臺灣博碩士論文加值系統

三氧礦化物 (Mineral trioxide aggregate, 簡稱MTA) 為矽酸鈣鹽水泥，因其良好的生物相容性、密封性、X光不透性與高鹼性等特性，已被廣泛應用於根管治療中。MTA主要成分為波特蘭水泥，並添加氧化鉍作為顯影材料提供足夠的X光不透性；本研究即以添加氧化鉿對氧化鉍進行改質，期望提升MTA材料之應用性。
本研究以硝酸鉍與硫酸鉿作為前驅物，利用溶膠凝膠法配合後續熱處理 (400 °C、500 °C、600 °C、700 °C與800 °C) 合成氧化鉍鉿複合粉體，所得粉體以熱重分析、X光繞射分析、掃描式電子顯微鏡與穿透式電子顯微鏡進行材料特性與晶體結構分析；接著將所得複合粉體作為MTA之顯影材料，根據MTA之組成 (75 wt.% 波特蘭水泥/20 wt.% 氧化鉍鉿複合粉體/5 wt.% 半水硫酸鈣) 製成試片，進行X光不透性分析，並以X光不透性挑選最佳組成比例，進行後續固化特性檢測、臨床應用特性分析與生物相容性評估。
實驗結果顯示：以溶膠凝膠法製備氧化鉍鉿複合粉體做為MTA之顯影材料 (radiopacifier) 時，添加適量的氧化鉿能提升其X光不透性，且其硬化時間與直徑抗拉強度皆優於標準氧化鉍MTA試片；進一步使用10 wt.% 氯化鈣水溶液與23.1 wt.% 乳酸葡萄糖酸鈣水溶液混合調拌時，皆能有效降低其硬化時間，且使用23.1 wt.% 乳酸葡萄糖酸鈣水溶液大幅提升了調拌時的操作性；生物相容性評估結果得知，本研究製備之氧化鉍鉿最佳組成參數，具有良好的生物相容性，能作為根管填充與顯影材料。

Mineral trioxide aggregate (MTA) has been classified as calcium silicate-based cement and its extensive endodontic therapy is attributed to its excellent advantages of biocompatibility, sealing ability, radiopacity, and alkalinity. MTA contains Portland cement as the main component and bismuth oxide (Bi2O3) as the radiopacifier. In the present study, hafnia was added into bismuth oxide to enhance the practical application of MTA.
In the present study, bismuth/hafnium oxide composite powder were synthesized from bismuth nitrate and hafnium sulfate with various Bi/Hf ratios by sol-gel process, and followed by calcining at different temperatures (400, 500, 600, 700, and 800 oC). The characteristic and crystal structure of as-prepared composite powder were investigated by thermogravimetry analysis, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Then, the MTA specimen were prepared according to the composition of MTA (75 wt.% Portland cement, 20 wt.% bismuth/hafnium oxide composite powders, and 5 wt.% calcium sulphate hemihydrate). The radiopacity of MTA sample was examined to determine the optimal composite composition. The solidification characteristics, characteristics during clinical application, and biocompatibility with selected samples were investigated.
The results suggest that: the addition of hafnia in the bismuth oxide powders can increase the radiopacity. The composite powder with 10 mole% hafnia addition and calcined at 700 oC exhibited the highest radiopacity of 6.26 ± 0.34 mmAl in the present study. Moreover, the Bi/Hf oxide composite powders revealed a relatively short setting time and a high DTS (diameter tensile strength) value, which were also better than the standard Bi2O3 MTA sample. The setting time can be reduce effectively by mixing with 10 wt.% CaCl2 solution or 23.1 wt.% calcium lactate gluconate (CLG) solution. In addition, the characteristic of MTA mixed with CLG solution improve the setting property significantly. MTA prepared by optimal bismuth/hafnium oxide composite powders exhibited also good biocompatibility and can be used as radiopacifier in MTA.

