J. Am. Ceram. Soc.
, 96 [10] 3223–3227 (2013)
Journal
Improved Heat Insulation and Mechanical Properties of Highly Porous YSZ
Ceramics After Silica Aerogels Impregnation
‡
State Key Lab of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University,
To further improve heat insulation and mechanical properties,
silica aerogels were impregnated into highly porous yttria-
stabilized zirconia (YSZ) ceramics with well-distributed pores
fabricated by tert-butyl alcohol -based gel-casting process and
pressureless sintering. Pore size distribution, room-temperature
thermal conductivities, and compressive strength of the YSZ
ceramics before and after impregnation with silica aerogels
were examined and compared, respectively. After impregnating
porous YSZ ceramics with silica aerogels, the porosity dis-
played a little decrease, whereas the pore size significantly
decreased by one order of magnitude. Based on this microstruc-
ture development, the room-temperature thermal conductivities
were significantly lowered and the compressive strength was
also promoted. Therefore, the heat insulation and mechanical
properties could be simultaneously improved by impregnating
porous ceramics with silica aerogels.
I. Introduction
Y TTRIA-STABILIZED zirconia (YSZ) has exhibited an
increasing interest for thermal isolation in high-
temperature processes, insulated engine components, and
refractory and thermal insulation due to its low thermal con-
ductivity and good mechanical performance. Furthermore,
introducing pores into the zirconia ceramics can obviously
decrease thermal conductivity because air trapped in the
pores is a better thermal insulator. There is currently a wide-
spread interest in fabricating porous zirconia ceramics with a
low thermal conductivity for their applications in bulk ther-
mal isolators. Schlichting et al.1 fabricated porous YSZ
ceramics using fugitive polymer method, where different
amounts of polymer spheres were included in the starting
powders before sintering, and their thermal conductivity was
measured. Deng et al.2 investigated the mechanical properties
of porous ZrO2 ceramics based on the microstructural analy-
ses. Hu et al.3 fabricated highly porous ZrO2 ceramics by a
TBA-based freeze-casting route. They created aligned chan-
nel pores and studied the microstructure and properties after
varying the experimental conditions. However, according to
the available published literatures,4–6 the strength of porous
ceramics decreases significantly with increasing porosity.
Therefore, the applications of porous zirconia ceramics for
heat insulation have been restricted because of their poor
strength. Lowering the thermal conductivity while preserving
strength is essential for developing porous zirconia ceramics
as thermal insulation materials.
P. Colombo—contributing editor
Manuscript No. 33307. Received June 3, 2013; approved July 17, 2013.
§
Present address: Materials Science and Engineering Program, Texas A&M Univer-
sity, 3003 TAMU, College Station, Texas, 77843-3003
†
Author to whom correspondence should be addressed. e-mail: wangca@tsinghua.
edu.cn.
3223
DOI: 10.1111/jace.12564
© 2013 The American Ceramic Society
Sa Li,‡ Chang-An Wang,‡,† and Liangfa Hu‡,§
Beijing 100084, China
Aerogels are also considered to be ideal candidates for
commercial thermal insulators due to their unique chemical
and textural characteristics.7,8 Many studies have long
focused on aerogels due to their extraordinary properties,
such as ultralarge specific surface area (500–1200 m2/g),
ultralow density (0.003–0.35 g/cm3), ultralow thermal con-
ductivity [0.012–0.1 W
(m
K)1], and ultrahigh porosity,
which originate from their mesoporous structure.9–12 How-
ever, a distinctive characteristic of aerogels is that they are
extremely brittle and weak because of poor mechanical prop-
erties. Improvement to the mechanical properties of aerogels
was realized by reinforcing their mesoporous structure with
polymers.13–17 Incorporating aerogels into other porous
materials, however, was rarely reported. It could be assumed
that incorporating silica aerogels, a better thermal insulator
than air, into the porous structure of porous zirconia ceram-
ics would reinforce the structure while further lowering the
thermal conductivity. In the previous research, the porous
YSZ ceramics with unidirectionally aligned pore channel
structure were fabricated by freeze casting and it was found
that impregnating aerogels into pores could further lower the
thermal conductivity while improving the mechanical proper-
ties.18,19 However, impregnation of silica aerogel into the
YSZ porous ceramics with uniformly distributed pores on
micrometer scale has never been tried by far and its feasibil-
