论文总字数：24012字

摘 要

本文介绍了测量分析微体积器件内部气体成分的方法，主要分为破坏法与非破坏法，对于一些材料坚固或成本较高的器件只能采用非破坏性方法来分析其内部气体成分。用非破坏性方法分析器件内部气体成分属于微量气体分析，介绍了微量气体分析的研究内容和研究现状。

本文中阐述并对比了非破坏分析中常用的方法，包括气相色谱法、光谱法和四极质谱法。其中，四极质谱法结构简单、灵敏度高、检测速度快，并且带有封闭式离子源的四极质谱仪能保持离子源内外较高的压强差，提高了测量微量气体时的灵敏度。

本文中对样品室的本底进行了测量分析，实验表明样品室真空性比较好，没有出现漏气，样品室的放气量极小对实验测量基本没有影响。对不漏气的样品进行了实验测量，结果表明样品材料表面吸附的气体主要为水汽，并且在放入真空系统中第二天样品材料表面脱附气体量大幅减少。

本文采用非破坏性分析中的四极质谱法对充有氢气的两个样品进行了实验分析，实验得出样品渗透出来的气体是可以测得的；气体信号强度较弱的情况下，可以通过积累法使气体富集，增强其信号强度；样品结构对渗透率的影响很大，不同结构的样品渗透率不同。

关键词：非破坏法、微量气体分析、四极质谱法、气体成分分析

Abstract

In this paper, the methods of measuring gas composition in micro volume devices were introduced, which mainly divided into destructive method and non-destructive method. For some devices with firm materials or high cost, only non-destructive methods can be used to analyze the internal gas composition. The analysis of gas composition in the device by non-destructive method belongs to trace gas analysis, introduced the research content and present situation of trace gas analysis.

The methods commonly used in non-destructive analysis are expounded and compared in this paper. These methods include gas chromatography, optical spectroscopy and quadrupole mass spectrometry. The quadrupole mass spectrometry has simple structure, high sensitivity and fast detection speed, and the quadrupole mass spectrometer with a closed ion source can maintain a high pressure difference between the inside and outside of the ion source, improving the sensitivity of the measurement of trace gases.

The background of the sample was analyzed in this paper, and the experiment showed that the sample room had a good vacuum, the minimum amount of air released from the sample chamber has little effect on the experimental measurement. The measurement result of airtight sample show that the adsorbed gas of the sample material is mainly water vapor, and the amount of desorption gas on the surface of the sample material was greatly reduced the next day after the sample was placed in the vacuum system.

In this paper, two samples filled with hydrogen were analyzed by quadrupole mass spectrometry in non-destructive analysis. The experimental results showed that the gas permeated from the sample can be measured; and when the gas signal strength is weak, the gas can be enriched through the accumulation method to enhance its signal strength. The sample structure has a great impact on the permeability, and the permeability of samples with different structures is different.

Key words: non-destructive method, trace gas analysis, quadrupole mass spectrometer, gas composition analysis

目 录

摘 要 I

Abstract II

第一章 绪论 1

1.1引言 1

1.2器件内部气体成分分析方法 1

1.3微量气体分析的研究内容和研究现状 2

1.4非破坏性分析常用方法 4

1.4.1气相色谱法 4

1.4.2光谱法 6

1.4.3四极质谱法 8

1.4.4几种方法的对比总结 9

1.5本文的研究目的和主要研究内容 10

第二章 实验设备及实验方法 11

2.1真空系统的设计与组装 11

2.2样品的测量 13

2.3本章小结 14

第三章 结果分析 15

3.1样品室本底测量分析 15

3.2空白样品的测量分析 16

3.3待测样品的测量分析 19

3.3.1样品1的测量分析 19

3.3.2样品2的测量分析 23

3.3.3误差分析 25

3.4本章小结 26

第四章 总结与展望 27

4.1全文总结 27

4.2展望 27

致 谢 28

参考文献 29

第一章 绪论

1.1引言

气体分析是指通过相应设备和技术手段对待测气体的组成成分进行定性、定量的分析方法。气体分析的应用范围极为广泛，在电子工业、医疗卫生、地质勘测、航空航天等方面都有着十分重要的作用。

气体分析包括常量气体分析与微量气体分析。相比于常量气体分析，微量气体分析所针对的待测气体的样品含量较小或是待测气体中某一组分的含量较小，一般其含量在ppm或ppb量级。并且由于其含量低，在真空系统中的易被干扰且保留时间会比较短。这就对微量气体的分析方法提出了高灵敏度、高准确度以及实时快速的要求。

1.2器件内部气体成分分析方法

对器件内部气体成分分析的方法有很多种，按是否损坏样品可分为破坏性分析和非破坏性分析。

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