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CERAMICS
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Ceramics International 40 (2014) 7661–7667
www.elsevier.com/locate/ceramint

Weibull distribution of the fracture strength of 99% alumina ceramic

reshaped by cold isostatic pressing
Yan Fu, Zhendong Tao, Xianqin Houn
Key Laboratory of Inorganic Functional Materials in Shandong Province, School of Material Science and Engineering, University of Jinan, Jinan 250022, China

Received 16 September 2013; received in revised form 5 December 2013; accepted 13 December 2013
Available online 21 December 2013

Abstract

The mechanical reliabilities of 99% alumina ceramics preformed by dry pressing using various pressures and reshaped by cold isostatic
pressing (CIP) at 150 MPa are investigated using the maximum likelihood method for the estimation of the Weibull parameters of the results. The
results indicate that among the various values of dry pressing and sintering temperatures applied, a maximum Weibull modulus of 13.9974 and
high reliability were attained for 75 MPa dry pressing followed by subsequent 150 MPa cold isostatic pressing (CIP) and a 1580 1C sintering
temperature. In addition, excessive preforming pressure caused dangerous flaws, called hardening defects, which were not repaired automatically
by the CIP and sintering process, thus acting as a source of fracture and reducing the reliability of the specimen strength.
& 2014 Published by Elsevier Ltd and Techna Group S.r.l.

Keywords: Weibull distribution; Cold isostatic pressing; 99% alumina ceramic; Fracture strength; Maximum likelihood estimation

1. Introduction a certain stress value of the material can be withstood before

Griffith strength theory accounts for the fracture of brittle
materials that is usually initiated from tiny cracks and flaws that
are distributed in the material in a disorderly and unsystematic
manner [1]. Fracture strength is one of the vital mechanical
properties of structural ceramics [2]. The strength of materials
depends on the size of the major flaw varying from one to
another, which leads to a discrete distribution of the fracture
strength. In this framework, an intimate correlation between the
flaw size and the scatter of the data of the strength is realized. The
fracture of ceramics originates from the presence of defects in the
microstructure that are mostly caused by the production process
of the material. Normally, the forming method, forming pressure
and sintering temperature are the sources of defects (large grains,
pores and cracks). Therefore, it is important to develop a
production process to obtain ceramics with good mechanical
properties and stable performances.
The reliability of alumina ceramics is mainly determined by
their fracture strength and Weibull modulus, which are greatly
affected by the forming process. Reliability means ensuring that
n
Corresponding author. Tel.: þ 86 13705403795; fax: þ 86 0531 82767385.
E-mail addresses: mse_houxq@ujn.edu.cn, houxianqin@sohu.com (X. Hou).
failure occurs for a given probability of failure and confidence
level. Weibull was the first to use a statistical technique to
describe the scatter of fracture, and his fundamental assumption
was the weakest link hypothesis (the specimen fails if its
weakest volume element fails). In recent years, a significant
number of researchers have used the Weibull distribution as a
statistical tool to evaluate the performance of ceramics. Because
the location parameter for brittle materials is usually observed to
be zero [3], the two-parameter Weibull distribution is used
for the present calculations [3]. Thus, the value of the shape
parameter characterizes the spread of the fracture strength.
Seidel et al. [4] studied the effect of processing on the reliability
of alumina ceramics in 1996, demonstrating that the change
in the forming method used in his study was of no help in
increasing the Weibull modulus, and the reason for the increase
in strength was the elimination of soft agglomerates. Nevarez-
Rascon et al. [5] used the Weibull distribution to evaluate the
compressive strength, hardness and fracture toughness of
ZTA and ATZ nanocomposites reinforced by Al2O3 whiskers.
Danzer [6] studied the correlation between fracture and defect
statistics and discussed the Weibull distribution of very small
specimens. Studies demonstrated that the defect density predicted
by the Weibull distribution was higher and that some interaction

