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Article

Synthesis and Characterization of Alumina


Zirconia Composite Material
Doped with Silica
Manas Ranjan Majhi1, S Viswakarma2, NS Meheta3, K Sauravh4, S Singh5

Abstract
Present research work deals with synthesis of alumina zirconia silica Composite material by
mixed powder composed of varying weight percentage of alumina and silica with fixed 30%
weight composition of zirconia. The characteristics such as bulk density, apparent porosity, linear
shrinkage and weight loss behaviour, XRD, bending strength and micro structures of different
samples were analysed comparatively with gradual increment of silica content from 0 to 4wt%
into base composition. After sintering at 1200°C, samples shows significant change in its physical
and microstructural properties such as densification and reduction in apparent porosity, XRD
pattern reveal zirconium aluminium oxide phase with conversion of monoclinic zirconia to
tetragonal phase and bending strength ware also improved apparently. Micro structure analysis
of sintered composite gives relative grain sizes and phases present in different samples which
shows improved bonding between the matrixes with silica addition.

Keywords: Alumina Zirconia, Silica, XRD pattern


Introduction
There are some common refractories which are commonly used in composites for their property of withstanding
high temperature without showing any sign of melting or deformation also with better mechanical and physical
properties.1 The composites made using these ceramic materials are widely used in industrial applications.
Specifically, they are used in the steel industry, cement industry, glass industry etc. Refractory materials with ZrO2
contents ranging from 30 to 42wt % are manufactured by melting and casting, and are characterized by high
corrosion resistance toward several types of aggressive environments.2,3 However it was seen experimentally, the
presence of ZrO2 in AZS refractories causes a significant change in volume of about 3-5% above 1000°C due to
tetragonal to monoclinic phase transformation in ZrO2, which corresponds to a martensitic transformation.4-5
During cooling of the material, the martensitic transformation causes the formation of micro cracks and porosity,
with a decrease in mechanical strength, associated with a reduction in its Young‘s modulus.7,8 The present work
deals with improving mechanical and physical properties with silica addition.9,10

1,2,3,4,5
Department of Ceramic Engineering, Indian Institute of Technology (BHU), Varanasi, Uttar Pradesh, India.
Correspondence: Mr. Manas Ranjan Majhi, Indian Institute of Technology (BHU), Varanasi, Uttar Pradesh, India.
E-mail Id: mrmajhi.cer@itbhu.ac.in
Orcid Id: http://orcid.org/0000-0001-9081-0469

How to cite this article: Majhi MR, Viswakarma S, Meheta NS et al. Synthesis and Characterization of Alumina Zirconia
Composite Material Doped with Silica. J Adv Res Glass Leath Plast Tech 2017; 2(1&2): 18-24.

© ADR Journals 2017. All Rights Reserved.


J. Adv. Res. Glass Leath. Plast. Tech. 2017; 2(1&2) Majhi MR et al.

Experimental Procedure Sample Characterization


Composition of Material After preparation and sintering the sample were
Table 1.Batch Composition characterized i.e. Bulk density, apparent density,
Sample No. Alumina Zirconia Silica linear shrinkage, weight loss. Phase determination by
(wt. %) (wt %) (wt %) XRD analysis the main aim of project is to improve the
1 70 30 0 properties of material after adding 2%, 4% of silica as
2 68 30 2 an additive.
3 66 30 4
Results and Discussion
Experimental Procedure Bulk Density Measurement
Al2O3 (70wt %) + ZrO2 (30wt %) <100gm> mix with Bulk density of all the sintered samples were
2wt%, 4wt% of silica with additive of 2% PVA which determined and analysed comparatively for their
act as binder. Mix powder press in steel die (1.5cm) by values. The bulk density of the composite
hydraulic pressure at 15tonn/sq. inch, for making continuously increases with increased silica content
powder in pellet form, all pellets pressed at constant which are listed below.
rate of load as 1 minute time (holding time).
Table 2.Bulk Density of Different Samples
These pellets are sintered at a temperature of 1200°C. Sample No. Bulk density (gm/cc)
Fired at required temperature with shocking time 1 1.61
period of 30 min. measured weight loss, linear 2 1.71
shrinkage properly using veneer scale before and after 3 1.85
sintering. Determine the behaviour of bulk density,
weight losses, linear shrinkage, and apparent porosity

Figure 1.Bulk Density vs. Silica wt%

Measurement of Apparent Porosity Table 2.Apparent porosity of different samples


Sample No. Apparent porosity (%)
Apparent porosity of all sintered samples is 1 19.03
determined and analysed comparatively for their 2 10.62
values. The apparent porosity of the composite 3 6.84
continuously increases with decrease bulk density.
The apparent porosity of the composite continuously A graph plotted between bulk density values with
decreases with increased silica content which are increasing silica composition which is given below:
listed below:

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Majhi MR et al. J. Adv. Res. Glass Leath. Plast. Tech. 2017; 2(1&2)

20
18
16
14
12
Apparent porosity10
(in %) 8
6
4
2
0
Silica 0% Silica 2% Silica 4%

Figure 2.Apparent Porosity vs. silica %

The densification of Alumina zirconia silica composite decreased porosity and improved densification of the
material was confirmed, apparent porosity decreased Alumina zirconia silica composite material.
with the increase of silica content but bulk density
increases. Increased densification with increased silica Weight Loss Calculation
due to the presence of discrete secondary zirconia
phase. Retarded grain growth did not allow pores to Weights of all samples are taken before and after
become trapped within the grains. As a result the sintering, hence giving the percentage of weight loss
pores did not grow in size but were eliminated from in different compositions which are given below in
the surface of the grains. This phenomenon led to table.
Table 3.Weight loss Percentage
Sample no. Initial weight Final weight Weight loss %
Batch 1 1 4.503 4.074 9.53
2 5.137 4.654 9.402
Batch 2 1 3.247 2.994 7.79
2 4.125 3.935 4.606
Batch 3 1 3.199 3.026 5.408
2 3.796 3.684 2.95

