Materials Science and Engineering C 29 (2009) 1144–1149

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Materials Science and Engineering C

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / m s e c

Microwave sintering of calcium phosphate ceramics

Abhijit Chanda a, Sudip Dasgupta b, Susmita Bose b,⁎, Amit Bandyopadhyay b,⁎
a
Department of Mechanical Engineering, Jadavpur University, Kolkata-700032, India
b
W. M. Keck Biomedical Materials Research Laboratory, School of Mechanical and Materials Engineering, Washington State University, Pullman, WA 99164, USA

a r t i c l e i n f o a b s t r a c t

Article history: Microwave sintering of hydroxyapatite (HAP) and tri-calcium phosphate (TCP) ceramics were studied using
Received 4 June 2008 a commercial 2.45 GHz, 3 KW fully automated microwave system. Four different powder compositions, apart
Accepted 1 September 2008 from pure HAP and TCP, were prepared with small amount of different oxide additives e.g., magnesium oxide,
Available online 13 September 2008
zinc oxide and titanium oxide. All samples were densified at 1250 °C for 30 min. Sintered samples had high
density and homogeneous microstructure for all compositions. Phase analysis using XRD showed no major
Keywords:
Hydroxyapatite
variations from starting materials. Presence of additives increased compressive strength between 100 and
Tri-calcium phosphate 200%. Fractured surfaces showed clear signs of intergranular fracture in undoped HAP and TCP while in
Microwave sintering doped samples, fracture modes were either transgranular or mixed mode. In comparison to conventional
Mechanical properties sintering, microwave sintering of calcium phosphate ceramics was found to be economically exciting due to
substantial reduction in processing time and energy expenditure due to volumetric heating of samples.
© 2008 Elsevier B.V. All rights reserved.

1. Introduction
During the last four decades, phosphate ceramics like calcium
hydroxyapatite (HAP) and tri-calcium phosphate (TCP) gained
significant popularity as biomaterials. HAP is a bioactive ceramics
while TCP is a bioresorbable one. Both compositions have been
increasingly used to repair or replace diseased or damaged parts of
human musculoskeletal system [1–4]. Both HAp and TCP show
excellent biocompatibility in vivo. HAp is also compositionally similar
to the inorganic mineral phase of bone. One of the two major
challenges in the area of these phosphate bioceramics is to make them
more osteo-mimic i.e., to ensure more resemblance with human bone,
and the other being enhancement of mechanical properties to
function properly within human body under varying stress pattern [4].
Clinically calcium phosphate biomaterials are used in number of
physical forms e.g., granular, porous or as a deposited coating.
Granular, dense or porous forms of such phosphate ceramics are
generally prepared through conventional powder compaction routes
followed by sintering in electrically heated furnace, which is a time-
consuming as well as energy-intensive procedure. As an alternative,
researchers have been exploring the possibility of using microwave
heating for sintering of phosphate ceramics to reduce processing time
and cost. Microwave heating is fundamentally different from conven-
tional radiant heating furnaces due to volumetric heating. Conven-
tional furnaces heat samples using surface heating mechanism, and
depending on the rate of heating, a large thermal gradient from the
⁎ Corresponding author. S. Bose is to be contacted at Tel.: +1 509 335 7461. A.
Bandyopadhyay, Tel.: +1 509 335 4862; fax: +1 509 335 4662.
E-mail addresses: amitband@wsu.edu (A. Bandyopadhyay), sbose@wsu.edu (S. Bose).
surface to the center can generate within a sample, particularly for
poor thermal conducting materials. However, volumetric heating
through microwave ensures uniform heating and almost no thermal
gradient, which allows higher heating rates, and reduce the proces-
sing time. For oxide ceramics, microwave heating is being used for the
last two decades [5–7] but microwave sintering of phosphate ceramics
is relatively newer proposition [8–10]. Microwave sintering of calcium
hydroxyapatite was first reported by Fang et al. [8]. A 500 W, 2.45 GHz
microwave oven was used and showed that microwave could ensure
high density, better microstructure, higher strength for HAP within a
relatively shorter time than conventional furnace. Most of the
microwave sintering studies mainly concentrated on pure HAP or
TCP, although it has been reported in recent past that judicious
introduction of certain metallic ions into these biomaterials not only
make them more osteo-mimic and biocompatible but also improve
their mechanical strength [11–15]. The present work aims at
microwave sintering of calcium phosphate ceramics, both HAP and
TCP, pure as well as doped, and their effect on microstructure and
mechanical properties. Results are compared with conventionally
sintered samples to appreciate the economic advantage for microwave
sintering of HAP and TCP ceramics.
2. Experimental procedure
2.1. Sample preparation
Starting powders were calcium hydroxyapatite (HAP) and tri-
calcium phosphate (TCP) with particle size of 600 nm procured from
Berkeley Advanced Biomaterials Inc. (Berkeley, CA). Three different
oxide additives e.g., magnesium oxide (MgO) (96% + purity), zinc oxide

