Ceramics International xxx (xxxx) xxx–xxx

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

The effect of wet foam stability on the microstructure and strength of porous
ceramics
Jin Zhaoa,b, Chi Yangc, Shunzo Shimaia, Xiupeng Guand, Guohong Zhoua,e, Jian Zhanga,e,
⁎
Juan Liua,e, Shiwei Wanga,e,
a
Key Laboratory of Transparent and Opto-functional Advanced Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050,
China
b
University of Chinese Academy of Sciences, Beijing 100049, China
c
Beijing Institute of Space Long March Vehicle, Beijing 100076, China
d
Beijing LDS Technology Co. LTD, Beijing 100101, China
e
State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050,
China

A R T I C L E I N F O A B S T R A C T

Keywords: Wet foam stability is of prime importance in fabricating porous ceramics with the desired microstructure and
Direct foaming mechanical properties. In this research, wet foams were fabricated via direct foaming after separately adding an
Foam stability anionic surfactant (TLS) and a cationic surfactant (DTAC) into alumina slurries with a copolymer of isobutylene
Porous ceramics and maleic anhydride (PIBM) as both the dispersant and the gelling agent. The foam stability was evaluated by a
Cell size
stability analyzer. The bubble size rapidly increased in the wet foam with TLS as the foam stabilizer and many
Compressive strength
large bubbles appeared within 60 min. The wet foam containing DTAC was very stable. Cationic DTAC increased
the hydrophobicity of alumina particles by interacting with the anionic PIBM adsorbed on the particles. The
hydrophobically modified particles acted as the foam stabilizer and enhanced the wet foam stability.
Furthermore, the fast gelling speed of the slurry containing DTAC also enhanced the wet foam stability. The
average cell size of the ceramic with 82.9% porosity from the wet foam with TLS was 188 µm and the com-
pressive strength was 9.7 MPa. The counterparts from the wet foam with DTAC were 54 µm of average cell size
and 18.1 MPa of compressive strength. The superior stability of wet foam brought about a smaller cell size and
higher strength of the resultant ceramic.

1. Introduction foam is thermodynamically unstable. The gelling system used in direct

Porous ceramics possess unique properties including high surface
area and low thermal conductivity due to their cellular microstructure
compared to dense ceramics. These enable them to have important roles
in many industrial applications including molten metal filtration, water
purification, catalyst support, high-temperature thermal insulation, and
bone tissue replacement depending on their porosity, cell size, and
structure [1–3].
Some techniques have been developed to fabricate porous ceramics
including sacrificial template, extrusion molding, and direct foaming.
Direct foaming is a simple and cost-effective method that has been
extensively used to fabricate various porous ceramics such as alumina,
silicon carbide, and mullite [4–7]. Wet foam with surfactant as the
stabilizer must be rapidly solidified by a gelling system because the
foaming includes free radical polymerization of acrylamide [5] or me-
thacrylamide [6], nucleophilic polymerization of epoxy resin and
amine [8], and spontaneous gelation of PIBM (a copolymer of iso-
butylene and maleic anhydride) [7,9,10]. On the other hand, particle-
stabilized foams have also been widely researched to fabricate porous
ceramics [11–14] since ultrastable foams were first reported [15]. The
particles used as the foam stabilizer were hydrophobically modified by
adjusting the slurry pH value and using short-chain amphoteric mole-
cules such as butyric acid and propyl gallate.
Wet foam stability is of prime importance when one wants to fab-
ricate porous ceramics with the desired microstructure and mechanical
properties. However, relatively little attention has been given to char-
acterization of foam stability. Gonzenbach et al. [16] measured average
bubble size by optical microscopy, and Sarkar et al. [17] measured the

⁎
Corresponding author at: Key Laboratory of Transparent and Opto-functional Advanced Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai
200050, China.
E-mail address: swwang51@mail.sic.ac.cn (S. Wang).

