椭偏仪在位表征电化学沉积的系统搭建（十四）- 在位监控装置的设计

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椭偏仪在位表征电化学沉积的系统搭建（十四）- 在位监控装置的设计

之前简要介绍了在镀Au的硅片基底上用电化学方法沉积Cu₂O薄膜并进行椭偏测试的制备过程、表征方法和实验中所用的试剂及设备，对基底电极Au/Si清洗和制备过程进行了详细描写，接着介绍了形貌表征及电化学测试等手段，如：椭偏仪测试与建模拟合，X-ray进行对样品的物相分析，SEM可观察薄膜的微观形貌。这些测试可以分析出Cu₂O薄膜的光学形貌等特点。

而在椭偏仪在位监测中，装置的设计是重点，要考虑池体的大小、溶液的容量、光路经过的介质、电极的放置等问题，本章主要介绍实验装置的设计、改进以及对应的一些测试实验。

3.1开放容器

在开始设计装置之前，用玻璃培养皿进行了实验，实验的目的是看不同溶液厚度对椭偏仪所测数据的影响。以醋酸钠、醋酸铅(1MNaCH₃COO、10mMPbPb[CH₃COO]₂)为溶液，镀金硅(Au/Si)为基底，进行不同溶液厚度的椭偏测试。

把25px×30px的Au/Si基底放入直径为260px的培养皿底，其厚度0.53mm，则体积是0.064cm³。经过计算光经过溶液后打在基底上再返回，要使得在溶液中经过的光程是25px、50px、75px、100px、125px和150px，则要向对应培养皿中加入18.9cm³、33.5cm³、48.0cm³、62.5cm³、77.1cm³和91.6cm³的溶液。在培养皿中先后加入上述体积的溶液，进行入射角度为70°，波长范围为300nm-800nm的椭偏测量，测试得到的椭偏参数如图3-1所示。

图3-1不同溶液厚度的椭偏仪测试(a)Psi；(b)Delta

从图3-1(a)可知，随着溶液的加入，溶液中的光程从0变化到150px。其中光程为25px、75px时测得的结果比0时要小，且曲线趋势也不同；光程为50px、100px、125px、150px时测得的数据比0时要大，且曲线的变化趋势大致相同，随着溶液的增加，差值增加，但是在加到5、150px时达到了极值，从图中可以看到5、150px时结果靠得非常近。

从图3-1(b)图可知，随着溶液的加入，溶液中的光程从0变化到150px。其中光程为25px，75px时测得的结果比0时要小，且曲线趋势和也相同。光程为50px、100px、125px、150px时测得的数据比0时要大，且曲线的变化趋势大致相同，随着溶液的增加，差值增加，但是在加到5、150px时达到了极值，从图中可以看到125px、150px时结果靠得非常近。

综上所述，加入透明溶液对基底进行测试是可行的，但是溶液厚度会对测量结果带来数值上的上下移动，溶液达到一定厚度后测试得到的数据会趋于稳定。在该波段溶液的存在会带来数据的波动。虽然敞开器皿作为池体很简单方便，但是它也存在溶液敞开会有溶液紊动，且存在测试时间长、溶液易被污染等对测试不利的因素，故需要重新设计其他电解池。

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