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7662 Y. Fu et al. / Ceramics International 40 (2014) 7661–7667

among the defects should occur for a very small amount of
specimens. Fan et al. [7] discussed the porosity dependence of the
Weibull modulus for hydroxyapatite and other brittle materials. In
their study, a total of 540 hydroxyapatite specimens were sintered
and fractured to extensively study the Weibull modulus. Warren
[8] discussed the effect of the test method and threshold stress on
the Weibull modulus of fracture of brittle materials. He demon-
strated that the Weibull modulus determined using different testing
techniques for fracture strength would be the same if there was no
threshold stress for fracture; in contrast, if this threshold stress did
exist, the test methods would affect the value of the Weibull
modulus even though specimens were formed using the same
method.
In this paper, the cumulative distribution function, a two-
parameter Weibull distribution, is used to assess the mechan-
ical reliabilities of 99% alumina ceramics preformed by dry
pressing with various pressures and reshaped by cold isostatic
pressing (CIP) at 150 MPa. With the analysis of the Weibull
parameters, the forming parameter of a 99% alumina ceramic
with high reliability is investigated.
2. Experimental procedures
2.1. Specimen preparation
Through spray granulation, pure (99%) alumina powder (Zhe-
jiang Ultrafine Powder & Chemicals Co., Ltd.) with an average
size of 100 μm was preformed into rectangular bars with dimen-
sions of 45  8  6 mm3 via dry pressing. The pressures used for
the dry pressing were 50 MPa (group A), 75 MPa (group B) and
100 MPa (group C). The bar-shaped compacts were then reshaped
by CIP at 150 MPa. To compare these samples with the specimens
reshaped by CIP, control experiments were established. Specimens
were formed by dry pressing only at 100 MPa (group D). The
number of specimens in each group was 100. Specimens of each
group were divided into five equal parts and sintered in an electric
furnace at 1500 1C, 1520 1C, 1540 1C, 1560 1C and 1580 1C. The
specimens were then polished and numbered for various tests to
determine their firing shrinkage, bulk density and fracture strength.
where s is the fracture strength, F is the applied force at the
fracture point, s is the span between supports, b is the width of the
specimen, and h is the thickness of the specimen.
The Weibull distribution [9–16] has been widely used to
analyze the scatter of fracture strength. Weibull parameters are
linked with the reliability of specimens. The Weibull distribu-
tion in this study is determined for four groups.
In terms of the Weibull distribution, the Weibull modulus,
m, is of great importance, where m can be defined in the two-
parameter Weibull distribution:
FðxÞ ¼ P ¼ 1  exp½  ðs=sc Þm : ð2Þ
where P is the cumulative probability of failure, m is the
Weibull modulus or the Weibull shape parameter, s is the
fracture strength, and sc is the characteristic strength or scale
parameter.
3. Results
As observed in Fig. 1, the XRD patterns of the raw material (the
lattice constants are a¼ 5.028 Å, b¼ 5.028 Å, and c¼ 13.730 Å)
and the specimens sintered at 1500 1C and 1580 1C (the lattice
constants are a¼ 4.758 Å, b¼ 4.758 Å, and c¼ 12.991 Å) display
distinct diffraction peaks. The primary phase can be identified as
α-Al2O3, which has a hexagonal structure. The peaks at 2θ¼
43.351, 35.121, 57.491, and 25.571 [17] correspond to the
characteristic diffraction peaks of α-Al2O3. No peaks of another
phase can be detected. When the sintering temperature reaches
1500 1C, the distinct diffraction peaks are the same as those of the
specimen sintered at 1580 1C. However, both sets of peaks are
shifted to the right compared with the X-ray diffraction pattern of
the raw material, which might be caused by the diminution of the
lattice constants. In addition, the orientation of grain growth might
lead to the shift of the diffraction peaks. Moreover, a small quantity
of fluxing agent in the raw material might form a solid solution,
which could also cause the diffraction peaks to shift. Furthermore,

