采用一次阳极氧化制备Sm3+/Ni2+共掺杂氧化铈膜;二次阳极氧化制备Sm3+ /Ni2+/Ca2+共掺杂氧化铈膜。分别研究了阳极氧化时间、氨水浓度、电流密度、CSm3+、CNi2+、CCa2+对Sm3+/Ni2+、Sm3+/Ni2+/Ca2+共掺杂氧
摘要:本文采用一次阳极氧化制备Sm3+/Ni2+共掺杂氧化铈膜;二次阳极氧化制备Sm3+/Ni2+/Ca2+共掺杂氧化铈膜。分别研究了阳极氧化时间、氨水浓度、电流密度、CSm3+、CNi2+、CCa2+对Sm3+/Ni2+、Sm3+/Ni2+/Ca2+共掺杂氧化铈膜厚的影响;分别研究了CSm3+、CNi2+、CCa2+对Sm3+/Ni2+、Sm3+/Ni2+/Ca2+共掺杂氧化铈膜组成的影响;研究CSm3+、CNi2+、CCa2+与温度对Sm3+/Ni2+、Sm3+/Ni2+/Ca2+共掺杂氧化铈膜电导率的影响;分别研究了热处理温度对Sm3+/Ni2+/Ca2+共掺杂氧化铈膜的晶型结构和IR谱图的影响;研究了Sm3+/Ca2+/Ni2+共掺杂氧化铈膜的微观结构。研究结果表明:在较佳工艺条件:电流密为0.5 mA/cm2、阳极氧化时间4 h、阳极氧化温度26 ℃下,当CNH3∙H2O为2.3542 mol/L、CSm3+、CNi2+分别为2.0800、3.5500 mmol/L,制备的Sm3+/Ni2+共掺杂氧化铈膜厚度达到最大值为16.8 μm;当CNH3∙H2O为2.2421 mol/L、CSm3+、CCa2+分别为5.9429、5.1587 mmol/L,制备的Sm3+/Ni2+/Ca2+共掺杂氧化铈膜厚度达到最大值33.2 μm。EDX结果表明:一次阳极氧化制备的膜为Sm3+/Ni2+共掺杂氧化铈膜;二次阳极氧化制备的膜为Sm3+/Ni2+/Ca2+共掺杂氧化铈膜;电解液中CSm3+、CNi2+、CCa2+的增加,Sm3+/Ni2+、Sm3+/Ni2+/Ca2+共掺杂氧化铈膜中Sm3+、Ni2+、Ca2+的含量增大。在600℃下,当CSm3+、CNi2+分别为2.0800、3.5500 mmol/L时,Sm3+/Ni2+共掺杂氧化铈膜的电导率达到最大值为1.30×10-2 S/cm;当CSm3+、CCa2+浓度分别为5.9429、5.5187 mmol/L时,Sm3+/Ni2+/Ca2+共掺杂氧化铈膜的电导率达到最大值为1.30×10-2 S/cm。XRD结果表明:制备的Sm3+/Ni2+/Ca2+共掺杂氧化铈膜为立方萤石结构。IR结果表明:未热处理的Sm3+/Ni2+/Ca2+共掺杂氧化铈膜吸附有水和乙二醇;在大于300 ℃热处理后,Sm3+/Ni2+/Ca2+共掺杂氧化铈膜上的水和乙二醇已基本脱附。SEM结果表明:制备的Sm3+/Ni2+/Ca2+共掺杂氧化铈膜为多孔结构。
关键词:氧化铈; 共掺杂; 阳极氧化法
Investigation on that performance of cerium oxide multirole co-doped with samarium, nickel and calcium
Abstract: Sm3+/Ni2+ co - doped cerium oxide film was prepared by primary anodic oxidation. Sm3+/Ni2+/Ca2+ co - doped cerium oxide film was prepared by secondary anodic oxidation. The effects of anodic oxidation time, ammonia concentration, current density, CSm3+, CNi2+ and CCa2+ on Sm3+/Ni2+, Sm3+/Ni2+/Ca2+ cooped cerium oxide film thickness were studied. The effects of CSm3+, CNi2+ and CCa2+ on the composition of Sm3+/Ni2+, Sm3+/Ni2+/Ca2+co-doped cerium oxide film were studied. The effects of CSm3+, CNi2+, CCa2+ and temperature on the conductivity of Sm3+/Ni2+, Sm3+/Ni2+/Ca2+ co-doped cerium oxide film was studied. The effect of heat treatment temperature on the crystal structure and IR spectrum of Sm3+/Ni2+/Ca2+ co - doped cerium oxide film was studied. The microstructure of Sm3+/Ni2+/Ca2+ co - doped cerium oxide film was studied. The results show that the current density is 0.5 mA /cm2 and the anodic oxidation time is 4 h under better technological conditions, anodic oxidation, anodic oxidation time 26 temperatures. When CNH3∙ H2O is 2.3542 mol/L, CSm3+ and CNi2+ are 2.0800 and 3.5500 mmol /L respectively, the Sm3+/Ni2+ copolymerize cerium oxide film thickness obtained reached a maximum of 16.8 μm. When CNH3∙ H2O is 2.2421 mol/L, CSm3+ and CCa2+ are 5.9429 and 5.1587 mmol/L respectively, the Sm3+/Ni2+/Ca2+ co-doped cerium oxide film thickness reached the maximum of 33.2 μm. The EDX results showed that Sm3+/Ni2+co - doped cerium oxide film was prepared by primary anodic oxidation. Sm3+/Ni2+/Ca2+ co-doped cerium oxide film was prepared by subordinate anodic oxidation. The contents of Sm3+, Ni2+ and Ca2+ in the electrolyte increased, and the contents of Sm3+, Ni2+, Sm3+/Ni2+/Ca2+ in the co-doped cerium oxide film increased. Under 600 ℃, when CSm3+, CNi2+ were 2.004, 1.7899 mmol/ L, Sm3+/Ni2+ total conductivity of doped cerium oxide film reached a maximum of 1.30 x 10-2 S/cm; When the concentrations of CSm3+ and CCa2+ were 4.5243 and 2.6423 mmol/L respectively, the conductivity of Sm3+/Ni2+/Ca2+ co-doped cerium oxide film reached the maximum value of 1.30 x 10-2 S/cm. The XRD results showed that the Sm3+/Ni2+/Ca2+ co - doped cerium oxide film was a cubic fluorite structure. The IR results showed that the unheated Sm3+/Ni2+/Ca2+ co-doped cerium oxide film adsorbed water and ethylene glycol. In more than 300 after heat treatment, Sm3+/Ni2+/Ca2+ doped cerium oxide film on the water and ethylene glycol has been attached. SEM results showed that the Sm3+/Ni2+/Ca2+ co - doped cerium oxide film was porous.