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J Porous Mater (2011) 18:195–203

DOI 10.1007/s10934-010-9370-8

Porous ceramics with controllable properties prepared by protein


foaming-consolidation method
Ahmad Fadli • Iis Sopyan

Published online: 11 March 2010


Ó Springer Science+Business Media, LLC 2010

Abstract A new protein foaming-consolidation method 1 Introduction


for preparing porous alumina was developed using egg
yolk both as consolidating and foaming agent. This method Porous ceramics have become important materials for
allows the control of properties of porous alumina not only various applications such as catalyst, porous burners,
by varying alumina-to-yolk ratio but also by managing the membrane, kiln furniture, and bioceramics [1–5]. Each
foaming process. After drying, the green bodies were application needs specific features and properties of porous
burned at 600 °C for 1 h to remove the pore creating agent, ceramics; they may differ in terms of porosity, strength,
followed by sintering at 1,550 °C for 2 h. The porous pore size distribution, pore morphology and pore connec-
alumina ceramics with pore sizes of 25–1,000 lm and tivity. For effective thermal insulation, for example, it is
relative density of 29–50% were obtained. The compres- favorable to have closed porosity whereas for filters and
sive strength of the sintered samples varied within the membranes open porosity is a must. In the bioceramics
range of 1.1–5.7 MPa, corresponding to porosity of 40– field it is desirable to use porous ceramic implants with
71%. The addition of dispersant with different concentra- certain porosity to promote integration with biological
tion into alumina slurries shifted the rheological properties tissues [6].
from shear thinning behavior to a Newtonian fluid, which Processes like replication method and the foaming
resulted in changes in the pore sizes of the resulting method have been used for preparation of porous ceramics.
ceramics. The main advantages of the process are the Schwartzwalder and Somers [7] reported the replication of
simplicity of the process and the low-cost processing polymer foams, as one of the first manufacturing tech-
equipment/materials needed. These results have opened a niques developed for producing ceramics with controlled
novel preparative way for porous ceramics especially alu- macroporosity. They started using polymeric sponges as
mina-based porous materials designed for biomedical templates to prepare ceramic cellular structures of various
applications. pore sizes, porosities, and chemical compositions. In the
polymeric replica approach, a highly porous polymeric
Keywords Protein foaming-consolidation  Egg yolk  sponge (typically polyurethane) is initially soaked into a
Alumina  Porous ceramics  Compressive strength  ceramic suspension until the internal pore cavities are filled
Porosity with suspension. The polymeric sponge is then removed
from the suspension and the excess slurry squeezed out.
This is followed by firing to completely vaporize and burn
A. Fadli  I. Sopyan (&)
out the organic material as well as to vitrify the ceramics.
Department of Manufacturing and Materials Engineering,
Faculty of Engineering, International Islamic University In the foaming method, porous ceramics are prepared by
Malaysia, 50728 Kuala Lumpur, Malaysia mixing ceramic powder with organic materials as a pore-
e-mail: sopyan@iiu.edu.my forming agent, which are followed by combustion of the
mixture, leaving pores within the ceramic body. This
A. Fadli
Department of Chemical Engineering, Faculty of Engineering, technique allows easy and fast production of highly porous
Riau University, Pekanbaru 28293, Indonesia ceramics materials with generally less open and dense

