椭偏仪在位表征电化学沉积的系统搭建（十一）- 工作电极的制备与椭偏仪在位监控

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椭偏仪在位表征电化学沉积的系统搭建（十一）- 工作电极的制备与椭偏仪在位监控

2.1工作电极的制备

实验中所用的工作电极为在Si(100)上磁控溅射100-200nm厚的Au，其制备流程如下：

(1)清洗

由于在生产保存与运输的过程中会使得硅片上残留无机、有机和其他灰尘颗粒污物，其对硅上的镀膜有着较大影响，故而镀膜之前需要对硅片进行清洗。清洗步骤：1.首先在丙酮中用超声清洗仪超声5-10分钟；2.然后用去离子水超声同样的时间；3.接着在酒精中超声清洗；4.zui后再用去离子水超声清洗。在完成以上步骤去除硅片表面的残留污染物后，将其置于鼓风干燥箱干燥即可。

(2)磁控溅射

由于金的晶格常数和硅的晶格常数存在较高的不匹配度，所以需要在硅片上镀一层Ta作过渡金属层增加薄膜之间的附着力。操作步骤：首先，将处理好的硅片放在样品托上，靶材Ta和靶材金均放在直流靶上，关闭腔体进行抽真空，使真空度达到3×10^-5Pa；然后打开氩气使腔体得工作压强是0.5Pa，接着开启直流电源，在可以观察到起辉后，于室温下进行溅射。首先在磁控溅射功率70W、氩气流速为35sccm条件下 溅射10nm的Ta层作为过渡层，然后在磁控溅射功率30W、氩气流速为25sccm条件下溅射生长100nm的金层作为该实验的基底。

2.2椭偏仪在位监控

2.2.1椭偏仪

图2-1是实验用的椭偏仪测试装置部分的实物图，其型号是Ellip-SR-I。可以看到该部分由基座、样品台、入射臂、出射臂探测器和角度盘组成。其中角度盘的精度是5°，即入射角度的变化是以5°为单位进行调节的，其调节范围在0-90°。如图2-1所示，为了保证垂直入射出射，样品台的高度可以进行调节，此外整个样品台面还可以在竖直方向上进行。当进行样品测试时，第1步就是进出准直的调节，即使样品测试面在水平，当入射光垂直入射时可以垂直反射。

图2-1椭偏仪实物图

2.2.2在位监控

1、Pb溶液体系

在进行不同浓度溶液：5/10/15/20mMPb(CH₃COO)₂和1MCH₃COONa混合溶液的实验，Pb薄膜的沉积实验用的是10mMPb(CH₃COO)₂和1MCH₃COONa混合溶液。该混合溶液透明，但是由于CH₃COO^-的存在，溶液体系不稳定性，每次实验时都需要即时配制溶液。

2、Cu₂O薄膜监控

进行Cu₂O薄膜沉积时用的是0.02MCu(CH₃COO)₂，0.1MCH₃COONa混合溶液，该溶液是浅蓝色的，同样存在不稳定性，实验都需要重新配制。

椭偏仪进行Cu₂O薄膜监控示意图2-2所示，沉积的装置放在椭偏仪的样品台上，在电化学沉积的同时进行椭偏仪测试，即可实现薄膜沉积的在位监测。

实验中根据设计的电解池，使用CHI-660D电化学工作站设备采用恒流进行电化学沉积Cu₂O薄膜，对沉积电流及沉积时间等参数的调节来调控Cu₂O薄膜的生长。在进行电化学沉积过程中同时进行椭偏仪的监测，第1组实验是准在位测试，即每沉积180s后进行一次300nm到800nm的椭偏测试，测试的时间点分别是0s、180s、360s、540s、900s及1080s。第二组实验是连续沉积1080s，在这期间同时进行椭偏测试，该组测试椭偏仪取点时间大约是13s每个点。

图2-2椭偏仪在位监测示意图

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