0928-4931/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msec.2008.09.008
 A. Chanda et al. / Materials Science and Engineering C 29 (2009) 1144–1149 1145

(ZnO) (99% + purity) and titanium oxide (TiO2) (96%+ purity) were
used to prepare two doped compositions of HAP and TCP each and
shown in Table 1. All these oxide powders were procured from Fisher
Scientific (Fair Lawn, NJ). Powders were weighed and mixed in 250 mL
polypropylene Nalgene bottles with 5 mm diameter zirconia milling
media. After dopant addition, dry ball milling was done for 7 h for each
composition. After ball milling, measured amount of powders were
uniaxially pressed. Two types of compacts e.g., disc and cylinders were
prepared through uniaxial pressing. Disc compacts were of 13 mm in
diameter and 3 mm thick, whereas cylinders were of 6 mm in
diameter and 11 mm long. All samples were compacted with the same
uniaxial pressure of 150 MPa using different stainless steel molds. Disc
compacts were used for microstructural analysis and microhardness
measurement, and cylindrical specimens were used for measuring
compressive strength. After uniaxial pressing, all compacts were
subjected to a cold isostatic pressing (CIP) at 350 MPa for 15 min.
CIP'ed samples were sintered in a 2.45 GHz, 3 KW fully automated
commercial microwave sintering furnace (MW-L0316V, Changsha
Longtech Co Ltd., China). Samples were placed on a silicon carbide
plate. They were surrounded by a hollow silicon carbide cylinder,
Fig. 1. Typical heating and cooling cycles with microwave furnace (MW) and conventional
which was used as the susceptor to enhance microwave heating electrical heating furnace (Conv.).
through efficient coupling. The entire assembly was covered with
ceramic fiber insulation. Sample temperature was measured con-
tinuously with the help of an optical pyrometer from the top with an specimens in a mortar. Phase analysis was done using a Philips PW
accuracy of ± 1 °C. The operating power of the microwave system was 3040/00 X'pert MPD system (Philips, Eindoven, The Netherlands) at
optimized through a number of trial runs and finally it was set to a room temperature using CoK∞ radiation with a Ni-filter. All test runs
three-stage operation to avoid overheating and cracking of samples. were carried out over a 2θ range of 20° to 60° at a step size of 0.02° (2θ)
Initially the power was set at 2000 W and then after reaching 800 °C, it and a count time of 0.5 s per step. Phases were compared between the
was increased to 2700 W, and finally when the desired temperature microwave-sintered and the conventionally sintered samples.
was attained, the power was adjusted to maintain a constant
temperature over the entire soaking time. After a number of trial 2.4. Microstructural analysis
runs, sintering temperature for both HAP and TCP (doped and
undoped) samples in the microwave system was fixed at 1250 °C Scanning electron microscope (SEM) was used to analyze micro-
with a soaking time of 30 min. A typical heating schedule of the structure of pure and doped microwave-sintered HAP and TCP
microwave (MW) furnace is shown in contrast with a conventional specimens in as prepared condition. Average grain sizes of the
heating cycle in Fig. 1. sintered discs were measured from SEM micrograph using linear
interception method. Furthermore, the fracture-surfaces of the
2.2. Densification study compressive strength specimens were studied to identify the mode
of fracture.
Bulk density of samples was measured following both uniaxial and
cold isostatic pressing. For sintered specimens, bulk and apparent 2.5. Mechanical property measurements
densities were measured using dimensional measurement and Archi-
medean principle. Three samples were measured from each composi- Compressive strength of all microwave-sintered HAP and TCP
tion for density measurements and an average data was reported. For samples were measured with a screw driven Instron universal testing
disc and cylinders, both radial and longitudinal shrinkages were machine (Instron, UK) with a constant crosshead speed of 0.002 mm/
calculated from green and sintered dimensions. To compare densifica- s. Test-specimens were made with a length to diameter ratio of 1.5 to
tion of microwave-sintered samples with conventional sintering, a batch 1.8. For each composition, minimum three samples were used.
of samples were prepared following the same processing steps and then Microhardness of the sintered and polished discs were measured
sintered in a muffle furnace at 1250 °C for 2 h. with a Vickers microhardness tester (Leco Corporation, Michigan,
USA) with a load range of 100 g to 500 g. For each specimen, at least
2.3. Phase analysis five indentations were made with each load and for each composition.
Moreover, tests were repeated on three different samples of the same
X-ray diffraction was used to evaluate phases in the sintered composition.
samples. Powdered samples were prepared by crushing the sintered
3. Results

