普铝中Fe，Si元素的激光诱导击穿光谱测试条件及定量分析研究

doi:10.3964/j.issn.1000-0593(2019)04-1267-07

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Abstract In order to promote the application of LIBS technology in electrolytic aluminum industry, give full play to its advantages of rapidness, no preparation and multi-element simultaneous detection. The contents of Fe and Si elements in general aluminium procuced from electrolysis process were detected by means of laser induced breakdown for the first time, and the reasonable experimental conditions were explored, the calibration curves were established and the content of Fe and Si in general aluminium were quantitatively analyzed based on reasonable experimental conditions. The accuracy of LIBS measurement results were examined according to national standard GB / T 7999—2015 “optical emission spectrometric analysis method of aluminum and aluminum alloy”. The fundamental frequency 1 064 nm laser produced by Nd∶YAG pulsed laser device as the excitation source producing plasma，the spectral informations were detected and recorded by multi-channel grating spectrometer and ICCD detector. First of all, LIBS spectral line was detected and the spectral line was assigned, the line of Al Ⅰ 266.04 nm, Si Ⅰ 288.15 nm and Fe Ⅰ 259.92 nm were selected for quantitative analysis through comprehensive consideration. The influence of trigger delay time, 1Q delay time, laser setting voltage on the spectral signal intensity and SNR were researched respectively in the paper. The experimental results show that the trigger delay time of 4 μs, 1Q delay time of 170~190 μs, the laser set voltage of 560 V are the reasonable experimental parameters for Si and Fe element quantitative analysis in this paper. According to the relationship between spectral intensity and elemental concentration, the calibration curves were cestablished by the internal standard method. The correlation coefficients were 0.952 11 and 0.919 72, and the relative standard deviation were 6.34% and 7.25% for Fe and Si elements respectively. There was a good linear relationship between concentration and spectral intensity, and the 12 samples were quantitatively analyzed base on the above model. The relative error of Fe content is 0~17.3% and the relative error of Si content is 0~14.3% compared with the results obtained by OES. The measurement results 100% comply with the allowable requirements for Si content in 12 samples, and the results 91.7% meet the allowable difference requirements according to national atandard GB/T 7999—2015 “optical emission spectrometric analysis method of aluminum and aluminum alloy”. The experimental results show that, LIBS technology has a certain value of promotion and using in the electrolytic aluminum industry for Fe and Si elements detection.

Key words：Laser induced breakdown spectroscopy; Aluminium electrolysis; General aluminium; Fe and Si elements; Quantitative analysis

Received: 2018-03-05 Accepted: 2018-07-19

ZTFLH:

O433.4，O657.3

Corresponding Authors: HU Xiao-jun E-mail: huxiaojun@ustb.edu.cn

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https://www.gpxygpfx.com/EN/10.3964/j.issn.1000-0593(2019)04-1267-07 OR https://www.gpxygpfx.com/EN/Y2019/V39/I04/1267

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