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ABSTRACT: The influence of dispersant concentration on the physical properties of porous alumina ceramics formed
by the protein foamingconsolidation method has been studied. Slurries of alumina powders, yolk, and dispersant
were prepared by rigorously stirring the mixture for 3 h with an alumina-to-yolk ratio of 1 : 1 in weight and dispersant
concentration of 0.010.05 wt.%. The resulting slip was poured into cylindrical shaped molds and followed by foaming
and consolidation through drying at 180 C for 1 h. The dried green bodies of the samples were then burned to remove
the pore-creating agent at 600 C for 1 h, followed by sintering at 1550 C for 2 h. The density of sintered alumina
ceramics could be controlled by varying the dispersant concentration of the slurry. Measurement of the average pore
size distribution showed that macropores of the sintered alumina porous bodies increased with decreasing density
and were found in the range of 54.4 12 to 424.5 25 m. The compressive strength was 4.6 0.8 MPa at 54.5%
porosity and it decreased significantly to 0.8 0.1 MPa at 71.8% porosity. A shrinkage of 29.3 2.7% was observed
for the sample prepared using the slurry without dispersant and it increased to 35.8 0.9% when the dispersant of
0.03% was added. 2011 Curtin University of Technology and John Wiley & Sons, Ltd.
KEYWORDS: protein foamingconsolidation; ceramics; porosity; characterization
INTRODUCTION
Porous ceramics have great potential in many
applications in which chemical, thermal, or mechanical
stresses make metallic or polymeric materials unsuitable, as in thermally insulating applications, as filters,
membranes, and gas burner, or as bioceramics. The
requirements for the ceramic matrix and the pore structure may vary depending on the type of application. For
effective thermal insulation closed porosity is favorable,
whereas filters and membranes require open porosity.
In the bioceramics field, it is desirable to use porous
ceramic implants with certain porosity to promote integration with biological tissues.[1]
A number of routes such as polymeric foam impregnation, gel casting, and freeze drying have been used for
the consolidation of the powder suspensions into porous
bodies. In polymeric foam impregnation, a ceramic slip
is forced to penetrate a polymer; after drying, the polymer is removed by a burn-out operation and the ceramic
*Correspondence to: Iis Sopyan, Department of Manufacturing and
Materials Engineering, Faculty of Engineering, International Islamic
University Malaysia, 50728 Kuala Lumpur, Malaysia.
E-mail: sopyan@iiu.edu.my
2011 Curtin University of Technology and John Wiley & Sons, Ltd.
Curtin University is a trademark of Curtin University of Technology
864
A. FADLI et al.
EXPERIMENTAL
Materials
Commercial alumina powder (Sigma-Aldrich, Inc., St.
Louis, MO, USA), with a characteristic mean diameter of 0.25 m (measured using a Malvern Instruments nanosizer, NanoS model) and a surface area
2011 Curtin University of Technology and John Wiley & Sons, Ltd.
Characterization
The rheological property of the slurries was measured
in a ThermoHaake VT 550 viscotester with a measuring system of concentric cylinders using sensor type of
SV-DIN. All rheological measurements were conducted
at a shear rate from 10 to 700 s1 at ambient temperature. The viscosity values were derived from shear
stress plots vs shear rates. The total porosity of the
as-sintered alumina ceramics was determined by the
apparent density and dimensions of the specimens. The
Asia-Pac. J. Chem. Eng. 2011; 6: 863869
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMINGCONSOLIDATION METHOD
apparent density of sintered samples obtained was measured using Archimedes principles in an Electronic densimeter (Alfa Mirage, MD300S model). The theoretical
density of fully densified alumina (3.98 g cm3 ) was
used as reference to calculate the total volume fraction
of porosity.
Each sintered porous alumina sample was crosssectioned and coated with carbon before being subjected to analysis of surface morphology using scanning
electron microscopy (SEM) (JEOL, 5600 model) and
field emission scanning electron microscopy (FESEM)
(JEOL, JSM 6700 F model). The SEM measurement
was done on five different parts of each sample to
precisely evaluate the pore size, pore interconnection,
and grain morphology. The mechanical strength of the
porous bodies was measured using a universal testing
machine (Lloyd, LR10K plus model) through diametrical compression on samples of 3 : 2 height-to-diameter
ratios (15 mm in height and 10 mm in diameter). Five
scaffold specimens were used to determine the average
maximum compressive strength.