2.2. Specimen characterization and Weibull analysis

X-ray diffraction (XRD, Bruker AXS, D-76181 Karlsruhe,

Germany) was used to analyze the crystalline phase of the raw
materials and fired specimens; a scanning electron microscopy
system (SEM, FEI, QUANTA FEG 250, America) was used to
examine the microstructural features of the fractured speci-
mens. The volume density of the specimens was measured
using the Archimedes method. The fracture strength of the
specimens was tested using the three-point bending test with a
support distance of 30 mm on a universal testing machine
(MTS, CMT5504, China).
All the specimens were bent to fracture with the loading center
perpendicular to the widest surface. The fracture strength was
calculated using the following equation: Fig. 1. X-ray diffraction patterns of material powder (a¼ 5.028 Å, b¼5.028 Å,
c¼13.730 Å) and specimens sintered at 1500 1C and 1580 1C (a¼4.758 Å,
s ¼ 3Fs=ð2bh2 Þ: ð1Þ b¼ 4.758 Å, c¼12.991 Å).
 Y. Fu et al. / Ceramics International 40 (2014) 7661–7667 7663

Fig. 2. Fracture strength for (a) group A, (b) group B, (c) group C and (d) group D.

undeveloped grain growth in the specimens sintered at 1500 1C

causes the intensities of the peaks to decrease. xi=[σ1 σ2 …σ20];
Fig. 2 shows the fracture strength for the four groups of
specimens sintered at five different temperatures. As observed
in Fig. 2, the fracture strength appears to be affected by the Plati=wblfit(xi)
preforming pressure. The data of group B show the most stable
state when the sintering temperature is 1580 1C.
In each group, a two-parameter Weibull distribution was applied Plati=A(σ0) B(m)
to analyze the fracture strength data for each validly fractured
specimen. A total of 400 specimens yielded a valid fracture. For
simplicity and accuracy, the maximum likelihood estimation was [M,V]=weibstat(A,B)
used to estimate the Weibull modulus and scale parameter [18].
MATLAB was used to write a program to estimate the Weibull
parameters. The detailed commands are shown in Fig. 3. M=expectation,V=variance
The Weibull modulus, scale parameter, expectation and
variance are determined after entering the values of the fracture Fig. 3. The detailed commands for the maximum likelihood estimation in
strength of each group. The detailed data are presented in MATLAB.
Table 1.
As observed in Table 1, the Weibull modulus appears to be when the preforming pressure is relatively lower. In addition, the
affected by the pressure of dry pressing. Ignoring some of the Weibull moduli of specimens sintered before 1580 1C differ
individual data points, the Weibull moduli of the specimens irregularly, which might be caused by the incomplete densification
reshaped by CIP in this experiment are relatively high, except of specimens, grain growth and other reasons. In terms of (1) and
for that of group C, indicating that one type of defect dominates the (2), it is important to note that the values of the Weibull moduli
fracture process in almost all of the specimens preformed by CIP are relatively higher except when the dry pressing pressure was
7664 Y. Fu et al. / Ceramics International 40 (2014) 7661–7667

Table 1
Weibull modulus, s0, expectation M, and variance V for (a) group A, (b) group
B, (c) group C and (d) group D.

T/1C s0/MPa m M V

(a)
1580 225.7056 8.8553 0.5131 0.0048
1560 227.5228 12.3756 0.6188 0.0037
1540 220.4052 12.4386 0.6219 0.0037
1520 217.7454 10.7151 0.5773 0.0042
1500 194.7364 11.6710 0.6094 0.0040

(b)
1580 224.6861 13.9974 0.6544 0.0033
1560 209.7745 11.7054 0.6064 0.0039
1540 213.0256 9.0371 0.5233 0.0048
1520 216.9435 12.6666 0.6279 0.0036
1500 185.7625 7.8912 0.4854 0.0053

