博碩士論文 982203008 詳細資訊


姓名 楊巧薇(Ciao-Wei Yang)  查詢紙本館藏   畢業系所 化學學系
論文名稱 含有機胺配位基金屬鍺酸鹽的合成與鑑定
(Synthesis and Characterization of Metal Germanates Incorporating Organic Amine Ligands)
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摘要(中) 本論文合成6個新穎結構的化合物,A系列合成有機胺金屬鍺酸鹽化合物:Zn2Ge4O10(NH2CH2CH2CH2NH2) (A1)、ZnGe2O5(NH2CH2CH2NH2) (A2)、β-In2Ge6O15(NH2CH2CH2NH2)2 (A3)以及γ-In2Ge6O15(NH2CH2CH2NH2)2 (A4);B系列合成鋅金屬有機鍺酸鹽化合物:ZnE2Ge2O3 (B1)以及Zn2EGeO3 (B2)。此兩系列的化合物利用單晶X光繞射法解析出化合物的結構及化學式,並進行結構上的深入探討,以粉末X光繞射分析確定樣品純度後進行儀器的量測,例如:元素分析、紅外線光譜分析、熱重分析。
A系列主要介紹使用不同的金屬 ( Zn與In ) 與二氧化鍺,藉由中溫溶劑熱法來合成四個新穎結構的有機胺金屬鍺酸鹽化合物,化合物A1與A2是使用有機胺作為溶劑,則化合物A3與A4則使用2-methylpentamethylenediamine作為溶劑,A1是由ZnO4N雙三角錐以共邊的方式形成無限延伸的鏈狀結構並與[Ge4O10]的層狀結構相互連接形成的三維結構;A2是由ZnO2N2四面體與[Ge2O5]的層狀結構相互連接形成的三維結構;則A3與A4是polymorphs皆是由In2O6N4的雙具體與鍺酸鹽的層狀結構相互連接形成的三維結構。
B系列主要介紹使用有機鍺作為起始物與鋅金屬在中溫水熱法下進行反應,因此獲得兩個新穎結構的鋅金屬有機鍺酸鹽化合物,化合物B1是藉由E官能基連接鍺酸鹽層和ZnO4四面體所形成三維的結構;B1是由混金屬層和E官能基連接形成的三維結構。
摘要(英) There are six novel compounds. The series A denotes organic amine metal-germanate, Zn2Ge4O10(NH2CH2CH2CH2NH2) (A1)、ZnGe2O5(NH2CH2CH2NH2) (A2)、β-In2Ge6O15(NH2CH2CH2NH2)2 (A3) and γ-In2Ge6O15(NH2CH2CH2NH2)2 (A4). The series B denotes zinc-organogermanate, ZnE2Ge2O3 (B1) and Zn2EGeO3 (B2). All structures are determined by single-crystal X-ray diffraction, and the details of these structures are discussed. The purity of each compound was confirmed by thepowder X-ray diffraction analysis, and the properties of these compounds were further characterized by different instrumental measurements, such as element analysis, infrared spectra analysis, and thermogravimetric analysis.
The A series were synthesized under solvothermal conditions by choosing different metals and organic amines to form organic amine metal-germanate. Compound A1 and A2 used organic animes as solvents, while compound A3 and A4 used 2-methylpentamethylenediamine as solvent. A1 strucutre is characterized by infinite chain formed of edge-sharing ZnO4N trigonal bipyramds and [Ge4O10] layers to form 3D framework. A2 strucutre is characterized by ZnO2N2 tetrahedra and [Ge2O5] chains to form 3D framework. A3 and A4 are polymorphs. Their strucutres are characterized by In2O6N4 dimers and germanates layers to form 3D framework.
The B series were synthesized hydrothermal conditions by choosing zinc metal and organogermanate to form zinc-organogermanate. B1 structure is characterized by E goups linked to germanate layers and ZnO4 tetrahedra into 3D framework. B2 structure is characterized by E groups linked to mixed metal layers into 3D framework.
關鍵字(中) ★ 孔洞材料
★ 有機胺金屬鍺酸鹽
★ 溶劑熱法
★ 水熱法
關鍵字(英) ★ hydrothermal
★ solvothermal
★ organic amine metal-germanate
★ porous materials
論文目次 謝誌 i
摘要 ii
Abstract iv
目錄 v
圖目錄 viii
表目錄 xii
第一章 緒論 1
1-1簡介 1
1-2 論文研究動機 9
1-3 合成方式 10
1-3-1 水熱法 10
1-3-2 助熔劑長晶法 14
1-3-3 藥品一覽表 16
1-4 鑑定方法 17
1-4-1 儀器測量簡介 17
1-4-2 單晶X-ray繞射儀與解構分析 17
1-4-3 粉末X-ray繞射儀 20
1-4-4 元素分析 21
1-4-5 X-ray能量散佈分析(EDX) 21
1-4-6 熱重分析 21
1-4-7 紅外線光譜儀 21
1-5 研究成果與摘要 23
第二章 有機胺金屬鍺酸鹽化合物 25
2-1 簡介 25
2-2 實驗部分 36
2-2-1 合成 36
2-2-2 單晶X-ray結構解析 38
2-3 化合物鑑定 41
2-3-1 粉末X-ray繞射分析 41
2-3-2 X-ray能量散佈分析 46
2-3-3 元素分析 46
2-3-5 紅外光譜分析 47
2-3-5熱重分析 51
2-4 結構描述 54
2-4-1 Zn2Ge4O10(NH2CH2CH2CH2NH2) (A1) 之結構描述 54
2-4-2 ZnGe2O5(NH2CH2CH2NH2) (A2) 之結構描述 58
2-4-3 β-In2Ge6O15(NH2CH2CH2NH2)2 (A3)之結構描述 61
2-4-4 γ-In2Ge6O15(NH2CH2CH2NH2)2(A4)之結構描述 64
2-5 結果與討論 67
第三章 鋅金屬有機鍺酸鹽化合物 69
3-1 簡介 69
3-2 實驗部分 72
3-2-1 合成 72
3-2-2 單晶X-ray結構解析 73
3-3 化合物鑑定 75
3-3-1 粉末X-ray繞射分析 75
3-3-2 X-ray能量散佈分析 76
3-3-3 元素分析 76
3-3-5 紅外光譜分析 76
3-3-5熱重分析 78
3-3 結構描述 81
3-3-1 ZnE2Ge2O3 (B1)之結構描述 81
3-3-2 Zn2EGeO3 (B2) 之結構描述 85
3-4 結果與討論 88
第四章 總結 90
參考文獻 93
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指導教授 李光華(Kwang-Hwa Lii) 審核日期 2011-7-14
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