http://dx.doi.org/10.1016/j.ceramint.2017.09.169
Received 28 July 2017; Received in revised form 19 August 2017; Accepted 21 September 2017
0272-8842/ © 2017 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Zhao, J., Ceramics International (2017), http://dx.doi.org/10.1016/j.ceramint.2017.09.169
J. Zhao et al.
volume variation of wet foam to evaluate foam stability. In bubble size
measurements, only local points of the wet foam were observed, and
many measurements were necessary to obtain reliable data. In volume
measurements, macro-level foam variation cannot reveal the micro-
level bubble evolution. Furthermore, the impact of foam stability on the
microstructure and properties of the resultant porous ceramics has not
yet been systemically evaluated.
Turbiscan stability analyzer has been successfully used to analyze
the stability of various concentrated colloidal dispersions and emulsions
as well as foams [18–20], but it has not yet been used in the wet foam
for porous ceramics. The aim of this research was to evaluate the sta-
bility of two kinds of wet foams via stability analysis and to correlate
the foam stability with the microstructure and mechanical properties of
the resultant porous ceramics. The foams were fabricated by adding an
anionic surfactant and a cationic surfactant into alumina slurries with
PIBM as both the dispersant and the gelling agent, respectively. The
porosity, cell size, and compressive strength of the resultant porous
alumina ceramics from different wet foams were compared and corre-
lated with the wet foam stability.
2. Materials and methods
2.1. Materials preparation
A commercial alumina powder (AES-11, Sumitomo Chemical,
Tokyo, Japan; average particle size 450 nm) was used as the raw ma-
terial. PIBM (Isobam104, Kuraray, Osaka, Japan; M.W. 55000–65000)
was used as both the dispersant and the gelling agent. An anionic sur-
factant, triethanolamine lauryl sulfate (EMAL TD, Kao Chemical,
Tokyo, Japan; noted as TLS), and a cationic surfactant, dodecyl-
trimethylammonium chloride (QUARTAMIN 24P, Kao Chemical,
Tokyo, Japan; noted as DTAC), were used as the foaming agents.
Ultrapure water was used throughout the experiments.
Alumina slurries with 40 vol% solids loading and different contents
of PIBM (relative to alumina powder) were prepared by milling for one
hour in a planetary ball mill. Wet foams were fabricated via direct
foaming with a kitchen mixer at 600 rpm for 4 min after adding TLS
and DTAC (relative to water in the slurry) into the slurries, respectively.
Then the wet foams were cast into plastic molds. After about 10 h′
setting, they were demolded and dried at room temperature for 2 days.
Finally, porous alumina ceramics were obtained after sintering at 1550
° C for 3 h in air.
2.2. Materials characterization
The interaction between surfactant and PIBM adsorbed on alumina
particles was characterized via the zeta potential of alumina particles in
a diluted suspension containing 0.2 g/L alumina powder with a zeta
potential analyzer (Zetaplus, Brookhaven, NY, USA).
Wet foams with about 65 vol% air from the slurries with 40 vol%
solids loading and 0.25 wt% PIBM were employed to evaluate the foam
stability by a stability analyzer (Turbiscan Tower, Formulaction,
Toulouse, France). After direct foaming, the wet foam was instantly and
carefully transferred into a cylindrical vial with 25.5 mm internal dia-
meter, and the height of the wet foam was 45 mm. An 880 nm source
was used as the incident light to scan the sample layer-by-layer with
40 µm intervals from the bottom of the vial. The backscattered light
(45° from the incident, noted as BS ) was measured to reveal the foam
