1. Process Control Using FT-IR Analysis of BaTiO3 from Ultrasonically Activated BaCO3 And TiO2
Hatice Zehra AKBAS
Department of Physics, Faculty of Science and Letters, Mustafa Kemal University, Hatay
Zeki AYDIN
Ismail Hakkı KARAHAN
Department of Chemistry, Faculty of Science and Letters, Mustafa Kemal University, Hatay
Tuncay DILSIZOGLU
Selvin TURGUT
MARGEM, Mustafa Kemal University, Hatay
 (corresponding author)

2. INTRODUCTION
BaTiO3 powders are particularly important family of the functional lead-free ceramics.
The powders have been using many electronic applications.
The commercial powders have about 1 μm particle size.
The decreasing grain size of the powders is required to achieve dense ceramics.
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
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3. INTRODUCTION
Therefore, the methods of decreasing BaTiO3 powders size have been attracting because of their application in fundamental research.
High-intensity ultrasonic waves (ultrasonication) are one of the advanced processes to obtain a sub-micron size of powders.
Ultrasonication is not only de-agglomerating the powders but also activating them in liquid..
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4. AIMS The aims of this work are using FT-IR spectrum:
to control the formation of barium titanate ceramic from BaCO3 and TiO2 powders by the solid-state reaction that modified using an ultrasonic method,
to investigate BaCO3 impurities in BaTiO3,
the effects of ultrasonication on lattice dynamics properties of BaTiO3 in different mediums (de-ionized water and acetone)
4) the effects of ultrasonication times on lattice dynamics properties of BaTiO3
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5. Ultrasonication High-intensity ultrasonic processor UP200S
- Hielscher Ultrasonics GmbH, Germany
Power : 200W
Frequency : 24kHz
Sonotrode diameter : 40 mm
Working mode : Continues (Cycle : 1)
Time : 5 minutes
30 minutes
The powders were mixed in deionized water and acetone.
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
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6. Ultrasonic processor http://www.hielscher.com, 31.08.2014.
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
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7. Heating and cooling rates in this processes is about 1010 K/s.
Collapsing bubbles produces mikro/nano dots with local high temperatures (roughly 5000 K) and intense pressure (roughly 1000 atm),
Heating and cooling rates in this processes is about 1010 K/s.
As a result, it has enough energy to activate and to de-agglomerate the grains.
Suslick, K. S. et al. Phil. Trans. R. Soc. Lond. A 357, (1999).
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
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8. Structural analysis:
After ultrasonication, the powder mixtures were dried and heated at 1100 °C for 4 hours in alumina crucibles.
Fourier Transform Infrared Spectroscopy (FT-IR) (Shimadzu, IRAffinity-1S, Japon) was confirmed the structure of the powders in the range of cm-1.
Grapher 11 (Golden Software, US) software program used to analyze the dataset.
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
October 26-28, 2016

9. RESULTS AND DISCUSSION
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10. FT-IR patterns of the powders
BaCO3
TiO2
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11. BaTiO3 with different homogenization time
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12. BaTiO3 with two different liquids medium
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13. BaTiO3 with different homogenization time in two different liquids medium
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14. FT-IR results : BaCO3 (Alfa Aesar) TiO2 BaTiO3 Bound Alfa Aesar
40mm 30m
Water
40mm 5m
Acetone
420
430
460 , 500, 530, 560
585, 695
470 -
Fingerprint of BaCO3
555, 600,
675
559, 597, 649
559 , 597,
649
559 ,597,
Fingerprint of
Ti-O-Ti and
Ti-O
855
C-C
1060
1050 or
C-O
1420
s [COO-]
1426
1460
O-H
1650
1673
C=O
1750
as [COO-]
2360
Ti-O or
O=C=O
2358
2315
2980
3000
3700
FT-IR results :
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15. CONCLUSION
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16. FT-IR analysis can determine free or bound BaCO3 impurities in BaTiO3.
BaTiO3 from BaCO3 and TiO2 powders can be prepared by the solid-state reaction with short homogenization time using high intense ultrasonic waves.
Ultrasonication mediums and times were changed the lattice dynamics properties of BaTiO3.
The formation of barium titanate ceramic from BaCO3 and TiO2 powders by the solid-state reaction can be controlled using FT-IR spectrum.
FT-IR analysis can determine free or bound BaCO3 impurities in BaTiO3.
Free BaCO3 impurities in BaTiO3 could not find after ultrasonication.