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struts which results in lower permeability but higher alumina were controlled by adjusting the drying tempera-
strength [8]. ture of slurry [16]. In this report we wish to present the
Lyckfeldt et al. reported a starch consolidation method for effect of foaming process condition and composition
preparation of porous ceramics. In this process, native and between yolk and alumina powder on physical properties
chemically modified potato starch granules were incorpo- of the obtained porous alumina.
rated into aqueous ceramic powder suspensions and the
slurry was further consolidated into near-net-shape bodies by
heating in the temperature range of 60–80 °C. The process 2 Experimental
produces porous ceramics with 30–70% porosities and pore
size depends on the size of starch granules which is nearly 2.1 Materials
50 lm [9]. Preparation of porous ceramics with hierarchical
structure has also been reported using foaming and consol- The starting materials used to prepare the porous ceramics
idation method. In this case, a ceramic powder suspension were a commercial alumina powder (Sigma–Aldrich, Inc.
containing cassava starch is foamed by using a liquid USA), with an average particle size of 0.25 lm (measured
detergent followed by consolidated in a microwave at 400 W using a Malvern Instruments nanosizer, NanoS model) and
[10]. The usages of ovalbumine as foaming agent have been a specific surface area of 0.39 m2/g (measured by N2
tried by some researcher groups [11]. However, due to its adsorption method on a Quantachrome surface area ana-
high foaming capacity, it was hardly to be suitable to make lyzer, Autosorb-1 model). Scanning electron microscope
porous ceramics with controlled porosity. (SEM) measurements showed that most of the particles
Recently, there is an increasing attention in using pro- have irregular size and shape. Protein used was yolk that
teins as additives to make porous materials. Proteins are freshly isolated from chicken egg. Darvan 821 A (R. T.
high molecular compounds, which are formally understood Vanderbilt, Norwalk, CT) was selected as the dispersant
as products of amino acids condensation. The main chain because of its ability in stabilizing dispersion of alumina in
of protein molecule is characterized by covalent peptide protein -water suspension [11].
bonds, while their (conformation) is stabilized by weak,
mostly non-covalent bonds. A change in the situation of 2.2 Preparation of porous ceramics
these bonds leads to a change in physical and chemical
properties of the molecule. The thermal activated loss of The flow chart in Fig. 1 describes an overview of the
this structure is called denaturation. Proteins are prone to process. Slurries were prepared by dispersing the alumina
foaming because of their amphilic character [12]. When powder and yolk with an alumina-to- yolk ratios of 1.00,
adding a protein to a ceramic slip through a mixing oper- 0.83, 0.75, and 0.65 in weight. The slurries were magnet-
ation, air bubbles are introduced, and the protein molecules ically stirred in a beaker glass for 3 h with a rate of
are adsorbed at the interface between air and water via 150 rpm. Into the slurry, the dispersant of 0.01–0.05 wt%
hydrophobic areas, and a partial unfolding (surface dena- concentrations was added. The slurries were cast in
turation) occurs. The increase in the surface tension caused cylindrical open stainless steel mold (ø & 1.3 mm,
by protein adsorption facilitates the formation of the new h & 1.4 mm). Covering the molds with castor oil made
interfaces and more bubbles are created. The ability of demolding easier. Thermal foaming-consolidating was
protein molecules to form and stabilize foam depends on done in an air oven (Memmert, 100-800 model) at range
the diffusion rate and denaturation ability [12]. temperatures of 110–180 °C for 1 h. The yolks were
Garrn et al. [13] reported the usage of protein (Bovine removed by burn-out in a SiC furnace (Protherm, PLF 160/
Serum Albumine, BSA) as binders for producing alumina 5 model) at 600° for a period of 1 h at 10 °C/min rate.
foams. The combination of foaming and increased stiffness Then heating was continued at a rate of 2 °C/min up to
gave a stable protein-ceramic foam structure. A fine cel- 1,550 °C ended by 2 h dwell time at the temperature.
lular foam structure of approximately 50–300 lm cell
diameters and 8–20% relative densities was obtained [13]. 2.3 Determination of foaming capacity
We have succeeded in developing a novel method for
preparation of porous alumina using egg yolk as both The foaming capacity of slurries was evaluated by mea-
consolidating and foaming agent [14]. Egg yolk is a suring the change in volume of slurry as a function of
complex association of water (50%), lipids (33%) and drying time. 10 mL slurries contained in a 100 mL glass
proteins (17%) [15]. It has been well known that the lipids measuring cylinder was placed in a temperature-controller
phase in egg yolk would reduce the foaming capacity of air oven for 60 min. The temperature was varied between
protein in making pores. Previously, we have reported that 100 and 180 °C. The change in slurries volume was
the porosities and compressive strengths of the porous monitored for every specified time intervals. The foaming

