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Article history:
Received 1 May 2015
Received in revised form 8 June 2015
Accepted 15 June 2015
Available online 18 June 2015
Keywords:
Zirconia reinforced alumina
BoxBehnken design
Micro Vickers hardness
Compressive strength
Regression
Multi response optimization
Response Surface Methodology and Grey
Relational Analysis
a b s t r a c t
In this work the effect of powder forming process parameters of zirconia reinforced alumina composites on micro
hardness and compressive strength was studied. The weight percentages of zirconia added to alumina, compaction pressure and sintering temperature are the process parameters selected for this analysis. Using Box
Behnken technique in Response Surface Methodology (RSM), seventeen experimental runs are developed. The
sintering temperature and weight percentage of zirconia added to alumina are found to inuence the responses.
The inuencing parameters were identied by using analysis of variance and Grey Relational Analysis (GRA). The
regression model for both micro hardness and compressive strength are developed. The increasing amount of
zirconia added to alumina matrix is found to enhance the compressive strength of the composite and reduces
the hardness of composite. Also, multi response optimization to obtain higher hardness and compressive
strength are done using both RSM and GRA.
2015 Elsevier Ltd. All rights reserved.
1. Introduction
Zirconia reinforced alumina (ZTA) are ceramic composites that are
widely used for knee and hip joint prostheses [1] and as insert materials
in machining tools [2]. The wide spectrum of applications has created
more interest in the detailed study of the composite. To develop ZTA
composite with higher reliability and improved performance detailed
investigation of the various physical and mechanical characteristics is
required. The nal composite characteristics depend on the material
characteristics of the matrix, reinforcements and the fabrication
techniques. Material characteristics such as hardness, yield stress, endurance limit creep and resistance to crack growth can be predicted
from indentation studies [3]. ZTA composites prepared by 5, 10 and
20 wt.% of zirconia reinforced with alumina by powder processing
showed decreasing hardness. But, powder synthesized by colloidal processing showed decreasing hardness up to 10 wt.% and increased above
10 wt.% [4]. The powder injection molding process was used to prepare
ZTA composites with different binders and sintering temperature of
1400 C and 1600 C soaking time of 2 hours. A maximum hardened
value of 1582.4 HV was reported at the sintering temperature of
1600 C [5]. The ZTA composites, green bodies were sintered from
1475 C to 1575 C with a temperature increment of 25 C after the
slip casting process. The hardness value decreased from 1900 HV10
to 1785 HV10 for sintering temperature of 1425 C and 1575 C
Corresponding author.
E-mail address: renoldelsen@gmail.com (S.R. Elsen).
http://dx.doi.org/10.1016/j.ijrmhm.2015.06.007
0263-4368/ 2015 Elsevier Ltd. All rights reserved.
160
S.R. Elsen, T. Ramesh / Int. Journal of Refractory Metals and Hard Materials 52 (2015) 159164
Table 1
Process design layout using Box Behnken design and test results.
Run Variables
Responses
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
CS
MVH
Wt.%
MPa
MPa
HV
10
15
5
10
15
5
10
10
15
5
10
10
10
5
15
10
10
100
130
130
160
100
160
130
130
160
100
130
130
130
130
130
100
160
1200
1200
1200
1200
1400
1400
1400
1400
1400
1400
1400
1400
1400
1600
1600
1600
1600
8.094853
12.80896
7.338466
9.073013
119.3591
71.9682
88.70822
96.85784
143.6895
88.27868
112.8129
113.4199
123.9988
237.514
292.054
283.753
264.161
122.93 25.
66 13.82
207.075 23.62
129.8 26.71
972.4 15.1
1170 62.93
1085 2.83
1056 40.79
1054.22 44
1127 21.69
1112 30.1
1019 23.8
1024.325 50.21
1934 17.7
1524 1.54
1676.4 11.6
1627.83 4
Table 2
ANOVA for response surface quadratic model compressive strength.
Source
Sum of square
DF
Mean square
F-value
p-Value
Prob b F
Model
AComposition
BPressure
CTemperature
AB
AC
BC
A2
B2
C2
Residual
Lack of Fit
Pure error
Cor total
1.49E5
4503.58
1.61
1.41E5
1.39
601.95
0.081
89.37
75.5
3441.53
840.6
827.39
13.21
1.50E5
9
1
1
1
1
1
1
1
1
1
7
3
4
16
16,579.58
4503.58
1.61
1.41E5
1.39
601.95
0.081
89.37
75.5
3441.53
120.09
275.8
3.3
138.06
37.5
0.013
1169.95
0.012
5.01
6.77E-4
0.74
0.63
28.66
83.52
b0.0001
0.0005
0.9109
b0.0001
0.9173
0.0602
0.98
0.4169
0.4539
0.0011
0.0005
Standard deviation:10.9583, R-squared:0.9943, mean:126.7249, adjusted Rsquared:0.9871, C.V. %:8.6473, predicted R-squared:0.9116, PRESS:13,258.9299,
adequate precision:37.181.
