【摘要】：當(dāng)前能譜儀(EDS)在顯微成分分析中獲得廣泛應(yīng)用,但對同一個(gè)分析樣品,不同的分析者會(huì)做出不同的分析結(jié)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(shù)是否合理,樣品自身?xiàng)l件處理是否得當(dāng)均會(huì)直接影響到分析結(jié)果的準(zhǔn)確性;因此提高定量分析結(jié)果的準(zhǔn)確性很有必要,操作參數(shù)的選擇、技巧的運(yùn)用以及樣品自身?xiàng)l件的處理是值得探討的。本文從樣品制備、SEM和EDS工作參數(shù)的選擇和能譜的分析與處理等對EDS定量分析準(zhǔn)確度影響因素進(jìn)行了探討。本論文使用的設(shè)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(nèi)容如下:(1)峰漂移會(huì)影響定量分析結(jié)果,因此在進(jìn)行相關(guān)實(shí)驗(yàn)之前,需要進(jìn)行峰位校正,確定峰位擬合完美。進(jìn)行點(diǎn)分析時(shí),分析模式選用縮小光柵模式。獲取峰位后先進(jìn)行峰自動(dòng)識(shí)別和可視化峰剝離,若有誤差再進(jìn)行手動(dòng)標(biāo)定。對于工作參數(shù)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(shí)間和計(jì)數(shù)率的變動(dòng),從而影響搜集時(shí)間的選擇。這四個(gè)工作參數(shù)對含量精確度均有影響,但影響能力是否顯著需要進(jìn)行驗(yàn)證;該實(shí)驗(yàn)借助SPSS軟件完成正交設(shè)計(jì)實(shí)驗(yàn),實(shí)驗(yàn)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(shù)的影響力仍有區(qū)別。(2)明確工作參數(shù)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(dǎo)電性,這樣避免荷電現(xiàn)象的出現(xiàn);樣品各元素含量要均勻性分布,這利用軟件進(jìn)行均勻性檢驗(yàn)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(diào)整放大倍數(shù)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(diào)整加速電壓,即可分別觀察;長時(shí)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(dāng)樣品尺寸明顯小于樣品臺(tái)的尺寸,自身高度較小時(shí),成分含量會(huì)受到樣品臺(tái)的影響。表面傾斜的樣品會(huì)使X射線的吸收路程會(huì)減小,導(dǎo)致輕元素含量增加。樣品表面的凹凸會(huì)明顯影響X射線的產(chǎn)生和激發(fā),因此可對試樣表面進(jìn)行研磨處理。對于帶腔體的樣品,當(dāng)失效區(qū)域距離腔體壁的間距不小于腔體壁高度時(shí),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(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.62

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