EDS分析的若干影響因素研究
發(fā)布時間：2018-10-25 16:12
【摘要】：當前能譜儀(EDS)在顯微成分分析中獲得廣泛應用,但對同一個分析樣品,不同的分析者會做出不同的分析結果,元素含量差異較大。選擇的掃描電子顯微鏡(SEM)和能譜儀參數是否合理,樣品自身條件處理是否得當均會直接影響到分析結果的準確性;因此提高定量分析結果的準確性很有必要,操作參數的選擇、技巧的運用以及樣品自身條件的處理是值得探討的。本文從樣品制備、SEM和EDS工作參數的選擇和能譜的分析與處理等對EDS定量分析準確度影響因素進行了探討。本論文使用的設備主要為日本電子JEM-6490型SEM,美國EDAX-Genesis型X射線EDS。具體研究內容如下:(1)峰漂移會影響定量分析結果,因此在進行相關實驗之前,需要進行峰位校正,確定峰位擬合完美。進行點分析時,分析模式選用縮小光柵模式。獲取峰位后先進行峰自動識別和可視化峰剝離,若有誤差再進行手動標定。對于工作參數的選擇來說,用低加速電壓分析輕元素,高加速電壓分析重元素;工作距離的大小改變特征射線的出射角;束斑控制著死時間和計數率的變動,從而影響搜集時間的選擇。這四個工作參數對含量精確度均有影響,但影響能力是否顯著需要進行驗證;該實驗借助SPSS軟件完成正交設計實驗,實驗表明這些因素對含量的影響并不顯著,但對每一種元素而言,各參數的影響力仍有區(qū)別。(2)明確工作參數對定量分析呈非顯著性影響后,開始探究樣品物理狀況對定量分析的影響。樣品首先需滿足有導電性,這樣避免荷電現象的出現;樣品各元素含量要均勻性分布,這利用軟件進行均勻性檢驗確定,這可以排除含量分布不均勻帶來的影響。樣品表面總存在污染,對于局部性污染,可以調整放大倍數控制觀察視野,來分別測試污染和基體;若是全區(qū)性碳污染,只需調整加速電壓,即可分別觀察;長時間的抽真空對降低碳含量作用不明顯。對于小尺寸的樣品,但當樣品尺寸明顯小于樣品臺的尺寸,自身高度較小時,成分含量會受到樣品臺的影響。表面傾斜的樣品會使X射線的吸收路程會減小,導致輕元素含量增加。樣品表面的凹凸會明顯影響X射線的產生和激發(fā),因此可對試樣表面進行研磨處理。對于帶腔體的樣品,當失效區(qū)域距離腔體壁的間距不小于腔體壁高度時,不易受到腔體壁的遮擋作用。
[Abstract]:At present, (EDS) is widely used in microanalysis, but for the same analytical sample, different analyzers will make different analytical results, and the content of elements will vary greatly. Whether the parameters of the scanning electron microscope (SEM) and the energy spectrometer are reasonable or not, and whether the sample's own conditions are properly handled will directly affect the accuracy of the analytical results, so it is necessary to improve the accuracy of the quantitative analysis results and the choice of the operating parameters. The application of the technique and the treatment of the sample's own condition are worth discussing. In this paper, the factors influencing the accuracy of EDS quantitative analysis are discussed from the aspects of sample preparation, selection of working parameters of SEM and EDS, and analysis and treatment of energy spectrum. The main equipment used in this thesis is Japanese electronic JEM-6490 SEM, American EDAX-Genesis X-ray EDS.. The specific research contents are as follows: (1) the peak drift will affect the quantitative analysis results, so before the relevant experiments, the peak position correction is needed to determine the perfect fitting of the peak position. For point analysis, the analysis mode is reduced grating mode. After the peak position is obtained, the peak is automatically identified and visualized, and then calibrated manually if there is any error. For the choice of working parameters, the light element is analyzed with low acceleration voltage, the heavy element is analyzed with high acceleration voltage, the output angle of characteristic ray is changed by the size of working distance, and the dead time and counting rate are controlled by beam spot. This affects the choice of collection time. These four working parameters have an effect on the accuracy of the content, but the influence ability needs to be verified, and the orthogonal design experiment with SPSS software shows that the influence of these factors on the content is not significant. However, for each element, the influence of each parameter is still different. (2) after determining the non-significant influence of working parameters on quantitative analysis, we begin to explore the effect of sample physical condition on quantitative analysis. In order to avoid the phenomenon of charge, the content of elements in the sample should be uniformly distributed, which can be determined by software homogeneity test, which can eliminate the influence of uneven distribution of content. There is always contamination on the surface of the sample. For the local pollution, we can adjust the magnification to control the observation field to test the pollution and the matrix separately, if the whole area of carbon pollution, we only need to adjust the acceleration voltage, we can observe separately. The effect of vacuum for a long time on reducing carbon content is not obvious. For small size samples, however, when the sample size is obviously smaller than that of the sample table, and the height of the sample is small, the composition content will be affected by the sample table. The sample with inclined surface reduces the absorption distance of X-ray and increases the content of light elements. The bump and concave of the surface of the sample can obviously affect the generation and excitation of X-ray, so the surface of the sample can be ground. For the sample with cavity, when the distance between the failure region and the cavity wall is not less than the height of the cavity wall, it is not easy to be blocked by the cavity wall.
