钙镍钐共掺杂氧化铈薄膜制备工艺的研究

通过一步阳极氧化法制备了钙、镍、钐共掺杂氧化铈薄膜,通过改变阳极氧化工艺参数电流密度、阳极氧化温度、氨水浓度、阳极氧化时间、热处理温度和Sm3+、Ca2+、Ni2+的浓度来观察Sm3+/Ca2+/N


摘要:本文通过一步阳极氧化法制备了钙、镍、钐共掺杂氧化铈薄膜,通过改变阳极氧化工艺参数电流密度、阳极氧化温度、氨水浓度、阳极氧化时间、热处理温度和Sm3+、Ca2+、Ni2+的浓度来观察Sm3+/Ca2+/Ni2+共掺杂氧化铈膜的膜厚度、电导率、膜成分、表面形貌、结构性能的改变情况。并分别用SEM、XRD和IRDE等仪器对氧化铈膜进行表征。

最终得出较佳的实验条件为:电流密度0.50 mA/cm2、阳极氧化温度26 ℃、氨水浓度2.2157 mol/L、Sm3+浓度4.6222 mmol/L、Ca2+浓度6.3726 mmol/L、Ni2+浓度5.0315 mmol/L、阳极氧化时间8 h。在此条件下的研究结果表明Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度为30.5 μm,其在热处理温度600 ℃下的电导率为1.75×10-2 S/cm,Sm3+/Ca2+/Ni2+共掺杂氧化铈膜为立方萤石结构,并且其表面具有多孔结构。经过了300 ℃热处理后的,Sm3+/Ca2+/Ni2+共掺杂氧化铈薄膜上的乙二醇和水基本脱离吸附。400 ℃热处理2 h以后的CeO2具有完整的晶型。

本文的创新点是钙、镍、钐共掺杂氧化铈薄膜制备工艺的研究未见报道。

关键词:SOFC;阳极氧化;氧化铈;立方萤石

Study on Preparation Technology of Cerium Oxide Film Co-doped with Sm3+,Ca2+ and Ni2+  

Abstract: Lining-up the Cerium oxide film Co-doped with Sm3+ , Ca2+ and Ni2+ by one-step anodic oxidation . It was observed the film thickness, conductivity, membrane composition, surface morphology, and structural properties of the changes by changing the parameter current density, anodizing temperature, ammonia concentration, anodizing time, heat treatment temperature and concentration of Sm3+, Ca2+ and Ni2+.The Cerium oxide membrane was characterized by SEM, XRD and IRDE respectively.

Finally, the better experimental condition was obtained: current density 0.50 mA/cm2, anodizing temperature 26 °C, ammonia concentration 2.2157 mol/L, Sm3+ concentration 4.6222 mmol/L, Ca2+ concentration 6.3726 mmol/L, Ni2+ concentration 5.03 15 mmol/L, anodizing concentration time 8 h. The result under this condition showed that the thickness of the Cerium oxide film co-doped with Sm3+ , Ca2+ and Ni2+ was 30.5 μm, and it's conductivity was 1.75 × 10-2 S / cm at the heat treatment temperature of 600 °C .The membrane of Cerium oxide film Co-doped with Sm3+ , Ca2+ and Ni2+ was a cubic fluorite structure and it's surface had a porous structure. After heat been treatment at 300 °C, the ethylene glycol and the water on the co-doped Cerium oxide film were  dissociated from adsorption basically. CeO2  had a complete crystal shape after it was heated at 400 °C.

The innovation of the study is that it has never been reported on the preparation of Cerium oxide films with Sm3+ , Ca2+ and Ni2+.

Key words:  SOFC ;  anodic oxidation ;  Cerium oxide ;  Cubic fluorite

目录

第一章 绪论 1

1.1 研究背景 1

1.2 固体氧化物燃料电池概述 1

1.2.1 固体氧化物燃料电池工作原理 1

1.2.2 固体氧化物燃料电池材料 2

1.3 固体氧化物燃料电池的发展趋势 1

1.4 论文研究内容 1

第二章 实验部分 2

2.1 实验试剂及仪器 2

2.2 Sm3+/Ca2+/Ni2+共掺杂氧化铈膜的制备 2

2.2.1 实验装置 2

2.2.2 溶液的配制 3

2.2.3 Sm3+/Ca2+/Ni2+共掺杂氧化铈膜的制备 3

2.3 阳极氧化工艺参数对Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度的影响 4

2.3.1 电流密度对Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度的影响 4

2.3.2 阳极氧化温度对Sm3+/Ca2+/Ni2+共掺杂氧化铈厚度的影响 4

2.3.3氨水浓度对Sm3+/Ca2+/Ni2+共掺杂氧化铈厚度的影响 4

2.3.4 阳极氧化时间对Sm3+/Ca2+/Ni2+共掺杂氧化铈厚度的影响 4

2.3.5 Sm3+浓度对Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度的影响 4

2.3.6 Ca2+浓度对Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度的影响 4

2.3.7 Ni2+浓度对Sm3+/Ca2+/Ni2+共掺杂氧化铈膜厚度的影响 4