微乳液反应合成纳米（生物）陶瓷粉末（ZrO₂, SiO₂）的研究

【作者】 骆锋；

【导师】 阮建明；

【作者基本信息】 中南大学 ， 材料学， 2004， 硕士

【摘要】 本课题对液相法制备无机纳米粉末及其改性开展了研究工作。通过实验研究了配制微乳液体系的条件；选用硅酸盐溶液／环己烷／聚乙二醇辛基苯基醚／正戊醇体系的微乳液体系，制备了纳米SiO₂粉末并对其进行了表面改性及生物学上应用的研究；同时采用微乳液法和化学共沉淀法制备了纯纳米ZrO₂粉末以及掺杂有CaO的纳米ZrO₂-CaO纳米粉末，研究了掺杂对ZrO₂物相的稳定作用；考察了一系列工艺条件尤其是共沸蒸馏脱水工艺对粉末制备的影响，对制得的无机纳米粉末进行了表征。 研究表明：在实验条件下，可配制环己烷／OP乳化剂／正戊醇／去离子水的微乳液体系来制备无机纳米粉末；采用可溶性硅酸盐溶液／OP乳化剂／正戊醇／环己烷的微乳液体系能够制备出比表面积在400～650m²／g左右，粒径可控制在15～30nm左右的纳米SiO₂粒子；通过硅烷偶联剂对纳米SiO₂粉末的改性取得了一定的效果，偶联剂特征基团与SiO₂颗粒表面存在一定的结合，多聚赖氨酸-SiO₂纳米复合载体能有效转移质粒DNA进入HNE1细胞，并能产生较好的绿色荧光蛋白表达。 在可溶性锆盐溶液／环己烷／聚乙二醇辛基苯基醚／正戊醇的微乳液体系中可以制备粒径小于40nm的超细分散纳米ZrO₂粉末，颗粒大小分布狭窄，分散性较好；以氯氧化锆、硝酸钙和氨水为原料，掺杂5％摩尔硝酸钙与共沸蒸馏分散相结合，用化学共沉淀法制备纳米ZrO₂-CaO粉末，在600℃至1100℃温度范围内热处理后可得到四方相ZrO₂，而采用微乳液法制备的纳米ZrO₂-CaO粉末经过1000℃焙烧后全部为稳定的立方相结构；经过共沸蒸馏后粉末表面被有机的正丁醇分子所包围，因此能有效脱除液相法所制备的无机纳米凝胶表面的吸附水，防止在干燥和焙烧时硬团聚体的形成，得到比表面积较大、粒径较小的纳米粉末。更多还原

【Abstract】 In this paper, preparation of inorganic nanometer powders with liquid phase method and modification was studied. The formation of microemulsion was investigated; the microemulsion system of silicate solution, cyclohexane, OP-10, and n-pentanol was selected to prepare nanometer silica particles, and the modification and application in biology of nanometer silica particles were studied; nanometer ZrO2 and ZrO2-CaO particles were prepared by microemulsion method and chemical co-precipitation method, the effect of adulteration on ZrO2 phase stabilization was studied; the effects of a series of conditions especially azeotropic distillation on the property of powders were studied, the powders were characterized.The research indicated that: The microemulsion system of silicate solution, cyclohexane, OP-10, and deionizing water can be selected to prepare inorganic nanometer powders experimentally; nanometer silica particles with the size 15~30nm and the specific surface area of powder is up to 400~650m2/g were prepared with the microemulsion system of silicate solution, cyclohexane, OP-10, and n-pentanol; nanometer silica particles modified by silane coupling agent had gained a little effect, nanometer poly-L-lysine/SiO2 composite carrier could transfer DNA into HNE1 cell efficiently and get good green fluorescent protein expression.The size of nanometer ZrO2 particles smaller than 40nm were prepared by microemulsion reaction method, where the microemulsion system includes ZrOCl2-8H2O solution, n-pentanol, OP-10, and cycloherane; with zirconium oxychloride and amonium as the raw materials, nanometer ZrO2-CaO particles were prepared by chemical co-precipitation method under the doping of nitrate of lime and azeotropic distillation, the stable region of tetragonal phase is from 600℃ to 1100℃, nanometer ZrO2-CaO particles by microemulsion method and calcined at 1000℃ were all cube phase structure; the azeotropic distillation process could effectively dehydrate hydrous inorganic nanometer powders and prevent the formation of the hardagglomerates during the evaporation.更多还原