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alumina-to-yolk ratio on the viscosity alumina slurries. For


comparison purpose, the viscosity of alumina suspension
with dispersant addition is also plotted in Fig. 2. It can be
seen clearly that the slurries without dispersant addition
showed pseudoplastic flow behavior. Though the slurries
showed small difference in viscosity (9.3–12.4 Pa s) at low
shear rate (10 s-1), the viscosity values of the slurries are
close at high shear rate. Pseudoplasticity in ceramics
slurries usually arises because of the existence of an
interparticle network, which undergoes a gradual break-
down with increasing shear rate, causing the typically
observed decrease in viscosity of slurries. It can be also
seen from Fig. 2 that addition of dispersant into slurries
with 1.00 alumina-to-yolk ratio altered flow behavior from
shear thinning to a Newtonian fluid. A viscosity of as high
as 12.4 Pa s was observed for the slurry without dispersant
content at low shear rate (10 s-1) but it decreased signifi-
Fig. 1 Preparation process of porous alumina ceramics by protein cantly to 2.0 Pa s when 0.05 wt% dispersant was added.
foaming-consolidation method The viscosity value of the all slurries at high shear rate
(700 s-1) was in the range 0.9–1.9 Pa s and it was still
capacity is evaluated in terms of the volume ratio of suitable for casting.
foamed slurry to the original one [17]. The pseudoplasticity in ceramic can be characterized by
non-Newtonian index n calculated according to the power
2.4 Characterization law model as per the following equation [18]:
g ¼ kcn1 ð1Þ
The rheological property of the slurries was measured in a
ThermoHaake VT 550 viscotester with a measuring system where g is the viscosity of the slurry, c the applied shear
of concentric cylinders using sensor cone type of SV-DIN. rate, k and n are the consistency factor and non-Newtonian
Thermogravimetry analysis was carried out in a Perkin index, respectively. Highly shear thinning slurries, with a
Elmer TG/DTA (Pyris Diamond model) to understand the strong inter-particle network, show a rapid decrease in
details of the yolk burn-out in ambient air at a heating rate viscosity with an increase in shear rate, corresponding to a
of 10 °C/min. The apparent density of sintered samples lower value on the non-Newtonian index, n, and slurries
obtained was measured in Electronic densimeter (Alfa with weak or no inter-particle network become closer
Mirage, MD300S model). The theoretical density of fully to the Newtonian behaviour with n values approaching
densified alumina (3.98 g/cm3) was used as the reference to 1.0 [18]. However, in suspensions containing yolk the
calculate the total volume fraction of porosity. The pore
size, interconnection among pore and also the grain
structure were examined using scanning electron micros-
copy (JEOL, 5600 model) and field emission scanning
electron microscopy (JEOL, JSM 6700 F model). The
mechanical strength of the porous bodies was measured
using a universal testing machine (Lloyd, LR10 K plus
model) through diametrical compression on samples of 3/2
height-to-width ratio. Five scaffold specimens were used to
determine the average maximum compressive strength.

3 Results and discussion

3.1 Rheological behavior


Fig. 2 Plots showing the change in viscosity of alumina slurries as a
The viscosity of the slurries were measured at various shear function of shear rate at various mixing conditions of alumina and
rates after 150 rpm for 3 h. Figure 2 shows the influence of yolk

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Table 1 The parameters n and k as a function of yolk and dispersant


contents in alumina suspensions
Alumina-to-yolk mass Dispersant k n
ratio (w/w) concentration (%)

0.65 0 74.2 0.32


0.75 0 47.3 0.41
1.00 0 37.6 0.51
1.00 0.03 8.5 0.71
1.00 0.04 3.9 0.81
1.00 0.05 3.1 0.82

