激光诱导击穿光谱技术的初步研究
摘要
激光诱导击穿光谱技术（Laser Induced BreakdownSpectroscopy，简称LIBS）是一种全新的物质元素分析方法。与传统光谱分析方法相比，LIBS技术具有如下特点：具有全元素和远程分析能力；样品无需预处理且分析速度快；能够分析任何物理状态的材料；既可以表面分析也可以逐层分析等。LIBS技术的分析结果不仅依赖于被测物质的物理化学特性，而且也依赖于激光器的参数，同时被测物质所处环境也直接影响分析结果。为了促进LIBS技术的实用化，激光诱导等离子体的特性有待深入研究。
本论文首先回顾了LIBS技术国内外研究现状及存在的问题，同时介绍了激光诱导击穿光谱技术用于物质分析的理论基础，重点研究了激光诱导等离子体的数据处理方法，激光诱导等离子体特征参数随激光功率密度的变化规律以及特征参数的空间分布规律，重点研究了三种不同的定量分析方法。最后一部分研究内容是基于LIBS技术分析了秦岭岩石成分、实验室热水壶水垢成分、鸡蛋壳元素成分和氯化铜溶液成分，同时利用LIBS技术对紫铜和黄铜以及一元硬币和五角硬币的成分进行了对比研究。论文的最后对研究内容进行了总结和展望。本论文的主要工作和创新结果包括以下几个方面：
介绍了激光诱导等离子体的产生机理及特点，分析了信背比与时间延迟的关系，提出了提高信噪比的方法。重点分析了背景辐射的产生机理，并采用多项式拟合扣除等离子连续背景辐射的方法。采用了一种改进的迭代Boltzmann方法精确求解等离子体的电子温度，利用电子密度与谱线的Stark展宽之间的近似线性关系简易求解等离子体的电子密度。
通过改变激光脉冲能量得到不同激光功率密度，利用激光维持爆轰波模型（LSDW）和激光维持辐射波模型（LSRW）解释了激光诱导等离子体辐射强度随功率密度的变化规律。实验发现，功率密度由3.7GW/cm2变到15.9GW/cm2时，等离子体的特征参数的增长率大于功率密度由15.9GW/cm2增强到21.9GW/cm2时的增长率。
在等离子体空间分布方面，实验发现在距离靶面1.5mm高度处等离子体谱线的信号最强，靶面附近和等离子体顶端的信号强度较弱。与等离子谱线强度的分布相似，实验证明等离子体的电子温度在距离靶面1.5mm处达到最大，而在等离子体两端处较低。通过测量铝原子谱线394.40nm的Stark展宽，实验发现在样品表面，激光产生的等离子体局限于较小区域，电子密度达到0.29*1017cm~(-3)，随着等离子体的膨胀，电子密度逐渐降低，在等离子体的顶端，电子密度值降低到0.17*1017cm~(-3)。
基于定性和定量分析，实验证明，在误差范围内，激光诱导产生的等离子体基本满足局部热力学平衡模型（Local Thermodynamic Equilibrium Model，简称LTE）和光学薄（Optically thin）模型。
以铝合金标样E311、E312、E313、E314、E315和E316为研究对象，采用传统定标方法和内标法，分别对元素硅、铁、铜、锰、镁、镍、锌和钛进行了定量分析。实验证明：对于含量较低的元素，内标法强于传统标准曲线法。基于传统定标方法，元素硅、铁、铜、锰、镁、镍、锌和钛的探测限（Wt%）分别是0.0412、0.0894、0.0601、0.0172、0.0334、0.0477、0.0196和0.0050。鉴于实际应用中很难找到对应的标样，论文初步研究了自由定标方法。
利用LIBS技术，探测出秦岭岩石中含有元素钙、铁、碳、钠、硅、铝、铜和镁，利用迭代Boltzmann方法求得秦岭岩石等离子体的电子温度是16853K，电子密度是2.86*1018cm-3。利用LIBS技术研究了办公室水壶中水垢等离子体，并探测出钙、镁、碳、硅和铝元素，计算得到水垢等离子体的特征参数分别是4793K和6.1*1018cm-3。通过激光诱导鸡蛋壳等离子体的分析，钙元素、铁元素、碳元素和硅元素得到证认，通过钙元素谱线的分析求得鸡蛋壳等离子体的电子温度是7250K，电子密度是6.1*1016cm-3。利用LIBS技术我们还分析了氯化铜溶液的元素成分及其特征参数。此外，利用LIBS技术，我们还对比研究了紫铜与黄铜、一元硬币与五角硬币等离子体的光谱，比较了它们的特征参数并分析了它们不同的物理原因。
Laser-Induced Breakdown Spectroscopy (LIBS) is a relatively new powerfulspectrochemical analytical technique. Compared with conventional spectroscopictechniques, LIBS offers many well-known advantages such as its versatility, nosample preparation, non-contact optical nature, simplicity and rapid analysis and soon. However, the interaction of focused laser radiation with materials is socomplicated that the plasma formation is still not explained satisfactorily so far.Previous works have demonstrated that the characteristics of laser-induced plasma notonly depend on laser beam properties (pulse duration, laser power and wavelength),but also on the physical and chemical properties of the sample, as well as the sampleenvironment. For the practical application of this technique, the characteristics ofLIBS need further study.
