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  hatice-akbas@windowslive.com (corresponding author)

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 October 26-28, 2016

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.. IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

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 IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

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 October 26-28, 2016

Ultrasonic processor http://www.hielscher.com, 31.08.2014. IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

Heating and cooling rates in this processes is about 1010 K/s. http://www.food.hacettepe.edu.tr/turkish/ouyeleri/gmu809/Ultrason%2012.pdf, 28.02.2014. http://www.variclean.eu/site/theory-ultrasonic-technology, 28.02.2014. 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. http://www.variclean.eu/site/theory-ultrasonic-technology, 28.02.2014. Suslick, K. S. et al. Phil. Trans. R. Soc. Lond. A 357, 335-353 (1999). http://www.hielscher.com, 31.08.2014. IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

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 400-4000 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

RESULTS AND DISCUSSION IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

FT-IR patterns of the powders BaCO3 TiO2 IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016 10

BaTiO3 with different homogenization time IMSEC 2016:1st International Mediterranean Science and Engineering Congress 11 October 26-28, 2016

BaTiO3 with two different liquids medium IMSEC 2016:1st International Mediterranean Science and Engineering Congress 12 October 26-28, 2016

BaTiO3 with different homogenization time in two different liquids medium IMSEC 2016:1st International Mediterranean Science and Engineering Congress 13 October 26-28, 2016

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 2905 2973 2980 3000 3700 FT-IR results : IMSEC 2016:1st International Mediterranean Science and Engineering Congress 14 October 26-28, 2016

CONCLUSION IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

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 October 26-28, 2016

REFERENCES IMSEC 2016:1st International Mediterranean Science and Engineering Congress October 26-28, 2016

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Acknowledgement This work is supported by grant 114F393 from The Scientific and Technological Research Council of Turkey (TÜBİTAK). October 26-28, 2016 IMSEC 2016:1st International Mediterranean Science and Engineering Congress

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