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ASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING

Asia-Pac. J. Chem. Eng. (2011)


Published online in Wiley Online Library
(wileyonlinelibrary.com) DOI:10.1002/apj.526

Special Theme Research Article


Porous alumina through protein foaming–consolidation
method: effect of dispersant concentration on the physical
properties
Ahmad Fadli,1,2 Iis Sopyan,1 * Maizirwan Mel3 and Zuraida Ahmad1
1
Department of Manufacturing and Materials Engineering, Faculty of Engineering, International Islamic University Malaysia, 50728 Kuala Lumpur,
Malaysia
2
Department of Chemical Engineering, Faculty of Engineering, Riau University, 28293 Pekanbaru, Indonesia
3
Department of Biotechnology Engineering, Faculty of Engineering, International Islamic University Malaysia, 50728 Kuala Lumpur, Malaysia
Received 2 November 2009; Revised 7 September 2010; Accepted 28 September 2010

ABSTRACT: The influence of dispersant concentration on the physical properties of porous alumina ceramics formed
by the protein foaming–consolidation 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 0.01–0.05 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 µm. 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 foaming–consolidation; ceramics; porosity; characterization

INTRODUCTION material is sintered, resulting in a material with open


porosity.[2] In gel casting, a ceramic powder suspen-
Porous ceramics have great potential in many sion containing an organic monomer and a cross-linking
applications in which chemical, thermal, or mechanical agent is foamed by using a blowing agent followed by
stresses make metallic or polymeric materials unsuit- setting through in situ polymerization on the monomer.
able, as in thermally insulating applications, as filters, Gel casting produces porous ceramics with a combi-
membranes, and gas burner, or as bioceramics. The nation of open and closed pore microstructures hav-
requirements for the ceramic matrix and the pore struc- ing superior mechanical properties in a wide range of
ture may vary depending on the type of application. For porosities. However, the process has limitations with
effective thermal insulation closed porosity is favorable, respect to the control of pore size.[3] In the freeze dry-
whereas filters and membranes require open porosity. ing process, controlled crystallization of ice is used for
In the bioceramics field, it is desirable to use porous consolidation of aqueous powder suspensions into bod-
ceramic implants with certain porosity to promote inte- ies, and sublimation of the ice crystals under reduced
gration with biological tissues.[1] pressure resulted in a porous structure.[4]
A number of routes such as polymeric foam impreg-
Preparation of the trimodal pore ceramic structure
nation, gel casting, and freeze drying have been used for
has been recently reported using the foaming and
the consolidation of the powder suspensions into porous
bodies. In polymeric foam impregnation, a ceramic slip starch consolidation method.[5] Different particles such
is forced to penetrate a polymer; after drying, the poly- as poppy seeds, polystyrene, polyvinyl acetate (PVAC),
mer is removed by a burn-out operation and the ceramic and wheat particles were used as a pore-forming
agent or template for producing porous ceramics.[6 – 9]
Proteins such as ovalbumin and bovine serum albu-
*Correspondence to: Iis Sopyan, Department of Manufacturing and min have been used for the foaming and setting of
Materials Engineering, Faculty of Engineering, International Islamic
University Malaysia, 50728 Kuala Lumpur, Malaysia. aqueous ceramic powder suspensions for preparation of
E-mail: sopyan@iiu.edu.my porous ceramics.[10,11] Lyckfeldt and Ferreira reported
 2011 Curtin University of Technology and John Wiley & Sons, Ltd.
Curtin University is a trademark of Curtin University of Technology
A. FADLI et al. Asia-Pacific Journal of Chemical Engineering

