对CU20薄膜沉积进行在位监控即可以承接前期研究，又可以作为在位沉积案例实现本研究系统搭建，所以此次研究以CU20薄膜沉积为表征对象。
椭偏仪在位表征电化学沉积的系统搭建（二十一）- 不同沉积条件CU20制备
CU20作为一种半导体材料，实验组前期对其进行了系统的研究。其中电化学沉积CU20薄膜对沉积条件如沉积电压、沉积温度和溶液pH值等十分敏感，且不同条件下沉积得到的CU20薄膜的催化性质有差异。对CU20薄膜沉积进行在位监控即可以承接前期研究，又可以作为在位沉积案例实现本研究系统搭建，所以此次研究以CU20薄膜沉积为表征对象。
本文主要是应用所设计的电解池进行薄膜的沉积并实现椭偏仪的在位监测和对所得到的数据进行拟合分析，构建出简单可行的椭偏仪在位表征体系。首先，进行了不同电流的恒压沉积且对成分进行了分析，确定了后续实验的沉积电流。其次是进行了准在位测试，即在沉积180s、360s、540s、720s、900s、1080s后分别进行了椭偏仪全谱(300nm-800nm)测试。zui后进行了380nm的单波长实时在位椭偏仪监控。
如图4-1(a)，是用圆形微腔体两电极体系下得到的CV图，其中电解液为0.02M CU(CH3COO)2和0.1M CH3COONa，工作电极是Au/Si，对电极为Pt丝环，开始电位为-0.6V，扫描范围-0.6-0.6V，扫描速率为5mV/s。该体系下得到的电流密度较小，在10-4mAcm-2数量级，这比实验组前期用三电极体系得到的电流密度小3个数量级。同时随着电位的移动，在0.04V附近出现了还原峰，0.89V附近出现了氧化峰。
图4-1(b)是不同电流沉积下测试得到的XRD。用流动型微腔池体进行了不同沉积电流的薄膜沉积，电解液为0.02M CU(CH3COO)2，0.1M CH3COONa。沉积电流分别为-0.4mA、-1mA、-2mA、-3mA，沉积18分钟，然后进行了X-ray测试，如图4-1所示。由图谱可知在-0.4mA的电压下沉积得到的是CU20，而1mA、2mA、3mA时沉积得到的是Cu和CU20的混合相。由此在后续的椭偏仪在位监测中可以据此选择沉积电流，实现CU20及Cu和CU20的混合相的沉积与监测。
图4-1 (a)微腔CU(CH3COO)2-CH3COONa的CV图（以Pt丝为对电极）;
(b)不同电流条件下的XRD
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