S.R. Elsen, T. Ramesh / Int. Journal of Refractory Metals and Hard Materials 52 (2015) 159164
161
Table 3
ANOVA for response surface quadratic model Vickers hardness.
Source
Sum of square
DF
Mean square
F-value
p-Value Prob b F
Model
AComposition
BPressure
CTemperature
AB
AC
BC
A2
B2
C2
Residual
Lack of Fit
Pure error
Cor total
5,032,364.484
85,114.22258
13.36445
4,867,863.023
6.5025
22,339.03891
14.8225
5692.576581
32.05958059
52,784.42603
6641.238606
6496.364106
144.8745
5,039,005.722
9
1
1
1
1
1
1
1
1
1
7
3
4
16
559,151.6093
85,114.22258
13.36445
4,867,863.023
6.5025
22,339.03891
14.8225
5692.576581
32.05958059
52,784.42603
948.7483723
2165.454702
36.218625
589.357121
89.7121145
0.0140864
5130.82622
0.00685377
23.5457995
0.01562322
6.00009101
0.03379145
55.6358541
59.7884294
b0.0001
b0.0001
0.9088
b0.0001
0.9363
0.0018
0.9040
0.0441
0.8593
b0.0001
0.00088
Standard deviation:30.8017, R-squared:0.9986, mean:978.78, adjusted R-squared:0.9969, C.V. %:3.1469, predicted R-squared:0.9793, PRES:104,168.1921, adequate
precision:75.269.
310
248
186
124
62
0
1600.00
15.00
1520.00
13.00
1440.00
C: Temperature (C)
11.00
1360.00
9.00
1280.00
7.00
1200.00
5.00
A: composition (wt%)
Fig. 2. Compressive strength response plot based on the composition of zirconia and sintering temperature.
2
The conformation study of Vickers hardness by ANOVA is given in
Table 3. The F-value of the micro Vickers hardness model was predicated by ANOVA to be 589.357121 which exhibit the signicance of the
model. The possibility of F-value this large that can occur due to noise
is 0.01 percentages. From the analysis Prob N F value smaller than 0.05
is found for the weight percentage of zirconia in alumina (A), sintering
temperature (C) combined effect of (A and C) and sintering
temperature2 (C2) which indicates the signicant model terms. The
compaction pressure (B) and other interaction terms have no inuence
on the micro Vickers hardness of the composite material. The predicted
R-squared value of 0.9793 is in agreement with an adjusted R-squared
value of 0.9969. The adequate precision value 75.269 measures the
signal to noise ratio, is greater than 4 is desirable and the model can
be used to navigate the design space. The Eq. (3) in terms of coded
factors and Eq. (4) with actual factors can be used to predict the
response to the provided levels of each factor.
MVH 1068:88102:68A 779:55C67:23 A C157:88C2 :
162
S.R. Elsen, T. Ramesh / Int. Journal of Refractory Metals and Hard Materials 52 (2015) 159164
addition of ZrO2 in the matrix causes the zirconia ions (Zr4+) to hinder
the grain boundary sliding of alumina [10]. Also, due to pinning effect
ZrO2 checks the grain growth of alumina during sintering which is
also a possible strengthening effect of the composite. Compressive
strength is enhanced from 7.33 MPa to 292.05 MPa for increasing
sintering temperature from 1200 C to 1600 C respectively. At
1200 C sintering temperature, more voids were observed (Fig. 3) and
also the grain boundary diffusion between the particles is minimal,
this causes immediate failure and minimal compressive strength. The
1400 C sintered sample has shown comparatively improved grain
boundary diffusion between the particles with voids (Fig. 4). Also higher
compressive strength was observed compared to 1200 C sintered samples. At 1600 C, proper grain boundary diffusion with few voids is observed as shown in Fig. 5. The collective effects of both weight
percentage of zirconia added to alumina and sintering temperature on
micro Vickers hardness of the zirconia that reinforced alumina ceramic
are given in Fig. 6. The sintering temperature is found to be the most inuential factor, and the hardness value increases with the increase in
temperature. This is due to the fact that 98% theoretical density with
less porosity is achieved at 1600 C. From the response plot, it is
observed that the hardness is increased from 96 HV at 1200 C to
1860 HV at 1600 C for 5 wt.% of zirconia added to alumina. The hardness value is found to be reduced by the addition of zirconia also
predicted by the response surface plot and similar behavior was reported by Arab et al. [14]. However, the hardness is decreased from 1860 HV
at 5 wt.% of zirconia to 1524 HV for 15 wt.% of zirconia at 1600 C by 18%.
