Int.

Journal of Refractory Metals and Hard Materials 54 (2016) 383394

Contents lists available at ScienceDirect

Int. Journal of Refractory Metals and Hard Materials

journal homepage: www.elsevier.com/locate/IJRMHM

Shrinkage characteristics studies on conventional sintered zirconia

toughened alumina using computed tomography imaging technique
S. Renold Elsen , T. Ramesh
Dept. of Mechanical Engineering, NIT Trichy, India

a r t i c l e

i n f o

Article history:
Received 1 July 2015
Received in revised form 10 September 2015
Accepted 26 September 2015
Available online xxxx
Keywords:
Zirconia toughened alumina (ZTA)
CT imaging
MIMICS
Response surface methodology
BoxBehnken design

a b s t r a c t
Shrinkage is an important issue during sintering of ceramics as it affects the structural and mechanical properties.
In the current work, the shrinkage characteristics of sintered zirconia toughened alumina (ZTA) compact
produced by conventional powder forming process was investigated by using computed tomography imaging
technique. The effect of process parameters such as weight percentage of zirconia added to toughened alumina,
compaction pressure, and sintering temperature on ZTA was studied. The BoxBehnken technique in response
surface methodology was used to develop the experimental design to analyze the shrinkage phenomena. The
sintered samples were subjected to computed tomography scan and analyzed by using MIMICS Software wherein the three dimensional shrinkage of the ZTA composites was done. The mathematical regression model relating
powder forming process parameters to the shrinkage was developed. It was observed that due to the effect of
gravity, shrinkage is found to be 20% in the top for 1600 C sintered sample. From the study shrinkage of the
sintered ZTA was inuenced by the sintering temperature. Being a non-contact type digital measurement
method the odds of error created by instrument or human was avoided. Shrinkage of three directional complex
shapes can also be identied effectively with the help of solid modeling packages.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
Zirconia toughened alumina composites are used for a variety of
application such as implants [1], machining inserts [2,3], creep resistant
materials [4], armor material in defense application. Ceramic composite
fabricated by conventional sintering technique is an economical and
simple method to form dense material. The powders are packed by
compaction are bonded together during sintering. Fairly, a large amount
of shrinkage is observed due to the removal of pores among powder
particles in ceramic compacts. The reduction of the inter particle
surfaces due to surface tension is the driving force of shrinkage [5]. It
is caused due to the decrease in pore volume, porosity, and with
increase in temperature [6]. It is essential to assess the shrinkage mechanism to predict the performance of sintering techniques. Prediction of
the shrinkage characteristics of ceramic composites is important for
the production of defect free near net shape nal sintered product.
The thermo-mechanical behavior of ceramics was found to be altered
with the change in porosity as the interfaces between particles are
consumed. Shrinkage in the compacts occurs anisotropically during
sintering of the elongated shaped particles, while difference is observed
for spherical shaped particles made with similar processing condition
[7]. Shrinkage anisotropy is found to have a linear relationship with particle orientation for spherical and elongated particle of ceramic compact
Corresponding author.
E-mail address: renoldelsen@gmail.com (S. Renold Elsen).

http://dx.doi.org/10.1016/j.ijrmhm.2015.09.008
0263-4368/ 2015 Elsevier Ltd. All rights reserved.

[8]. The -alumina of particle sizes 0.25, 0.31 and 0.61 m was subjected
to sintering studies. By varying the temperature from 1050 C to 1400 C it
exhibits a low linear shrinkage at 1050 C as reported by Bisset et al. [9].
The shrinkage is also varied during sintering by the addition of additives
in the composites. Particle size of the additive also affects the shrinkage
behavior of composites [10]. Elevated sintering temperatures and prolonged soaking time contribute to higher shrinkage rate in ceramics [11].
2. Literature survey
Based on the complexity of proles and required accuracy different
measurement techniques can be employed to assess the shrinkage characteristics of composites. The inuences of powder injection molding
process parameters on shrinkage for FeNi samples were found using
a Vernier caliper and micrometer [12]. The shrinkage for alumina
ceramics used for MEMS application was measured with a resolution
of 1 m using a charge coupled device microscope [13]. The linear
shrinkage of ceramic composites found using dilatometer at different
temperature was used to estimate density and activation energy
[1415]. Watanabe et al. studied the two-dimensional shrinkage of
complex shaped structure formed by metal injection molding. This
was done using a multi reference digital image in-situ and noncontact type shrinkage studies for up to 1370 C using this method
[16].A novel technique in dilatometer, which exploits white-light noncontact surface prolometry, is applied for measuring shrinkage rate
in small cylindrical powder [17] with an z-resolution of less than