【學位授予單位】：電子科技大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.62
本文編號：2294205
[Abstract]:At present, (EDS) is widely used in microanalysis, but for the same analytical sample, different analyzers will make different analytical results, and the content of elements will vary greatly. Whether the parameters of the scanning electron microscope (SEM) and the energy spectrometer are reasonable or not, and whether the sample's own conditions are properly handled will directly affect the accuracy of the analytical results, so it is necessary to improve the accuracy of the quantitative analysis results and the choice of the operating parameters. The application of the technique and the treatment of the sample's own condition are worth discussing. In this paper, the factors influencing the accuracy of EDS quantitative analysis are discussed from the aspects of sample preparation, selection of working parameters of SEM and EDS, and analysis and treatment of energy spectrum. The main equipment used in this thesis is Japanese electronic JEM-6490 SEM, American EDAX-Genesis X-ray EDS.. The specific research contents are as follows: (1) the peak drift will affect the quantitative analysis results, so before the relevant experiments, the peak position correction is needed to determine the perfect fitting of the peak position. For point analysis, the analysis mode is reduced grating mode. After the peak position is obtained, the peak is automatically identified and visualized, and then calibrated manually if there is any error. For the choice of working parameters, the light element is analyzed with low acceleration voltage, the heavy element is analyzed with high acceleration voltage, the output angle of characteristic ray is changed by the size of working distance, and the dead time and counting rate are controlled by beam spot. This affects the choice of collection time. These four working parameters have an effect on the accuracy of the content, but the influence ability needs to be verified, and the orthogonal design experiment with SPSS software shows that the influence of these factors on the content is not significant. However, for each element, the influence of each parameter is still different. (2) after determining the non-significant influence of working parameters on quantitative analysis, we begin to explore the effect of sample physical condition on quantitative analysis. In order to avoid the phenomenon of charge, the content of elements in the sample should be uniformly distributed, which can be determined by software homogeneity test, which can eliminate the influence of uneven distribution of content. There is always contamination on the surface of the sample. For the local pollution, we can adjust the magnification to control the observation field to test the pollution and the matrix separately, if the whole area of carbon pollution, we only need to adjust the acceleration voltage, we can observe separately. The effect of vacuum for a long time on reducing carbon content is not obvious. For small size samples, however, when the sample size is obviously smaller than that of the sample table, and the height of the sample is small, the composition content will be affected by the sample table. The sample with inclined surface reduces the absorption distance of X-ray and increases the content of light elements. The bump and concave of the surface of the sample can obviously affect the generation and excitation of X-ray, so the surface of the sample can be ground. For the sample with cavity, when the distance between the failure region and the cavity wall is not less than the height of the cavity wall, it is not easy to be blocked by the cavity wall.
【學位授予單位】：電子科技大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.62
【參考文獻】
相關期刊論文 前10條
1 馮善娥;高偉建;;掃描電鏡附EDS能譜儀的使用與維護[J];分析測試技術與儀器;2014年02期
2 劉松;;鋼中C元素EDS分析準確度的影響因素[J];失效分析與預防;2014年02期
3 章小余;趙志娟;劉芬;;樣品高度對XPS測試的影響[J];分析測試技術與儀器;2013年04期
4 田弋緯;陳紹楷;苗壯;常璐;胡濤濤;;影響EDS分析準確性的因素探討[J];西安文理學院學報(自然科學版);2010年03期
5 葉建海;包生祥;王嬌;張德政;;提高能譜無標樣定量分析準確度的參數選擇[J];分析測試技術與儀器;2010年02期
6 王英姿;侯憲欽;;帶能譜分析的掃描電子顯微鏡在材料分析中的應用[J];制造技術與機床;2007年09期
7 張步升;樣品表面傾角對能譜定量分析精度的影響[J];理化檢驗(物理分冊);1997年07期
8 洪建明，趙曉寧;能譜分析中應注意的幾個問題[J];電子顯微學報;1994年06期
9 張淑芳;冀克儉;李學;張銀生;;加速電壓和樣品表面粗糙度對EDS分析精度的影響[J];電子顯微學報;1993年04期
10 王典亮;洪班德;;原子序數及測試參數對塊狀樣品X射線強度比的影響[J];冶金分析與測試(冶金物理測試分冊);1984年05期
相關碩士學位論文 前2條
1 李世嵐;電子薄膜的電子探針能譜分析技術研究[D];電子科技大學;2008年
2 趙鴻飛;X射線能譜精確定量技術的研究[D];天津大學;2007年
，本文編號：2294205
本文鏈接：http://sikaile.net/kejilunwen/huaxue/2294205.html
教材專著
