此篇論文包含兩部份材料檢測。第一部分為聚丁二酸二丁酯共聚少量2-甲基二丙酯。第二部份為由五種牙科用鑄造合金與一種二氧化鋯陶瓷製作共六種植牙牙冠之研究。
共聚酯合成後以NMR檢測為89 mol%丁二酸二丁酯與11 mol% 2-甲基二丙酯所組成，且單體是以無序排列存在，以微差式掃描熱卡儀(DSC)研究等溫結晶動力學其溫度 (Tc) 範圍由75至91 °C，完成等溫結晶後再以DSC改變Tc、結晶時間與掃描速率觀察熔融行為。DSC可看出三個熔融峰，多重熔融行為研究顯示溫度較高之二個熔融峰且認為是由主要結晶(Primary)與再結晶或晶體層板厚度不同所造成，當Tc愈高，再結晶現象趨緩最後則消失。利用Hoffman-Weeks線性外插法得到平衡熔點為118.4 °C。以光學顯微鏡配合CCD鏡頭紀錄並計算出Tc在69與91 °C間之球晶成長速率，將球晶成長速率作動力學分析可得到regime II-III轉移溫度約為77.2 °C。
將五種鑄造合金分別做成10 × 9 × 4 mm塊材。塊材製作過程與牙冠皆相同。將表面經氧化處理後以X光光電子能譜儀(XPS)與掃描式電子顯微鏡(SEM)分析；塊材經燒附陶瓷後厚度約為5.5 mm，將側向橫截面利用電子探微儀(EPMA)做分析。另將五種合金與二氧化鋯製作標準上顎骨前臼齒牙冠。將牙冠置於訂製之夾具上配合萬用材料試驗機以0.5 mm/min施加載重於咬合面中間直到斷裂，計算各合金牙冠斷裂時之平均載重且利用one-way analysis of variance (ANOVA)與Tukey test作多重比較(α=0.05)，另將斷裂試片表面利用SEM觀察，結果發現XPS、SEM與EPMA指出合金表面(或合金與陶瓷界面)有銦(or/and 錫、鋅等)的氧化層，觀察由合金內至界面金屬元素含量變化，發現金屬氧化物逐漸增加，貴金屬則逐漸減少。藉由XPS、SEM與EPMA檢測金屬-陶瓷界面以了解牙冠之破壞強度與破壞路徑間關係。

This thesis contains two parts of materials characterization. Part I is a poly(butylene succinate) copolymer with minor amount of 2-methyl-propylene succinate. In the second part, six kinds of implant crowns made from five dental casting alloys and one Zircoina ceramic are studied.
Copolyester was synthesized and characterized as having 89.0 mol% butylene succinate units and 11.0 mol% 2-methyl-propylene succinate units in a random sequence, revealed by NMR. Isothermal crystallization kinetics was studied in the temperature range (Tc) from 75 to 91 °C using differential scanning calorimeter (DSC). The melting behavior after isothermal crystallization was studied by using DSC by varying the Tc, the crystallization time and the scanning rate. DSC curves showed triple melting peaks. Multiple melting behaviors indicate that the upper melting peaks are associated with the primary and the recrystallized crystals, or the crystals with different lamellar thickness. As the Tc increases, the contribution of recrystallization slowly decreases and finally disappears. A Hoffman-Weeks linear plot gives an equilibrium melting temperature of 118.4 °C. The spherulitic growth rates of this copolyester were measured at Tc between 69 and 91 °C using an optical microscope equipped with a CCD camera. The kinetic analysis of the growth rates gave a regime II-III transition temperature at about 77.2 °C.
Rectangular specimens of 10 × 9 × 4 mm were made of five kinds of casting alloys, separately. They were treated in the same procedures as crowns did. Their surfaces after oxidation were analyzed using x-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Rectangular specimens after applying porcelains were ~5.5 mm thick. The cross-section areas were studied by electron probe micro analyzer (EPMA). Standardized maxillary premolar crowns were fabricated with five different alloys and one Zircoina ceramic. The crown specimens were positioned in a custom testing apparatus and vertically loaded on the middle of the occlusal surface with a universal testing machine at a crosshead speed of 0.5 mm/min until fracture. Mean values of load at fracture were calculated in each alloy and compared with a one-way analysis of variance and Tukey test (α=0.05). The fracture surfaces were examined using SEM. The results of XPS, SEM and EPMA indicate that on the surface there was an oxidation layer (or interface between metal and ceramic) of indium (or/and tin, zinc, etc.). The concentration of oxide metal increased, whereas that of precious metal decreased, from bulk to interface. The fracture strength and the fracture path of the crowns were correlated with the metal-ceramic interface of the rectangular specimens that was characterized using XPS, SEM and EPMA.