stability (Fig. 1). The data acquisition had 3 min intervals and lasted
22 h. In these wet foams, the bubble size (several ten microns) was
about 100 times larger than the particle size (~450 nm). The signal
variation caused by the particles in the wet foams was neglected. The
BS signal at the beginning of the measurement (t = 0) was subtracted
from those measured with increasing time, and the results were pre-
sented as ∆BS (%) profile versus the sample height at different time.
Negative ∆BS values indicated an increase in bubble size. The
2
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Fig. 1. Schematic illustration of foam stability measurement in Turbiscan stability ana-
lyzer.
fluctuation in ∆BS profile indicated heterogeneous bubble sizes in the
wet foam. In addition, there is a stability criteria named Turbiscan
Stability Index (noted as TSI ) [21], which reveals the stability of the
sample from a macro level. Lower TSI values indicate more stable wet
foam.
The effect of TLS and DTAC on the viscosity and gelation of alumina
slurries was characterized via a rheometer (Haake Viscotester iQ Air,
Thermo Electron GmbH, Karlsruhe, Germany) with a parallel plate
(20 mm in diameter). Alumina slurries with 40 vol% solids loading and
0.25 wt% PIBM were prepared by ball milling. The TLS and DTAC were
respectively added into the slurries and mixed with a glass rod for
10 min followed by degassing to remove air in the slurries. The visc-
osity of the slurries was determined with a continuous shear rate mode
increasing from 1 to 400 1/s. The gelation of the slurries was char-
acterized by measuring the storage modulus of the slurries at 25 ° C in
oscillatory mode with a frequency of 1.0 Hz and a constant strain of
0.4%.
The relative density and porosity of the porous ceramics were de-
termined via the mass-to-volume ratio and the theoretical density of α-
alumina (3.98 g/cm3). Scanning electron microscopy (JSM-6390LV,
JEOL, Tokyo, Japan) was used to observe the cell structure of the
porous ceramics. The average cell size and size distribution were de-
termined by measuring the diameters of 100 cells in the SEM images.
Five cylindrical test pieces with a diameter of 18 mm and a height of
20 mm were drilled out from one porous bulk for compressive strength
measurements via a universal testing machine (Instron 5500, Norwood,
MA) with a loading speed of 1.0 mm/min.
3. Results and discussion
3.1. Effect of surfactant on zeta potential
Fig. 2 shows the effect of two kinds of surfactants on the zeta po-
tential of alumina particles upon addition of PIBM. In the suspension
containing TLS, the zeta potential remained negative when the TLS
concentration increased from 0 to 84 ppm. However, in the suspension
containing DTAC, the potential signal changed from negative to posi-
tive. Taking the suspension with 0.2 wt% PIBM as an example, the zeta
potential varied from −23.5 to 11.1 mV with only 10 ppm DTAC ad-
dition. The potential variation in the suspension with 0.3 wt% PIBM
was similar to that with 0.2 wt% PIBM.
The PIBM used here is an anionic polyelectrolyte and generated
carboxyl groups (R-COO-) in the alumina suspension adsorbed on alu-
mina particle surface via electrostatic attraction leading to a negative
zeta potential of alumina particles. TLS is an anionic surfactant, and
therefore the zeta potential remained negative. In contrast, DTAC is a
J. Zhao et al.
Fig. 2. The effect of surfactant on zeta potential of alumina particles.
cationic surfactant, and dodecyltrimethylammonium ions (DTA+) in
the suspension could combine with the R-COO- of the PIBM chain and