Table 1
The compositional characteristics, microstructural features, physi-
Different compositions of calcium phosphate ceramics used for this study. cal and mechanical properties of different compositions listed in
Table 1 were presented and discussed with reference to conventional
Compositions Percentage of additives Percentage of metallic ions
sintering as well as MW-sintering data. From the list of dopants shown
introduced introduced
in Table 1, the percentage addition of metallic ions were calculated and
Pure HAP (HAP-I) Nil Nil
HAP with MgO (HAP-II) 1 wt.% MgO 0.6 wt.% Mg found to be 0.6 wt.% Mg in case of HAP-II, 0.6 wt.% Ti in TCP-II, 0.6 wt.%
HAP with MgO+ZnO (HAP-III) 1 wt.% MgO+0.25 wt.% ZnO 0.6 wt.% Mg, 0.2 wt.% Zn Mg and 0.25 wt.% Zn in HAP-III and TCP-III.
Pure TCP (TCP-I) Nil Nil The radial and longitudinal shrinkages of the microwave-sintered
TCP with TiO2 (TCP-II) 1 wt.% TiO2 0.6 wt.% Ti samples were presented in Table 2. With HAP, doped and undoped,
TCP with MgO+ZnO (TCP-III) 1 wt.% MgO+0.25 wt.% ZnO 0.6 wt.% Mg, 0.2 wt.% Zn
shrinkages were higher with both types of specimen. Fig. 2 clearly
1146 A. Chanda et al. / Materials Science and Engineering C 29 (2009) 1144–1149

Table 2 Table 3
Radial and longitudinal shrinkages of disc and cylindrical samples of different compositions. Bulk densities of microwave-sintered and conventionally sintered disc and cylindrical
specimens.
Composition Disc specimen Cylindrical specimen
Radial Longitudinal Radial Longitudinal Compositions Microwave-sintered Conventionally sintered
shrinkage shrinkage shrinkage shrinkage Disc Cylinder Disc Cylinder
HAP-I 15.61 9.41 15.11 8.22 HAP-I 94.1 ± 2.0 94.3 ± 1.67 94.1 ± 2.6 93.9 ± 1.88
HAP-II 13.5 12.95 16.24 8.91 HAP-II 87.6 ± 2.6 95.5 ± 2.34 89.3 ± 3.4 92.3 ± 2.15
HAP-III 11.82 11.11 14.89 8.43 HAP-III 88.1 ± 1.1 95.1 ± 3.5 90.2 ± 3.4 91.5 ± 2.23
TCP-I 12.07 10.8 11.2 7.23 TCP-I 81.6 ± 1.76. 82.0 ± 1.45 82.2 ± 2.44 82.9 ± 1.78
TCP-II 7.7 9.73 12.7 7.82 TCP-II 87.0 ± 2.1 87.6 ± 2.11 87.2 ± 3.12 87.5 ± 2.45
TCP-III 11.81 12.00 13.1 8.31 TCP-III 89.1 ± 0.78 89.9 ± 1.5 87.6 ± 2.11 88.9 ± 3.0

