椭偏仪准在位监测薄膜的沉积。利用微腔电解池进行Au基底上薄膜的恒流沉积（-0.4mA)。并在沉积时间为180s、360s、540s、900s、1080s时进行椭偏仪全谱表征（300-800nm)。
椭偏仪在位表征电化学沉积的系统搭建（六）- 在位监测电化学沉积
2.3在位监测电化学沉积
目前报道过的在位监测手段主要有电化学在位拉曼光谱法、在位傅里叶红外光谱仪法、石英晶振仪法、质谱仪法、在位椭偏仪法。
电化学在位拉曼光谱法，其原理是通过介质分子对入射光发出频率的有明显变化的散射现象，用单色入射光（圆偏振光与线偏振光)来激发由电极电位控制的电极表面，然后测定出散射得到的光谱信号，如频率、强度及偏振性能变化与电极的电位或者电流强度的变化关系。
在位傅里叶红外光谱仪法(FTIRS)是由Bewick等人在20世纪80年代早期首创的。在位傅里叶变换红外光谱仪可以获取电极上中性和离子吸附物的分子信息，以及参与电化学反应的溶液种类。大量的研究已将在位FTIRS由光滑的表面向粗糙的表面扩展，由静态条件向动态条件扩展，由水相系统向非水相系统扩展。利用在位FTIRS技术可以得到的电化学双分子层等图像信息，达到对电催化反应以及带电界面过程更深刻的理解。
图1-11两种在位FTIRS电池设计图
两种在位FTIRS电池设计方法已经被开发出来，以减少电解质的强红外吸收，即内部和外部反射装置，其原理图如图1-11所示。该方法适用于多种电极材料，包括金属单晶电极、纳米材料电极、氧化物材料电极和碳材料电极，并能同时测定电化学反应中吸附物和溶液的种类。在位FTIRS也采用衰减全反射(ATR)模式的内反射结构，在高折射率的红外透明母棱镜上沉积一层金属薄膜作为工作电极。由于红外光束从电极背面(通过棱镜)聚焦在界面上，然后检测到反射辐射，因此溶液层的厚度对入射、出射光的影响可避免，故而液层的厚度将不再受到限制。然而，这种内部反射结构的电极材料仅限于红外窗口棱镜上的一个薄膜(小于100nm)，仅限于溅射或化学沉积的少数金属(Au、Pt、Pd等)。
石英晶振仪是一种非常灵敏的质量天平，可以测量单位面积内质量的毫微克水平变化。石英是一种压电材料，通常通过金属电极施加适当的电压，可以使其以规定的频率振荡。在电极表面添加或去除少量的质量可以影响振荡的频率。这种频率的变化可以实时监测，以获得电极表面发生的分子相互作用或反应的有用信息，如薄膜生长、氧化、腐蚀或衰减等。因此可以把石英晶振仪作为工作电极衬底，从而用于监控薄膜生长过程中的薄膜厚度。石英晶振仪能给出沉积的量的多少，但是无法给出生长的模式，因此通常用于配合其他的测试方法，如椭偏仪。
质谱仪法是通过用电场、磁场把运动的带电荷原子、分子和离子等粒子，按其比荷进行分离检测的方法。不同带电粒子其质荷比不同，偏转的时间也不同，质谱仪就可以将这些不同的时间、位置等信息转变成光学数据，通过质谱图呈现出来，这样混合物中的各种成分就可以被解析观察。可以用于解构在电化学过程中溶液的变化等。
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