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10 nm. Maca et al. [18] used the data from dilatometric shrinkage to
develop a plot for densication curves with an automatic procedure.
The shrinkage studies were performed with a CCD camera and video
frame grabber on WC6% Co cylindrical specimen during sintering by
Gasik and Zhang using the data obtained from optical dilatometer
[19]. Cristofolini et al. used coordinate measuring machine (CMM) to
evaluate the dimensional deviation and geometrical variation of steel
part formed by powder metallurgy route [20]. The shrinkage analyses
to examine the 3 dimensional shrinkage behavior of alumina during
the sintering were made by digitizing them using a gray-code fringe
projection and detection by a CCD camera [21]. A wide-range of work
on axial and radial shrinkage behavior for ceramics and glass powder
compacts reinforced with alumina-platelets during the sintering were
carried out by Boccaccini et al. using hot stage microscopy (HSM)
[2224]. The shrinkage behavior of porcelain stoneware was obtained
using HSM photos showed that the sample expanded at 1000 C
exhibits no signicant shrinkage up to 1120 C. The decrease in sample
height started from 1120 C and increased exponentially up to 1220 C,
at which the maximum shrinkage was observed [25]. Designs of experiments (DOE) methods were used to model the shrinkage of powder
compacts by varying the parameters. Factorial design was used to
study the shrinkage of powder injection molding with four process
parameters such as the debinding method, sintering heating rate, hold
temperature, and time [12]. Taguchi technique was chosen to study
and optimize the shrinkage behavior of selective laser sintering (SLS).
The empirical relationships between different SLS process parameters
such as scan length, laser beam power, hatch spacing, laser beam
speed, and part bed temperature to predict shrinkage was developed
[26]. RSM was used to identify the inuencing process parameters of
the shrinkage for the ZTA ceramic composites. Although a lot of
techniques were used to model the shrinkage behavior of ceramics,
literature is still limited on computed tomography (CT) based methods
for studying the three dimensional shrinkage. Hence, the present work
has been envisaged to investigate the shrinkage of ZTA using CT imaging
technique, which is a new approach.
3. Materials and method
3.1. Experimental design by response surface methodology (RSM)
RSM is a combination of mathematical and statistical procedures
used to analyze the inuence of multiple variables on a single or
multiple responses [27]. Response surface methodology (RSM), is a
design of experiment method used to model a phenomenon, evaluate
the performance, analyze the behavior and optimize the inuencing
factors [28]. Design of experiment technique called BoxBehnken
design (BBD) is selected for shrinkage study. BBD for three parameters
such as composition, compaction pressure and sintering temperature,
each of three levels with shrinkage as the response was studied. The
BBD allows the usage of relatively least combinations of process parameters to determine the response function. In various experimental
conditions, it is possible to express the independent process parameter
involved into a quantitative form given in Eq. (1).
Y K x1 ; x2 ; ; xk er

Fig. 1. XRD pattern of starting powders alumina and zirconia.