Fig. 3 The effect of drying temperature on volume increase of slurry


pseudoplasticity arises not only from gradual breakdown of at 1.00 alumina mass-to-yolk ratio without dispersant addition
the inter-particle network of ceramic grains but also from
alignment of the yolk molecule at high shear rates. form a continuous viscoelastic film. For effective foam
The calculated n index for the 1.00 alumina-to-yolk ratio formation, proteins must be capable of migrating and ori-
slurries with 0.03–0.05 wt% dispersant is in range of 0.71– entating rapidly to form encapsulating films around the gas
0.82, thus indicating a behavior closer to Newtonian bubbles to prevent destabilization. Foams may destabilize
(Table 1). On the other hand, n values for slurries without due to: (1) diffusion of gas from small to large bubbles or
dispersant addition and varied yolk are in the range of to the atmosphere, termed Ostwald ripening or dispropor-
0.32–0.51 indicating the shear thinning behavior. The tionation; (2) drainage of liquid from and through the foam
calculated k parameter, which is a consistency factor in layer due to gravity; and (3) coalescence of bubbles due to
the power law model, decreased almost linearly with the instability of the film between them [20].
increasing dispersant concentrations but increased with the The amphiphilic character of protein molecule causes a
increasing yolk contents in the ceramic suspension. decrease in surface tension, thus leading to possibly better
foaming properties [20, 21]. The foaming capacity values
3.2 Foaming of slurry determined from volume increase of slurry was 2.2, 1.97
and 1.7 v/v for slurry alumina-to-yolk ratios 0.65, 0.83 and
Figure 3 shows the effect of drying temperature on volume 1.00 respectively. The foaming ability of slurries became
increase of slurry at 1.00 alumina mass-to- yolk ratio intensive with the increased yolk content.
without dispersant addition. It is well known that heat- The volume increases for slurry without and with 0.01%
treatment can induce protein denaturation, thus leading to dispersant addition at 60 min drying are presented in
changes in the functional properties of the treated proteins Table 2. The foaming experiments involving slurries con-
[19]. During the process of denaturation, secondary va- taining dispersant (Darvan 821 A) showed that the foaming
lency bonds such as hydrogen bridge bonds, ionic bonds, capacity increased with dispersant addition of 0.01 wt% in
hydrophobic bonds and disulphide bridges are partially the slurry in the range of drying temperature 110–180 °C.
modified. In consequence of the partially or totally Compared to the slurries without dispersant which pro-
unfolding, larger random coil structures are formed. duces volume increase in the range 1.0–2.0 (v/v) the slur-
Between these unfolded protein chains new bonds are ries containing dispersant of 0.01% has improved foaming
statistically formed. This leads to consolidation and a capacity from 1.3 to 2.2 (v/v). It could be deducted that
decrease in solubility [12]. dispersant molecules will decrease the viscosity of slurry
Generally, foaming of slurry took place in three stages: (see Fig. 2) and accelerate transfer proteins from interior of
pre-heating of slurry without increasing volume, foaming the slurry towards the newly created surface, thus
stage with the strongly increased until reaches a maximal decreasing the surface tensions and increasing the foaming
value and then undergoes a plateau (stabilizing stage). capacity.
During the pre-heating period, the structural properties of The foam stability is the ability to retain air for a certain
protein were induced by heating, leading to changes in the period of time [22]. For certain drying time, the surface
functional properties. Subsequently, during foam forma- tensions minimal value, hence the foaming capacity keeps
tion, proteins will (1) diffuse to the air–water interface, steady and stable. Foam stability relates to the stability
concentrate and reduce surface tension; (2) partially unfold lamellae and the ability to retain the gas for a given time.
and reorient such that the polar groups are directed towards Foam stability is a reflection of foam film characteristics
the polar phase; and (3) interact with one another via non- such as impermeability to gas, viscoelastic characteristics
covalent interactions and potentially covalent bonds to and mechanical strength of the film [20].

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Table 2 The effect of the addition of 0.01 wt% dispersant into the
slurry on foaming capacity at 60 min drying
Drying Volume increase (v/v)
temperature (°C)
Added with 0.01% Without
dispersant dispersant

100 1.30 1.09


110 1.55 1.32
160 1.81 1.78
180 2.19 2.00

The stability of the foam relates to the decrease of foam


volume with time. We found that the green bodies after
demolding would be collapse when it dried less than
Fig. 5 TG curve of egg yolk
20 min time, whereas after drying time more than 20 min,
the green bodies would be steady. A photograph of typical
Thus, the heating was set up to 600 °C with a dwell time of
green bodies produced from the suspension after 13 and
1 h to allow ample time for the complete burnout of the
40 min drying is shown in Fig. 4.
yolk for creating pores.
3.3 Burn-out
3.4 Sintering
In general, foamed green body is easy to debinder than
Prepared alumina samples after sintering were performed
dense body, for it contains abundant cells and channels to
without significant deformations which indicated good
let organic components occupy and escape. Thermal
homogeneity of the materials. Figure 6 shows three sin-
analysis was used to optimize the burn-out schedule of the
tered porous alumina samples with cylindrical shape.
foamed body.
The relative density and shrinkage of sintered samples
Figure 5 shows a TGA curve for yolk carried out in air.
using slurry without dispersant addition is listed in Table 3.
The figure revealed that the first drop in TG appeared at
Sintered ceramics prepared in this work exhibited relative
*100 °C with a 51% weight loss which is due to water
densities in the range 29–50%, increased with varying
evaporation. The second drop occurs in the range of
alumina content. It can be explained that high alumina
*100–340 °C and experienced ca 24% weight loss which
substance of the slurry resulted in high viscosity, hence a
attributed to the removal of lipids. In the temperature range
decrease in foaming capacity. In addition, high solid frac-
of 340–550 °C, the decomposition of proteins occurred
tion itself also lead to high density of cell struts.
with a weight loss of 25%. From the graph, it is also evi-
Furthermore, with the increase of yolk content, the
dent that at 550 °C, the yolk was completely burned out.
sintered alumina shrunk increasingly. The shrinkage of
samples changed from 29 to 40% when the alumina-to-
yolk ratio decreased from 1.00 to 0.65. A substantial
shrinkage occurred as the proteins were removed.

