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Starting with the Name of ALLAH the

most merciful and mighty


M.phil Physics Synopsis
Preparation and microwave dielectric properties of
(1-x)Mg0.95Ni0.05Ti0.98Zr0.02O3 -xCaTiO3
Ceramics
Submitted by:
Asif Nawaz Khan
Registeration No: 9544-B-2003
CESET Islamabad: Session 2013 - 2015

Research supervisor:
Prof Dr. Ehsan Ullah Khan (Ex- professor CESET Islamabad)

Research Co-Supervisor:
Dr. Abdul Manan (Assistant professor University of Science & Technology Bannu)
INTRODUCTION:
Dielectric ceramics have been studied extensively and employed in the
microwave devices applications as dielectric resonators, dielectric filters,
dielectric antennas etc. [1]
for example Wireless communication is driven by the unique dielectric properties
of ceramics.
These properties includes:
i. High dielectric constant (ɛr) for reducing the size of devices.
ii. High unloaded quality factor multiplied by the resonant frequency (Qufo) or
low loss for selectivity.
iii. Near zero temperature coefficient of resonant frequency (τf) for stability of
the resonant frequency [2].
The utilized frequency range has been increased from 900 MHz to 2.4, 5.2 or
even to 5.8 GHz due to occupation of Low frequency bands. Therefore, low
dielectric constant materials are needed for applications at these high frequencies
[3].
There are many materials with complex structure is investigated for high
frequencies applications [4-8]. For example
Ba(Zn1/3Ta2/3)O3 and Ba(Mg1/3Ta2/3)O3 showed the highest Qufo values ranging
from 105 GHz to about 2x105 GHz [9,10] but these materials contain tantalum
which is very expensive and required high sintering temperature (1600-1650 oC)
require long time about 50hrs to obtain optimum densities.
Similarly MgTiO3 is one of the low cost material having ɛr =17,
Qufo~ 16x104 GHz and a τf ~ -50 ppm/⁰C [10].
The Qufo of MgTiO3 has been improved by various cationic substitutions at the A
and B site causing local lattice distortion, which is greater than the effect of
impurity in MgTiO3.
By partial replacement of Mg by Ni Co, Mn, Zn, at the A-site results in
improvement in the Qufo value (1.8x105-2.64x105 GHz) of pure MgTiO3 [11, 12]
for example Ni based MgTiO3 i.e. Mg0.95Ni0.05TiO3 possess excellent microwave
dielectric properties with ɛr ~17.2, Qufo~1.8x105 GHz and τf ~ -45 ppm/oC [13].
However, the high negative value of τf makes Mg0.95Ni0.05TiO3 impractical for
applications.
. To makes it feasible, it is required to tune the τf through zero by either suitable
cationic substitution or mixing with materials having high positive τf .
There are may material which have studied to get the required result are:

i. Mixing of Nd0.5Na0.5TiO3 with Mg0.95Ni0.05TiO3 i.e 0.81Mg0.95Ni0.05TiO3-


0.19Nd0.5Na0.5TiO3 ceramics results in ɛr ~25.61, Qufo ~ 6.9x104 GHz, and a τf ~ -
6 ppm/oC [14].

ii. Similarly with the addition of La0.5Na0.5TiO3 to Mg0.95Ni0.05TiO3 i.e


0.87Mg0.95Ni0.05TiO3–0.13La0.5Na0.5TiO3 results in to ɛr ~ 23.22, a Qufo ~ 8.6x104
GHz, and a τf ~ 2.8 ppm/°C sintered at 1275°C for 4 h [15].
iii. Shen et al. reported ɛr~22.9, Qufo~ 9.2x104 GHz, τf ~ −5.4 ppm/°C for
0.9Mg0.95Ni0.05TiO3–0.1Ca0.8Sm0.4/3TiO3 ceramics sintered at 1275 °C for 4 h
[16].

iv. Manan et al. partially substituted Zr for Ti and reported ɛr ~17, Qufo~195000
GHz and τf ~ -46 ppm/oC for Mg0.95Ni0.05Ti0.98Zr0.02O3 [17]. However, the high
negative value of τf makes Mg0.95Ni0.05Ti0.98Zr0.02O3 impractical for applications.

V. Similarly addition of SrTiO3 to the Mg0.95Ni0.05Ti0.98Zr0.02O3 i.e 0.04SrTiO3-


0.96Mg0.95Ni0.05Ti0.98Zr0.02O3 results in to ɛr ~ 20, Qufo ~ 8.5x104 GHz and τf ~3
ppm/oC [18].
The material which we have selected for our reaserch work is CaTiO3 having εr ∼
170, Qufo value ∼ 3600 GHz at 7 GHz and τf ∼ + 800 ppm/◦C) [19].
Research Plan:
The research project will be completed in three phases

Phase.1: In this phase, literature review for the project will be carried out.