a starch consolidation process for preparation of porous of 0.39 m2 /g (measured by N2 adsorption method on
ceramics.[12] a Quantachrome surface area analyzer, Autosorb-1
Porous alumina scaffolds have been applied to tissue model), was used as raw material. The protein used
engineering. The scaffold is used for bone replacement was yolk that was freshly isolated from chicken egg
and orthopedic surgery because it facilitates fast cell procured from the local market. The egg yolk con-
proliferation and has good biocompatibility, inertness, sisted of 25 wt.% proteins and 24 wt.% lipids as well
and better chemical stability.[13 – 16] In order to fulfill as 51 wt.% water [estimated gravimetrically by heating
the different demands of many applications, various at 1000 ◦ C at a heating rate of 10 ◦ C/min in a Perkin
techniques have been developed, allowing the design Elmer TG/DTA (Pyris Diamond model)]. Darvan 821A
and fabrication of porous alumina ceramics with tai- (40 wt.% aqueous solution of ammonium polyacrylate;
lored porosities, interconnectivities, mechanical proper- R.T. Vanderbilt, Norwalk, CT, USA) was selected as
ties, surface chemistry, and biocompatibility.[17] the dispersant.
Studies have shown that the rheology of the slip prior
to foaming is extremely important in determining the
structure of the resulting foam.[18] Generally, ceramic
slurries should contain a minimum amount of water Preparation of ceramic body
for molding because the shrinkage by drying decreases.
However, lower water content results in lower fluidity Slurries were prepared by dispersing the alumina pow-
of the slurries and it is necessary to use a dispersant to der, yolk, and dispersant with an alumina-to-yolk weight
maintain high fluidity.[19] ratio of 1 : 1. The dispersant concentrations were varied
Recently, we have succeeded in developing a novel from 0.01 to 0.05 wt.% (to 100 wt.% alumina powder)
method for the preparation of porous alumina with con- and one slurry was prepared without dispersant content.
trollable physical properties using egg yolk as both The slurries were stirred in a glass beaker for 3 h at a
consolidating and foaming agent.[20] The advantage of rate of 150 rpm. The slurries were cast in cylindrical
this method is that pore creation can be done at very open stainless steel molds and heated in an air oven
low temperatures (110–180 ◦ C)[20] compared with con- (Memmert, 100–800 model) at 180 ◦ C for 1 h. Cas-
ventional methods (500–600 ◦ C).[6 – 9,12] In the direct tor oil was used as lubricant for easy mold removal.
protein foaming method using egg white protein, pores The dried samples were then heated in a SiC furnace
were generated via foaming by stirring or milling, fol- (Protherm, PLF 160/5 model) at a 10 ◦ C/min rate up
lowed by drying for consolidation or gelation,[10,11] to 600 ◦ C for removal of the yolk and followed by
whereas in our work, both foaming and consolidation 1 h holding. Then, heating was continued at a rate of
occurred during drying. Therefore, control of porosity 2 ◦ C/min up to 1550 ◦ C and ended with 2 h dwell time
can be achieved by controlling the composition of the at the temperature.
slurry in the earlier method and by composition of slurry
and drying temperature as well in our work. Egg yolk is
a complex association of lipids (33% by weight), pro- Determination of foaming capacity
teins (17%), and water (50%).[21] This work suggested
that egg yolk delayed foaming during stirring. The lipid The foaming capacity of slurries was evaluated by
phase in egg yolk would lessen the foaming capacity of measuring the change in volume of slurry as a function
proteins in creating pores.[22] of drying time. A volume of 10 mL of slurry contained
In our earlier work, we have reported the effect in a 100-mL glass measuring cylinder was placed in
of time and temperature of foaming on the physical a temperature-controlled air oven for 60 min at 180 ◦ C.
properties of porous alumina.[23] A dispersant, Darvan The change in slurry volume was monitored at specified
821A, was added to increase the slurry’s stability, thus time intervals.
improving the foaming capacity and physical properties
of the porous alumina. This report presents the effect
of dispersant concentration on the physical properties
Characterization
of sintered products.
The rheological property of the slurries was measured
EXPERIMENTAL in a ThermoHaake VT 550 viscotester with a measur-
ing system of concentric cylinders using sensor type of
Materials SV-DIN. All rheological measurements were conducted
at a shear rate from 10 to 700 s−1 at ambient temper-
Commercial alumina powder (Sigma-Aldrich, Inc., St. ature. The viscosity values were derived from shear
Louis, MO, USA), with a characteristic mean diam- stress plots vs shear rates. The total porosity of the
eter of 0.25 µm (measured using a Malvern Instru- as-sintered alumina ceramics was determined by the
ments nanosizer, NanoS model) and a surface area apparent density and dimensions of the specimens. The
 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMING–CONSOLIDATION METHOD