The plot shows a gradual decrease in the response as the weight percentage of zirconia added to alumina factor is increased. The
composite prepared by the powder injection molding process with
95% theoretical density exhibited 1582.4 HV [5]. A maximum hardness
of 1934 HV has been achieved for 96.5% theoretical density of the nal
composite material.
1860.5
1419.38
978.25
537.125
96
1600.00
15.00
1520.00
13.00
1440.00
11.00
1360.00
C: Temperature (C)
9.00
1280.00
7.00
1200.00
A: composition (wt%)
5.00
S.R. Elsen, T. Ramesh / Int. Journal of Refractory Metals and Hard Materials 52 (2015) 159164
Table 4
Constraints and limits for compressive strength and Vickers micro hardness.
Constraints
163
Table 7
Response table for Grey relational grade.
Limits
Name
Goal
Lower limit
Upper limit
A: Composition
B: Compaction pressure
C: Temperature
Compressive strength
Vickers hardness
Is in range
Is in range
Is in range
Maximum
Maximum
5 (wt.% of zirconia)
100 MPa
1200 C
292.054 (MPa)
1934 (HV)
15 (wt.% of zirconia)
160 MPa
1600 C
Process parameter
Level 1
Level 2
Level 3
Range (maximumminimum value)
Order
0.537241
0.53939*
0.523843
0.015547
2
0.53903*
0.53733
0.526566
0.010764
3
0.338162
0.477832
0.841994*
0.503832
1
Table 8
Comparison of conrmation experiments with the results.
Table 5
Optimized value for responses and highest value of desirability.
Process parameter
Response
C
Compressive
strength
Micro Vickers
hardness
MPa
MPa
HV
100.001
1600
292.054
1623.828
Wt.%
11.815
Exp. no
Desirability
0.912
indicates that the factor compaction pressure has no effect on the response.
1
2
3
Obtained
Predicated
Error
Obtained
Predicated
Error
273.0705
276.0202
264.0168
292.054
292.054
292.054
6.5%
5.49%
9.6%
1575.113
1581.608
1560.499
1623.83
1623.83
1623.83
3%
2.6%
3.9%
by using the higher the better condition is given by Eqs. (5) and (6).
NCSi
CSi minCSi
:
maxCSi minCSi
NMVHi
MVHi minMVHi
:
maxMVHi minMVHi
oi MVH 1NMVHi :
oi CSmin oi CSmax
:
oi CS oi CSmax
i MVH
oi MVHmin oi MVHmax
:
oi MVH oi MVHmax
10
Table 6
Calculated normalized value Grey relational co-efcient, grade values and rank of process design layout.
Run
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
Pressure
Temperature
Reference sequence
Deviation sequence
GRC after
weighted
(Wt.% of ZrO2)
(MPa)
(C)
N(CS)
N(MVH)
oi(CS)
oi(MVH)
CS
MVH
2
3
1
2
3
1
2
2
3
1
2
2
2
1
3
2
2
1
2
2
3
1
3
2
2
3
1
2
2
2
2
2
1
3
1
1
1
1
2
2
2
2
2
2
2
2
2
3
3
3
3
0.00266
0.01921
0
0.00609
0.39345
0.227
0.28579
0.31442
0.4789
0.28428
0.37046
0.37259
0.40974
0.80844
1
0.97084
0.90203
0.05204
0
0.11086
0.06109
0.60407
0.72851
0.67647
0.66063
0.6086
0.71041
0.66968
0.67647
0.6629
1
0.81448
0.9095
0.89367
0.99734
0.98079
1
0.99391
0.60655
0.773
0.71421
0.68558
0.5211
0.71572
0.62954
0.62741
0.59026
0.19156
0
0.02916
0.09797
0.947964
1
0.88914
0.938914
0.395928
0.271493
0.323529
0.339367
0.391403
0.289593
0.330317
0.323529
0.337104
0
0.18552
0.090498
0.106335
0.3339
0.3377
0.3333
0.3347
0.4519
0.3928
0.4118
0.4217
0.4897
0.4113
0.4427
0.4435
0.4586
0.7230
1.0000
0.9449
0.8362
0.3402
0.3333
0.3510
0.3411
0.4927
0.5501
0.5238
0.5155
0.5149
0.5365
0.5319
0.5051
0.5066
1.0000
0.6949
0.7838
0.7531
GRG
Rank
0.3371
0.3355
0.3422
0.3379
0.4723
0.4714
0.4678
0.4686
0.5023
0.4739
0.4873
0.4743
0.4826
0.8615
0.8475
0.8644
0.7946
16
17
14
15
10
11
13
12
5
9
6
8
7
2
3
1
4
164
S.R. Elsen, T. Ramesh / Int. Journal of Refractory Metals and Hard Materials 52 (2015) 159164
n
1X
f CS i MVHg:
n i1 i
11
Acknowledgement
The authors wish to thank Dr. P. Senthil, Assistant Professor, Production Engineering, NIT Trichy for extending the micro Vickers hardness
facility to carry out the tests which were procured by funding project
reference No (SR/FT/ET-033/2009).