3.2. Experimental details

The commercial grade of alpha phase alumina (-Al2O3) and cubic
phase zirconia (ZrO2) were used in the present work. The mean crystallite size and phases for alumina and zirconia identied from XRD results
were 40 nm and 56 nm, respectively (Fig. 1). Powders of alumina with
different weight ratio (5, 10 and 15%) of zirconia are blended together
using Ball mill for 2 h with 10 min milling and 10 min stoppage with
charge to powder ratio of 1:1. The blended powder is then poured
into the 10 mm diameter circular cavity die and compacted. Cylindrical
ZTA green compacts with diameter 10 mm and length 40 mm for 6 g of
powder were obtained for various loads of 120, 140 and 160 MPa as
shown in Fig. 2. The temperature at which the shrinkage initiates for
alpha-alumina is at 1100 C to 1150 C [29], which are independent of
the particle size and atmosphere. At 1600 C, a maximum density is
reported for ZTA composite [30]. Therefore, 1200 C is selected as the
initial temperature level and 1600 C is selected as the nal temperature
level. The compacts are sintered at temperatures of (1200 C, 1400 C,
and 1600 C) at 5 C raise in temperature per minute with a soaking
period of 5 h in the box furnace. All the specimens were prepared
according to the experimental runs developed by the DESIGN EXPERT
8. The controlling parameter set for running the design matrix is given
in Table 1. Physical and mechanical characteristic of the ZTA composite
fabricated by the same process is published in [31,28] respectively.

where, the response is Y and x1, x2,, xk of k quantitative factors and er

measures the experimental errors, this function is called response
surface function. The mathematical form of is unknown; it can
be approximately satisfactory within the experimental region by
polynomial. The regression equation of second order polynomial was
used to represent the response surface Y as given by Eq. (2).
Y 0

k
X
i1

i xi

k
X
i1

i x2i

k
1
X

k
X

i1 ji1

ij xi x j

2
Fig. 2. Green compact of the specimen.

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385

Table 1
Controlling parameters and their levels for the shrinkage study.
Symbol

A
B
C

Variables

Composition of ZrO2 in Al2O3

Compaction pressure
Sintering temperature

Units

Weight %
MPa
C

Experimental level
Low level
(1)

Mid level
(0)

High level
(1)

5
100
1200

10
130
1400

15
160
1600

3.3. Computed tomography scan

3.4. Microstructural analysis

Computed tomography (CT) is a popular technique for three dimensional medical imaging. It is extensively used to create accurate three
dimensional models of organs for various diagnosis and analyses [32
34]. In this technique, a multi direction projection in the form of slice
is acquired over a different range of angular orientations from the CT
scan. Using the MIMICS software, the three dimensional models from
CT image was developed. The procedure for creation of three dimensional models is given in sequence as shown in Fig. 2. The CT scan has
registration accuracy along with precision of 0.02 0.09 mm [35].
SIEMENS sensation 64 CT scanner was used to scan the specimen
(Fig. 3). These samples were positioned in the machine bed after careful
labeling. The slice interval of 0.65 mm was set with the image matrix
512 512. Then, the samples were subjected to scanning and generation of the data on the right hand side monitor as shown in the Fig. 4.
The number of slices obtained from the scan was 3226 and the captured
images were stored in DICOM 3.0 format and used for further study. The
3D geometry of all the samples generated from the CT les with the help
of MIMICS software. The top, middle and bottom dimensions of the
samples were measured using MIMICS software. It is then subtracted
from the initial dimension of the green compact to obtain the dimensional changes due to shrinkage.

High resolution scanning electron microscopy (HRSEM) micrographs of the test samples were acquired using a Carl Zeiss Supra 40
with an accelerating tension of 3 kV. The ZTA16, ZTA17 and ZTA9
samples for different sintering temperature of 1200, 1400 and 1600 C
respectively with 10 wt.% of zirconia were selected for HR SEM analysis.
Samples were gold-coated using a sputtering unit before SEM analysis.
The images captured by SEM are used to determine the microstructural
behavior inuencing shrinkage of the ZTA composite. The grain size
analyses were done based on the intercept method (ASTM: E112-12
standards) and the grain growth studies were reported.
4. Results and discussion
The shrinkage characteristic of conventionally sintered ZTA by
powder forming process was investigated by using CT scan imaging
technique. The complete experimental runs with process parameter
and the response analyzed using BBD is provided in Table 2. From the
analyses the sintered cylindrical specimen measured least dimension
(8 mm) at the top for the 1600 C sintered specimens. The maximum
shrinkage percentage of 20% is observed and is very similar to 18% for
sintered alumina compact at 1600 C [7]. The improved shrinkage

Fig. 3. Production of 3D model samples.