denoted the radial shrinkage of a typical, sintered HAP sample. For
compressive strength specimens i.e., cylindrical specimens, having
higher length to diameter ratio, the difference between radial and
longitudinal shrinkage was more pronounced. In almost all the
compositions, irrespective of length to diameter ratio, radial shrin-
kages were found to be more than the corresponding longitudinal
shrinkage values.
Green densities of all compositions, after uniaxial pressing, were
between 43 and 45% of theoretical density (TD), and following cold
isostatic pressing between 57 and 60% of TD. However, sintered
densities of these samples varied significantly between HAP and TCP.
Table 3 presented the sintered densities data of samples as a
percentage of theoretical density. Theoretical density of HAP was
considered as 3.16 g/cc and that for TCP was 3.07 g/cc. Sintered
densities of some of the compositions showed marked variations with
geometry. In case of HAP-I, sintered density was consistently ~94%
while for other two cases e.g., HAP-II and HAP-III, densities of
cylindrical specimens were considerably higher than corresponding
values for disc specimens. It may be noted that those specimens with
compositions HAP-II and HAP-III showed higher shrinkages too, both
radially and longitudinally. With 1 wt.% MgO doping in HAP,
maximum sintered density of 95.5% was observed with cylindrical
samples. With binary dopant in HAP III, density was as high as 95.1%.
In case of different TCP compositions, there was not much of variation
in density with geometry. In TCP-I, density was consistently on the
lower side, ~ 82%TD. With the introduction of dopants i.e., TCP-II and
TCP-III, density increased by 5% and 7%, respectively, but it did not
show any variation with specimen-geometry. Table 3 showed
comparative data on densification for microwave and conventionally
sintered samples. It revealed that densities of all samples were highly
comparable between the two sintering cycles. In case of HAP-II and
HAP-III there was some reduction in density with disc specimens in
microwave in comparison to conventionally sintered samples; how-
ever with cylindrical specimens i.e., high length to diameter ratio,
densities of these compositions were quite similar.
Fig. 3a and b show the comparative XRD plots for microwave-
sintered and conventionally sintered HAP and TCP compacts, and it is
evident that no significant change in phase formation had occurred
due to microwave sintering. Fig. 4a to f show the microstructures of
different compositions observed under SEM. From these figures, it was
clear that in most cases, the grains were nearly equiaxed in shape
except in HAP-II, where some elongated grains were observed, in
Fig. 4b. The average grain sizes in case of HAP-I, HAP-II and HAP-III are
4.5 ± 1.8 μm, 5.8 ± 1.8 μm and 3.3 ± 1.5 μm, respectively. In HAP-II, the
elongated grains were of varying length ranging from 15 μm to 35 μm,
and between 2 and 5 μm wide. These grains were found to form a
typical close-net dendritic structure. In TCP-I, average grain size was
3.8 ±1.6 μm as shown in Fig. 4d. In this case, a lot of porosity with
interconnectivity were observed. In TiO2 doped TCP [TCP-II], grain size
showed a wider scatter with several bigger grains along with some
smaller ones, shown in Fig. 4e. The average grain size was measured to
be 4.8 ± 3.1 μm. In the case of TCP with binary dopants (TCP-III), the
grain size was low 3.2 ± 1.8 μm and uniform. Like HAP-III, in TCP-III
too, small particulate phase was widely found across the surface of the
grain boundaries as well as within the grains.
Compressive strength and microhardness data are presented in
Table 4. HAP-I showed the highest hardness. With the addition of
dopants, hardness decreased. In HAP-II and HAP-III, average micro-
hardness values were significantly lower than that of pure HAP. In TCP
compositions, the average values of microhardness with doped
compositions showed a decreasing trend though the range of variation
was not so high.
From Table 4, it can be observed that with both HAP and TCP,
introduction of dopants increased compressive strength. In case of
HAP, this increase was as high as nearly 100% with 1 wt.% MgO (HAP-II)
and nearly 200% with binary dopant i.e., 1 wt.% MgO and 0.25 wt.% ZnO
(HAP-III). In TCP, there was also considerable increase in compressive
strength e.g., 130% in TCP-II, and nearly 100% in TCP-III. Similar type of
strength enhancement of TCP with conventional sintering with
identical dopant additions was reported earlier [11,12,16]. Fracture
surface of broken samples of HAP-III composition revealed transgra-
nular crack propagation in Fig. 5a due to the presence of strong
particulate second phase along the grain boundaries. In contrast, in the
case of HAP-I and TCP-I, the fracture modes were found to be
intergranular in nature and shown in Fig. 5b and c. In other
compositions no specific features were observed as such except a
mixed mode i.e., partially transgranular and partially intergranular in
nature. Another important observation made during compressive
strength-testing was that all samples failed along planes parallel to the
direction of loading. This was due to the tensile residual stress
component of the applied compressive stress perpendicular to the
loading axis [17,18].

4. Discussion

From our results, it was evident that calcium phosphate ceramics

Fig. 2. Green and microwave-sintered HAP-I specimens.
with different compositions possess good sinterability under micro-
wave heating. It resulted in uniform microstructure and comparable
densification to conventional sintering process. Mechanical proper-
ties, strongly influenced by densification, were found to be compar-
able if not better than those of conventionally sintered samples with
 A. Chanda et al. / Materials Science and Engineering C 29 (2009) 1144–1149 1147

Fig. 3. X-ray diffraction plots of MW-sintered calcium phosphate ceramics. (a) HAP—pure and doped (JCPDS file # 09-0432), (b) TCP—pure and doped (JCPDS file # 09-0169).