3.5 Microstucture

Figure 7 shows the FESEM pictures of macrostructures of


porous alumina prepared from different slurry composi-
tions. It shows the macropores of 50–600 lm diameters in
average (Fig. 7a, b).
Figure 7c and d show the FESEM images of the
microstructure of sample after sintering at 1,550 °C. As the
amount of yolk increased more micropores are found, thus
showing poorer densification of particles. It could be
deducted that high yolk content resulted in low viscosity,
Fig. 4 Comparison between green bodies of porous alumina with
1.00 alumina-to-yolk mass ratio and 0.01 wt% dispersant concentra- which corresponded to high foaming capacity and low
tion after drying times at a 13 and b 40 min density. Moreover, the grain size of porous alumina walls

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mainly attributed to protein removal (Fig. 8a). As a result,


pores of small sizes and ununiform shape are generated. On
the other hand, when dried at 150 and 180 °C, protein
foaming took place well and produced most pores with
spherical shape in the porous bodies (Fig. 8b, c).
Figure 8d shows side view SEM image of sintered
samples prepared using the slurry dried at 180 °C. We can
see that pores sizes is in the range of 50–200 lm and it
indicated that the alumina body has open pore with good
interconnectivity. In tissue engineering, particularly poros-
ity, pore size distribution, pore morphology and orientation,
as well as the degree of pore interconnectivity significantly
Fig. 6 The sintered porous alumina ceramics with cylindrical shape
made by protein foaming-consolidation method affect bone penetration in macropore of implants, thus
mediating implant-tissue osseointegration [23].
Dissimilarity in pore distribution was found in samples;
Table 3 Relative density and shrinkage of sintered alumina at vari- the upper part of porous bodies shows higher porosity than
ous alumina-to-yolk mass ratio without dispersant addition the lower part due to insufficient slurry stability during the
Mass ratio of Shrinkage Relative drying process. The stability of slurry was not fully
alumina-to-yolk (vol%) density (%) achieved because alumina particles tend to agglomerate
(w/w) and to precipitate over slurry foaming process. Conse-
quently, slurry in upper part which containing high yolk
0.65 39.9 29.4
was more exhaustively foamed than the lower part.
0.75 36.4 47.2
Generally the foaming process has to be carried out prior
0.83 32.5 49.5
to the stiffening of the protein. At low temperatures
1.00 29.3 45.2
the material has still a remaining extensibility which allows
the deformation of the bodies. This is comparable with the
shown irregular and in some parts small particles adsorb on moment of dough rupture in the process of baking bread,
the large grains. There is much bonding area among grains. which is caused by similar mechanism [24]. Thus, control
It is well known that more bonding area usually leads to of drying process is crucial for producing foams of high
higher strength between particles; consequently the frac- structural integrity and good mechanical properties. The
ture of alumina bodies mainly happens at the particles dispersant concentration played an important role in
boundary. determining the microstructure of the sintered porous alu-
In particular, the effect of drying time on the pore size of mina, as shown in Fig. 9.
alumina bodies has been investigated using SEM analysis. All samples were prepared using slurries with alumina-
From the macrostructure images indicated that the pore to-yolk ratio of 1.00 and then dried at 180 °C. It can be
size of alumina bodies increased with drying time. The seen that the pore size of alumina bodies increased with
slurries were dried at 180 °C with alumina to yolk mass dispersant concentration. As the dispersant content was
ratio of 1.00. It is clear that the pore size is determined by increased, the pores became bigger, more interconnected
drying time; hence higher drying time leads to higher with less dense and thinner pore walls, important factors
foaming capacity (see Fig. 3) and corresponding with that influence the mechanical properties of the porous
bigger pore size. materials. Besides, the morphology of pores was altered
Figure 8 shows top view SEM images of sintered alu- from spherical to polygonal shape. The pore size of sin-
mina porous bodies with the green bodies dried at tem- tered bodies was in the range of 200–1,000 lm. It can be
peratures of 110 (a), 150 (b) and 180 °C (c). As the drying explained that low viscosity of the slurry resulted in high
temperature increased, the pore size of porous alumina foaming capacity, hence increased the pore generation.
bodies increased as well. Sintered porous alumina prepared Samples produced by the above technique have porosity up
in this work showed an increase in pore size from 25 to to 78% when 0.01wt.% dispersant was added. The apparent
375 lm as drying temperature increased from 110 to densities of sintered alumina as a function of dispersant
180 °C. It can be explained that slurry drying at low addition with constant alumina to yolk mass ratio were
temperatures resulted in low foaming capacity, hence poor found in the range 0.7–1.8 g/cm3. These results suggest
pore generation. When dried at 110 °C, the alumina slurry that porous alumina can be a potential candidate for
was slightly foamed with volume increasing of 1.1 (v/v; see floating microcarrier application especially in a bioreactor
Fig. 3), thus the created pores of sintered bodies were cell culture.