Linear Shrinkage Measurement show shrinkage behaviour after sintering because of


moisture elimination which was earlier present in
Linear dimensions such as length, width, thickness are green body. Different samples of different batch are
taken before and after sintering. These dimensions dimensionally measured which are obtained as given
below:
Table 4.Linear Shrinkage Percentage
Sample no. Initial final Shrinkage (%)
1 Length 41.41 40.6 1.96
Width 10.58 10.41 1.61
Thickness 6.1 6.02 1.31
2 Length 41.41 40.77 1.55
Width 10.58 10.42 1.51
Thickness 4.31 4.26 1.16
3 Length 41.41 40.84 1.38
Width 10.58 10.45 1.23
Thickness 5.07 5.02 0.99

It is found that Shrinkage values for linear dimensions material. The above tabulated values of shrinkage
decrease on increasing silica value in the composite values graphically represented as below:

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J. Adv. Res. Glass Leath. Plast. Tech. 2017; 2(1&2) Majhi MR et al.

2.5

1.5
Length Shrinkage
%

Width Shrinkage % 1

Thickness
Shrinkage %
0.5

0
Sample No. 1 Sample No 2 Sample No 3

Figure 3.Shrinkage Percentage Values of Different Samples

XRD Analysis the XRD pattern of base composition sintered powder.


Powder X-ray diffraction pattern of the sample show
XRD Analysis of Base Composition different phases that is because of converting ZrO2
into tetragonal form (t) and there is also a small peak
Powder X-ray diffraction patterns are carried out for of monoclinic (m) phase is present in the graph. The
all compositions using ‘Rigaku High Resolution Powder ZrO2 is stabilized because of alumina presence in
X-ray Diffractometer’ with Cu Kα1 radiation and Ni- composition. All peaks of Zirconium Aluminium oxide
filter is employed at room temperature. Fig. shows phase is matched with JCPDS file no. 820494.

Figure 4.XRD Pattern of Base Composition (Alumina Zirconia Composite)

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Majhi MR et al. J. Adv. Res. Glass Leath. Plast. Tech. 2017; 2(1&2)

The pattern shows no any residual alumina phase. The XRD Analysis after 2% and 4% Silica Addition
XRD patterns were recorded in the 2- theta range of
10-80 degree. It is seen that some unreacted SiO2 remains in the
samples as residual form fired at relatively lower
temperatures such as 1200°C, since there is no
reaction taken place with silica.

Figure 5.XRD Pattern with Silica Addition

But it gives the scope for further phase formation at point bending set up which are tabulated as below:
higher temperature range with increasing values of
silica content. In present case phases remains same as Table 5.Bending Strength Values for Different Samples
obtained earlier. The XRD pattern does not change Sample No. Bending Strength (MPa)
with slight change of silica addition as from 2% to 4% 1 59.51
in base composition of Alumina Zirconia Composite 2 205.60
material; however it enhances the mechanical 3 232.62
properties as seen previously. The XRD pattern with
silica addition is shown in Fig. 5. These bending strength shows increment in their
values with increasing silica value in their
Modulus of Rupture/ Flexural Strength composition. This is because of the fact that silica
content increases mechanical behaviour of base
Flexural strength or bending strength of different composition that is Alumina zirconia composite.
samples of different batch are calculated from three
70

60 59.62

50 51.6

Bendin 40
39.51
g
Strengt
h 30
(MPa)

20

10

0
0 2 4
Silica %
Figure 6.Bending Strength vs. Silica Composition at 1200°C

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J. Adv. Res. Glass Leath. Plast. Tech. 2017; 2(1&2) Majhi MR et al.

Hence, higher densification with increased silica From sample 1 to 3 due to densification and decrease
content helps in improving bending strength of in porosity value more uniform matrix of the
Alumina Zirconia Silica composite material. Variation composite material is obtained. It gives clear
in bending strength has shown graphically as above. indication of improvement in mechanical properties
such as bending strength because of improved
Microstructure Characterization bonding between the matrixes which is lesser in base
composition of alumina zirconia composite. It clearly
The microstructure of Alumina zirconia silica shows changes in its microstructure by following
composite has been examined for each batch graphs:
composition with slight increment of silica content.

Figure 7.Microstructure in Alumina Zirconia Silica Composite

This microscopy can be utilized in finding the length of The bulk density of the composite material increase
required phase or voids. Some of the lengths with increase the silica percentage in base
measured in each samples are obtained as below: composition of alumina zirconia composite material.
Apparent porosity decreases with increasing silica
Table 6.Micro Measurement Data in Different Samples percentage because of retarded grain growth which
Measurement Name Sample No. Length (Micron) does not allow pores to become trapped within the
L1 1 3.530 grains. As a result, the pores do not grow in size and
2 3.046 are also eliminated from the surface of the grains.
3 1.857 Percentage linear shrinkage decreases with increasing
L2 1 6.746 silica content. There is slight weight reduction of every
2 1.732 sample after sintering at 1200°C. From the XRD
3 2.716 analysis, it is confirmed that different phases are
L3 1 1.500 developed after sintering. Strength of the material
2 3.267 increases with increasing silica content. Bending
3 3.233 strength of base composition i.e. alumina zirconia
L4 1 26.072 composite is low when there is no presence of silica
2 3.775 content in it. Microstructure comparisons of different
3 0.866 samples clearly identify the improved physical and
mechanical properties.
Conclusions References
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