possibly adsorb on the negatively charged points of alumina particle
surface via electrostatic attraction. This led to a variation in the zeta
potential from negative to positive. Meanwhile, the tails of the DTA+
ions increased the hydrophobicity of the particles, which influenced
wet foam stability and slurry gelation.
3.2. Effect of surfactant on foam stability
Fig. 3 shows ∆BS (Y-axis) obtained from wet foams with TLS and
Fig. 3. ∆BS of wet alumina foams with (a) TLS and (b) DTAC at different time.
3
Ceramics International xxx (xxxx) xxx–xxx
Fig. 4. TSI of wet alumina foams versus time.
DTAC respectively versus sample height (X-axis) at different time (t).
The ∆BS value in the wet foam with TLS was about 1% and there were
many peaks in the ∆BS profile after 15 min (Fig. 3(a)). This implied a
rapid increase of bubble size just after foaming. The ∆BS value further
increased, and the peaks in the ∆BS profile were more striking after
60 min. This indicated that the bubble size increased with time and
many large bubbles appeared at many points in the wet foam. In con-
trast, the ∆BS value of the wet foam with DTAC was only about 0.2%
after 60 min (Fig. 3(b)). This indicated that the wet foam with DTAC
was very stable.
Fig. 4 shows the variation of the TSI with time and reveals the
destabilization kinetics of the two wet foams. The TSI of the wet foam
with TLS increased rapidly and reached 1.39 after 100 min followed by
a slow increase and a plateau. In comparison, the TSI of the wet foam
with DTAC was only 0.09 after 100 min and less than 0.15 over all the
measurements. This also indicated that the stability of the wet foam
with DTAC was significantly better than that with TLS.
Cationic DTAC interacted with the anionic PIBM adsorbed on alu-
mina particles and increased the hydrophobicity of the particles. The
partially hydrophobic particles acted as the foam stabilizer and en-
hanced the wet foam stability. The excellent stability of the wet foam
with DTAC would favorably retard the germination of coalescence and
coarsening in the wet foam after foaming and control the cell structure
of the resultant ceramic.
3.3. Effect of surfactant on viscosity and gelation
Fig. 5(a) shows the effect of TLS and DTAC on the viscosity of
alumina slurries. The slurry without addition of surfactant possessed a
shear-thinning property, and the viscosity was 1.1 Pa·s at a shear rate of
100 1/s. Upon addition of 0.038 wt% TLS, the viscosity of the slurry
was almost the same as that without surfactant. Upon addition of
0.042 wt% DTAC, the slurry also presented a shear-thinning property,
but the viscosity was smaller than that without surfactant at a high
shear rate. For example, the viscosity of the slurry with DTAC addition
was only 0.6 Pa·s at the shear rate of 100 1/s. This may be attributed to
a relatively easy movement of water around the DTAC-modified PIBM.
Fig. 5(b) shows the effect of TLS and DTAC on the storage modulus
of alumina slurries. The storage modulus of the slurry without surfac-
tant addition began to increase around 6 h. With 0.038 wt% TLS in the
slurry, the storage modulus began to increase at about 3 h and reached
about 330 Pa after 4 h. This is similar to a previous report [9] and might
be due to an esterification reaction between PIBM and TLS. With
0.042 wt% DTAC in the slurry, the storage modulus rapidly increased to
436 Pa within 15 min. This was mainly attributed to the hydrophobic
interaction between DTAC-modified PIBM molecules adsorbed on alu-
mina particles. The rapid increase in the storage modulus of the slurry
J. Zhao et al. Ceramics International xxx (xxxx) xxx–xxx