References
[1] M. Bocanegra-Bernal, C. Domnguez-Rios, A. Garcia-Reyes, A. Aguilar-Elguezabal, J.
Echeberria, A. Nevarez-Rascon, Fracture toughness of an -al2o3 ceramic for joint
prostheses under sinter and sinter-hip conditions, Int. J. Refract. Met. Hard Mater.
27 (4) (2009) 722728.
[2] N. Mandal, B. Doloi, B. Mondal, Predictive modeling of surface roughness in high
speed machining of aisi 4340 steel using yttria stabilized zirconia toughened alumina turning insert, Int. J. Refract. Met. Hard Mater. 38 (2013) 4046.
[3] D. Casellas, I. Rfols, L. Llanes, M. Anglada, Fracture toughness of zirconiaalumina
composites, Int. J. Refract. Met. Hard Mater. 17 (1) (1999) 1120.
[4] A. Rafferty, A. Alsebaie, A. Olabi, T. Prescott, Properties of zirconia-toughenedalumina prepared via powder processing and colloidal processing routes, J. Colloid
Interface Sci. 329 (2) (2009) 310315.
[5] S. Md Ani, A. Muchtar, N. Muhamad, J.A. Ghani, Fabrication of zirconia-toughened
alumina parts by powder injection molding process: optimized processing parameters, Ceram. Int. 40 (1) (2014) 273280.
[6] F. Kern, P. Palmero, F.G. Marro, A. Mestra, Processing of aluminazirconia composites by surface modication route with enhanced hardness and wear resistance,
Ceram. Int. 41 (1) (2015) 889898.
[7] H.L. Calambs Pulgarin, M.P. Albano, Sintering, microstructure and hardness of
different aluminazirconia composites, Ceram. Int. 40 (4) (2014) 52895298.
[8] J. Lankford, Compressive strength and microplasticity in polycrystalline alumina, J.
Mater. Sci. 12 (4) (1977) 791796.
[9] E. Calvi, L. Joly-Pottuz, C. Esnouf, P. Clment, V. Garnier, J. Chevalier, Y. Jorand, A.
Malchre, T. Epicier, K. Masenelli-Varlot, Real time tem observation of alumina ceramic nano-particles during compression, J. Eur. Ceram. Soc. 32 (10) (2012)
20672071.
[10] O. Flacher, J. Blandin, K. Plucknett, Effects of zirconia additions on the superplasticity
of alumina zirconia composites, Mater. Sci. Eng. A 221 (1) (1996) 102112.
[11] G. Liu, D. Zhang, C. Meggs, T.W. Button, Porous Al2O3 ZrO2 composites fabricated by
an ice template method, Scr. Mater. 62 (7) (2010) 466468.
[12] R. Liu, Y. Li, C.-A. Wang, S. Tie, Fabrication of porous aluminazirconia ceramics by
gel-casting and inltration methods, Mater. Des. 63 (2014) 15.
[13] S.Renold Elsen, T. Ramesh, B. Aravinth, Optimization of process parameters of zirconia reinforced alumina by powder forming process using response surface method,
Adv. Mater. Res. 984 (2014) 129139.
[14] Ali Arab, Zainal Arin Ahmad, Roslan Ahmad, Effects of yttria stabilized zirconia (3YTZP) percentages on the ZTA dynamic mechanical properties, Int. J. Refract. Met.
Hard Mater. 50 (1) (2015) 157162.
[15] N. Mandal, B. Doloi, B. Mondal, Development of ank wear prediction model of zirconia toughened alumina (ZTA) cutting tool using response surface methodology,
Int. J. Refract. Met. Hard Mater. 29 (2) (2011) 273280.
[16] A. Haq, P. Marimuthu Noorul, R. Jeyapaul, Multi response optimization of machining
parameters of drilling Al/SiC metal matrix composite using grey relational analysis
in the Taguchi method, Int. J. Adv. Manuf. Technol. 37 (34) (2008) 250255.