椭偏仪在位表征电化学沉积的系统搭建（二十）- 长方形流动微腔

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椭偏仪在位表征电化学沉积的系统搭建（二十）- 长方形流动微腔

3.3.2长方形流动微腔

为了解决溶液微圆形腔体溶液注入困难、溶液少及反应产生气泡的问题，进一步对腔体进行改进，得到微流腔体。图3-18是微流腔体制作过程示意图，首先准备好ITO、EVA胶膜、特氟龙细管、Au/Si，把EVA胶膜切成内为25px×62.5px，外为37.5px×75px的长方形，然后从上到下依次把ITO、EVA胶膜/特氟龙细管、Au/Si叠好置于加热平台，在150℃下加热，使得EVA软化粘合池体，zui后冷却得到成品。

该池体工作电极即为Au/Si基底，上端的ITO即为对电极，溶液的进出由两边的特氟龙细管实现，通常制作完成后的微腔厚度和特氟龙细管一致，约为1mm。该微腔具有液层薄、溶化充足且流动可以消除ITO上产生的气泡等优点。

图31-18流动型微腔示意图

用该池体对不同浓度醋酸铅溶液进行测试，得到的结果如图3-19所示。可以看到有无溶液加入，测试得到的椭偏参数峰位及数值上都存在差别。但是在加不同浓度的溶液(去离子水、1M醋酸钠、1M的醋酸钠和5/10/15/20mM的醋酸铅)后得到的椭偏参数数值和趋势都一致。这和前面所述的半圆弧型电解池在不同浓度的醋酸铅溶液中椭偏测试结果一致，同样说明在醋酸铅溶液中，其浓度椭偏测试参数的影响可忽略不计。

图3-19不同条件下EVA腔体椭偏测试结果(a)Psi；(b)Delta

如图3-20所示，是用该池体进行沉积薄膜的结果。电解液为0.02MCu(CH₃COO)_2，0.1MCH₃COONa，Au/Si为工作电极，ITO为对电极，-0.4mA恒压沉积。对比沉积前后腔体图可知，用该池体可以进行沉积。与前圆环电极对比可以看到，ITO上不再有气泡存在，因为产生的气泡都被流动的溶液带走了。因溶液可以流动，故可克服圆环电极溶液少的缺点。所以后续沉积薄膜实验的椭偏仪监测选用该流动池体进行。

图3-20流动型微腔(a)沉积前(b)沉积后实物图

3.4小结

本文主要介绍了研究中实验装置的设计及测试的过程，主要包含半圆弧型器件微元腔体器件。首先设计完成半圆弧器件，实现了把沉积过程和椭偏仪测试相结合，观察窗口选用石英玻璃，理论上zui大限度减小了光的损耗。但是它的池体设计太大使得溶液浪费且测试过程中基底的更换、池体的密封困难。然后完成圆环型微元腔体的设计及制作，其足够小的腔体减小了溶液对椭偏测试带来的影响。但是容纳的溶液会带来沉积离子不够的问题且经过实验发现对电极ITO上会出现气泡，影响椭偏测试，所以在此基础上设计制作完成了长方形微流腔体。该设计成功解决了气泡和溶液少所带来的问题，故而后续实验将采用长方形微流腔体。

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