誌謝 I
中文摘要 III
Abstract V
目錄 VII
表目錄 XII
圖目錄 XIII
第一章 前言 1
第二章 文獻回顧 3
2.1 根管治療 3
2.1.1 根管治療的原則 3
2.1.2 根管修補材料 5
2.2 三氧礦化物(Mineral trioxide aggregate, MTA) 7
2.2.1 MTA之發展與組成 7
2.2.2 MTA之X光不透性 9
2.2.3 MTA之生物相容性與動物實驗 11
2.3 MTA之水合反應(Hydration) 13
2.3.1 水合反應機制 14
2.3.2 影響水合作用的因素 16
2.3.3 不同水溶液對MTA固化之影響 17
2.4 顯影材料 (Radiopacifier) 23
2.4.1 氧化鉍 24
2.4.2 氧化鋯 28
2.4.3 氧化鉿 30
2.5 陶瓷粉體的製備方法 31
2.5.1 溶膠凝膠法 33
2.5.2 噴霧熱解法 37
第三章 實驗步驟 40
3.1 實驗流程 40
3.2 溶膠凝膠法製備Bi2-xHfxO3+x/2複合粉體 42
3.3 粉體之特性分析 44
3.3.1 熱重分析 （TGA） 44
3.3.2 X-ray繞射分析 （XRD） 44
3.3.3 掃描式電子顯微鏡 （SEM） 45
3.3.4 穿透式電子顯微鏡 （TEM） 45
3.4 MTA 樣品之製備與分析 46
3.5 MTA之固化特性分析 47
3.5.1 X 光不透性 (Radiopacity) 分析 47
3.5.2 硬化時間 (Setting time) 48
3.5.3 直徑抗拉強度 (Diameter tensile strength) 49
3.6 MTA 臨床應用上之特性分析 50
3.6.1 水合溫度變化量測 (Temperture Change) 51
3.6.2 酸鹼值量測 (pH value of Leachate solution) 51
3.7 MTA 之生物相容性評估分析 52
3.7.1 細胞毒性分析 53
3.7.2 細胞增生分析 58
3.7.3 細胞貼附 60
第四章 結果與討論 61
4.1 Bi2-xHfxO3+x/2複合粉體之特性分析 61
4.1.1 Bi2-xHfxO3+x/2複合粉體之熱分析 61
4.1.2 Bi2-xHfxO3+x/2複合粉體之X光繞射分析 62
4.1.3 Bi2-xHfxO3+x/2複合粉體之SEM分析 66
4.1.4 Bi2-xHfxO3+x/2複合粉體之TEM分析 72
4.2 Bi2-xHfxO3+x/2複合粉體之MTA樣品固化特性分析 74
4.2.1 X 光不透性 74
4.2.2 硬化時間 79
4.2.3 直徑抗拉強度 83
4.3 Bi2-xHfxO3+x/2複合粉體之MTA樣品臨床應用分析 86
4.3.1 溫度變化量測 (Temperature change) 86
4.3.2 酸鹼值量測 (pH value of leachate solution) 87
4.4 Bi2-xHfxO3+x/2複合粉體之MTA樣品生物評估分析 89
4.4.1 MTT 細胞毒性分析 89
4.4.2 LDH 細胞毒性分析 90
4.4.3 WST-1 細胞增生 91
4.4.4 細胞貼附觀察 92
第五章 結論 94
參考文獻 96
 
附錄 108
A. Zr1-xHfxO2複合粉體之製備 108
A.1 噴霧熱解法製備Zr1-xHfxO2複合粉體 108
B. Zr1-xHfxO2複合粉體之特性分析 110
B.1 噴霧熱解法製備氧化鋯鉿複合粉體之熱分析 110
B.2 Zr1-xHfxO2複合粉體之X光繞射分析 111
B.3 Zr1-xHfxO2複合粉體之SEM分析 114
B.4 Zr1-xHfxO2複合粉體之TEM分析 116
C. Zr1-xHfxO2複合粉體之MTA樣品固化特性分析 119
C.1 X 光不透性 119
C.2 硬化時間 123
C.3 直徑抗拉強度 126
D. Zr1-xHfxO2複合粉體之MTA樣品生物評估分析 128
D.1 MTT細胞毒性分析 128
D.2 LDH細胞毒性分析 129
D.3 WST-1細胞增生 130
D.4 細胞貼附觀察 131

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