Abstract

Titanium oxide nanoparticles are synthesized in a molten mixture of alkali chlorides and nitrates. X-ray diffraction analysis, Raman spectroscopy, and scanning electron microscopy are used to identify the oxide powders. Titanium oxides of various modifications and compositions are synthesized by anodic polarization of high-purity titanium in a molten eutectic mixture of cesium and sodium chlorides containing 5 wt % sodium nitrate. Polarization is carried out under galvanostatic conditions at a current density of 3.5 mA/cm² and a temperature of 540–700°C in an argon atmosphere. The phase composition of the oxidation products depends on the synthesis temperature. The particle size is controlled by varying the density and temperature. X-ray diffraction analysis and Raman spectroscopy show that the sample synthesized at a temperature of 540°C is single-phase and consists of Cs_1.36Ti_6.64O₁₆. The samples synthesized at temperatures of 600 and 650°C form the TiO₂ phase in mixed anatase and rutile modifications. The sample synthesized at a temperature of 700°C consists of TiO₂ titanium dioxide (rutile and brookite modification) and NaTi₈O₁₃. According to scanning electron microscopy, the particle size decreases when the synthesis temperature increases. The sample synthesized at a temperature of 540°C and annealed at a temperature of 200°C contains a mixture of the nano- and microparticles of cesium trititanate (over 50 nm). The titanium dioxide particle size is 20 nm in the sample synthesized at a temperature of 600°C and is 10–20 nm in the samples synthesized at temperatures of 650 and 700°C.

中文翻译：

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在碱金属氯化物和硝酸盐的熔融混合物中电化学合成氧化钛纳米粉末

摘要

氧化钛纳米颗粒是在碱金属氯化物和硝酸盐的熔融混合物中合成的。X 射线衍射分析、拉曼光谱和扫描电子显微镜用于鉴定氧化物粉末。通过在含有 5% 硝酸钠的氯化铯和氯化钠的熔融共晶混合物中对高纯度钛进行阳极极化来合成各种变型和组成的氧化钛。极化在恒电流条件下以 3.5 mA/cm ²的电流密度进行在氩气气氛中温度为 540–700°C。氧化产物的相组成取决于合成温度。通过改变密度和温度来控制粒度。X 射线衍射分析和拉曼光谱表明，在 540°C 温度下合成的样品是单相的，由 Cs _1.36 Ti _6.64 O _{16 组成}。在 600 和 650°C 的温度下合成的样品形成混合锐钛矿和金红石改性的 TiO ₂相。在 700°C 温度下合成的样品由 TiO ₂二氧化钛（金红石和板钛矿改性）和 NaTi ₈ O _{13 组成}. 根据扫描电子显微镜，当合成温度升高时，粒径减小。在 540°C 的温度下合成并在 200°C 的温度下退火的样品包含三钛酸铯（超过 50 nm）的纳米颗粒和微粒的混合物。在 600°C 温度下合成的样品中二氧化钛粒径为 20 nm，在 650 和 700°C 温度下合成的样品中二氧化钛粒径为 10–20 nm。