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为了探索在固体表面制作周期微结构的快速、低成本的新方法，并了解表面周期微结构对激光诱导击穿光谱（LIBS）信号增强的物理机制，本文利用200目的球形铜粉在聚氯乙烯片上压印出半球形表面周期微结构，再利用电镀方法制作出复制有该微结构的镍板。通过对比观测光滑表面镍板和带有半球形表面周期微结构的镍板不同的LIBS信号增强效果、测量其等离子体的温度和电子密度变化，分析得出样品被照射表面积的增加是半球形表面周期微结构引起LIBS信号增强的主要原因。还与具有一定深度的圆柱形表面周期微结构的实验现象和信号增强机制进行了对比分析，表明微结构的深度有助于获得更好的信号增强效果，为后续的微结构参数设计提供了有益的参考。最后还应用表面增强LIBS技术分析了水中的铅元素。结果表明：当前条件下，带有半球形表面周期微结构的镍板与光滑表面的镍板相比，基于Pb I 405.78 nm分析线，铅的分析灵敏度可改善约23倍，重复测量时信号强度的可重复性也获得了一定程度的改善。In order to develop a rapid and cost-effective new approach to produce periodic microstructures on solid surfaces, and help to understand the physical mechanism of the enhancement of laser-induced breakdown spectroscopy (LIBS) signals induced by surface periodic microstructures, in this article, spherical copper powder with about 74 μm diameter was used to imprint semispherical surface periodic microstructures on polyvinyl chloride (PVC) sheets under 15 T pressures. A platinum conducting layer about 100 nm thickness was coated on the PVC surface using a vacuum sputter coater and then nickel plates with the replicated microstructures on one surface were prepared using electroplating method. The signal enhancement effect induced by micro-structured surface in LIBS was experimentally observed and compared with that achieved while using flat surface nickel plate, the temperature and electron density of the induced plasma was measured according to Boltzmann plot method and the Stark broadening of Hα line of hydrogen. By systematically analyzing these results, it is concluded that the main physical mechanism of the signal enhancement in LIBS caused by the semi-spherical surface periodic microstructure is due to the increased surface area of the sample can be irradiated by the laser beam, leading to mass increase for the ablated sample material if compared with that of flat surface irradiated by the same laser beam. Comparative analysis was also conducted with experimental phenomena and signal enhancement mechanisms of using cylindrical surface periodic microstructures with a certain depth (20 μm diameter, 15 μm depth and 40 μm period ). It was found that the depth of the microstructure helps to achieve better signal enhancement effects. This provides useful references for subsequent microstructure parameter design in the future. Finally, lead in aqueous solution samples was detected with surface-enhanced LIBS (SENLIBS) technique, while Pb I 405.78 nm line was selected as the analytical line. In comparison with flat surface nickel substrate, 23-folds detection sensitivity and slightly improved signal reproducibility can be achieved while using nickel substrates with hemispherical surface periodic microstructure. The results indicate that nickel plates with hemispherical surface periodic microstructure show better analytical performance than flat surface nickel plates in elemental analysis of aqueous solution samples by SENLIBS.
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Keywords:
- Laser-induced breakdown spectroscopy /
- Surface-enhancement /
- Surface periodic micro-structures /
- Signal enhancement mechanism
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