Pechini sol gel method for the synthesis of titanates

Cesium and sodium titanates with the respective stoichiometries of CsxTi2-x/4□x/4O4 (x ≈ 0.7) and Na2Ti6O13 was synthesized by making use of the Pechini sol-gel method. The subsequent direct intercalation of hydrazine hydrate in both cesium and sodium titanates proved unsuccessful while direct intercalation of ammonium into cesium titanate was achieved. The protonated form of cesium titanate was successfully intercalated with hydrazine hydrate. X-ray diffraction (XRD) results of the synthesised hydrazinium and ammonium titanate showed a high degree of peak correlation when compared with each other. Thermogravimetric (TG) analysis showed the thermal release and potential decomposition of hydrazinium titanate to be at a lower temperature than reported by Britvin, et al. [1]. Raman analysis of the nitrogen derivative titanates showed a significant difference in obtained spectra. Density functional theory (DFT) calculations showed correlation with the observed Raman vibrations.

本研究采用佩奇尼溶胶-凝胶法（Pechini sol-gel method）合成了化学计量比分别为CsₓTi₂₋ₓ/₄□ₓ/₄O₄（x≈0.7）与Na₂Ti₆O₁₃的铯钛酸盐与钠钛酸盐。后续针对两种钛酸盐直接插层水合肼的实验均未获得成功，而将铵根直接插层至铯钛酸盐中的实验取得了成功。质子化铯钛酸盐可顺利与水合肼完成插层反应。X射线衍射（X-ray diffraction, XRD）测试结果显示，所合成的肼基钛酸盐与铵基钛酸盐的衍射峰具有高度相关性。热重分析（Thermogravimetric, TG）结果表明，肼基钛酸盐的热释放与潜在分解温度低于Britvin等人[1]的已有报道。对两类含氮衍生物钛酸盐的拉曼光谱分析显示，所得光谱存在显著差异。密度泛函理论（Density Functional Theory, DFT）计算结果与实验观测到的拉曼振动峰具有良好匹配性。