ity as well as the corresponding influence on thermal and
mechanical performance have never been explored.
In this work, porous YSZ ceramics with uniformly distrib-
uted pores were prepared, and then silica aerogels were
impregnated into the as-prepared samples. The obtained por-
ous YSZ/silica aerogels composite materials are expected to
combine lower thermal conductivity and higher compressive
strength. As the thermal conductivity of porous YSZ ceram-
ics is strongly related to the porosity features, it is important
to be able to design the thermal properties of these materials
as well as to theoretically interpret the experimental results.
The objective of this study was to clarify the effects of micro-
structures on the thermal conductivity and mechanical prop-
erty of porous ceramics.
II. Experimental Procedure
(1) Preparing Porous YSZ Ceramics with Uniformly
Distributed Pores
Commercially available 8 mol% YSZ powder (AR grade;
Shanghai Chemical Regent Co., Shanghai, China) was used
as the starting material, which has an average particle size of
1.26 lm and a specific surface area of 6.49 m2/g. Tert-butyl
alcohol (TBA; chemical purity, Beijing Yili Chemical Co.,
Beijing, China) was used as a shaping solvent and pore-form-
ing agent in gel-casting process. A premix solution of mono-
mers and cross-linker was prepared in TBA with a concentration
of 14.5 wt% of acrylamide (AM, C2H3CONH2) and 0.5 wt%
N,N′-methylenebisacrylamide [MBAM, (C2H3CONH)2CH2].
Initiator and catalyst for the gelation reaction are ammo-
nium persulfate and N,N,N,N- tetramethylethylenediamine
3224 Journal of the American Ceramic Society—Li et al.
(TEMED), respectively. All chemicals used in this study are
of analytical grade. The TBA-based gel-casting technique
typically consists of preparing a liquid suspension (slurry),
molding, drying, binder removal, and sintering. Slurries with
15 vol% solid loading, including YSZ powders, TBA, and
AM were prepared by ball-milling for 5 h. To adjust the sus-
pension to a proper flowability during casting, the selected
alkali solution was added into the slurries. After ball-milling,
initiator and catalyst were mixed into the slurries. The slur-
ries were poured into molds and dried at 52°C in nitrogen
atmosphere. During the drying procedure, the polymerization
of AM occurred and TBA gradually volatilized. Green
bodies were then produced. Subsequently, they were sintered
at different temperatures of 1350°C, 1400°C, 1450°C,
1500°C, and 1550°C for 2 h in air.
(2) Impregnating Porous YSZ Ceramics with Silica
Aerogels
Silicon precursor, tetraethoxysilane, was dissolved in metha-
nol. Ammonia solution (NH4OH) as a catalyst was added
into the solution while vigorously stirring. The mixed solution
was poured into a container with the porous YSZ ceramics
and immersed in the pores of the porous YSZ ceramics by
application of vacuum to the container. A wet gel was formed
in the pores of the porous YSZ ceramics by hydrolysis and
condensation of the solution within 12 h. The wet gel was
(a)
(c)
(e)
Fig. 1. SEM micrographs of porous YSZ specimens at different sintering temperatures: (a) 1350°C, (b) 1400°C, (c) 1450°C, (d) 1500°C, (e)
1550°C, and (f) impregnation of sample (e).
Vol. 96, No. 10
then aged in a pure ethanol bath for 40 h, followed by a
supercritical drying process, which was performed in an auto-
clave with a diameter of 105 mm and a depth of 100 mm.
The temperature and pressure in the autoclave were raised to
be 260°C and 7.8 MPa above the critical point of ethanol
(Tc = 243°C; pc = 6.3 MPa),20 respectively. The obtained sil-
ica aerogels were distributed in the interparticle packing pores
of the porous YSZ ceramics. To understand the properties of
the silica aerogel that was impregnated into the porous YSZ
ceramics, including porosity and thermal conductivity, we
separately synthesized silica aerogel without impregnation
through the same method mentioned above. It turns out that
the silica aerogel used in this study has a porosity of 81% and
thermal conductivity of 0.079 W
(m
K)1.
(3) Characterization
Microstructure was observed using a scanning electron micro-
scope (SEM; JSM 6700F, JEOL, Tokyo, Japan). Pore size
distribution of the porous YSZ ceramics was analyzed by a
mercury intrusion porosimeter (AutoPore-IV9510, Micromer-
itics Instrument Corp., Norcross, GA). The mesopores in the
silica aerogels are hardly detectable with the mercury intru-
sion method due to crushing of the silica aerogels during
intrusion of mercury into the silica aerogels. For this reason,
the average pore size distribution of silica aerogels was deter-
mined by N2 adsorption at 77 K instead of mercury intrusion.
(b)
(d)
(f)
October 2013 Porous YSZ Ceramics 3225