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Fig. 4. Picture of the data generation from CT scan in control room.

at the top of the sintered cylindrical specimen is observed, on the

Shrinkage top column in Table 2. This was due to the effect of gravity
which causes non-uniformities in shrinkage and compact aspect ratio
as reported in the literature [36,37]. The unied model using nite
element analysis method also predicts more shrinkage at the top and
lower shrinkage at the bottom. As predicted by Chen et al. [38], a conical
shape is formed by diameter changes along the length after sintering of
cylindrical shaped parts. The shrinkage at 1600 C of 2 mm is more compared to 1400 C and is very low for 1200 C with 0.3 mm shrinkage
which is in accordance with the reported literature [39].
4.1. Conformation of the model by ANOVA methods for radial shrinkage at
the top
The model is considered to be signicant from Table 3 as the model
F-value is also 361.15, there is only a 0.01% probability that such large
value could occur due to noise. Also from the analysis temperatures (C
and C2) were found to be signicant terms. The predicted R-squared

value of 0.9979 for the investigation is in harmony with adjusted

R-squared value of 0.9951. The signal to noise ratio calculated by
adequate precision is 52.947, which indicates an adequate signal as it
measures more than four. In the analysis the temperature is found to
be signicant model. The response surface and contour in Figs. 57
show the interaction effects between compaction pressure and composition for shrinkage in the top region at varying temperatures of 1200 C,
1400 C and 1600 C, respectively. The shrinkage of 0.16 mm to 0.36 mm
is found for the ZTA at the top from the analysis for 1200 C from Fig. 5.
The shrinkage for ZTA was found to be from 1.4 mm to 1.5 mm for
sintering temperature of 1400 C Fig. 6, also a maximum shrinkage of
1.81 mm to 2.01 mm for 1600 C Fig. 7. Eqs. (3) and (4), express the
empirical relation in terms of coded factors and actual factors for shrinkage at the top, respectively.
Shrinkage Top 1:48 0:83  C0:015  A2 0:015  B2 0:36  C2
0:050  A  B0:050  B  C

Table 2
Process design layout using BoxBehnken design & test results.
Variables

Responses

Run

Composition of ZrO2 in Al2O3

Weight percentage

Pressure
MPa

Temperature
C

Shrinkage bottom
mm

Shrinkage middle
mm

Shrinkage top
mm

ZTA1
ZTA2
ZTA3
ZTA4
ZTA5
ZTA6
ZTA7
ZTA8
ZTA9
ZTA10
ZTA11
ZTA12
ZTA13
ZTA14
ZTA15
ZTA16
ZTA17

10
5
10
15
10
10
15
5
10
15
5
15
10
10
5
10
10

160
130
130
130
130
130
130
130
100
160
100
100
160
130
160
100
130

1600
1600
1400
1600
1400
1400
1200
1200
1600
1400
1400
1400
1200
1400
1400
1200
1400

1.8
1.8
1.3
1.8
1.4
1.4
0.2
0.2
1.9
1.3
1.3
1.3
0.2
1.4
1.2
0.1
1.4

1.9
1.9
1.4
1.9
1.4
1.4
0.2
0.2
1.9
1.4
1.4
1.4
0.2
1.4
1.3
0.1
1.4

1.9
1.9
1.4
1.9
1.5
1.5
0.3
0.3
2
1.5
1.5
1.4
0.3
1.5
1.4
0.2
1.5

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387

Table 3
ANOVA model for shrinkage at the top (response surface quadratic).
Source

Sum of squares

Degrees of freedom

Mean square

F value

p-Value prob N F

Model
A-comp
B-pre
C-tem
AB
AC
BC
A2
B2
C2
Residual
Lack of t
Pure error
Cor total

6.036412
0
0
5.445
0.000947
0.000947
0.560947
0.01
0
0.01
0.013
0.005
0.008
6.049412

9
1
1
1
1
1
1
1
1
1
7
3
4
16

0.670712
0
0
5.445
0.000947
0.000947
0.560947
0.01
0
0.01
0.001857
0.001667
0.002

361.1528
0
0
2931.923
0.510121
0.510121
302.0486
5.384615
0
5.384615

b0.0001
1.0000
1.0000
b0.0001
0.4982
0.4982
b0.0001
0.0534
1.0000
0.0534

0.833333

0.5413

Std. dev. 0.043, R-squared 0.9979, mean 1.29, adjusted R-squared 0.9951, C.V. 3.33, predicted R-squared 0.9847, PRESS 0.093, adequate precision 52.947.