Firstly, the present conditions and theoretical foundation of LIBS were given.Then, the data processing methods, variations of the plasma parameters (line intensity,electron temperature and electron number density) with the laser power density andtheir spatial distributions were studied. At the same time, three quantitative analysismethods (traditional calibration curve, internal standardization method andcalibration-free method) were analyzed based on a set of six standard samples ofaluminum alloy. Using LIBS, the elemental compositions of the Qin Mountain rock,water scale, egg shell, CuCl2, copper and brass, oneyuan coin and wujiao coin werestudied and their plasma parameters were calculated also. The following works weredone in this thesis.
The physics of plasma relevant to laser-induced breakdown spectroscopy hasbeen discussed. The relationship of the ratio of signal to background emissionwas analyzed and the method of improving SNR was provided. In order tocalculate and subtract the continuum emission more precisely, the polynomialfunction was used to fit the background. An iterative Boltzmann plot method wasused to calculate the laser-ablated plasma temperature, and the electron numberdensity in plasma was determined based on Stark broadening.
To study the effect of the laser irradiance on the plasma parameters, the aluminum alloy was irradiated with different laser power densities (3.7,6.3,9.7,12.4,15.9,19,21.9GW/cm2). The emission curves showed a rapid linear increase at lowpower densities, and started to bend when the6.3GW/cm2was reached with aflat region. When the laser power densities above9.7GW/cm2, a new increase ofthe emission intensities was produced. The laser-supported detonation wave atlow power densities and the laser-supported radiation wave at high powerdensities were used to explain the behavior of the laser-induced plasma,respectively. The electron temperature and electron density increased morequickly when the laser power density changed from15.9GW/cm2to21.9GW/cm2than from3.7GW/cm2to15.9GW/cm2.
All the signals increased rapidly near the target surface, and reached themaximum at a distance about1.5mm from the target surface, then decreased withthe increasing of the distance. A slight decrease of temperature both at the plasmaedge and close to the target surface was observed, as was consistent with thespatial variation of the line emission intensity. The electron density at the distanceof0.1mm above the target surface was approximately0.29*1017cm-3anddecreased to about0.17*1017cm-3at the distance of4.0mm.
Based on qualitative and quantitative analysis, the laser-induced plasma satisfiedLTE and optically thin models within experimental errors.
With a set of six standard samples of aluminum alloy, calibration curves werepresented for samples containing Si, Fe, Cu, Mn, Mg, Ni, Zn, Ti using twoquantitative analysis methods (traditional calibration curve, internalstandardization method). Based on experimental results, the limits of detection(Wt%) of trace elements were0.0412,0.0894,0.0601,0.0172,0.0334,0.0477,0.0196and0.0050, respectively. At the same time, the calibration-free methodwas also studied.
The composition of Qin Mountain rock was studied using a1064nm pulsedNd:YAG laser for the first time. Elements Ca, Mg, Cu, Fe, C, Na, Si and Al wereidentified qualitatively. The electron temperature and electron density wereinferred to be16835K and2.86*1018cm-3. Elements Ca, Mg, C, Si and Al wereidentified in the water scale by the analysis of the plasma spectra. The plasmatemperature4793K was inferred using the iterative Boltzmann plot method withten neutral calcium lines, while the electron density6.1*1018cm-3was obtainedfrom the Stark broadening of the profile of Mg I285.21nm. Based on the plasma spectra of egg shell, elements iron, oxygen, silicon, carbon and calcium wereidentified, and its parameters were7250K and6.1*1016cm-3, respectively.Using LIBS, the CuCl2, copper and brass, one-yuan coin and wu-jiao coin werealso studied.