The porosity was obtained from the ratio of the bulk density, (a)
measured from the sample mass and dimension, to the theo-
retical one of this YSZ material (6.0 g/cm3). Three samples
were examined to determine the average porosity. Thermal
conductivity at room temperature was measured on
5 mm 9 5 mm 9 3 mm machined specimens, using a Ther-
mal Transport Option of Physical Properties Measurement
System (Model 6000; Quantum Design, San Diego, CA). For
the compressive strength measurements, samples with a diam-
eter of 6 mm and a height of 12 mm were loaded with a
crosshead speed of 0.05 mm/min (Instron 3369; Instron
Corp., Norwood, MA). Five specimens were used to obtain
average values and standard deviations.

III. Results and Discussion

(1) Microstructure
The microstructure change in the porous YSZ ceramics
with impregnation of silica aerogels was investigated using (b)
SEM. As can be observed from Figs. 1(a)–(e), the intercon-
nected pores were homogeneously dispersed in the zirconia
matrix and adjacent grains interconnected to form a strong
skeleton. In addition, the grains enlarged and the porosity
decreased as the sintering temperature increased from
1350°C to 1550°C. Compared with Fig. 1(e), impregnation
with silica aerogels in the well-distributed pores of the por-
ous YSZ ceramics was obviously observed in Fig. 1(f). Sil-
ica aerogel occupied most of the intraparticle pore volume,
resulting in a significant decrease in pore size. Since the
similarity of the SEM images after the impregnation, the
microstructure of samples sintered at 1550°C is shown here
for brevity. Figure 2(a) shows the pore size variations in
porous YSZ ceramics with different sintering temperatures
before and after impregnation with silica aerogels. As the
sintering temperature increased from 1350°C to 1550°C, the
pore size decreased from 1.92 to 0.69 lm due to the pro-
cess of sintering densification. On the other hand, the pore
size of samples with different sintering temperatures drops (c)
to a similar dimension, about 0.18 lm, after impregnation,
forming a YSZ–aerogel–air three-phase system. Figure 2(b)
shows a typical pore size distribution determined by mer-
cury intrusion method for porous YSZ ceramics sintered at
1350°C before and after impregnation. Both cases presented
monomodal pore size distributions, which reached a peak
of 1.92 and 0.18 lm before and after impregnation, respec-
tively. Each peak revealed a narrow half-peak width, signi-
fying a narrow pore size distribution. It should be noted
that the pore size of the mesoporous silica aerogels was
not observed in this figure because the mesopores of the
silica aerogels are hardly detected with mercury intrusion
method. The pore size distribution of silica aerogels was
determined by N2 adsorption and then calculated using the
KJS method,21 as revealed in Fig. 2(c), in which a single
peak near 50 nm was observed. It could be concluded that
two types of pores were detected by pore size distribution
determinations of the porous YSZ ceramics impregnated Fig. 2. (a) Porosity variation after impregnation of silica aerogel,
with silica aerogels. The results were consistent with the (b) typical pore size distribution of porous YSZ ceramics with
observations in Fig. 1(f). uniformly distributed pores before and after impregnation with silica
aerogels determined by mercury intrusion porosimeter method, (c)
determined by N2 adsorption at 77 K.