0.05 wt.% dispersant concentration behaved as a Newtonian fluid. Pseudoplasticity in ceramic slurries usually arises because of the existence of an inter-particle
network, which undergoes a gradual breakdown with
increasing shear rate, causing the typically observed
decrease in viscosity of slurries. The viscosity value of
the slurries at high shear rate (700 s1 ) was in the range
of 0.91.7 Pa s and it was still suitable for casting.
The measured flow curves for slurries were fitted with
a power law model[24] :
= k n1
(1)
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A. FADLI et al.
other words, the composition has destabilized the particle supermolecular structure, leading yolk dispersions
in water to exhibit weak gel properties.[26]
Foaming capacity
Figure 4 shows the effect of dispersant concentration
on the foaming capacity of the slurry after being dried
at 180 C for 1 h. The foaming capacity is evaluated in
terms of the volume ratio of the foamed slurry to the
original one.
The foaming capacity of the slurry without dispersant
content was lower than that with dispersant. As the
dispersant content was increased to 0.03 wt.%, the
volume of slurry was 2.5 times that of the original
one. It could be inferred that dispersant molecules will
decrease the viscosity of slurry (Fig. 1) and accelerate
transfer of proteins from the interior of the slurry toward
the newly created surface, thus decreasing the surface
tensions and increasing the foaming capacity.
Foaming by addition of a surfactant is a simple
process and has been described previously by Sevulpeda
and Binner.[28] Foam volume was found to reach a
maximum after 5 min. Several factors introduced in
the fabrication process can affect the cell size of the
foamed ceramics. These include rheology of the slip
prior to foaming, the foam volume, and also the type
of surfactant used. All of these mechanisms alter the
process of bubble formation and coalescence. Foaming
in the presence of the methylcellulose resulted in
foamed ceramics generated in a matter of minutes with
optimal pore and window sizes for osteoconduction.
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMINGCONSOLIDATION METHOD
45.4 3.3
28.2 2.2
20.9 2.3
17.5 2.8
54.4 12
175.0 07
319.5 18
424.5 25
2011 Curtin University of Technology and John Wiley & Sons, Ltd.
6.1
4.0
7.5
7.5
high foaming capacity, thereby increasing the pore generation. Errors quoted are standard errors of the mean.
Porosity of the samples increased as the dispersant
concentration increased. Porosity of the samples prepared from the slurry without dispersant content and the
slurry with dispersant concentration of 0.03% was in the
range 54.571.8%. Generally, the strength of a porous
ceramic is strongly affected not only by the strength of
the ceramic wall (or strut) but also by the surface flaws
on the strut. In order to evaluate the mechanical properties of the samples, compressive strength tests were
conducted. The stress increased linearly with the elastic
response for all the fabricated samples and then dropped
rapidly owing to fast fracture. The compressive strength
was remarkably increased from 0.8 to 4.6 MPa, with
the porosity decreasing from 71.8 to 54.5%, as shown
in Fig. 8.
The dependence of compressive strength on porosity
can be described by several models. For highly porous
ceramic structures with interconnected pores, Gibson
and Ashby considered the macrofracture (crushing) of a
porous structure as a result of the bending microfracture
of the struts and derived the following formula[29] :
= 0 (1 P )3/2
Error
(2)
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CONCLUSIONS
The effect of dispersant concentrations on physical
properties of porous alumina was studied by discussing
five factors: rheological behavior, foaming capacity,
shrinkage, relative density, and strength.
Asia-Pac. J. Chem. Eng. 2011; 6: 863869
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMINGCONSOLIDATION METHOD
Figure 9. High connectivity of the porous alumina sample (a) and grain
structure of walls (b).
Acknowledgements
The authors would like to thank the faculty of Engineering and Research Management Center, International
Islamic University, Malaysia, for their financial support
(EDW B 0901-197) when the work was implemented.
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[5] X. Mao, S. Wang, S. Shimai. Ceram. Int., 2008; 34, 107112.
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