金属氧化物纳米薄膜的LIBS分析技术研究
发布时间：2018-08-17 11:53
【摘要】：激光诱导击穿光谱(Laser induced breakdown spectroscopy,LIBS)技术,是一种利用聚焦后的脉冲激光烧蚀样品,产生瞬态高温等离子体,通过测量等离子体冷却时发射的原子或离子光谱来实现样品成分分析的技术。自其诞生以来,LIBS技术凭借其实时、快速、可远程非接触测量,免样品处理,微量烧蚀,探测范围宽,可现场应用等优点得到快速发展,在各个领域得到广泛应用。但将LIBS技术应用于纳米薄膜质量检测时,有很多关键问题亟需解决。本文针对纳米薄膜质量分析中的实际应用需求,将LIBS分析技术与薄膜分析技术结合,对结合过程中存在的关键科学问题和技术问题进行了深入的研究。文章从分析系统的设计实现,各种参数的影响,等离子体特性的多角度分析和系统的检测能力等几个方面进行了研究和讨论。针对纳米材料本身的结构特性和LIBS技术的烧蚀特点,本文设计实现了一套利用定位系统辅助定位的LIBS薄膜综合分析系统。利用该系统,本文针对LIBS检测的重复性进行了实验研究,并计算了强度的相对标准偏差(RSD),结果小于2%,证明了所搭建的系统具有较好的重复性和稳定性,可用于纳米薄膜质量分析。同时,还根据实际测试的结果,完善了激发和收集光路的设计。本文利用搭建的系统,深入分析了各种不同实验参数(激光能量、激光聚焦点到样品表面距离(LFTSD)参数、聚焦条件、收集光路等)对等离子体演化和光谱辐射特性的影响。实验数据表明,LFTSD参数是影响激光-物质相互作用过程、等离子体形态以及等离子体光谱发射等过程的主要因素之一。在低能量(1 mJ),LFTSD=0处获得了一系列硅元素的谱线,并利用这些谱线计算了电子温度(17445 K),同时利用硅的两条谱线(250.69 nm和252.85nm)和Hα线计算了电子密度(1.66×1017cm-3、1.47×1017cm-3和7.5×1017cm-3),验证了产生的等离子体满足局部热力学(LTE)条件。针对实验中和分析中遇到的一些问题,本文对搭建的系统进行了改进和完善,采用位置灵敏传感器(PSD)定位单元和等离子体时空分辨分析单元,对关键的LFTSD参数和等离子体诊断光路进行了优化。利用新系统和新制备的样品,验证了系统的稳定性(光谱强度RSD小于1.5%),并研究了利用硅元素校正前后谱线强度与样品组分间的关系。结果表明,经校正后,谱线强度与薄膜组分浓度间呈较好的线性关系(90%以上)。最后,对全文内容进行了总结,分析了本文工作的创新点。根据实际应用需求,对下一步的研究内容进行了展望。
[Abstract]:Laser induced breakdown spectroscopy (Laser induced breakdown spectroscope) technique is a kind of transient high temperature plasma produced by pulsed laser ablation of samples after focusing. A technique for sample composition analysis by measuring the atomic or ionic spectra emitted by a plasma during cooling. Since its birth, LIBS technology has been rapidly developed with its advantages of real-time, fast, remote non-contact measurement, sample free treatment, micro-ablation, wide detection range, and can be applied in various fields. However, there are many key problems to be solved when LIBS technology is applied to the quality detection of nanocrystalline films. In this paper, the key scientific and technical problems existing in the process of nano-film quality analysis are deeply studied by combining the LIBS analysis technology with the thin film analysis technology in order to meet the practical application needs in the analysis of the quality of nanocrystalline films. The design and implementation of the analysis system, the influence of various parameters, the multi-angle analysis of plasma characteristics and the detection ability of the system are studied and discussed in this paper. According to the structural characteristics of nanomaterials and the ablative characteristics of LIBS technology, a comprehensive analysis system for LIBS thin films is designed and implemented by using positioning system. By using this system, the repeatability of LIBS detection is studied experimentally, and the relative standard deviation (RSD),) results of strength are calculated. It is proved that the system has good repeatability and stability. It can be used to analyze the quality of nanometer film. At the same time, according to the actual test results, the design of excitation and collection light path is improved. In this paper, the effects of various experimental parameters (laser energy, laser focus distance to surface (LFTSD) parameter, focusing condition, collection path, etc.) on plasma evolution and spectral radiation characteristics are analyzed. The experimental data show that the parameters of LFTSD are one of the main factors affecting the laser-matter interaction, plasma morphology and plasma spectral emission. At the low energy (1 MJ) LFT SD0, a series of Si spectral lines have been obtained. The electron temperature (17445 K),) and the electron densities (1.66 脳 1017cm-347 脳 1017cm-3 and 7.5 脳 1017cm-3) of silicon (250.69 nm and 252.85nm) and H 伪 (1.66 脳 1017cm-347 脳 1017cm-3 and 7.5 脳 1017cm-3) have been calculated simultaneously. It is verified that the produced plasma satisfies the local thermodynamic (LTE) condition. Aiming at some problems encountered in the experiment and analysis, the system is improved and perfected in this paper. The position sensitive sensor (PSD) positioning unit and the plasma space-time resolution analysis unit are used. The key parameters of LFTSD and the optical path of plasma diagnosis are optimized. The stability of the system (the spectral intensity RSD is less than 1.5%) was verified by using the new system and the newly prepared samples. The relationship between the spectral line strength and the composition of the sample before and after correction with the silicon element was studied. The results show that there is a good linear relationship between the spectral line strength and the composition concentration of the film (more than 90%). Finally, the content of this paper is summarized, and the innovation of this paper is analyzed. According to the practical application requirements, the future research content is prospected.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383