Phase.2: In this phase, the desired compositions will be prepared and analyzed
using various techniques, mentioned earlier.

Phase.3: In this phase the data will be published in a peer-reviewed international


Journal of Physics or Materials Science and the data will finally be gathered in the
form of thesis
Methodology:
1.Both Mg0.95Ni0.05Ti0.98Zr0.02O3 and CaTiO3 ceramics will be prepared
separately.
2. High purity raw materials of TiO2, NiO, MgO, ZrO and CaCO3 in
stoichiometry ratios will be weighted and mixed.
3. The mixtures for the preparation of both the ceramics will be ball
milled for 10h using ZrO2 ball as grinding media and isopropanol as
lubricant to make fine freely moving slurries.
4. The slurries will be dried over-night in an oven ~95oC which will be
followed by sieving to get fine powders.
5. The mixed and milled powders will be calcined at 1100⁰C studied in
a literature at heating/cooling rate of 5⁰C/min for 5h.
6. The calcined powders will be re-milled to dissociate the agglomerates if any.
7. The calcined reagents will be mixed in the desired composition of (1-
x)(Mg0.95Ni0.05Ti0.98Zr0.02O3-x CaTiO3 (x =0, 0.05, 0.10, 0.15, 0.2) and ground
into fine powders for 1and half hours.
8. The finely grounded calcined powders will be pressed into pellets and sintered
in a range of temperature i.e. 1300oC to 1400oC to get optimum dense samples.
9. The Phase analyses of the calcined and sintered samples will be carried out
using XRD.
10. Microstructure of the optimum dense samples will be investigated using

scanning electron microscope (SEM).


11. The microwave dielectric properties will be measured using vector network
analyzer.

References:
[1]. M.T. Sebastian “Dielectric Materials for Wireless Communication” 1st
Edition, Elsevier Science, 2008.
[2] I. M. Reaney, D. Iddles, J. Am. Ceram. Soc., 89 [7], 2063 (2006).
[3] C.L. Huang, S. S. Liu, J. Alloys. Compds., 471, L9 (2009.
[4] H. Tamura, T. Konoike, Y. Sakabe, K. Wakino, J. Am. Ceram. Soc., 67,
C59 (1984).
[5] S. Nomura, K. Kaneta, Jpn. J. Appl. Phys., 33, 507 (1984).
[6] M. Onada, J. Kuwata, K. Kaneta, K. Toyama, and S. Nomura, Jpn. J. App.
Phys., 21[12], 1707 (1982).
[7] B.K. Kim, H. Hamaguchi, I.T. Kim, K.S. Hong, J. Am. Ceram. Soc., 78, 3117
(1995).
[8] I. M. Reaney, I. Qazi, and W. E. Lee, J. Appl. Phys., 88[11], 6708 (2000).
[9] L. Chai, M.A. Akbas, P.K. Davies, and J.B. Parise, Mat. Res. Bull., 33, 1261
(1998).
[10] K. Wakino, Ferroelectrics., 91, 69(1989).
[11] E. S. Kim, C. J. Jeon, J. Euro. Ceram. Soc., 30, 341 (2010).
[12] C.L. Huang, S. S. Liu, Jpn. J. Appl. Phys., 46 [1], 283 (2007).
[13] J. H. Sohn, Y. Inaguma, S. O. Yoon, M. Itoh, T. Nakamura, S. J. Yoon,
H. J. Kim, Jpn. J. Appl. Phys., 33[9B], 5466 (1994).
[14] C. H. Shen, C. L. Huang, C. F. Shih, C. M Huang, Curr. Appl. Phys, 9 [5],
1042 (2009).
[15] C. H. Shen, C. L. Huang, C. F. Shih, C. M Huang, Int. J. Appl. Ceram.
Technol., 7 [S1], E64 (2010).
[16] C. H. Shen, C. L. Huang, J. Alloys. Compds., 477, 720 (2009).
[17] A. Manan, D. N. khan, A. Ullah, A. S. Ahmad, Mater. Sci. Pol., 33, 95
(2015).
[18] A. Manan, D. N. khan, A. Ullah, J. Mater. Sci: Mater Elect., 26, 2066
(2015).
[19] A Pashkin, S Kamba, M Berta, J Petzelt, G D C Csete de Gyorgyfalva, H
Zheng, H. Bagshaw, I. M. Reaney, J. Phys. D: Appl. Phys.,38, 741 (2005).
[20] J. Li T. Qiu, Intern. J. Miner. Metall. Mater., 19, 2045 (2012).
Thanks

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