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Synthesis and characteristics of near-stoichiometric barium titanate powder by low temperature hydrothermal reaction using titanium tetra(methoxyethoxide)

机译:四(甲氧基乙醇)钛的低温水热反应合成接近化学计量的钛酸钡粉末

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摘要

Near-stoichiometric BaTiO_(3) powders with ultrafine particle size and high crystallinity were prepared by low temperature hydrothermal reaction of Ba(OAc)_(2) and Ti(OCH_(2)CH_(2)OCH_(3))_(4). BaTiO_(3) particles were synthesized in the spherical, metastable cubic crystalline grains with size distribution between 60-90 nm in diameter. Ultrafine particle size was resulted from the control of the hydration rate and the decrease of Ti-O-Ti cross-linking extent of titanium precursor, Ti(OCH_(2)CH_(2)OCH_(3))_(4), which gives electronic, steric, and weakly chelating effect to titanium ion. Increasing the Ba/Ti mole ratio in reactant could not overcome the notorious Ba-deficiency but, improved stoichiometry and produced finer and less agglomerated particles. Interestingly, adding a slight pressure to autogeneous hydrothermal condition (total 4-10 atm) has yielded near-stoichiometric, highly crystalline, and less agglomerated BaTiO_(3) particles. These particles, which were in metastable cubic form as synthesized, initiated phasetransition to tetragonal form by calcination at below 400℃.
机译:通过Ba(OAc)_(2)和Ti(OCH_(2)CH_(2)OCH_(3))_(4)的低温水热反应制备了具有超细粒径和高结晶度的近化学计量BaTiO_(3)粉末)。 BaTiO_(3)颗粒是在球形,亚稳态立方晶粒中合成的,其晶粒直径分布在60-90 nm之间。通过控制水合速率和降低钛前体Ti(OCH_(2)CH_(2)OCH_(3))_(4)的Ti-O-Ti交联程度来获得超细粒径对钛离子产生电子,空间和弱螯合作用。提高反应物中的Ba / Ti摩尔比不能克服臭名昭著的Ba缺乏症,但可以提高化学计量比并产生更细和更少的团聚颗粒。有趣的是,对自生水热条件(总压力为4-10 atm)施加较小的压力已产生接近化学计量的,高度结晶的和较少聚集的BaTiO_(3)颗粒。这些在合成时呈亚稳态立方形式的颗粒通过在400℃以下的煅烧引发相转变为四方形式。

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