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利用乾膠長晶法合成抗腐蝕SiO2膜 = Synthesis SiO2 F...

國立高雄大學應用化學系碩士班

利用乾膠長晶法合成抗腐蝕SiO2膜 = Synthesis SiO2 Film by Dry-gel Method for Anti-corrosion Application

紀錄類型:	書目-語言資料,印刷品 : 單行本
並列題名:	Synthesis SiO2 Film by Dry-gel Method for Anti-corrosion Application
作者:	張簡文銓,
其他團體作者:	國立高雄大學
出版地:	[高雄市]
出版者:	撰者;
出版年:	2012[民101]
面頁冊數:	99面圖，表格 : 30公分;
標題:	固體轉換法
標題:	Dry Gel Method
電子資源:	http://handle.ncl.edu.tw/11296/ndltd/08464462740746080822
附註:	107年4月10日公開
附註:	參考書目：面86-91
摘要註:	本研究目的在於發展一種簡易的規則孔洞型薄膜製備方法，用以改良金屬基材表面性質，製備抗腐蝕膜，增強抗刮性能。吾人發展出乾膠長晶法，在鋁材上先行塗佈ZSM-5晶種前驅液，以固體轉換方式，藉由水作為蒸鍍液，直接長晶生成分子篩薄膜。另外，以一般常用的濕式水熱合成法在鋁片基材表面生長MFI沸石膜，在不同的反應時間下，可以生成不同厚度和顆粒大小。利用Tafel plot鑑定其抗腐蝕的能力，得知沸石膜厚度與其抗腐蝕能力並無明顯關係，只有極厚薄膜才會降低電流，具有更高的抗腐蝕能力。綜合比較兩種製備方法，結果發現乾膠長晶法生長之薄膜表面較為平整，呈現高度親水性質，在中性與酸性腐蝕溶液中的抗腐蝕能力優於濕式水熱合成法製備之沸石膜，其腐蝕機制來自於模板劑之封孔效應。以含烷基矽烷修飾沸石膜表面，可改良其疏水性質，提升其抗腐蝕能力。另外，吾人成功的在鋁片基材上成長介孔二氧化矽薄膜，Tafel plot測試結果顯示良好之抗腐蝕能力，介孔二氧化矽薄膜經由高溫鍛燒去除所含之十六烷基三甲基溴化銨(CTAB)之界面活性劑後，其抗腐蝕能力明顯降低。鍛燒後介孔二氧化矽薄膜可以回填不同之化合物，其抗腐蝕能力與化合物結構、分子尺寸有關，含浸benzotriazole防鏽劑並無明顯增強抗腐蝕能力效果，含浸C3與C12這兩種四級銨之抗腐蝕能力明顯不足，含浸C16四級銨CTAB則可以恢復其抗腐蝕能力，但不足量CTAB回填之抗腐蝕能力卻不佳，顯示介孔二氧化矽薄膜之抗腐蝕能力來自於界面活性劑封孔效應。 The purpose of this study is to develop a dry gel method for preparing order and porous films on metal substrates with improved surface properties as well as corrosion-resistant and scratch resistant properties. The dry gel method is firstly to coat the aluminum substrate with a zeolite seed precursor and then transform it directly to zeolite crystals in the presence of water vapor. On the other hand, by the conventional wet gel method, zeolite films grow via in-situ crystallization on top of aluminum substrates. Different thickness and crystal sizes can be controlled by varying synthesis recipes and reaction conditions and time. The anti-corrosion properties of various metal oxide films were evaluated electrochemically by means of Tafel plot. The anti-corrosion property of the as-synthesized zeolite films is attributed to the formation of nonporous passivation layers in the presence of structure directing agent for blocking Al substrates from the attack of air and humidity. The dry gel conversion of pre-deposited MFI zeolite precursor gel was demonstrated as an effective means for the preparation of anticorrosion coating on aluminum alloy. A 10 μm thick dense film, consisted of closely packed pure silica MFI nanocrystals was obtained in a short process time. The MFI film prepared by dry gel method is more smooth and hydrophilic than that prepared from wet gel method. A better anticorrosion performance was found comparing to the zeolite coating prepared by the conventional in-situ crystallization method in both NaCl and acidic solution. In case of wet gel method, very thick film is required for adequate corrosion resistance generating low corrosion current. There is no clear relationship between the thickness of the MFI membrane and its corrosion resistance. Modification of alkyl silanes on the MFI films prepared with both methods increases their hydrophobicity and thus corrosion resistance properties. The proposed dry gel method eliminates the suspended zeolite that always produces along with the conventional process, thus reduces waste. The need of a TEFOLN lined reactor could also be relaxed. Consequently, a zeolite anticorrosion coating can be applied more cost-effectively onto larger substrates. Furthermore, mesoporous silica film was successfully grown on aluminum substrate, showing good corrosion resistance properties. After removal of cetyltrimethylammoniumammonium bromide (CTAB) surfactant during high temperature calcination, mesoporous silica films lose their corrosion resistance properties. The corrosion resistance of the calcined mesoporous silica was restored by back loading to saturation with CTAB and benzotriazole (rust inhibitor). The corrosion resistance of the calcined mesoporous silica was poor in case of unsaturated loading or loading with quaternary C3 and C12 halide compounds. Therefore, surfactant molecules act as sealants mesoporous silica film and contribute corrosion resistance property.

