Application of Statistical Design to Optimize the Preparation of Barium Titanate Nanopowders via Oxalate Precursor Method

M.M. Rashad1, R.S. Mohammed1, A.A. El-Midany1, A.T. Kandil2 and I.A. Ibrahim1

1Central Metallurgical Research and Development Institute, P.O. Box: 87 Helwan, 11421 Cairo, Egypt

2Inorganic & Nuclear Chemistry Dept., Faculty of Science, Helwan University, Cairo, Egypt

Abstract

Nanocrystalline barium titanate (BaTiO3) powders have been synthesized by oxalate precursor method. Statistical design (Box-Behnken) is used to study the effect of main three parameters: calcination temperature (800-1200C), calcination time (0.5-4 hrs), and oxalic acid mole ratio (0.5-1.5) related to barium and titanium added at constant Ba/Ti mole ratio 1 on the formation of BT powders. Barium titanate particles were characterized using X-ray diffraction (XRD), and scanning electron microscope (SEM). The statistical design showed that conversion of barium titanate increases by decreasing the oxalic acid mole ratio and decreasing the calcination temperature and calcination time. XRD showed that single phase of barium titanate is formed at calcination temperature starting from 800C, oxalic acid mole ratio 0.5 and calcination time 2.25 hrs. The average crystallite sizes at different conditions are in the range between 36 to 91 nm. SEM micrographs showed that the produced pure BT nanopowders were formed in the tetragonal structure shape.