Shrinkage Top 23:605000:031333  Composition 0:012667

 Compaction pressure 0:030758  Temperature6  104
 Composition2 1:67  105  Compaction pressure2 9:125
 106  Temperature2 3:33  104  Composition
 Compaction pressure 2:78  1019  Composition
 Temperature8:33  106  Compaction pressure
 Temperature

4.2. Conformation of the model by ANOVA methods for radial shrinkage at

the middle
The model F-value is 672.32 is considered to be signicant from
Table 4 and the probability is only 0.01% for such large value could
occur due to noise. The Temperature (C and C2) were found to be a
signicant terms from the analysis of variance. The R-squared value
predicted from the investigation was 0.9988 and it is in harmony with
adjusted R-squared value of 0.9974. The adequate precision is 71.201,
which is more than four indicates an adequate signal. The response
surface and contour in Fig. 8 show the variation of shrinkage from
0.125 mm to 0.225 mm for the interaction effects between compaction

pressure and composition on the middle at 1200 C. The surface graph

shows a least shrinkage value comparatively. The shrinkage was
predicted to be 1.3375 mm to 1.41875 mm in Fig. 9 for the sintering temperature of 1400 C. The surface graph (Fig. 10) for sintering temperature
of 1600 C, in the middle region gives shrinkage of 1.825 mm to 1.925 mm
which exhibits maximum shrinkage compared to lower sintering temperature. The following equation expresses the empirical relation in terms of
coded factors for shrinkage at the middle is given in Eqs. (5) and (6) respectively.
Shrinkage middle 1:40 0:012  A 0:86  C0:025  B2 0:35  C2
0:025  A  B0:025  B  C

5
Shrinkage middle 22:823610:019167  Composition 0:011389
 Compaction pressure 0:029354Temperature 2:35172
 1016  Composition2  2:77778  105
 Compaction pressure2 8:75000  106 Temperature2
1:66667  104  Composition  Compaction pressure
3:33067  1019  Composition  Temperature4:16667
 106  Compaction pressure  Temperature

Fig. 5. Response surface and contour graph of shrinkage for interaction effects between compaction pressure and composition at 1200 C on the top.

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Fig. 6. Response surface and contour graph of shrinkage for interaction effects between compaction pressure and composition at 1400 C on the top.

4.3. Conformation of the model by ANOVA methods for radial shrinkage at

the bottom
The model is signicant the model F-value is 298.8216 from Table 5
as also, there is 0.01% probability that such large value could occur due
to noise. The analysis showed temperature (C and C2) to be a signicant
term. The R2 value of 0.9778 was predicted from the investigation is
in harmony with adjusted R2 value of 0.9941. The adequate precision
calculated signal to noise ratio was 48.489 and is more than four,

which indicates an adequate signal as it measures. The following

equation expresses the empirical relation in terms of coded factors
for shrinkage at the middle is given in Eqs. (7) and (8) respectively.

Shrinkage bottom 1:38 0:013  A0:012  B 0:83  C0:053  A2

0:053  B2 0:33  C2 0:025  A  B0:050  B  C

Fig. 7. Response surface and contour graph of shrinkage for interaction effects between compaction pressure and composition at 1600 C on the top.

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389

Table 4
ANOVA model for shrinkage at the middle.
Source

Sum of squares

Degrees of freedom

Mean square

F value

p-Value prob N F

Model
A-comp
B-pre
C-tem
AB
AC
BC
A2
B2
C2
Residual
Lack of t
Pure error
Cor total

6.483088
0.00125
0
5.95125
0
0.002632
0.515789
0.0025
0
0.0025
0.0075
0.0075
0
6.490588

9
1
1
1
1
1
1
1
1
1
7
3
4
16

0.720343
0.00125
0
5.95125
0
0.002632
0.515789
0.0025
0
0.0025
0.001071
0.0025
0

672.3203
1.166667
0
5554.5
0
2.45614
481.4035
2.333333
0
2.333333

b0.0001
0.3159
1.0000
b0.0001
1.0000
0.1611
b0.0001
0.1705
1.0000
0.1705

Standard deviation 0.033, R2 0.9988, mean 1.22, adjusted R2 0.9974, C.V. 2.68, predicted R2 0.9815, PRESS 0.12, adequate precision 71.201.