IMSEC 2016:1st International Mediterranean Science and Engineering Congress
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17. REFERENCES
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18. [1]. Koziej, D. , Lauria, A. and Niederberger, M
[1] Koziej, D., Lauria, A. and Niederberger, M. (2014) 25th Anniversary article: Metal oxide particles in materials science: Addressing all length scales. Advanced Materials, 26, 235–57.
[2] Potong, R., Rianyoi, R., Ngamjarurojana, A., Yimnirun, R., Guo, R., Bhalla, A.S. et al. (2013) Effect of Particle Size on Dielectric Properties and Hysteresis Behavior of 0-3 Barium Zirconate Titanate-Portland Cement Composites. Integrated Ferroelectrics, 148, 131–7.
[3] Reddy, Y.K.V. (2006) Synthesis and characterization of BaTiO 3 and SrTiO 3 thin film capacitors with RuO 2 electrodes.
[4] Kim, J. (2002) Synthesis of porous (Ba, Sr) TiO 3 ceramics and PTCR characteristics. Materials Chemistry and Physics, 78, 154–9.
[5] Roy, A.K., Prasad, K. and Prasad, A. (2013) Piezoelectric, impedance, electric modulus and AC conductivity studies on (Bi0.5Na0.5)0.95Ba0.05TiO3 ceramic. Processing and Application of Ceramics, 7, 81–91.
[6] Suslick, K.S., Didenko, Y., Fang, M.M., Hyeon, T., Kolbeck, K.J., McNamara III, W.B. et al. (1999) Acoustic cavitation and its chemical consequences. Philosophical Transactions of the Royal Society A, 357, 335–53.
[7] Ashokkumar, M. (2011) The characterization of acoustic cavitation bubbles–an overview. Ultrasonics Sonochemistry, 18, 864–72.
[8] Ashokkumar, M., Lee, J., Kentish, S. and Grieser, F. (2007) Bubbles in an acoustic field: an overview. Ultrasonics Sonochemistry, 14, 470–5.
[9] Marković, S., Mitrić, M., Starcević, G. and Uskoković, D. (2008) Ultrasonic de-agglomeration of barium titanate powder. Ultrasonics Sonochemistry, 15, 16–20.
[10] Marković, S., Miljković, M., Jovalekić, Č., Mentus, S. and Uskoković, D. (2009) Densification, Microstructure, and Electrical Properties of BaTiO 3 (BT) Ceramics Prepared from Ultrasonically De-Agglomerated BT Powders. Materials and Manufacturing Processes, Taylor & Francis Group. 24, 1114–23.
[11] Alavi, M. and Morsali, A. (2008) Syntheses of BaCO 3 nanostructures by ultrasonic method. Ultrasonics Sonochemistry, 15, 833–8.
[12] Infrared spectroscopy correlation table [ Spectroscopic_Parameters/Infrared_Spectroscopy_Absorption_Table].
[13] Infrared Spectroscopy Absorption Table [ _correlation_table].
[14] Trivedi, M., Nayak, G., Patil, S., Tallapragada, R. and Latiyal. (2015) Impact of Biofield Treatment on Atomic and Structural Characteristics of Barium Titanate Powder. Industrial Engineering & Management, 4.
[15] Ashiri, R. (2013) Detailed FT-IR spectroscopy characterization and thermal analysis of synthesis of barium titanate nanoscale particles through a newly developed process. Vibrational Spectroscopy, 66, 24–9.
[16] Kuruva, P., Rajaputra, U.M.S., Sanyadanam, S. and Sarabu, R.M. (2013) Effect of microwave sintering on grain size and dielectric properties of barium titanate. Turkish Journal of Physics, 37, 312–21.
[17] Deshmane, V.G. and Adewuyi, Y.G. (2012) Synthesis of thermally stable, high surface area, nanocrystalline mesoporous tetragonal zirconium dioxide (ZrO2): Effects of different process parameters. Microporous and Mesoporous Materials, Elsevier Inc. 148, 88–100.
[18] Ferreira, J.M.F., Olhero, S.M. and Kaushal, A. (2013) Is the ubiquitous presence of barium carbonate responsible for the poor aqueous processing ability of barium titanate? Journal of the European Ceramic Society, 33, 2509–17.
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19. Acknowledgement
This work is supported by grant 114F393 from The Scientific and Technological Research Council of Turkey (TÜBİTAK).
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20. THANK YOU FOR YOUR ATTENTION ANY QUESTION
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