apparent density of sintered samples obtained was mea- 0.05 wt.% dispersant concentration behaved as a New-
sured using Archimedes principles in an Electronic den- tonian fluid. Pseudoplasticity in ceramic slurries usu-
simeter (Alfa Mirage, MD300S model). The theoretical ally arises because of the existence of an inter-particle
density of fully densified alumina (3.98 g cm−3 ) was network, which undergoes a gradual breakdown with
used as reference to calculate the total volume fraction increasing shear rate, causing the typically observed
of porosity. decrease in viscosity of slurries. The viscosity value of
Each sintered porous alumina sample was cross- the slurries at high shear rate (700 s−1 ) was in the range
sectioned and coated with carbon before being sub- of 0.9–1.7 Pa s and it was still suitable for casting.
jected to analysis of surface morphology using scanning The measured flow curves for slurries were fitted with
electron microscopy (SEM) (JEOL, 5600 model) and a power law model[24] :
field emission scanning electron microscopy (FESEM)
(JEOL, JSM 6700 F model). The SEM measurement η = k γ n−1 (1)
was done on five different parts of each sample to
precisely evaluate the pore size, pore interconnection, where η is the viscosity of the slurry, γ the applied
and grain morphology. The mechanical strength of the shear rate, and k and n are the consistency factor
porous bodies was measured using a universal testing and non-Newtonian index, respectively. The extent of
machine (Lloyd, LR10K plus model) through diametri- pseudoplasticity could be due to the non-Newtonian
cal compression on samples of 3 : 2 height-to-diameter index, n, as defined by the power law model. The non-
ratios (15 mm in height and 10 mm in diameter). Five Newtonian index, n, is indicative of the inter-particle
scaffold specimens were used to determine the average network strength in the slurries. Highly shear thinning
maximum compressive strength. slurries, with a strong inter-particle network, show a
rapid decrease in viscosity with an increase in shear rate,
corresponding to a lower value on the non-Newtonian
index, n, and slurries with weak or no inter-particle
RESULTS AND DISCUSSION network exhibit closer to Newtonian behavior with n
values approaching 1.0.[25]
Rheological properties The non-Newtonian index is shown in Fig. 2 as
a function of deviation in dispersant amount. The
calculated n index for slurry without dispersant content
Figure 1 shows the rheological flow curves of slurries
is 0.51. Further, addition of dispersant up to 0.5 wt.%
with different dispersant concentrations. The viscosity
results in increases in n index, which reaches the value
of the slurries was measured at various shear rates after
0.82, indicating behavior closer to Newtonian. On the
150 rpm stirring for 3 h at ambient temperature. The
other hand, the calculated k parameter, which is a
viscosity of the slurries containing the same alumina-to-
consistency factor in the power law model, decreases
yolk ratio decreased with increasing dispersant amount. almost linearly with increasing dispersant concentration
The viscosity of slurry with dispersant concentration of in the ceramic slurry.
0.03 wt.% and without dispersant content showed shear Figure 3 shows the influence of stirring time on the
thinning (pseudoplastic flow) behavior, i.e. apparent vis- viscosity of ceramic slurry at 0.01 and 0.04 wt.% dis-
cosity decreases with shear rate, whereas the slurry with persant at a shear rate of 10 s−1 . It can be seen that the
viscosity of 0.04 wt.% dispersant slurry is lower than

Figure 1. Rheological flow curves of slurries with different Figure 2. The parameters n and k as a function of
dispersant concentrations. dispersant concentration in slurries.
 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj
A. FADLI et al. Asia-Pacific Journal of Chemical Engineering

Figure 3. The viscosity of ceramic slurry vs stirring time


(shear rate = 10 s−1 ). Figure 4. Relationship between dispersant content in
slurries and volume increase.

