摘要：本实验使用阳极氧化法制备Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜，研究阳极氧化工艺（电流密度、温度、氨水浓度、时间、Gd3+、Ni2+、Ca2+离子浓度）对制备Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜厚度的影响，Gd3+、Ni2+、Ca2+浓度与温度对阳极氧化法制备Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜电导率的影响，Gd3+、Ni2+、Ca2+浓度对Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜成分的影响，热处理温度对Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜晶型结构和IR谱图的影响，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜的形貌分析。结果表明，制备该膜较佳的实验条件为电流密度为0.5mA/cm2，温度为26℃，氨水浓度选择2.510mol/L，阳极氧化时间选择8h。在上述的较佳实验条件下当Gd3+浓度为4.4879mmol/L时，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜厚度达到最大值29.8μm，并且温度为600℃，达到最高电导率为1.12×10-2S/cm；当Ni2+浓度为3.4080mmol/L时，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜厚度达到最大值29.3μm，并且温度为600℃，达到最高电导率为2.03×10-2S/cm；当Ca2+浓度为3.8845mmol/L时，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜厚度达到最大值21.9μm，并且温度为600℃，达到最高电导率为2.23×10-2S/cm。成分分析结果表明该膜为Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜，电解液中随着Gd3+、Ni2+、Ca2+浓度的增大，膜上相对应的Gd3+、Ni2+、Ca2+含量也会增大。经过200℃，300℃和400℃热处理后晶型结构为立方萤石结构，温度到达600℃时，晶型结构更完整，25℃的IR谱图表明，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜的表面仍然吸附着水和乙二醇，300℃以上高温处理后IR谱图只有氧化铈的吸收峰，乙二醇和水脱附完全，Gd3+/ Ni2+/ Ca2+共掺杂氧化铈膜的微观形貌为多孔结构。

关键词：CeO2薄膜 共掺杂 阳极氧化

Study on Properties of Erbium, Nickel and Calcium Codoped Oxide Films

Abstract: In this experiment, Gd3+/Ni2+/Ca2+ cooped yttrium oxide film was prepared by anodic oxidation, and the anodization process (current density, temperature, ammonia concentration, time, Gd3+, Ni2+, Ca2+ concentration) was studied to prepare Gd3+/Ni2+/Ca2+ Effect of doped yttrium oxide film thickness, Gd3+, Ni2+, Ca2+ concentration and temperature on the conductivity of Gd3+/Ni2+/Ca2+ co-doped yttrium oxide film prepared by anodic oxidation, Gd3+, Ni2+, Ca2+ concentration versus Gd3+/Ni2+/Ca2+ Effects of co-doped yttrium oxide film composition, heat treatment temperature on crystal structure and IR spectrum of Gd3+/Ni2+/Ca2+ co-doped yttrium oxide film, morphology analysis of Gd3+/Ni2+/Ca2+co-doped yttrium oxide film. The results showed that the optimal experimental conditions for the preparation of the membrane were the case that the current density was 0.5mA/cm2, the temperature was 26°C, the ammonia concentration was 2.510mol/L, and the anodizing time was 8h. Under the above optimal experimental conditions, the Gd3+/Ni2+/Ca2+cooped yttrium oxide film thickness reached a maximum of 29.8 μm when the Gd3+ concentration was 4.4879 mmol/L, and the temperature was 600°C, reaching a maximum conductivity of 1.12×10-2S/cm; when Ni2+ concentration is 3.4080mmol/L, the thickness of Gd3+/Ni2+/Ca2+ co-doped yttrium oxide film reaches a maximum of 29.3μm, and the temperature is 600°C, reaching a maximum conductivity of 2.03×10-2S/ cm; when Ca2+ concentration is 3.8845mmol/L, the thickness of Gd3+/Ni2+/Ca2+cooped yttrium oxide film reaches a maximum of 21.9μm, and the temperature is 600°C, and the maximum conductivity is 2.23×10-2S/cm. The results of compositional analysis indicate that the film is a Gd3+/Ni2+/Ca2+ cooped yttrium oxide film. With increasing concentrations of Gd3+, Ni2+, and Ca2+ in the electrolyte, the corresponding Gd3+, Ni2+, and Ca2+ contents on the film will expand. The crystal structure after heat treatment at 200°C, 300°C and 400°C is cubic fluorite structure. When the temperature reaches 600°C, the crystal structure is more complete. IR spectrum at 25°C shows that Gd3+/Ni2+/Ca2+ cooped yttrium oxide Water and glycol are still adsorbed on the surface of the membrane. After the treatment at a high temperature above 300°C. The IR spectrum shows only the absorption peak of yttrium oxide, and glycol and water desorption is complete. The microstructure of Gd3+/Ni2+/Ca2+ codoped yttria films is porous.