椭偏仪在位表征电化学沉积的系统搭建（二十二）- 沉积前装置的椭偏数据

正文

椭偏仪在位表征电化学沉积的系统搭建（二十二）- 沉积前装置的椭偏数据

1形貌分析

图4-2(a)是准在位监测后沉积1080s时测试得到的SEM图，在1μm放大倍数下看到沉积的薄膜颗粒大小不等（~10-10³nm），形态上为不规则的块状。实验组前期用三电极体系(Au/Si工作电极，Pt网对电极，Ag/AgCl参比电极)恒压法(-0.05V)常温下(T=20℃)沉积30分钟得到的结果如图4-2(b)所示。与恒压沉积相比，沉积薄膜粒径不均匀性更强。

图4-2CU₂0薄膜的SEM图：(a)沉积1080s(b)实验组前期恒压常温沉积

2不同沉积时间椭偏数据的分析

对沉积时间为180s、360s、540s、720s、900s、1080s的CU₂0薄膜分别进行了椭偏仪全谱（300-800nm）测试，获得椭偏参数以及样品整体的反射率和光学常数。

2.1沉积前装置的椭偏数据

1、Psi、Delta、α、R实验数据在-0.4mA时进行两电极的恒流沉积，并在每沉积180s以后进行300nm到800nm的椭偏测试。在这个沉积电压下，不同时间沉积的库仑量如表4-1所示。由X-ray测试知该电流下沉积的为CU₂0，假设法拉第效率为100%，则所对应的生长速率分别为0.94nm/s，相应沉积时间下的CU₂0沉积厚度如表4-1所示。

如图4-3(a)所示，在沉积之前测试的Psi和Delta随波长增加而增加，在500nm处有跃迁，在长波段(600nm-800nm)存在波动。图4-3(b)是对应的吸收系数α和反射率R值随波长的变化图，可以看到R值在500nm处存在跃迁，趋近于zui大值1后，经文献查阅知这属于基底Au的反射特性。说明没有沉积之前所得到的椭偏测试结果主要反应的是衬底的信息，ITO和溶液对其影响甚小，也进一步证明该流动型装置用于监测薄膜沉积是可行的。对于α值，在370nm和600nm附近存在吸收峰，其和文献中报道的ITO玻璃基板上Au纳米膜的连续可见光吸收光谱出现的峰位十分接近，相对于文献其峰位发生蓝移且两峰值存在差异，这可能是由于Au薄膜上溶液和ITO带来的影响。

图4-3 沉积0s时(a)Psi和Delta(b)R随波长变化

2.2装置对应的光学常数

图4-4(a)是沉积之前测试得到的n、k随波长的变化图，从图中可以看到短波段图线较平滑，长波段数据波动大。n值在500nm附近出现峰，k值在600nm附近出现峰。500nm处n值存在跃迁，说明该处附近可能有等离子体共振峰的出现。

图4-4(b)是沉积之前测试得到的、，从图中可以看到短波段数据曲线平滑，长波段数据波动大。、均在500nm附近出现峰，这归因于Au表面等离子体共振。

图4-4 沉积0s时的n、k、、随波长的变化

经过以上分析可知，在该体系下(ITO-溶液-Au/Si)，较短波段得到的椭偏参数比较光滑，在较长波段得到椭偏数据波动比较大。与较短波段相比长波段得到的数据误差更小，该测试系统更适合较短波段测试。

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