(c)
1580 284.2463 4.0112 0.2217 0.0038
Fig. 4. SEM image of the raw material.
1560 309.0777 6.7623 0.3999 0.0048
1540 245.0394 6.8940 0.4208 0.0051
1520 212.7108 5.3475 0.3383 0.0053
1500 193.1959 8.8155 0.5207 0.0050 porosity of the specimens, well-grown grains and a uniform grain
(d)
size. All of these factors lead to a higher reliability of specimens
1580 287.4833 6.6126 0.3962 0.0049 preformed by dry pressing (75 MPa) and reshaped by CIP
1560 239.9311 5.6315 0.3493 0.0051 (150 MPa) with a high Weibull modulus compared with
1540 213.5262 9.6625 0.5453 0.0046 Fig. 4a (incomplete growth of the grain and grain boundary)
1520 198.0753 6.5439 0.4154 0.0055 and Fig. 5c (oversintering of the grain and the hardening defect).
1500 194.6201 7.1417 0.4476 0.0055
Comparing Fig. 5c with Fig. 5d, oversintering of the grain and
the hardening defect of Fig. 5c lead to a lower Weibull modulus
in the specimens preformed by dry pressing (100 MPa) and
75 MPa combined with CIP at a sintering temperature of 1500 1C. reshaped by CIP than in the specimens formed by dry pressing
It is obvious that the value of the Weibull modulus is relatively (100 MPa) only, even though it has a higher bulk density and
high, up to 13.9974 (the preforming pressure was 75 MPa, the CIP firing shrinkage (Fig. 6, Fig. 7).
pressure was 150 MPa, and the sintering temperature was Fig. 6 shows the firing shrinkage [19] for the 4 groups of
1580 1C), indicating that the fracture strength values are centra- specimens. The specimens preformed by dry pressing and
lized, which is apparent in Fig. 2. The Weibull modulus of (4) is reshaped by CIP exhibit a higher value of firing shrinkage than
relatively lower than that of (1) and (2). The Weibull modulus those formed by dry pressing only except when the preforming
provides paramount information about the scatter of the fracture pressure is 100 MPa. In this case, the shrinkage is lower than
strength, but it cannot dominate the reliability of ceramics alone. in the specimens formed by dry pressing only at 1500 1C.
To determine the reliability of the specimens or the synergistic In addition, the firing shrinkage for specimens formed at
action of the shape parameter and scale parameter, the expectation different pressures increases with increasing sintering tempera-
and the variance should be investigated. ture. A high sintering temperature (below the melting point)
As observed in Table 1, when the preforming pressure is contributes to molecular motion and sintering.
75 MPa, the subsequent CIP pressure is 150 MPa and the Fig. 7 shows the bulk density for the 4 groups of specimens.
sintering temperature is 1580 1C, the reliability is the highest As observed in Fig. 7, the specimens preformed by dry pressing
(the expectation is the highest, the variance is the lowest and and reshaped by CIP exhibit a higher bulk density than those
the shape parameter is the highest). formed by dry pressing only; however, when the preforming
Fig. 4 shows the microstructure of the raw material with an pressure is lower and the sintering temperature is 1580 1C, the
average size of 100 μm. Fig. 5 shows the fracture surfaces for value of the bulk density is higher. In addition, the bulk density of
specimens with the same value of fracture strength formed using the specimens sintered below 1580 1C does not correspond to the
different methods and sintered at 1580 1C. In Fig. 5d, crack-like shrinkage. This result may occur because the bulk density was
voids entrapped in grains are present, and intergranular fracture is measured using the Archimedes method. The density is thus
dominant. In addition, the size of the grains is not uniform, which measured with apparent porosity, ignoring the closed pores that
indicates that specimens formed by dry pressing only with the might be caused by hardening defects and crack-like voids.
pressure of 100 MPa have a non-homogeneous microstructure, In addition, the contact angle between the grain (undeveloped
leading to a decrease in the Weibull modulus and an enlargement growth) and the pore is too small to overcome the energy of grain
in the range of the fracture strength. In Fig. 5b, an appropriate boundary migration (removed with grain boundary movement).
preforming pressure (75 MPa) yields better densification, less The expansion of pores at the high temperature will lead to the
 Y. Fu et al. / Ceramics International 40 (2014) 7661–7667 7665

Fig. 5. SEM images under the same magnification (5 μm) of fracture surface for specimens sintered at 1580 1C. (a) formed by dry pressing only at 100 MPa,
(b) preformed by dry pressing at 50 MPa and preshaped by CIP at 150 MPa, (c) preformed by dry pressing at 75 MPa and preshaped by CIP at 150 MPa and
(d) preformed by dry pressing at 100 MPa and preshaped by CIP at 150 MPa.