(2) Room-Temperature Thermal Conductivity

Figure 3 shows the room-temperature thermal conductivity
of porous YSZ ceramics with well-distributed pores before
and after impregnation with silica aerogels. All the samples
had very low thermal conductivities [0.090–0.141 W
(m
K)1
before impregnation and 0.057–0.084 W
(m
K)1 after
impregnation], which were much lower than those reported
porous zirconia ceramics.22 At a given porosity, the thermal
conductivity of porous YSZ ceramics after impregnation with
silica aerogels was much lower than that before impregna-
tion. Particularly, after impregnating porous YSZ ceramics
with silica aerogels, the thermal conductivities decreased
from 0.090–0.141 W
(m
K)1 to 0.057–0.084 W
(m
K)1.
Many thermal conductivity models to describe porous
ceramics have been proposed. The in-series and in-parallel
models proposed by Voigt-Reuss are the simplest models,
which give the two extreme limits for the thermal conductivity
of a two-phase composite.23 Hashin and Shtrikman24 derived
effective conductivity bounds that were the narrowest possible
bounds for macroscopically homogeneous, isotropic, two-
phase materials that could be derived from the components’
3226 Journal of the American Ceramic Society—Li et al. Vol. 96, No. 10

volume fractions and conductivities. As for a heterogeneous compressive strength of the porous YSZ ceramics with
material in which the two components are distributed porosity. The compressive strength of the porous YSZ
randomly, with neither phase being necessarily continuous or ceramics with a porosity of 62.9% was 30 MPa before
dispersed, the Effective Medium Theory (EMT) equation impregnation, whereas the value increases to 66 MPa after
could well predict the effective conductivity.25 In this work, the impregnation. As the porosity increased, the compressive
YSZ porous ceramic before impregnation is a two-component strength decreased remarkably. In the porous YSZ ceramics,
system, and the thermal conductivity can be calculated using which contained 77% pores, the compressive strength was
the EMT equation. However, most of the open pores would be about 3 MPa. With the decrease in the porosity, the pore
filled with silica aerogel after the impregnation, and therefore
the composite material is a three-phase system. We perform a
two-step calculation based on EMT to calculate the thermal (a)
conductivity for such a model. Firstly, the thermal conductiv-
ity of the mixture constituted by the solid part and the
mesoporous network is calculated.
kYSZ  k1 kaerogel  k1
fYSZ þ faerogel ¼0 (1)
kYSZ þ 2k1 kaerogel þ 2k1
where kYSZ, kaerogel, and k1 are thermal conductivity of YSZ
solid phase, aerogel, and effective conductivity of the two-
phase composite, respectively. fYSZ and faerogel, respectively,
represent the volume fractions of YSZ phase and aerogel.
Secondly, the effective thermal conductivity of the sample
is determined by using the previous calculated value and the
volume of the mesopores.

k1  k2 kair  k2
ð1  fair Þ þ fair ¼0 (2)
k1 þ 2k2 kair þ 2k2
where fair stands for the porosity after aerogel impregnation; (b)
kair and k2 are the thermal conductivity of air and effective
conductivity of the three-phase composite, respectively. In
addition, as the aerogel occupies part of the pore, the follow-
ing relationship among faerogel, fair, and fYSZ exists:

fair þ faerogel þ fYSZ ¼ 1 (3)

The thermal conductivities of aerogel, YSZ, and air are

0.079, 1.80, and 0.026 W
(m
K)1, respectively. We substi-
tuted those data to the above equations to obtain the pre-
dicted value by a two-step EMT. Fig. 3 reveals the thermal
conductivities of porous YSZ ceramics before impregnation,
after impregnation, and calculated by EMT as a function of
pore volume fraction. As can be seen, the measured values of
samples after aerogel impregnation generally match the calcu-
lated effective thermal conductivity based on a two-step EMT.