of compressive strength of the high porosity ceramic. Consequently, the

ceramic with 82.9% porosity showed only 9.7 MPa compressive
strength (T3 in Table 1).
Table 2 shows the porosity, cell size, and compressive strength of
porous alumina ceramics from wet foams with DTAC. Fig. 7 shows the
cell structure and cell size distribution of these ceramics.
The concentration of PIBM and DTAC in the slurries influenced the
porosity and cell size of the resultant ceramics. With the same amount
of PIBM in the slurries, the increase in DTAC concentration increased
the porosity and decreased the average cell size. For slurries with 0.2 wt
% PIBM, the porosity increased from 68.3% to 80.7%, and the average
cell size decreased from 59 µm to 50 µm with an increase of DTAC from
0.021 wt% to 0.063 wt% (D1, D2, and D3 in Table 2, Fig. 7(a), (b) and
(c)). This was attributed to the increase in foaming ability and foam
stability with increasing DTAC concentration.
On the other hand, the increase in PIBM concentration in the slur-
ries with the same amount of DTAC increased the porosity and average
cell size of the resultant ceramics. The porosity of the resultant ceramics
from the slurries with 0.021 wt% DTAC increased from 68.3% to 72.9%
and 78.4% with an increase of PIBM from 0.2 wt% to 0.25 wt% and
0.3 wt%, and the average cell size increased from 59 µm to 64 µm and
89 µm (D1, D4, and D7 in Table 2, Fig. 7(a), (d) and (e)). The viscosity
of the slurry with high concentration PIBM was relatively low and re-
sulted in an increase in foaming ability of the slurry and porosity of the
resultant ceramic. Meanwhile, the relatively low viscosity also caused
drainage and coarsening in the wet foam. This led to the appearance of
some windows on the cell walls and an increase in the average cell size
as shown in Fig. 7(e).
The average cell size of the resultant ceramics from wet foams with
TLS was more than 120 µm (Table 1). However, that with DTAC was
smaller than 90 µm (Table 2). This was consistent with the bubble size
in the particle-stabilized foams [16]. The standard deviation of cell
sizes in the ceramics from wet foams with TLS was also bigger than that
Fig. 5. The effect of surfactant on (a) viscosity and (b) storage modulus of alumina with DTAC. The big standard deviation indicated that an obvious
slurries.
coarsening occurred in the wet foams with TLS. Consequently, the
ceramics from wet foams with DTAC showed higher compressive
with DTAC addition indicated a fast gelling speed. This also contributed strength than those with TLS, as shown in Fig. 8. The compressive
to the stability of the wet foam with DTAC. strength of the ceramic with 82.9% porosity from the wet foam with
DTAC (18.1 MPa) was much higher than that with TLS (9.7 MPa).
3.4. Porous alumina ceramics from wet foams with TLS and DTAC The difference in microstructure of the porous ceramics was caused
by the different stability mechanism and gelling speed of the wet foams.
Table 1 shows the porosity, cell size, and compressive strength of The TLS was used as the foam stabilizer, and it desorbed from the
porous alumina ceramics from wet foams with TLS. Fig. 6 shows the cell bubble interface easily due to the small adsorption energy (only a few
structure of these ceramics. kTs, k is the Boltzmann constant, and T is the temperature) [22]. This
With increasing TLS concentration from 0.038 wt% to 0.193 wt%, led to the occurrence of coalescence and coarsening in the wet foams
the porosity of the ceramics increased from 66.4% to 82.9%, and the (Fig. 3(a)). The resultant ceramics possessed large cells and windows on
average cell size increased from 124 µm to 188 µm. This is similar to the the cell walls in microstructure (Fig. 6(c)) and relatively low com-
previous research [9]. The foaming ability of the slurry increased with pressive strength (Fig. 8). In comparison, DTAC modified the PIBM
TLS concentration resulting in an increase in the porosity of the re- adsorbed on alumina particles and increased the hydrophobicity of the
sultant ceramic. The cell size markedly increased in the high porosity particles. The hydrophobically modified particles acted as the foam
ceramic (Fig. 6(c)). This was attributed to the relatively poor stability of stabilizer, whose adsorption energy was as high as thousands of kTs
the wet foam with TLS (Fig. 3(a)). The increase in porosity and cell size [22]. This resulted in an irreversible adsorption on the bubble interface
as well as large windows on the cell walls resulted in a marked decrease and excellent foam stability (Fig. 3(b)). Meanwhile, the hydrophobic
interaction between the particles increased the gelling speed (Fig. 5(b)),
Table 1
which was also beneficial for foam stability. As a result, the micro-
Porosity, cell size, and compressive strength of porous alumina ceramics from wet foams structure of the wet foam was inherited without severe coalescence and
with TLS. coarsening, and therefore the resultant ceramics possessed small cells
(Fig. 7) and high compressive strength (Fig. 8). In a word, for porous
Sample PIBM TLS Relative Porosity (%) Cell Size Compressive
ceramics fabricated from wet foams, the excellent foam stability and
(wt%) (wt Density (μm) Strength
%) (MPa) rapid gelling speed endowed the resultant porous ceramics with small
cells and high strength.
T1 0.25 0.038 0.34 66.4 124 ± 65 62.8 ± 5.7 According to the classic Gibson-Ashby model on brittle foams me-
T2 0.116 0.22 77.9 148 ± 76 26.4 ± 3.1
chanics [23], the relation between the compressive strength (σc ) and the
T3 0.193 0.17 82.9 188 ± 89 9.7 ± 0.7
relative density ( ρr ) of porous ceramics is described by:
Note: Cell size and compressive strength are shown in the form of average value and
standard deviation.
σc = Cσ0 ρrn (1)