Shrinkage bottom 22:90917 0:022833  Composition 0:024750

 Compaction pressure 0:028133  Temperature2:1
 103  Composition2 5:83333  105
 Compaction pressure2 8:18750  106  Temperature2
1:66667  104  Composition  Compaction pressure
2:91434  1019  Composition  Temperature8:33333
 106  Compaction pressure  Temperature

The response surface and contour in Fig. 11 show the variation of

shrinkage from 0.2365 mm to the least shrinkage of 0.0725 mm for
the interaction effects between compaction pressure and composition
on the middle at 1200 C. The shrinkage for the sintering temperature
of 1400 C was predicted to be 1.3812 mm to 1.225 mm from response
surface graph Fig. 12. The surface graph shown in Fig. 13 for sintering
temperature of 1600 C, in the middle region gives lower shrinkage
value of 1.672 mm to higher value of 1.925 mm which exhibits minimum
shrinkage compared to the upper and middle portion.

4.4. Inuence of process parameter

From the ANOVA results that temperature is found to plays a major
role in the shrinkage behavior of the zirconia reinforced alumina
composites. The maximum shrinkage is found at 1600 C sintering
temperature. The compaction pressure has no inuence on the shrinkage of the compact in the study as predicted by ANOVA. This is because
particleparticle interaction and densication is not achieved by the
compaction pressure of magnitude 160 MPa. The observation from
Figs. 7, 10 and 13 shows maximum shrinkage at all three stages (top,
middle and bottom) for the interaction between 15% weight percentage
of zirconia and maximum sintering temperatures of 1600 C. More
amount of zirconia in the alumina matrix causes pinning effect which
hinders the grain growth of alumina. The two adjacent particles diffuse
along the grain boundary to form the neck which reduces the distance
separating their mass centers thus effecting shrinkage in a powder
system. The shrinkage of a powder compact is dominated by the surface
diffusion of grains which causes the smaller grains found in between

Fig. 8. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1200 C on the middle.

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Fig. 9. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1400 C on the middle.

Fig. 10. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1600 C on the middle.
Table 5
ANOVA model for radial shrinkage at the bottom of the sample.
Source

Sum of squares

Degrees of freedom

Mean square

F value

p-value prob N F

Model
A-comp
B-pre
C-tem
AB
AC
BC
A2
B2
C2
Residual
Lack of t
Pure error
Cor total

5.955088
0.00125
0.00125
5.445
0.011605
0.011605
0.451605
0.0025
0
0.01
0.0155
0.0075
0.008
5.970588

9
1
1
1
1
1
1
1
1
1
7
3
4
16

0.661676
0.00125
0.00125
5.445
0.011605
0.011605
0.451605
0.0025
0
0.01
0.002214
0.0025
0.002

298.8216
0.564516
0.564516
2459.032
5.241087
5.241087
203.9508
1.129032
0
4.516129

b0.0001
0.4769
0.4769
b0.0001
0.0559
0.0559
b0.0001
0.3233
1.0000
0.0712

1.25

Standard deviation 0.047, R2 0.9974, mean 1.18, adjusted R2 0.9941, C.V. 4.00, predicted R2 0.9778, PRESS 0.13, adequate precision 48.489.

0.4028

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391

Fig. 11. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1200 C on the bottom.

