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被動(dòng)調(diào)Q激光誘導(dǎo)擊穿光譜探測(cè)研究

發(fā)布時(shí)間:2018-06-25 08:25

  本文選題:激光誘導(dǎo)擊穿光譜 + 等離子體; 參考:《哈爾濱工業(yè)大學(xué)》2017年碩士論文


【摘要】:激光誘導(dǎo)擊穿光譜技術(shù)(Laser-Induced Breakdown Spectroscopy,簡(jiǎn)稱(chēng)LIBS)是一種通過(guò)使用高能激光脈沖來(lái)激發(fā)樣品,并探測(cè)接收樣品原子發(fā)射光譜的技術(shù)。聚焦激光脈沖和樣品之間的相互作用產(chǎn)生了由電離物質(zhì)組成的等離子體,等離子體發(fā)射的光譜可以提供多種不同化學(xué)成分元素專(zhuān)屬的“光譜指紋”,檢測(cè)過(guò)程相對(duì)簡(jiǎn)單,能檢測(cè)分析很多物理形態(tài)下的樣品,對(duì)很多ppm量級(jí)元素有很好的檢測(cè)靈敏度,而且只消耗少量樣品(通常只有pg~ng量級(jí)形成等離子體)進(jìn)行分析,在檢測(cè)時(shí)通常可近似為無(wú)損檢測(cè),利用無(wú)需樣品預(yù)處理的優(yōu)勢(shì)可進(jìn)行遙感探測(cè)。首先,搭建了實(shí)驗(yàn)室常規(guī)使用的,基于主動(dòng)調(diào)Q激光器的單脈沖LIBS光譜探測(cè)系統(tǒng),使用DG535數(shù)字延時(shí)信號(hào)發(fā)生器,將激光器和光譜儀進(jìn)行同步,時(shí)間分辨光譜數(shù)據(jù),找到最佳信噪比延遲時(shí)間;其次,搭建了基于被動(dòng)調(diào)Q激光器的單脈沖LIBS系統(tǒng),設(shè)計(jì)了小型光電轉(zhuǎn)換模塊及數(shù)字延時(shí)模塊,使用泵浦氙燈作為觸發(fā)信號(hào)進(jìn)行光譜采集同步,找到最佳工作條件;最后,搭建了基于被動(dòng)調(diào)Q激光器的預(yù)燒蝕雙脈沖LIBS系統(tǒng),泵浦氙燈電壓達(dá)到570V時(shí),穩(wěn)定出輸出雙脈沖激光,雙脈沖間隔35μs~40μs,將第一束脈沖激光的漫反射光作為觸發(fā)信號(hào),經(jīng)光電轉(zhuǎn)換及數(shù)字延時(shí)后進(jìn)行光譜采集同步,找到最佳工作條件。分別使用上述三種LIBS系統(tǒng)進(jìn)行樣品燒蝕實(shí)驗(yàn)對(duì)比。首先,對(duì)純銅樣品進(jìn)行燒蝕,三種LIBS系統(tǒng)都可以得到純銅樣品光譜,雙脈沖LIBS系統(tǒng)可以得到信噪比更高,強(qiáng)度更強(qiáng)的光譜譜線(xiàn);其次,使用內(nèi)部標(biāo)定法對(duì)溶液中銅離子進(jìn)行檢測(cè)分析,將500ppm的MgCl_2溶液作為內(nèi)標(biāo)溶液,檢測(cè)不同濃度的CuCl_2溶液,以碳棒為基底,在水分蒸發(fā)后進(jìn)行燒蝕分析,得到雙脈沖LIBS系統(tǒng)對(duì)Cu元素的檢測(cè)限為5.87ppm;最后,對(duì)海水進(jìn)行元素光譜檢測(cè),兩種單脈沖LIBS系統(tǒng)只能檢測(cè)到海水中含量較高的元素,被動(dòng)調(diào)Q雙脈沖LIBS系統(tǒng)可以檢測(cè)出更多的元素,分別對(duì)威海小石島地區(qū)和麻子港生活污水入?谔幍暮KM(jìn)行檢測(cè)分析,發(fā)現(xiàn)麻子港處的Al、Fe、Cu元素含量相對(duì)較高,也說(shuō)明生活污水中上述元素含量相對(duì)較高。
[Abstract]:Laser-Induced Breakdown Spectroscopy (LIBS) is a technique that excites samples by using high-energy laser pulses and detects atomic emission spectra of receiving samples. The interaction between the focused laser pulse and the sample produces a plasma consisting of ionized substances. The spectrum emitted by the plasma can provide a "spectral fingerprint" that is specific to many different chemical elements, and the detection process is relatively simple. Can detect and analyze samples in many physical forms, have good sensitivity for many ppm orders of magnitude, and consume only a few samples (usually only pg~ng order of magnitude to form plasma) for analysis. In the detection process, it can be approximated as nondestructive testing, and remote sensing detection can be carried out by using the advantage of no sample pretreatment. First of all, a monopulse Libs spectral detection system based on active Q-switched laser is set up in the laboratory. The DG535 digital delay signal generator is used to synchronize the laser with the spectrometer and resolve the spectral data in time. The optimal SNR delay time is found. Secondly, a monopulse Libs system based on passive Q-switched laser is built, and a small photoelectric conversion module and a digital delay module are designed. The pump xenon lamp is used as the trigger signal for spectral acquisition synchronization. Finally, a pre-ablation double-pulse Libs system based on passive Q-switched laser is built. When the pump xenon lamp voltage reaches 570V, the output double-pulse laser is stabilized. The diffuse reflectance of the first pulsed laser is taken as the trigger signal, and the spectrum acquisition synchronizes after photoelectric conversion and digital delay, and the optimum working conditions are found. The above three Libs systems were used to compare the sample ablation experiments. First, the pure copper sample can be ablated, the spectrum of pure copper sample can be obtained by three kinds of Libs system, and the spectral lines with higher SNR and stronger intensity can be obtained by double pulse Libs system. The copper ions in the solution were detected and analyzed by internal calibration method. The 500ppm MgCl2 solution was used as the internal standard solution to detect the CuCl2 solution with different concentrations. The carbon rod was used as the substrate, and the ablation analysis was carried out after the evaporation of the water. The detection limit of Cu in dual-pulse Libs system is 5.87 ppm.Finally, the two monopulse LIBS systems can only detect the elements with high content in seawater. The passive Q-switched dual-pulse Libs system can detect more elements. The seawater in Xiaoshi Island area of Weihai and at the entrance of domestic sewage of Aizi Port has been detected and analyzed respectively. It is found that the content of Al _ (Fe) Fe _ (Cu) in the port is relatively high. It also shows that the content of above elements in domestic sewage is relatively high.
【學(xué)位授予單位】:哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類(lèi)號(hào)】:O657.319

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