羟基氧化铝纳米胶体的制备与表征
发布时间:2018-04-24 02:33
本文选题:羟基氧化铝 + 凝胶 ; 参考:《吉林大学》2015年硕士论文
【摘要】:本论文中所述的羟基氧化铝纳米胶体是指铝的氢氧化物、羟基氧化物及其各级脱水产物所形成的纳米胶体的统称,由于产物所含的Al、0、0H的比例不同,因而具有不同的结构和性质。这些胶体由于微观形貌可控,被广泛的用于结构陶瓷、催化剂、吸附剂以及微电子功能材料等,已成为当今材料科学领域的前沿研究课题之一。 在已有的制备方法中,大多数方法倾向于运用活性剂、沉淀剂、解胶剂等制备羟基氧化铝、氢氧化铝胶体。在实验过程中,还要控制pH值,反应时间也较长,反应步骤复杂,限制了这些胶体的生产与应用。因此,探究一种简单易行的方法具有十分重要的意义。本论文用溶剂热醇解法制备了不同形貌的羟基氧化铝胶体,主要研究内容和结果如下: (1)以无水氯化铝为铝源,分别与无水甲醇、无水乙醇、正丙醇在不同条件下进行反应,生成氢氧化铝纳米薄片。当反应温度降低到160℃时,无样品生成。说明无水氯化铝与醇类反应,生成羟基氧化铝胶体的下临界温度为160℃。 (2)通过X射线衍射、扫描电子显微镜和透射电子显微镜等技术对制备的样品进行表征,发现产物均为纳米片状结构,其结晶度随时间的延长和温度的升高而提高。 (3)以无水氯化铝为铝源,以甲醇为前驱物时,产物以氢氧化铝Al(OH)3为主;以乙醇、正丙醇为前驱物时,产物以氢氧化铝的各级脱水产物为主,并随温度升高和时间延长,最终转化为羟基氧化铝A1OOH。 (4)通过对观测到的现象进行系统分析,推演其反应机理,认为反应通过如下路径进行:AlCl3+3ROH→Al(OR)3+3HCl Al(OR)3+3ROH→Al(OH)+3ROR Al(OH)3→AlOOH+H2O 进而推演出片状纳米结构的生长机制:在温度较低、反应时间较短时,均生成块状Al(OH)3胶体,随着反应时间的延长,反应温度的升高,,发生不同级次的脱水,向AlOOH转化;由于AlOOH具有层状结构,在(010)表面羟基的作用下,块状Al(OH)3胶体最终分裂成片状纳米结构,温度越高,时间越长,纳米片越薄;由于表面羟基和范德华力的影响,这些纳米片在高温下发生弯曲,甚至包裹成球状。
[Abstract]:The hydroxyl alumina colloids in this thesis refer to the hydroxides of aluminum, hydroxyl oxides and the colloids formed by their dehydration products. The products have different structures and properties because of the different proportion of Al _ 2O _ 0 O _ (0) H in the products. These colloids have been widely used in structural ceramics, catalysts, adsorbents and microelectronic functional materials because of their controllable morphology, and have become one of the leading research topics in the field of material science. In the existing preparation methods, most of the methods tend to use active agents, precipitators and colloids to prepare hydroxyl alumina and aluminum hydroxide colloids. In the process of experiment, pH value should be controlled, the reaction time is longer and the reaction steps are complicated, which limits the production and application of these colloids. Therefore, it is of great significance to explore a simple and easy method. In this thesis, hydroxyl alumina colloids with different morphologies were prepared by solvothermal alcoholysis. The main contents and results are as follows: Using anhydrous aluminum chloride as aluminum source, anhydrous methanol, anhydrous ethanol and n-propanol were reacts under different conditions to produce aluminum hydroxide nanocrystals. When the reaction temperature was reduced to 160 鈩
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