larger grains perishes to restart the neck growth process. The pore
mobility is facilitated for the pores located at the grain boundary by
the pull created by moving grain boundary. The grain boundary diffusion is found to be minimal at 1200 C sintering temperature with
large number of voids. As the activation energy required for material
transportation mechanism is more the shrinkage of ZTA compacts is
found to be minimal. The neck growth is also found to be limited during
the partial diffusion of grain boundary between the particles will
remove the curvature in the surface. Because of this shrinkage of the
sintered samples at 1200 C is found to be poor and grain growth is
found to be minimal with grain size of 0.282 m (ASTM grain size number 21) and least densication as observed in Fig. 14. At 1400 C

sintering temperature, appreciable amount of grain boundary diffusion

is observed (Fig. 15) with comparatively minimal pores/voids. Few
pores have reached their equilibrium shapes due to the surface and
interfacial tension and still the pore phase is continuous. There is a
reduction in the cross section of pores compared to 1200 C and few
pores have become unstable and have left isolated pores as they pinch
off. After being pinched off from other pores, few of them become isolated
at the grain corners. The grain boundary diffusion has not occurred fully
and the presence of pores has to contribute to minimal shrinkage. The
grain growth is found to be normal with increased grain size of 0.55 m
(ASTM grain size number 19) compared to 1200 C sintered sample.
The SEM image (Fig. 16) of 1600 C sintered samples shows increased

Fig. 12. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1400 C on the bottom.

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Fig. 13. Surface graph for interaction effects of shrinkage for compaction pressure and composition at 1600 C on the bottom.

averages grain size, maximal pore healing with improved densication

and proper grain boundary diffusion. The voids and the pores found in
the other two cases are reduced and the grain size is found to be
increased to 1.42 m (ASTM grain size number 16). The coarsening mechanism is not found due to which smaller grains are consumed along with
the pores which causes reduction on sample volume which was observed
during macroscopic analysis. The pores found in grain corners of sample
sintered at 1400 C are not found in samples sintered at 1600 C. The
increase in temperature causes continuous shrinkage of pores which
causes the removal of porosity in the ZTA samples so maximum shrinkage has occurred. Shui et al. [7] reported that the study of both linear
and radial shrinkage of alumina compact during sintering. From the analysis it was observed that shrinkage percentage for both linear and radial
shrinkage of the alumina compact started to straighten out at 1550 C
after a steady fall. To investigate further, the exact temperature where
the maximum shrinkage has occurred two other temperatures 1560 C

and 1580 C has been selected in the range nearer to 1600 C. The experiments were carried out with 15 wt.% zirconia in the alumina matrix and
the shrinkage studies were carried out by using the Vernier Calipers.
Further, the grain boundary interactions, pore mobility and pore closure
of the samples were analyzed using SEM. The SEM image (Fig. 17)
shows the samples sintered at 1560 C with smaller grains. The grain
boundary diffusion is found to be good and the absences of pores are
observed. The SEM image shows samples sintered at 1580 C with comparatively larger grains (Fig. 18). The grain boundary diffusion is found
to be good and pores are also not found.

Fig. 14. HR SEM image of (ZTA16) sintered at 1200 C.

Fig. 15. HR SEM image of (ZTA17) sintered at 1400 C.

5. Conclusion
The shrinkage of alumina zirconia composites fabricated by powder
forming was investigated by using computed tomography technique.
The shrinkage measurement was carried out using three dimensional

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393

Fig. 16. HR SEM image of (ZTA9) sintered at 1600 C.

models developed from CT scan images and the following conclusions

are made:
The selected process parameter such as weight percentage of zirconia
added to alumina and compaction pressure does not inuence the
shrinkage characteristics of the ZTA compact.
The shrinkage of ZTA compact was found to be maximum for
the sintering temperature of 1600 C at the top, middle and bottom
portion of the compact.
The maximum shrinkage percentage of 20% is found to be at the top of
the cylindrical compact sintered at 1600 C.
The HR SEM image suggested that at 1600 C grain growth is the dominate factor which cause the maximum shrinkage.

Fig. 18. SEM image of ZTA sintered at 1580 C.

The temperature inuences the shrinkage behavior of ceramic

composites compared to other factors.
The change in weight percentage of zirconia in alumina matrix and
compaction pressure showed no inuence on the responses.

Also the advantage of the proposed new measurement method over

the other proposed and available methods were as follows:
The error created by measuring instruments and human is avoided
completely by this precise digital method.
Also measuring dimensions of green compacts which are fragile and
difcult for handling can be done with ease.
Even shrinkage of complex shapes along all three directions can be
assessed easily using commercial solid modeling packages.

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Fig. 17. SEM image of ZTA sintered at 1560 C.

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