Fig. 6. Firing shrinkage for 4 groups of specimens sintered at five different Fig. 7. Bulk density for 4 groups of specimens sintered at five different
temperatures. temperatures.

reduction of shrinkage. All of these factors cause the Weibull
modulus of specimens sintered below 1580 1C to differ irregu-
larly. In addition, the excessive pressure of preforming increases
the rate of densification, leading to the bulk density of the
specimens preformed by dry pressing with pressures of 50 MPa
and 75 MPa to be lower at 1500 1C. With increasing temperature,
the shrinkage increases until full sintering.
4. Discussion
The results reveal that both crack-like voids and inherent
hardening (Fig. 8) defects exist in the specimens reshaped by
CIP with an excessive preforming pressure (100 MPa), or dry
pressing, such that subsequent CIP with the reshaped pressure up
to 150 MPa could not restore the specimens. The defects cause
the Weibull modulus and reliability of group C to be lower than
7666 Y. Fu et al. / Ceramics International 40 (2014) 7661–7667
Excessive pressure
of preforming
Raw materials
(Spherical-like
particles)
Sintering process
Fig. 8. Forming process of hardening defect.
those formed by dry pressing only. To some extent, CIP cannot
restore the inherent hardening defect when the pressure of dry
pressing is oversized. CIP makes the defect die-hard such that
grain growth during the sintering process with densification of the
specimens is of no benefit. Furthermore, excessive preforming
pressure causes a point contact to irreversibly transform into line
contacts and face contacts, leading to a reduction in the mobility
of the powder. The energy of the sintering process might
decrease, and the hardening defect [20] cannot be restored
automatically. In addition, most of the soft defects produced by
the preforming process can be restored automatically during the
CIP process, and sintering contributes to increasing the Weibull
modulus when the preforming pressure is lower.
For the firing shrinkage, at the range of low temperature,
densification caused by pressure has a stronger effect on the
shrinkage of specimens than the temperature. When the
sintering temperature is 1580 1C, the effect of densification
caused by pressure on shrinkage and sintering is crucial.
In addition, the hardening defect produced by dry pressing with
excessive pressure is difficult to eradicate in the low temperature
phase. A lower preforming pressure increases the number of
pores between grains or large agglomerates that can be crushed
by CIP. CIP promotes the densification of compacts. A high
preforming pressure combined with CIP causes poor mobility of
the powder. A close connection between powders is helpful for
the densification of a green body and is beneficial to increase the
degree of firing shrinkage. A hardening defect produced by an
excessive preforming pressure is difficult to eliminate; thus,
with increasing preforming pressure, the degree of shrinkage
decreases, which is why specimens preformed by dry pressing
(100 MPa) and reshaped by CIP (150 MPa) have lower Weibull
moduli and reliabilities.
Thus, an appropriate dry pressing pressure and sintering
temperature are crucial to the shrinkage, bulk density, Weibull
modulus [21] and reliability when the specimens undergo a
subsequent CIP process [22,23].
5. Conclusions
The dry pressing pressure has considerable effects on the
microstructures and reliabilities of 99% alumina ceramics
reshaped by CIP. An appropriate dry pressing pressure
(75 MPa) and an appropriate sintering temperature (1580 1C)
promote densification and grain growth of the specimens.
Hardening defect
In addition, an appropriate preforming pressure (75 MPa) (dry
pressing) promoted an increase of the Weibull modulus of
specimens up to 13.9974 and improved the reliability of this
modulus; the expectation is 0.6544, and the variance is 0.0033.
An excessive preforming pressure (100 MPa) causes hardening
defects, and subsequent CIP cannot restore the dangerous
defect that results in a low Weibull modulus and low reliability
of the specimens.
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