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研究生:薛美雲
研究生(外文):Shiue, Meei-Yun
論文名稱:發展電熱式原子吸收光譜法及中子活化分析技術進行銻化銦半導體材料及高純度銀金屬材料中微量元素的分析研究
論文名稱(外文):Development of Electrothermal Atomic Absorption Spectrometry and Neutron Activation Analysis for the Determination of Trace Elements in InSb Semiconductor and High-Purity Ag Metal
指導教授:楊末雄, 王素蘭
指導教授(外文):Sue-Lein Wang
學位類別:博士
校院名稱:國立清華大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:1998
畢業學年度:86
語文別:中文
論文頁數:140
中文關鍵詞:電熱式原子吸收光譜銻化銦中子活化分析法電熱式-感應耦合電漿質譜儀
外文關鍵詞:Electrothermal Atomic Absorption Spectrometryindium antimonideneutron activation analysiselectrothermal inductively coupled plasma
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本研究利用電熱式原子吸收光譜法 (Electrothermal
AtomicAbsorption 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 of
electrothermalatomic absorption spectrometry (ETAAS) and neutron
activationanalysis (NAA) for the determination of trace elements
inhigh-purity materials including indium antimonide
semiconductorand silver metal. There consists of four main parts
in this work.Firstly, the effect of chemical modifiers including
palladium andpalladium/magnesium on the determination of Te by
electrothermal atomic absorption spectrometry was investigated.
The possible mechanisms of tellurium with these modifiers were
investigated with the assist of laser inductively coupled plasma
mass (LS-ICPMS), electrothermal vaporization inductively coupled
plasma mass (ETV-ICPMS) and scanning electron microscopy (SEM).
Secondly, a method of slurry preparation and direct injection
into the electrothermal atomizer for the determination of
tellurium in indium antimonide was developed. The quality of
analyte peak shape, precision, accuracy and limit of detection
achievable by the proposed method were evaluated and discussed.
Thirdly, methods for the determination of dopant concentration
of Te in InSb semiconductor material by electrothermal atomic
absorption spectrometry and radiochemical neutron activation
analysis were developed. And finally, a neutron activation
analysis technique for the determination of Au, Co, Cu, Fe, Hg
and Zn in high purity silver materials, based on prior isolation
of analytes from the silver matrix with two steps selective
precipitation separation, was proposed. The practical
applicability of the methods to real sample analysis was
evaluated and discussed.
COVER
TABLE OF CONTENTS
LIST OF TABLES
LIST OF FIGURES
CHAPTER 1: INTRIDUCTION
1.1 ROLE OF TRACE ANALYTICAL CHEMISTRY
1.2 PURPOSE OF THIS STUDY
1.3 METHODOLOGICAL DEVELOPMENT OF ETAAS
1.4 METHODOLOGICAL DEVELOPMENT OF NAA
1.5 THE CONTENTS OF THIS THESIS
1.6 REFERENCES
CHAPTER 2: PROPOSED MECHANISM OF PALLADIUM AND PALLADIUM MEGNESIUM NITRATE MODIFIERS INFLUENCE ON TELLARIUM ATOMIZATION IN ELECTORCHERMAL ATOMIC ABSORPTION SPECTRMETRY
ABSTRACT
2.1 INTRIDUCTION
2.2 EXPERIMENTAL
2.3 RESULTS AND DISCUSSION
2.4 CONCLUSIONS
2.5 REFERENCES
TABLES
FIGURES
CHAPTER 3: DETERMINATION OF TELLURIUM IN INDIUM ANTIMONIDE BY SLURRY SAMPLING ELECTROTHERMAL ATOMIC ABSORPTION SPECTRMETRY
ABSTRACT
3.1 INTRODUCTION
3.2 EXPERIMENTAL
3.3 RESULTS AND DISCUSSION
3.4 CONCLUSIONS
3.5 REFERENCES
TABLES
FIGURES
CHAPTER 4: DETERMINATION OF TELLURIUM IN INDIUM ANTIMONIDE SEMICONDUCTOR MATERIAL BY ELECTROTHERMAL ATOMIC ABSORPTION SPECTRMETRY AND RADIOCHEMICAL NEUTRON ACTIVATION ANALYSIS
ABSTRACT
4.1 INTRODUCTION
4.2 EXPERIMENTAL
4.3 RESULTS AND DISCUSSION
4.4 CONCLUSIONS
4.5 REFERENCES
TABLES
FIGURES
CHAPTER 5: DETERMINATION OF TRACE METAL IMPURITIES IN HIGH PURITY SILIVER VIA TWO STEP SELECTIVE PRECIPITATION SEPARATION FOLLOWED BY NEUTRON ACTIVATION ANALYSIS
ABSTRACT
5.1 INTRODUCTION
5.2 EXPERIMENTAL
5.3 RESULTS AND DISCUSSION
5.4 CONDLUSIONS
5.5 REFERENCES
TABLES
FIGURES
CHAPTER 6: CONCLUSIONS
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