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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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