that of 0.01 wt.% dispersant. Properties of protein-based other words, the composition has destabilized the par-
ticle supermolecular structure, leading yolk dispersions
suspensions such as stability, rheological behavior, and
in water to exhibit ‘weak’ gel properties.[26]
texture are intimately related to interactions taking place
among adsorbed protein molecules and within the inter-
facial film.[26] The main chain of protein molecule is
Foaming capacity
characterized by covalent peptide bonds, while their
conformation is stabilized by weak, mostly noncovalent Figure 4 shows the effect of dispersant concentration
bonds. Denaturation means loss of native structure and on the foaming capacity of the slurry after being dried
biological activity of a protein through a breakdown at 180 ◦ C for 1 h. The foaming capacity is evaluated in
of the structure. Noncovalent bonds, such as hydro- terms of the volume ratio of the foamed slurry to the
gen bonds, are broken and random coil or metastable original one.
forms are formed. Denaturation is generally reversible The foaming capacity of the slurry without dispersant
if the peptide chain is stabilized in its unfolded state, content was lower than that with dispersant. As the
which inhibits any intermolecular reactions. Irreversible dispersant content was increased to 0.03 wt.%, the
denaturation occurs when the unfolded peptide chain volume of slurry was 2.5 times that of the original
is stabilized by interactions with other chains.[27] This one. It could be inferred that dispersant molecules will
is the case of yolk, in which the denaturation exposes decrease the viscosity of slurry (Fig. 1) and accelerate
amino acid side chains, which, in turn, may take part transfer of proteins from the interior of the slurry toward
in intermolecular interactions as a result of the mix- the newly created surface, thus decreasing the surface
ing process. Figure 3 also shows that the viscosity of tensions and increasing the foaming capacity.
0.01 wt.% dispersant is slightly increased from 8 to Foaming by addition of a surfactant is a simple
10 Pa s when stirring time increases from 3 to 9 h, process and has been described previously by Sevulpeda
but it increases significantly to 27 Pa s at 24 h stir- and Binner.[28] Foam volume was found to reach a
ring time. It can be inferred that, when the stirring time maximum after 5 min. Several factors introduced in
of the slurry increases from 3 to 24 h, the polypeptide the fabrication process can affect the cell size of the
chains of protein molecules become tangled to form a foamed ceramics. These include rheology of the slip
three-dimensional gel network (coagulation) through the prior to foaming, the foam volume, and also the type
formation of new hydrogen bonds between the chains, of surfactant used. All of these mechanisms alter the
hence the slurry viscosity is increased.[27] process of bubble formation and coalescence. Foaming
On the other hand, increasing the stirring time from in the presence of the methylcellulose resulted in
3 to 24 h results in no significant changes in viscosity, foamed ceramics generated in a matter of minutes with
which reaches 4 Pa s for the alumina slurry contain- optimal pore and window sizes for osteoconduction.
ing 0.04 wt.% of dispersant. The viscosity trends of
0.01 and 0.04 wt.% of dispersant can be explained
from the Darvan 821 A dispersant composition. It con- Characterization of porous ceramics
tains 60 wt.% of water shifted rheological properties
of the slurry from shear thinning behavior to shear During the preparation of green bodies, yolk con-
independent flow behavior (Newtonian), hence the stir- stituents may have to function as both foaming and con-
ring time has no effect on viscosity of the slurry. In solidating agents. The majority of proteins in yolk are
 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMING–CONSOLIDATION METHOD

