- 學位論文
溶膠凝膠法製備具中孔洞結構白榴石牙科瓷之研究
Mesoporous Leucite Porcelain Synthesized by Sol-Gel Method
摘要
本實驗主要是以溶膠-凝膠法(Sol-gel)合成出具規則性排列之奈米中孔洞(mesopore)白榴石牙科瓷，實驗分成四個部份探討，分別是界面活性劑含量改變造成孔洞形成的影響因素，溫度的作用下探討孔洞的規則性現象，熟化環境溫度的變化是否能影響孔洞狀態及pH值對孔洞狀態的影響。 實驗結果顯示，可由XRD圖得知在900℃以上熱處理得到白榴石晶體。以三區塊共聚高分子作為天然模板，於室溫環境合成下可產出中孔洞粉末，由吸/脫附曲線圖形的趨勢走向，可以知道本實驗所製備的粉末內部有序中孔洞為圓柱狀通道孔洞型態，藉由恆溫吸/脫附儀的量測並配合BET與BJH理論，顯示所具有的中孔洞平均孔洞尺寸大小在7~8 nm之間，此外其他的結果，如界面活性劑添加量的多寡，可清楚顯示微胞堆積情況會影響中孔洞材料的結構，在P123莫爾分率為0.38孔洞數量最多且排列最佳。熱處理溫度對孔洞型態影響顯著，在650℃孔洞將完全被破壞。當60℃恆溫熟化在界面活性劑添加量為0.17~0.25莫爾比時有助於孔洞排列規則性，反之則不利。利用小角度繞射圖的結果分析後，可清楚得知熱處理溫度確實是具有明顯控制孔洞排列的能力。當鹽酸水溶液濃度增加時孔徑縮短，比表面積下降。由穿透式電子顯微鏡影像圖觀察證明，本實驗所製備的中孔洞粉末其孔洞型態為圓柱狀通道，孔洞排列方式則為二維-六角堆積型結構(2D-hexagonal)，是屬於對稱p6mm點群。最後在奈米銀填充所形成之奈米銀與中孔洞樣品複合粉末有抑菌效果，且奈米銀粒子粒徑大小為7~8 nm。
並列摘要
The purpose of this study was tried to fabricate the leucite porcelain with ordered mesoporous structure. We have four topics in this plan to discuss. A study amount on the basis of the interactions between inorganic-organic to form meso-structured composites.The reaction temperature is relatively order of mesostructure. The pore structures of mesoporous materials depend on the temperature changing and pore condition of mesoporous materials depend on the pH value of micells formation. The results shown the temperature of calcination over 900℃ leucite crystal was obtained. The triblock copolymer surfactant (P123) was employed as the structure agents for synthesizing the mesopore leucite at room temperature. According to the isothermal nitrogen adsorption-desorption curve and the Barrett- Emmett-Teller (BET) and Barrett-Joyner-Halanda (BJH) theories, the results shown that the mesoporous structure with the pore size of 7~8 nm. The concentration of the surfactant low micelle formation is difficult to great shape. P123 was 0.38 mol ratio to obtaine the best amount and order of mesopore. Pores were break down when the temperature of calcination were over 650℃.Decreasing surfactant mol ratio was helpful for order mesostructure formation when aging at 60℃.But it could be opposite when increasing surfactant. Then, poer size and the BET value were decreased with the increasing pH value. These results were confirmed by TEM and reveal a highly ordered 2D-hexagonal arrangement of one-dimensional channel with a symmetry p6mm space group.