[Abstract]:Laser induced breakdown spectroscopy (Laser induced breakdown spectroscope) technique is a kind of transient high temperature plasma produced by pulsed laser ablation of samples after focusing. A technique for sample composition analysis by measuring the atomic or ionic spectra emitted by a plasma during cooling. Since its birth, LIBS technology has been rapidly developed with its advantages of real-time, fast, remote non-contact measurement, sample free treatment, micro-ablation, wide detection range, and can be applied in various fields. However, there are many key problems to be solved when LIBS technology is applied to the quality detection of nanocrystalline films. In this paper, the key scientific and technical problems existing in the process of nano-film quality analysis are deeply studied by combining the LIBS analysis technology with the thin film analysis technology in order to meet the practical application needs in the analysis of the quality of nanocrystalline films. The design and implementation of the analysis system, the influence of various parameters, the multi-angle analysis of plasma characteristics and the detection ability of the system are studied and discussed in this paper. According to the structural characteristics of nanomaterials and the ablative characteristics of LIBS technology, a comprehensive analysis system for LIBS thin films is designed and implemented by using positioning system. By using this system, the repeatability of LIBS detection is studied experimentally, and the relative standard deviation (RSD),) results of strength are calculated. It is proved that the system has good repeatability and stability. It can be used to analyze the quality of nanometer film. At the same time, according to the actual test results, the design of excitation and collection light path is improved. In this paper, the effects of various experimental parameters (laser energy, laser focus distance to surface (LFTSD) parameter, focusing condition, collection path, etc.) on plasma evolution and spectral radiation characteristics are analyzed. The experimental data show that the parameters of LFTSD are one of the main factors affecting the laser-matter interaction, plasma morphology and plasma spectral emission. At the low energy (1 MJ) LFT SD0, a series of Si spectral lines have been obtained. The electron temperature (17445 K),) and the electron densities (1.66 脳 1017cm-347 脳 1017cm-3 and 7.5 脳 1017cm-3) of silicon (250.69 nm and 252.85nm) and H 伪 (1.66 脳 1017cm-347 脳 1017cm-3 and 7.5 脳 1017cm-3) have been calculated simultaneously. It is verified that the produced plasma satisfies the local thermodynamic (LTE) condition. Aiming at some problems encountered in the experiment and analysis, the system is improved and perfected in this paper. The position sensitive sensor (PSD) positioning unit and the plasma space-time resolution analysis unit are used. The key parameters of LFTSD and the optical path of plasma diagnosis are optimized. The stability of the system (the spectral intensity RSD is less than 1.5%) was verified by using the new system and the newly prepared samples. The relationship between the spectral line strength and the composition of the sample before and after correction with the silicon element was studied. The results show that there is a good linear relationship between the spectral line strength and the composition concentration of the film (more than 90%). Finally, the content of this paper is summarized, and the innovation of this paper is analyzed. According to the practical application requirements, the future research content is prospected.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383
【共引文献】
相关期刊论文 前10条
1 马靖,陆同兴;振铃光谱技术中腔内光场的涨落计算[J];安徽师范大学学报(自然科学版);2001年03期
2 唐晓闩,杨锐,郑贤锋,凤尔银,马靖,季学韩,崔执凤;激光烧蚀铝等离子体中离子特性的实验研究[J];安徽师范大学学报(自然科学版);2002年02期
3 李慧敏;傅院霞;张先q，
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