目 錄…………………………………………………………………………………Ⅰ
Scheme Contents……………………………………………………………………..Ⅳ
表目錄……………………………………………………………………………......Ⅳ
圖目錄……………………………………………………………………………......Ⅴ
摘要……………………………………………………………………………….….Ⅷ
Part I 聚丁二酸二丁酯共聚10 mol%聚丁二酸2甲基二丙酯之檢測與分析
第一章 序論
1.1簡介…………………………………………………………………........1
1.2 研究目的………………………………………………………………...2
1.3 實驗流程圖……………………………………………………………...3
第二章 文獻回顧
2.1 聚丁二酸二丁酯與聚丁二酸2-甲基二丙酯與其共聚酯之結晶結構...5
2.2高分子之結晶與熔融行為 (crystallization kinetics)…..………………..5
2.2.1 Avrami 方程式………………………………………................6
2.2.2 多重熔融峰之行為……………………………………................7
2.2.3 Hoffman-Weeks線性外插……………………………………...8
2.3 結晶成長速率與區型轉移(regime transition)之分析........................….9
2.3.1 偏光顯微鏡……………………………………………………..10
第三章 實驗
3.1 實驗材料…………………………………………………….…………13
3.2 實驗儀器與設備…………………………………………………….…13
3.3 樣品製備
3.3.1 樣品的純化…………………………………………………..…14
3.3.2 薄膜試片壓製…………………………………………………..14
3.4 性質檢測分析
3.4.1 分子量的量測………………………………………………..…15
3.4.2 化學結構分析……………………………………………..……15
3.4.3 玻璃轉移溫度(Tg)與熔融溫度(Tm)的量測…………………….15
3.4.4 熱穩定性………………………………………………………..16
3.5 等溫結晶動力學與熔融行為
3.5.1 等溫結晶動力學分析……………………………………….….16
3.5.2 熔融行為……………………………………………………......16
3.6 球晶成長速率、形態與區型轉移(regime transition)分析……………17
3.6.1 等溫結晶………………………………………………………..17
3.6.2 晶體結構………………………………………………………..17
第四章 結果與討論
4.1 分子量的量測……………………………………………………….…18
4.2 化學結構分析……………………………………………………….…18
4.3 熱穩定性分析……………………………………………………….…19
4.4 晶體結構……………………………………………………………….20
4.5 熱性質分析……………………………………………………….……20
4.6 等溫結晶動力學分析………………………………………………….20
4.7 熔融行為………………………………………………………….........21
4.8 等溫結晶之球晶成長速率與區型轉移分析…………………….……22
4.9 結晶形態………………………………………………………….……23
第五章 結論……………………………………………………………………...….24
參考文獻…………………………………………………………………………..…50

Part II 比較人工植牙不同金屬襯底牙冠陶瓷之氧化層與斷裂強度分析
第六章 序論
6.1 簡介…………………………………………………………………….54
6.2 研究目的……………………………………………………………….55
第七章 文獻回顧……………………………………………………………………56
第八章 實驗
8.1 實驗材料……………………………………………………………….60
8.2 實驗儀器與設備……………………………………………………….60
8.3 樣品製備……………………………………………………………….61
8.4 X光光電子能譜儀(XPS)..……………………………….…………..63
8.5 掃描式電子顯微鏡(SEM)…………………………………………..…63
8.6 電子探微儀(EPMA)..……………………………………………….....64
8.7 萬用材料試驗機………………………..……………………………...64
第九章 初步結果與討論
9.1 合金襯底之表面氧化物分析………………………………………….66
9.1.1 Argelite 50………………………………………………….….…66
9.1.2 Aquarius……….…………………………………………….…...67
9.2 烤瓷牙冠斷裂分析…………………………………………………….68
第十章 未來工作……………………………………………………………………69
參考文獻…………………………………………………………………………..…88

第一部份
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