有机样品中激光诱导等离子体时空分辨特性以及无机元素的定量分析
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摘要
本文主要阐述针对有机样品的激光诱导等离子体的机理,以及激光诱导击穿光谱(laser-induced breakdown spectroscopy-LIBS)对有机样品的定量分析。本文主要目的在于增加对一些基本物理机制的理解。这些物理机制主要包括激光与物质相互作用、等离子体的产生、演变和向环境气体的膨胀；本文还致力于如何提高激光诱导击穿光谱对有机样品的分析能力。激光在有机样品表面产生的等离子体与金属表面产生的等离子体有着明显的差别,特别是激光烧蚀样品的机制远比金属表面要复杂。正是由于有机样品的独特性,LIBS在此类样品的应用目前属于国际LIBS研究的热点。提高LIBS分析有机样品的能力在于怎么实现激光在有机样品表面产生的等离子体的时空分布稳定性和重现性。
针对LIBS对有机样品的应用,本文将按以下组织结构进行阐述：
首先,前言部分主要介绍当今LIBS的科学技术背景。第一章主要回顾一些理论知识,包括必要的激光诱导等离子体的产生和等离子体在背景气体中的膨胀过程,其中特别强调在有机样品中的应用。第二章着重于一种典型农业产品,马铃薯皮样品中等离子体的产生和演变。本文工作开始时,在软质并且潮湿的有机样品,如新鲜土豆中的等离子诱导的特点还是当时科研界的未知领域。这些特性的研究为在有机品中的痕量和超痕量金属元素定量分析提供了必要的理论基础。在阐述该样品中的等离子体特性后,本章节讨论了土豆皮中LIBS光谱特性,并且提取出半定量的分析结果。在第二章的研究基础上,本文第三章继续讨论LIBS对有机样品的定量分析。本章主要研究LIBS技术和电感耦合等离子体原子发射光谱(Inductively Coupled Plasma Atomic Emission Spectroscopy:ICP-AES)在对奶粉样品的定量分析结果的比较。该结果一方面是对LIBS技术对有机样品定量分析能力的评估,另一方面也验证了本文采用的无校准LIBS (Calibration Free-LIBS:CF-LIBS)技术手段和结果。不同于第二、三两章侧重于有机样品中的微量金属元素的测量,第四章研究的主要内容在于有机样品固有的有机结构,也就是被公认的四大有机元素C、H、O和N。由于激光烧蚀有机样品会有机结构的分解,在等离子体中这些元素可能以分子链的形式直接从样品中喷射出来；同时它们也可能通过碰撞重组,以新的分子形式存在。本章我们主要讨论这些分子的形成与激光烧蚀参数之间的联系,其中主要研究不同激光波长对样品烧蚀的影响。本文最后总结了上述工作并提出在此基础上的展望。
This PhD work was devoted to the understanding of the laser-induced plasma on organic materials and the application of laser-induced breakdown spectroscopy (LIBS) to quantitative analysis of these materials. It contributes to deepen our knowledge on the physical mechanisms involved in laser-matter interaction, plasma generation, evolution and expansion of the plasma into the ambient gas, with emphasis on plasmas induced on organic targets. It also intends to improve the performance of LIBS for the analysis of organic materials. The specificity for organic targets fits the current focus of the international community working on LIBS, to improve the control of the plasma induced on this kind of material which has a distinguished optical prosperity with respect to that of metals, better known for laser ablation. It addresses also the growing need to apply the LIBS technique to organic materials for different applications in the environmental, food, or biomedical domains.
The works in this thesis were therefore presented in this thesis document according to the following organization.
After the General Introduction which introduces the scientific and technological contexts, Chapter Ⅰ recalls the basic theoretical elements necessary to understand the phenomenon of plasma generation by laser ablation, and its evolution in the background gas. Ablation of organic material is emphasized. Procedures and techniques of diagnostics of laser-induced plasma were then presented with a focus on the transient and inhomogeneous nature of the expanding plasma. Chapter Ⅱ focuses on the generation and the evolution of the plasma induced on the skin of a potato, a typical sample of agricultural product. The characteristics of plasma induced on a soft and wet organic target, such as a fresh potato, was something unknown when the thesis work started. These characteristics provide the necessary basis for the quantitative analysis of the trace and ultra-trace metallic elements in these samples. Following this characterization, semi-quantitative analytical results were extracted from LIBS spectra corresponding to potato skin. Chapter Ⅲ is presented in the continuity of Chapter Ⅱ for the application of LIBS to the quantitative analysis of organic materials. A comparative study on the analytical results with LIBS and ICP-AES for milk powders allows an assessment of the performances of quantitative analysis by LIBS for organic materials, and a validation of the CF-LIBS procedure that we have developed. Different from Chapters Ⅱ and Ⅲ where attention was paid to trace metal elements, Chapter Ⅳ studies the behavior of the major elements that make up the matrix of organic material, which are4known organic elements:H, C, O, N. During the decomposition of organic material by laser ablation, these elements can be found in the form of molecular fragments, or recombined into molecular species. We then study in this Chapter the evolution of these species as a function of the laser ablation parameters, the laser wavelength in particular. The thesis document ends with a general conclusion and outlooks.