利用乾膠長晶法合成抗腐蝕SiO2膜 = Synthesis SiO2 Film by Dry-gel Method for Anti-corrosion Application
張簡, 文銓

利用乾膠長晶法合成抗腐蝕SiO2膜 = Synthesis SiO2 Film by Dry-gel Method for Anti-corrosion Application / 張簡文銓撰 - [高雄市] : 撰者, 2012[民101]. - 99面 ; 圖，表格 ; 30公分.
107年4月10日公開參考書目：面86-91.
固體轉換法Dry Gel Method

利用乾膠長晶法合成抗腐蝕SiO2膜 = Synthesis SiO2 Film by Dry-gel Method for Anti-corrosion Application
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330 $a 本研究目的在於發展一種簡易的規則孔洞型薄膜製備方法，用以改良金屬基材表面性質，製備抗腐蝕膜，增強抗刮性能。吾人發展出乾膠長晶法，在鋁材上先行塗佈ZSM-5晶種前驅液，以固體轉換方式，藉由水作為蒸鍍液，直接長晶生成分子篩薄膜。另外，以一般常用的濕式水熱合成法在鋁片基材表面生長MFI沸石膜，在不同的反應時間下，可以生成不同厚度和顆粒大小。利用Tafel plot鑑定其抗腐蝕的能力，得知沸石膜厚度與其抗腐蝕能力並無明顯關係，只有極厚薄膜才會降低電流，具有更高的抗腐蝕能力。綜合比較兩種製備方法，結果發現乾膠長晶法生長之薄膜表面較為平整，呈現高度親水性質，在中性與酸性腐蝕溶液中的抗腐蝕能力優於濕式水熱合成法製備之沸石膜，其腐蝕機制來自於模板劑之封孔效應。以含烷基矽烷修飾沸石膜表面，可改良其疏水性質，提升其抗腐蝕能力。另外，吾人成功的在鋁片基材上成長介孔二氧化矽薄膜，Tafel plot測試結果顯示良好之抗腐蝕能力，介孔二氧化矽薄膜經由高溫鍛燒去除所含之十六烷基三甲基溴化銨(CTAB)之界面活性劑後，其抗腐蝕能力明顯降低。鍛燒後介孔二氧化矽薄膜可以回填不同之化合物，其抗腐蝕能力與化合物結構、分子尺寸有關，含浸benzotriazole防鏽劑並無明顯增強抗腐蝕能力效果，含浸C3與C12這兩種四級銨之抗腐蝕能力明顯不足，含浸C16四級銨CTAB則可以恢復其抗腐蝕能力，但不足量CTAB回填之抗腐蝕能力卻不佳，顯示介孔二氧化矽薄膜之抗腐蝕能力來自於界面活性劑封孔效應。 The purpose of this study is to develop a dry gel method for preparing order and porous films on metal substrates with improved surface properties as well as corrosion-resistant and scratch resistant properties. The dry gel method is firstly to coat the aluminum substrate with a zeolite seed precursor and then transform it directly to zeolite crystals in the presence of water vapor. On the other hand, by the conventional wet gel method, zeolite films grow via in-situ crystallization on top of aluminum substrates. Different thickness and crystal sizes can be controlled by varying synthesis recipes and reaction conditions and time. The anti-corrosion properties of various metal oxide films were evaluated electrochemically by means of Tafel plot. The anti-corrosion property of the as-synthesized zeolite films is attributed to the formation of nonporous passivation layers in the presence of structure directing agent for blocking Al substrates from the attack of air and humidity. The dry gel conversion of pre-deposited MFI zeolite precursor gel was demonstrated as an effective means for the preparation of anticorrosion coating on aluminum alloy. A 10 μm thick dense film, consisted of closely packed pure silica MFI nanocrystals was obtained in a short process time. The MFI film prepared by dry gel method is more smooth and hydrophilic than that prepared from wet gel method. A better anticorrosion performance was found comparing to the zeolite coating prepared by the conventional in-situ crystallization method in both NaCl and acidic solution. In case of wet gel method, very thick film is required for adequate corrosion resistance generating low corrosion current. There is no clear relationship between the thickness of the MFI membrane and its corrosion resistance. Modification of alkyl silanes on the MFI films prepared with both methods increases their hydrophobicity and thus corrosion resistance properties. The proposed dry gel method eliminates the suspended zeolite that always produces along with the conventional process, thus reduces waste. The need of a TEFOLN lined reactor could also be relaxed. Consequently, a zeolite anticorrosion coating can be applied more cost-effectively onto larger substrates. Furthermore, mesoporous silica film was successfully grown on aluminum substrate, showing good corrosion resistance properties. After removal of cetyltrimethylammoniumammonium bromide (CTAB) surfactant during high temperature calcination, mesoporous silica films lose their corrosion resistance properties. The corrosion resistance of the calcined mesoporous silica was restored by back loading to saturation with CTAB and benzotriazole (rust inhibitor). The corrosion resistance of the calcined mesoporous silica was poor in case of unsaturated loading or loading with quaternary C3 and C12 halide compounds. Therefore, surfactant molecules act as sealants mesoporous silica film and contribute corrosion resistance property.
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