Abstract
本研究利用電熱式原子吸收光譜法 (ElectrothermalAtomicAbsorption Spectrometry, ETAAS) 及中子活化分析法(Neutronactivation analysis, NAA) 探討銻化銦半導體及高純度銀金屬材料中微量元素分析的方法。研究中建立泥漿樣品導入技術(Slurrysampling technique) 配合原子吸收光譜法，以及放射化學中子活化分析法(Radiochemical NAA, RNAA)進行樣品的分析。在 ETAAS的研究中，特別針對化學修飾劑對待測元素的作用機制進行探討。本論文分為四個部份。第一部份以電熱式原子吸收光譜法進行 Te元素分析的基礎探討。研究中除了探求 Pd 及 Pd-Mg 化學修飾劑對 Te 吸收訊號的影響外，同時利用雷射剝蝕-感應耦合電漿質譜儀(LA-ICP-MS)、電熱汽化-感應耦合電漿質譜儀 (ETV-ICP-MS) 以及電子顯微鏡(SEM)， 對修飾劑和分析物間可能的反應機制進行研究。第二部份則為發展固體樣品中微量元素的直測分析技術，利用泥漿導入技術配合ETAAS 探討 InSb 中 Te 摻雜元素的分析方法。研究的結果顯示，添加適量的Pd修飾劑可有效的降低基質干擾效應並提升分析靈敏度；對於InSb 中Te 的分析，其方法偵測極限可低達 0.4 ug/g。第三部份為發展 ETAAS 及 RNAA 對 InSb 半導體材料中Te 摻雜元素的分析方法。研究中探討各種可能對分析結果造成影響的因素，並探求方法應用的可行性。本論文最後一部份係以高純度銀樣品中微量雜質元素的分析為主題，利用選擇性沈澱方法先將待測元素從銀基質中分離，再以共沉方法濃縮後，再行中子活化進行元素的測定。結果顯示，樣品基質所造成之伽傌能譜干擾可有效地去除，各待測元素(Au, Co, Cu,Hg, Zn and Fe) 的偵測極限約可低達 0.001-10 ug/g 程度。The present study is aimed at development ofelectrothermalatomic absorption spectrometry (ETAAS) and neutronactivationanalysis (NAA) for the determination of trace elementsinhigh-purity materials including indium antimonidesemiconductorand silver metal. There consists of four main partsin this work.Firstly, the effect of chemical modifiers includingpalladium andpalladium/magnesium on the determination of Te byelectrothermal atomic absorption spectrometry was investigated.The possible mechanisms of tellurium with these modifiers wereinvestigated with the assist of laser inductively coupled plasmamass (LS-ICPMS), electrothermal vaporization inductively coupledplasma mass (ETV-ICPMS) and scanning electron microscopy (SEM).Secondly, a method of slurry preparation and direct injectioninto the electrothermal atomizer for the determination oftellurium in indium antimonide was developed. The quality ofanalyte peak shape, precision, accuracy and limit of detectionachievable by the proposed method were evaluated and discussed.Thirdly, methods for the determination of dopant concentrationof Te in InSb semiconductor material by electrothermal atomicabsorption spectrometry and radiochemical neutron activationanalysis were developed. And finally, a neutron activationanalysis technique for the determination of Au, Co, Cu, Fe, Hgand Zn in high purity silver materials, based on prior isolationof analytes from the silver matrix with two steps selectiveprecipitation separation, was proposed. The practicalapplicability of the methods to real sample analysis wasevaluated and discussed.