本论文首先回顾了LIBS技术国内外研究现状及存在的问题，同时介绍了激光诱导击穿光谱技术用于物质分析的理论基础，重点研究了激光诱导等离子体的数据处理方法，激光诱导等离子体特征参数随激光功率密度的变化规律以及特征参数的空间分布规律，重点研究了三种不同的定量分析方法。最后一部分研究内容是基于LIBS技术分析了秦岭岩石成分、实验室热水壶水垢成分、鸡蛋壳元素成分和氯化铜溶液成分，同时利用LIBS技术对紫铜和黄铜以及一元硬币和五角硬币的成分进行了对比研究。论文的最后对研究内容进行了总结和展望。本论文的主要工作和创新结果包括以下几个方面：
介绍了激光诱导等离子体的产生机理及特点，分析了信背比与时间延迟的关系，提出了提高信噪比的方法。重点分析了背景辐射的产生机理，并采用多项式拟合扣除等离子连续背景辐射的方法。采用了一种改进的迭代Boltzmann方法精确求解等离子体的电子温度，利用电子密度与谱线的Stark展宽之间的近似线性关系简易求解等离子体的电子密度。
通过改变激光脉冲能量得到不同激光功率密度，利用激光维持爆轰波模型（LSDW）和激光维持辐射波模型（LSRW）解释了激光诱导等离子体辐射强度随功率密度的变化规律。实验发现，功率密度由3.7GW/cm2变到15.9GW/cm2时，等离子体的特征参数的增长率大于功率密度由15.9GW/cm2增强到21.9GW/cm2时的增长率。
在等离子体空间分布方面，实验发现在距离靶面1.5mm高度处等离子体谱线的信号最强，靶面附近和等离子体顶端的信号强度较弱。与等离子谱线强度的分布相似，实验证明等离子体的电子温度在距离靶面1.5mm处达到最大，而在等离子体两端处较低。通过测量铝原子谱线394.40nm的Stark展宽，实验发现在样品表面，激光产生的等离子体局限于较小区域，电子密度达到0.29*1017cm~(-3)，随着等离子体的膨胀，电子密度逐渐降低，在等离子体的顶端，电子密度值降低到0.17*1017cm~(-3)。
基于定性和定量分析，实验证明，在误差范围内，激光诱导产生的等离子体基本满足局部热力学平衡模型（Local Thermodynamic Equilibrium Model，简称LTE）和光学薄（Optically thin）模型。
以铝合金标样E311、E312、E313、E314、E315和E316为研究对象，采用传统定标方法和内标法，分别对元素硅、铁、铜、锰、镁、镍、锌和钛进行了定量分析。实验证明：对于含量较低的元素，内标法强于传统标准曲线法。基于传统定标方法，元素硅、铁、铜、锰、镁、镍、锌和钛的探测限（Wt%）分别是0.0412、0.0894、0.0601、0.0172、0.0334、0.0477、0.0196和0.0050。鉴于实际应用中很难找到对应的标样，论文初步研究了自由定标方法。
利用LIBS技术，探测出秦岭岩石中含有元素钙、铁、碳、钠、硅、铝、铜和镁，利用迭代Boltzmann方法求得秦岭岩石等离子体的电子温度是16853K，电子密度是2.86*1018cm-3。利用LIBS技术研究了办公室水壶中水垢等离子体，并探测出钙、镁、碳、硅和铝元素，计算得到水垢等离子体的特征参数分别是4793K和6.1*1018cm-3。通过激光诱导鸡蛋壳等离子体的分析，钙元素、铁元素、碳元素和硅元素得到证认，通过钙元素谱线的分析求得鸡蛋壳等离子体的电子温度是7250K，电子密度是6.1*1016cm-3。利用LIBS技术我们还分析了氯化铜溶液的元素成分及其特征参数。此外，利用LIBS技术，我们还对比研究了紫铜与黄铜、一元硬币与五角硬币等离子体的光谱，比较了它们的特征参数并分析了它们不同的物理原因。
Laser-Induced Breakdown Spectroscopy (LIBS) is a relatively new powerfulspectrochemical analytical technique. Compared with conventional spectroscopictechniques, LIBS offers many well-known advantages such as its versatility, nosample preparation, non-contact optical nature, simplicity and rapid analysis and soon. However, the interaction of focused laser radiation with materials is socomplicated that the plasma formation is still not explained satisfactorily so far.Previous works have demonstrated that the characteristics of laser-induced plasma notonly depend on laser beam properties (pulse duration, laser power and wavelength),but also on the physical and chemical properties of the sample, as well as the sampleenvironment. For the practical application of this technique, the characteristics ofLIBS need further study.