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Fig. 7 FESEM cross-section of porous ceramics for alumina-to-yolk mass ratios of a 0.75 and b 0.65 and its grain morphology of c 0.75 and
d 0.65

Fig. 8 Top view SEM images of sintered alumina porous bodies with the green bodies dried at temperatures of 110 (a), 150 (b) and 180 °C (c).
Side view image for 180 °C drying is shown in (d)

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Fig. 9 SEM micrograph of sintered samples prepared using slurries with added dispersant concentrations of: a 0.01, b 0.03, c 0.04 and d 0.05
wt%

3.6 Mechanical strength strength of the ceramic wall (or strut) and the surface flaws
on the strut. Porosity is also considered to have a significant
In order to evaluate mechanical properties of the samples, impact on compressive strength.
compressive strength tests were conducted. The compres- The results of compressive strength measurement were
sive strength remarkably increased from 1.07 to 5.72 MPa fit to three mathematical models given in Table 4, to
with the decreasing porosity from 71 to 40 vol.%, as shown investigate the relationship between pore structure and
in Fig. 10. Many studies have been made to establish a compressive strength. In these equations, ‘‘rc’’ is defined as
relationship between strength and microstructural proper- the strength of a porous material. ‘‘rc0’’ is the theoretical
ties such as pore structure and pore size distribution. The strength of a material at zero porosity. Porosity is repre-
strength of a porous ceramic is strongly affected by the sented with ‘‘n’’ and ‘‘m’’ is a constant. Figure 10 shows
plots of porosity and compressive strength relationship for
the results of compressive strength measurements and the
three models. A smooth connection has been obtained
between relationship from experiment results and the
mathematical models. The error percentage of Balshin,
Ryshkewitch, and Hasselman models were 20, 25 and 18%,
respectively. Based on all models and the experiment facts,

Table 4 Mathematical models between porosity and compressive


strength [25]
Model Empirical equation

Balshin rc = rc0(1-n)m
Ryshkewitch rc = rc0 exp(-mn)
Hasselman rc = rc0–mn
Fig. 10 Relationship between porosity and compressive strength

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it can be deduced that the compressive strength of porous References


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good correlation has been obtained between the relation- 20. L.A. Glaser, A.T. Paulson, R.A. Speers, R.Y. Yada, D. Rousseau,
ship from experiment data and other mathematical models. Food Hydrocolloids 21, 495 (2007)
The present method is applicable to fabricate a floating 21. J.R. Clarkson, Z.F. Cui, R.C. Darton, J. Collid Interf. Sci. 215,
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microcarrier for cell culture in a bioreactor. 22. R.J. Pugh, Adv. Colloid Interface Sci. 64, 67 (1996)
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Acknowledgments The authors would like to thank Faculty of 24. I. Sopyan, M. Mel, S. Ramesh, K.A. Khalid, Sci. Technol. Adv.
Engineering and Research Management Center, International Islamic Mater. 8, 116 (2007)
University Malaysia for providing the financial support under the 25. A.U. Ozturk, B. Baradan, Comp. Mater. Sci. 43, 974 (2008)
research project No. EDW B 0901-197.

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