similar compositions. Generally densification in solid-state sintering
of ceramics involves several steps, however the first is neck formation
between the particles. In the present study, uniaxial pressing followed
by CIP'ing ensured intimate particle to particle contact in green
compacts. Near 60% green density prior to sintering was achieved for
all the specimens irrespective of compositions, which certainly
enhanced bonding between the particles. Solid state sintering, is a
diffusion-controlled process with different modes e.g., volume
diffusion, grain boundary diffusion, and surface diffusion, and in
iono-covalent ceramics, the diffusing species are anions and cations.
Microwaves, which are high frequency electromagnetic waves, are
reported to interact with such ionic species and induce motion in
them [19–21]. This induced motion tends to cause a departure from
natural equilibrium of the system and is resisted due to frictional,
1148 A. Chanda et al. / Materials Science and Engineering C 29 (2009) 1144–1149

Fig. 4. Microstructures of MW-sintered calcium phosphate ceramics. (a) HAP-I, (b) HAP-II, (c) HAP-III, (d) TCP-I, (e) TCP-II, (f) TCP-III.

elastic and inertial forces. Owing to this resistance, the electric field cylindrical, suffered cracking during heating and cooling cycle due
associated with the microwave radiation is attenuated and cause to typical non-uniform shrinkage in ceramics.
volumetric heating of material. Calcium phosphate ceramics such as Besides these, another important feature of microwave sintering
HAP and TCP used in the present study, being iono-covalent in nature, can be noted. Microwave heating cycle was found to be quite economic
are also expected to be microwave-sensitive. Furthermore the
presence of hydroxyl group in HAP-structure may have contributed Table 4
favorably to microwave heating and densification. The presence of Compressive strength and microhardness of different compositions.
various ions with the introduction of additives also enhances ionic
Composition Strength (MPa) Microhardness (HV)
transport and densification, though their concentration is quite low. In
HAP-I 101 ± 19.2 780 ± 160
addition to high densification, uniform microstructure and good HAP-II 199 ± 31.5 375 ± 70
mechanical properties, another aspect can be observed during the HAP-III 280 ± 60.2 465 ± 110
present study i.e., uniformity in shrinkage. Through proper optimiza- TCP-I 98 ± 16.5 409 ± 80
tion in heating rate by controlling the microwave power, it was TCP-II 227 ± 38.6 384 ± 90
TCP-III 193 ± 27.5 396 ± 75
ensured that none of our samples of either geometry, disc or
 A. Chanda et al. / Materials Science and Engineering C 29 (2009) 1144–1149 1149

tional sintering [22]. Due to the addition of dopants, an increase in

strength with HAP and TCP was expected. These dopants were used
before in calcium phosphate based ceramics using conventional
sintering and their influence on mechanical properties have also
been documented [11–13,18]. Our goal was to show that microwave as
a tool can be used to any broad composition range for calcium
phosphate ceramics towards densification. Compression strength of
doped and undoped HAP and TCP ceramics clearly supports that idea.
Moreover, compressive strength data showed good repeatability with
low scatter except in the case of HAP-III.
The general nature of variation of microhardness with composition
for HAP ceramics indicated somewhat an opposite trend to that
observed in the case of compressive strength. This difference can be
due to the difference in density of the two types of specimens—discs and
cylinders. In the case of compressive strength measurement, cylindrical
specimens were used and had higher density than disc specimens that
was used for microhardness measurements. However in the case of TCP,
microhardness numbers were comparable in all the cases.

5. Conclusions

The objective of the present work was to study microwave

sinterability of pure and doped calcium phosphate ceramics, namely
HAP and TCP. Our study clearly showed that both HAP and TCP, pure as
well as doped with oxide additives, could be sintered well with
microwaves. Microwave-sintered samples showed good densification,
uniform shrinkage without cracking with uniform microstructure.
Addition of additives in both HAP and TCP caused significant increase
(100–200%) in strength. Fracture modes were identified as inter-
granular in pure HAP and TCP while in other cases, they were
transgranular or mixed mode of fracture. Moreover, there was no
major change in phase due to microwave heating. Overall, microwave
heating could render good reproducible sinterability to these
phosphate ceramics. Microwave sintering achieved comparable
properties within 60 min instead of 8 h in conventional heating due
to significantly higher heating rates that can be used without cracking
because of uniform volumetric heating of samples.

Acknowledgements

The authors acknowledge experimental help from S. Dasgupta,

Z. Seeley, V. Krishna Balla, Dr. W. Xue and Dr. Valerie Lynch-Holm of WSU.
One of the authors (A. Chanda) is grateful to the TEQIP, JU for financial
help. Financial support from the W. M. Keck Foundation and the Office of
Naval Research (N00014-1-05-0583) are also acknowledged.

Fig. 5. Fractured surfaces of compressive strength samples. (a) HAP-I, (b) TCP-I, (c) HAP-II. References

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