(3) Compressive Strength

The compressive strength of porous YSZ ceramics also
depends on the porosity. Figure 4(a) shows the variation in (c)

Fig. 4. (a) Compressive strength of porous YSZ ceramics with

Fig. 3. Room-temperature thermal conductivity of porous YSZ uniformly distributed pores before and after impregnation with silica
ceramics with uniformly distributed pores before and after aerogels. Variation in the value of parameter b derived from Rice
impregnation with silica aerogels and calculated by EMT model. equation with increasing sintering temperature (b) and porosity (c).
October 2013 Porous YSZ Ceramics
became smaller, and the grains interconnected tightly to form
a strong skeleton, resulting in relatively high strength.
Generally, a number of expressions can be used to
describe the compressive strength–porosity behavior of por-
ous ceramics. One of the simplest methods was firstly pro-
posed by Ryshkewitch and Duckworth,4,5 and developed to
the Rice equation6:
r ¼ r0 expðbPÞ (4)
where r0 is the strength of a dense material, r is the strength
of the porous material with a porosity of P, and b is a
parameter depending on the structure and material composi-
tion. The value of the parameter b represents the susceptivity
of strength on porosity, i.e., the larger b value, the more sus-
ceptivity of strength on porosity.
Figure 4(b) shows the variation in the value of parameter b
derived from the Rice equation [i.e., Eq. (4)]. r and P are the
measured compressive strength and measured porosity of por-
ous YSZ ceramics. r0 is the compressive strength of dense
YSZ ceramics, which was taken as 2068 MPa for this YSZ
material.26 A general increasing trend of the value of parame-
ter b with decreasing sintering temperature was observed when
the temperature is higher than 1400°C, indicating that the
higher the sintering temperature, the weaker is the dependence
of strength on porosity; however, a sharp increase in the b
value occurs at 1350°C. Although similar results are found in
samples with silica aerogel impregnation, the b value is lower
than the respective one before impregnation, which also
reveals that interconnection of grains and total volume of
pores were two factors that influence the resultant strength of
sintered ceramics. Considering the fact that a change in speci-
men pore volume is attributed to an associated change in the
size of the effective or critical load-bearing area within the
specimen, the promoted compressive strength of porous YSZ
ceramics partly comes from the lower porosity brought by
impregnation with silica aerogels. The value of parameter b
(6.7–8.5) calculated from Eq. (4) indicated a moderate poros-
ity-dependent compressive strength of porous YSZ ceramics,
by comparing with the corresponding values of some other
porous ceramics (i.e., hydroxyapatite, b = 9.2–10.827; alumina,
b = 75; mullite, b = 5.6–6.228).
IV. Conclusions
Highly porous YSZ ceramics with well-distributed pores were
fabricated by TBA-based gel-casting process and pressureless
sintering. Silica aerogels were successfully impregnated into
the as-fabricated samples. It is found that the porosities were
decreased, whereas the room-temperature thermal conductiv-
ity was significantly lowered and the compressive strength was
promoted after impregnating with silica aerogels. Based on
the respective microstructure observation, a two-step EMT
equation was adopted to calculate the thermal conductivity of
the YSZ–air–aerogel system, and the simulation results are
more close to the measured ones. In addition, the introduction
of nanoscale porous aerogel also can enhance the compressive
strength while reducing the porosity sensitivity of the highly
porous YSZ ceramics.
Acknowledgment
The authors would like to thank the financial support from the National
Natural Science Foundation of China (NSFC–No. 90816019 and 51172119)
3227
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