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題 名 | 溶凝膠法製備Nano-pore氧化鋯薄膜=Synthesis of Nano-Pore Zirconia Membrane Using Sol-Gel Method |
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作 者 | 程麗純; 吳紀聖; | 書刊名 | 國立臺灣大學工程學刊 |
卷 期 | 78 2000.02[民89.02] |
頁 次 | 頁45-60 |
分類號 | 460.02 |
關鍵詞 | 氧化鋯薄膜; 溶凝膠法; 超過濾; 氣體滲透; Zirconia membrane; Sol-gel; Ultrafiltration; Gas permeation; |
語 文 | 中文(Chinese) |
中文摘要 | 本實驗在討論以鋯的醇氧化合物 (alkoxide) 經由溶膠凝膠法,製備納 米 (nano) 級的微孔型氧化鋯薄膜的方法。有別於常見的氧化鋯溶凝膠製程,本 實驗利用乙酸與丁醇進行酯化反應產生的水,與鋯之醇氧化合物進行水解反應。 由於乙酸也具有螯合物 (chelating agent) 的功能,因此可以降低醇氧化合物的高 水解速度,避免快速沉澱,可製備出均相的氧化鋯溶膠。經由氣相層析╱質譜 (GC/Mass) 分析,乙酸丁酯的生成證實了酯化反應的發生。溶膠的FT-IR分析也 證實乙酸在反應中扮演螯合物的角色。加入硝酸或水對溶膠進行peptization,可 以得到pH值分別為1以及5.5的兩種溶膠。利用旋轉塗佈法將各溶膠塗佈於 Whatman公司出品的氧化鋁薄膜上,在控制濕度及溫度的條件下乾燥,最後在 500°C煆燒後,可以由XRD與電子繞射圖分析得知氧化鋯可能為正方晶與立方 晶的混合晶相。由SEM的觀察發現,以硝酸進行peptization之溶膠可以在支撐 材上完整的披覆一層氧化鋯薄膜。由氮氣滲透法估算薄膜之流量平均孔徑 (flow average pore diameter) 約為3.63nm。未支撐 (unsupported) 的氧化鋯由氮氣吸附 法可得孔徑大小在1.5 ~ 3.5nm間。利用薄膜分離黃豆油與正己烷,可以得到37% 的阻隔率 (rejection),比未塗佈的支撐材高出許多,顯示薄膜沒有裂痕或缺陷。 TEM觀察粒徑大小約在5 ~ 10nm。然而以水進行peptization所得之溶膠有膠化 (gelation) 的趨勢。以此溶膠製成的氧化鋯薄膜,表面有少數的裂縫產生,會造 成支撐材結構的破壞,不但使得氣體滲透法出現反常的結果,進行黃豆油混合液 分離時,得到的阻隔率為負值。 |
英文摘要 | The objective of this study is to synthesize nano-pore zirconia membranes using Zr alkoxide via sol-gel route. Unlike the traditional technique, the hydrolyzing water is provided by the esterification of butanol and acetic acid. In addition, acetic acid also serves as chelating agent to stabilize the hydrolysis-condensation process so that the agglomeration of zirconia is minimized. Esterification is verified by the product, butyl acetate, determined by a GC/Mass. The chelating complex is evidenced from FTIR spectrum. The peptization is performed either adding HNO3 or H2O resulting two different sols with pH values, ~ 1 and ~ 5.5, respectively. Such sols are spin-coated on Whatman anodic discs, dried in controlled temperature and humidity, then calcined at 500°C to remove organic compounds. Zirconia might be transformed to the mixture of tetragonal and cubic forms that are indicated by XRD and electron diffraction pattern. SEM micrograph shows a uniform layer on disc which using sol peptized by HNO3. The flow average pore size of membrane is estimated 3.63nm by nitrogen gas permeation. The pore size distribution of unsupported zirconia ranges from 1.5 to 3.5nm measured by nitrogen adsorption. The rejection of soybean oil/hexane mixture reaches 37% which is much better than that of bare disc indicating that membrane is crack and defect free. TEM shows that average particle size is near 5 ~ 10nm. Gelation occurs in the sol peptized by H2O when setting for a period of time. Membrane prepared from H2O peptized sol can develop a few cracks, which cause the destruction of disc resulting anomalous gas permeation and the negative rejection of soybean oil/hexane. |
本系統中英文摘要資訊取自各篇刊載內容。