organized into micellar and granular structures together


with polar and nonpolar lipid molecules. Yolk coagu-
lation or gelation, as a result of heating, is an impor-
tant functional property of the yolk in the preparation
and texture modification of ceramic products. Gel net-
work structure formation by yolk is attributed to its
constituent protein denaturation, leading to molecular
interactions and the development of a hard and rubbery
structure.[26]
In the sintering process of green bodies, shrinkage
occurred. The linear shrinkage of samples at differ-
ent dispersant concentrations is shown in Fig. 5. With
the increase of dispersant concentrations, the sintered
alumina shrunk increasingly. Shrinkage of the porous Figure 6. Relative density of the sintered porous alumina
alumina prepared from slurry with dispersant concen- as a function of dispersant concentration.
trations from 0.00 to 0.03% is in the range 29.3 ± 2.7
to 35.8 ± 0.9 vol.%, respectively. A substantial shrink- Table 1. The average pore size of porous alumina
age occurred as the organic substances such as protein measured at various relative densities.
and lipid were removed. The shrinkage increased with
increasing dispersant content. Relative density (%) Pore size (µm) Error
Figure 6 shows the relative density of the sintered 45.4 ± 3.3 54.4 ± 12 6.1
alumina as a function of the dispersant concentration. It 28.2 ± 2.2 175.0 ± 07 4.0
can be seen that the relative densities were in the range 20.9 ± 2.3 319.5 ± 18 7.5
of 18 ± 2.8 to 45 ± 3.3%; it decreased with the disper- 17.5 ± 2.8 424.5 ± 25 7.5
sant concentrations of 0.00–0.05%. It could be consid-
ered that high dispersant concentration resulted in low
viscosity, which corresponded to high foaming capacity high foaming capacity, thereby increasing the pore gen-
and low relative density. So, the products with different eration. Errors quoted are standard errors of the mean.
relative densities could be easily obtained and controlled Porosity of the samples increased as the dispersant
by means of the slurries with different dispersants. concentration increased. Porosity of the samples pre-
Density played an important role in determining the pared from the slurry without dispersant content and the
microstructure of the sintered porous alumina, as shown slurry with dispersant concentration of 0.03% was in the
in Fig. 7 and Table 1. It can be seen that an increase in range 54.5–71.8%. Generally, the strength of a porous
the pore size of alumina bodies occurred when the den- ceramic is strongly affected not only by the strength of
sity decreased. The average pore size of sintered bodies the ceramic wall (or strut) but also by the surface flaws
was in the range of 54.4 ± 12 to 424.5 ± 25 µm. It can on the strut. In order to evaluate the mechanical prop-
be explained that low viscosity of the slurry resulted in erties 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] :

σ = σ0 (1 − P )3/2 (2)

where σ is the compressive strength of a porous


structure at porosity P and σ0 is the bending strength
of the strut material, which may contain micropores. It
Figure 5. Shrinkages of samples as a function of dispersant is obvious from Eqn (2) that increasing porosity leads
concentration. to decreasing strength.
 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj
A. FADLI et al. Asia-Pacific Journal of Chemical Engineering

Figure 7. SEM micrographs of porous alumina with relative densities of


(a) 45.4 ± 3.3%, (b) 28.2 ± 2.2%, (c) 20.9 ± 2.3%, and (d) 17.5 ± 2.8%.

bonding area also has an important effect on the


improvement of sample strength.
Ceramic microcarrier is predicted to meet the spe-
cial requirements of a microcarrier technique because
of its good mechanical properties as well as chemical
and thermal resistances. Moreover, in the application of
the cell culture using a stirred bioreactor, we need to
use floatable porous ceramics as a microcarrier media
for an optimum process of cell proliferation. We have
reported that porous alumina ceramics produced by the
current method are floatable as its density could reach
below 1.0 g cm−3 .[30] On account of its considerably
high compressive strength, we believe that our porous
Figure 8. Compressive strength of porous alumina as a alumina can be a potential candidate for floating micro-
function of porosity. carrier application, especially in a bioreactor cell cul-
ture. The future works should deal with biocompatibility
of our microcarriers. A group of investigators, how-
ever, proved that in vitro tests of porous alumina with
Figure 9(a) shows the FESEM photomicrograph of fibroblast exerted no acute cytotoxic effects, confirm-
the porous alumina sample prepared at the dispersant ing the excellent biocompatibility of porous alumina
concentration of 0.05%. Interconnectivity of the pores ceramics.[31]
through windows is clearly seen in the micrographs.
The grains of porous alumina walls are irregular and
some small particles adsorb on the large grains as CONCLUSIONS
shown in Fig. 9(b). There is more bonding area among
grains. It is well known that more bonding area usually The effect of dispersant concentrations on physical
leads to higher strength between particles; consequently, properties of porous alumina was studied by discussing
the fracture of alumina bodies mainly happens at the five factors: rheological behavior, foaming capacity,
particle boundaries. Hence, the increase of the grain’s shrinkage, relative density, and strength.
 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering POROUS ALUMINA THROUGH PROTEIN FOAMING–CONSOLIDATION METHOD

Figure 9. High connectivity of the porous alumina sample (a) and grain
structure of walls (b).

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 2011 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. (2011)
DOI: 10.1002/apj

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