Firstly, the present conditions and theoretical foundation of LIBS were given.Then, the data processing methods, variations of the plasma parameters (line intensity,electron temperature and electron number density) with the laser power density andtheir spatial distributions were studied. At the same time, three quantitative analysismethods (traditional calibration curve, internal standardization method andcalibration-free method) were analyzed based on a set of six standard samples ofaluminum alloy. Using LIBS, the elemental compositions of the Qin Mountain rock,water scale, egg shell, CuCl2, copper and brass, oneyuan coin and wujiao coin werestudied and their plasma parameters were calculated also. The following works weredone in this thesis.
The physics of plasma relevant to laser-induced breakdown spectroscopy hasbeen discussed. The relationship of the ratio of signal to background emissionwas analyzed and the method of improving SNR was provided. In order tocalculate and subtract the continuum emission more precisely, the polynomialfunction was used to fit the background. An iterative Boltzmann plot method wasused to calculate the laser-ablated plasma temperature, and the electron numberdensity in plasma was determined based on Stark broadening.
To study the effect of the laser irradiance on the plasma parameters, the aluminum alloy was irradiated with different laser power densities (3.7,6.3,9.7,12.4,15.9,19,21.9GW/cm2). The emission curves showed a rapid linear increase at lowpower densities, and started to bend when the6.3GW/cm2was reached with aflat region. When the laser power densities above9.7GW/cm2, a new increase ofthe emission intensities was produced. The laser-supported detonation wave atlow power densities and the laser-supported radiation wave at high powerdensities were used to explain the behavior of the laser-induced plasma,respectively. The electron temperature and electron density increased morequickly when the laser power density changed from15.9GW/cm2to21.9GW/cm2than from3.7GW/cm2to15.9GW/cm2.
All the signals increased rapidly near the target surface, and reached themaximum at a distance about1.5mm from the target surface, then decreased withthe increasing of the distance. A slight decrease of temperature both at the plasmaedge and close to the target surface was observed, as was consistent with thespatial variation of the line emission intensity. The electron density at the distanceof0.1mm above the target surface was approximately0.29*1017cm-3anddecreased to about0.17*1017cm-3at the distance of4.0mm.
Based on qualitative and quantitative analysis, the laser-induced plasma satisfiedLTE and optically thin models within experimental errors.
With a set of six standard samples of aluminum alloy, calibration curves werepresented for samples containing Si, Fe, Cu, Mn, Mg, Ni, Zn, Ti using twoquantitative analysis methods (traditional calibration curve, internalstandardization method). Based on experimental results, the limits of detection(Wt%) of trace elements were0.0412,0.0894,0.0601,0.0172,0.0334,0.0477,0.0196and0.0050, respectively. At the same time, the calibration-free methodwas also studied.
The composition of Qin Mountain rock was studied using a1064nm pulsedNd:YAG laser for the first time. Elements Ca, Mg, Cu, Fe, C, Na, Si and Al wereidentified qualitatively. The electron temperature and electron density wereinferred to be16835K and2.86*1018cm-3. Elements Ca, Mg, C, Si and Al wereidentified in the water scale by the analysis of the plasma spectra. The plasmatemperature4793K was inferred using the iterative Boltzmann plot method withten neutral calcium lines, while the electron density6.1*1018cm-3was obtainedfrom the Stark broadening of the profile of Mg I285.21nm. Based on the plasma spectra of egg shell, elements iron, oxygen, silicon, carbon and calcium wereidentified, and its parameters were7250K and6.1*1016cm-3, respectively.Using LIBS, the CuCl2, copper and brass, one-yuan coin and wu-jiao coin werealso studied.
引文
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