针对LIBS对有机样品的应用,本文将按以下组织结构进行阐述：
首先,前言部分主要介绍当今LIBS的科学技术背景。第一章主要回顾一些理论知识,包括必要的激光诱导等离子体的产生和等离子体在背景气体中的膨胀过程,其中特别强调在有机样品中的应用。第二章着重于一种典型农业产品,马铃薯皮样品中等离子体的产生和演变。本文工作开始时,在软质并且潮湿的有机样品,如新鲜土豆中的等离子诱导的特点还是当时科研界的未知领域。这些特性的研究为在有机品中的痕量和超痕量金属元素定量分析提供了必要的理论基础。在阐述该样品中的等离子体特性后,本章节讨论了土豆皮中LIBS光谱特性,并且提取出半定量的分析结果。在第二章的研究基础上,本文第三章继续讨论LIBS对有机样品的定量分析。本章主要研究LIBS技术和电感耦合等离子体原子发射光谱(Inductively Coupled Plasma Atomic Emission Spectroscopy:ICP-AES)在对奶粉样品的定量分析结果的比较。该结果一方面是对LIBS技术对有机样品定量分析能力的评估,另一方面也验证了本文采用的无校准LIBS (Calibration Free-LIBS:CF-LIBS)技术手段和结果。不同于第二、三两章侧重于有机样品中的微量金属元素的测量,第四章研究的主要内容在于有机样品固有的有机结构,也就是被公认的四大有机元素C、H、O和N。由于激光烧蚀有机样品会有机结构的分解,在等离子体中这些元素可能以分子链的形式直接从样品中喷射出来；同时它们也可能通过碰撞重组,以新的分子形式存在。本章我们主要讨论这些分子的形成与激光烧蚀参数之间的联系,其中主要研究不同激光波长对样品烧蚀的影响。本文最后总结了上述工作并提出在此基础上的展望。
This PhD work was devoted to the understanding of the laser-induced plasma on organic materials and the application of laser-induced breakdown spectroscopy (LIBS) to quantitative analysis of these materials. It contributes to deepen our knowledge on the physical mechanisms involved in laser-matter interaction, plasma generation, evolution and expansion of the plasma into the ambient gas, with emphasis on plasmas induced on organic targets. It also intends to improve the performance of LIBS for the analysis of organic materials. The specificity for organic targets fits the current focus of the international community working on LIBS, to improve the control of the plasma induced on this kind of material which has a distinguished optical prosperity with respect to that of metals, better known for laser ablation. It addresses also the growing need to apply the LIBS technique to organic materials for different applications in the environmental, food, or biomedical domains.
The works in this thesis were therefore presented in this thesis document according to the following organization.
After the General Introduction which introduces the scientific and technological contexts, Chapter Ⅰ recalls the basic theoretical elements necessary to understand the phenomenon of plasma generation by laser ablation, and its evolution in the background gas. Ablation of organic material is emphasized. Procedures and techniques of diagnostics of laser-induced plasma were then presented with a focus on the transient and inhomogeneous nature of the expanding plasma. Chapter Ⅱ focuses on the generation and the evolution of the plasma induced on the skin of a potato, a typical sample of agricultural product. The characteristics of plasma induced on a soft and wet organic target, such as a fresh potato, was something unknown when the thesis work started. These characteristics provide the necessary basis for the quantitative analysis of the trace and ultra-trace metallic elements in these samples. Following this characterization, semi-quantitative analytical results were extracted from LIBS spectra corresponding to potato skin. Chapter Ⅲ is presented in the continuity of Chapter Ⅱ for the application of LIBS to the quantitative analysis of organic materials. A comparative study on the analytical results with LIBS and ICP-AES for milk powders allows an assessment of the performances of quantitative analysis by LIBS for organic materials, and a validation of the CF-LIBS procedure that we have developed. Different from Chapters Ⅱ and Ⅲ where attention was paid to trace metal elements, Chapter Ⅳ studies the behavior of the major elements that make up the matrix of organic material, which are4known organic elements:H, C, O, N. During the decomposition of organic material by laser ablation, these elements can be found in the form of molecular fragments, or recombined into molecular species. We then study in this Chapter the evolution of these species as a function of the laser ablation parameters, the laser wavelength in particular. The thesis document ends with a general conclusion and outlooks.
引文
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