4
J. Zhao et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 6. SEM micrographs of porous alumina ceramics from wet foams with 0.25 wt% PIBM and different TLS concentrations: (a) 0.038 wt%, (b) 0.116 wt%, and (c) 0.193 wt%.

Table 2
Porosity, cell size, and compressive strength of porous alumina ceramics from wet foams
with DTAC.

Sample PIBM DTAC Relative Porosity (%) Cell Compressive

(wt%) (wt%) Density Size Strength
(μm) (MPa)

D1 0.2 0.021 0.32 68.3 59 ± 26 71.1 ± 12.8

D2 0.042 0.20 80.4 56 ± 34 28.8 ± 4.1
D3 0.063 0.19 80.7 50 ± 26 30.4 ± 3.1
D4 0.25 0.021 0.27 72.9 64 ± 30 67.2 ± 7.0
D5 0.042 0.19 80.7 61 ± 27 29.4 ± 7.3
D6 0.063 0.18 82.3 53 ± 30 24.6 ± 5.1
D7 0.3 0.021 0.22 78.4 89 ± 63 32.6 ± 4.3
D8 0.042 0.19 81.4 65 ± 31 21.8 ± 1.9
D9 0.063 0.17 82.9 54 ± 26 18.1 ± 3.0

Note: Cell size and compressive strength are shown in the form of average value and
standard deviation. Fig. 8. Compressive strength of porous alumina ceramics from different wet foams.

where σ0 is the bending strength of dense struts, and C and n are di-
attributed to the excellent stability of the wet foams with DTAC. Fur-
mensionless constants.
thermore, the process for porous ceramics in this research is facile, and
For the porous ceramics from wet foams with DTAC, the value of the
the additives are nontoxic. Therefore, this process can be used to fab-
exponent n was 2.4 by linearly fitting the data of the compressive
ricate high strength porous ceramics.
strength and the relative density in double log plot in Fig. 8. This ex-
ponent (2.4) was smaller than the previous value (2.9) [8], and the
compressive strength was higher than that with the same por- 4. Conclusions
osity—especially for porosity values higher than 80%. This was
The stability of wet alumina foams with different surfactants was

Fig. 7. SEM micrographs of porous alumina ceramics from wet foams with different PIBM and DTAC concentrations: (a) 0.2 wt% and 0.021 wt%, (b) 0.2 wt% and 0.042 wt%, (c) 0.2 wt%
and 0.063 wt%, (d) 0.25 wt% and 0.021 wt%, (e) 0.3 wt% and 0.021 wt%, and (f) cell size distribution of these porous ceramics.

5
J. Zhao et al.
evaluated with a stability analyzer. For wet foam containing an anionic
surfactant (TLS), the TLS molecules stabilized the foam. For wet foam
containing a cationic surfactant (DTAC), the DTAC molecules hydro-
phobically modified the alumina particles, and the particles acted as the
foam stabilizer. The stability of the wet foam with DTAC was sig-
nificantly better than that with TLS. The different stability of the wet
foams resulted in a difference in cell size and compressive strength of
the porous ceramics. The ceramic with 82.9% porosity from wet foam
with TLS possessed 188 µm average cell size and 9.7 MPa compressive
strength. The counterpart with DTAC possessed 54 µm average cell size
and 18.1 MPa compressive strength. The superior stability of wet foam
endows the resultant porous ceramic with a smaller cell size and higher
strength.
Acknowledgments
This work was supported by National Key R & D Program of China
(2017YFB0310501) and Science and Technology Commission of
Shanghai Municipality (14XD1421200).
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