[5] H. Wu; W. Liu; R. He; Z. Wu; Q. Jiang;
X. Song; Y. Chen; L. Cheng; S. Wu,
Fabrication of dense zirconia-toughened
alumina ceramics through a internal loop airlift reactors involving
stereolithography-based additive
manufacturing. Ceramics International
43 (2017), pp.968–972
[6] P. Maitia; M. Bhattacharyaa; P.S. Dasa;
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Indentation size effect and energy
balance issues in nanomechanical
behavior of ZTA ceramics. Ceramics
International 44 (2018), pp.9753-9772
[7] G.P. Cousland; X.Y. Cui; A.E. Smith;
A.P.J. Stampfl; C.M. Stampfl,
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[8] M.M. Renjo; L. Ćurković; K. Grilec,
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[9] A. Evcin, Investigation of the effects of
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Special Issue of the journal Materials: Mechanical Properties and Applications of Advanced Ceramics
Lidija Ćurković · Irena Zmak

The journal Materials (ISSN 1996-1944) is currently running a Special Issue titled Mechanical Properties and Applications of Advanced
Ceramics. As Guest Editors of this Special Issue, we would lik ... [more]

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Article

Structural and Microstructure Relationship with Fracture Toughness of CeO2 Addition into Zirconia To...

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10/12/22, 4:41 PM (PDF) Sintering of slip cast composite Al2O3-ZrO2 ceramics
December 2012 · Advanced Materials Research
Conference Paper Sintering of slip cast composite Al2O3-ZrO2 ceramics
Rejab Nik Akmar · Zahirani Ahmad Ahmad Azhar · Mani Maran Ratnam · Zainal Arifin Ahmad

The full-text
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CeO2 addition in zirconia
Read full-text toughened alumina citation
Download (ZTA) was examined.
CopyThe
linkCeO2 addition in weight percent (wt %) was
varied from 0 wt% to 15 wt%. The fabricated samples were sintered at a temperature of 1600°C. The sintered samples were
characterized their properties such as fracture toughness and phase determination. X-ray diffraction patterns confirm the constituent
phases present in ... [Show full abstract]

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Article Full-text available

The role of powder preparation method in enhancing fracture toughness of zirconia ceramics with low...

September 2015 · Journal of Ceramic Science and Technology

Igor Danilenko · Tetyana Konstantinova · G. K. Volkova · [...] · V. Glazunova

In most cases zirconia-alumina composites for scientific investigations and industry are prepared by means of mechanical mixing of
powders, compaction and sintering. In our opinion, this is one of the reasons for the low values for fracture toughness of the sintered
materials. In this study, we investigated the effect of nanopowder synthesis methods on the structure and mechanical properties of ...
[Show full abstract]

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Article Full-text available

Stabilization of Highly Concentrated Alumina Suspensions by Different Dispersants

October 2018 · Transactions of FAMENA

Ivana Sever · Irena Zmak · Lidija Ćurković · Zrinka Švagelj

Slip casting is a widely used colloidal technique for consolidation of ceramic powders from a suspension. The colloidal approach
ensures homogeneous microstructure of a green body, thereby reducing post-sintering machining and production costs. The process
consists of several steps. The first step is to mix the ceramic powder with a liquid, usually water, where the stabilization of the new ...
[Show full abstract]

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Composition Optimization of Alumina Suspensions which Contain Waste Alumina Powder

January 2018

Irena Zmak · Lidija Ćurković · Milan Vukšić

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Article Full-text available

Optimization of Sintering Process of Alumina Ceramics Using Response Surface Methodology

June 2021 · Sustainability

Lidija Ćurković · Irena Zmak · Darko Landek · [...] · Ivana Gabelica

In this work, alumina (Al2O3) ceramics were prepared using an environmentally friendly slip casting method. To this end, highly
concentrated (70 wt.%) aqueous suspensions of alumina (Al2O3) were prepared with different amounts of the ammonium salt of a
polycarboxylic acid, Dolapix CE 64, as an electrosteric dispersant. The stability of highly concentrated Al2O3 aqueous suspensions
was monitored ... [Show full abstract]

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Article Full-text available

Spark Plasma Sintering of dense alumina ceramics from industrial waste scraps
February 2021

Irena Zmak · Lidija Ćurković · Milan Vukšić · Andraz Kocjan

The implementation of environment-friendly manufacturing, which include the reuse and recycling of materials is nowadays crucial in
https://www.researchgate.net/publication/328335584_Sintering_of_slip_cast_composite_Al2O3-ZrO2_ceramics 10/11
10/12/22, 4:41 PM (PDF) Sintering of slip cast composite Al2O3-ZrO2 ceramics
order to meet the circular economy approach. The present study shows the possibility of recycling waste alumina scraps obtained after
Conference
the Paper Sintering
green machining ofduring
step slip cast
the composite Al2O3-ZrO2
manufacturing process ofceramics
alumina ceramics as a broken ware, which contained small amounts
(≤5 ... [Show full abstract]

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Last Updated: 05 Jul 2022

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