摘要
本论文以硝酸锌为主要原料,采用沉淀和水热处理相结合的方法,通过添加一定量的阳离子表面活性剂,控制反应条件,分别制备了Zr掺杂ZnO粉体,Zn-Ce复合氧化物粉体和Mn掺杂ZnO粉体三种系列材料。考察了掺杂量或复合组分在产物中的含量、水热反应温度、水热时间、掺杂或复合方式等因素对材料的影响,采用多种表征手段对材料组成和结构进行了表征。同时,采用涂布制膜技术,对纳米ZnO紫外屏蔽性能进行了系统考察。实验结果如下:
对于Zr掺杂ZnO:当Zr的掺杂量为3.5%时,在阳离子表面活性剂十六烷基三甲基溴化铵的作用下,在室温下经过沉淀生成氢氧化物后,再经过150℃水热处理0.5 h,所制备的复合氧化物样品的紫外屏蔽性能最强;Zn-Ce复合氧化物中CeO2的含量为12.5%时,在室温下生成氢氧化物,再经过120℃水热处理1 h,所制备的复合氧化物样品的紫外屏蔽性能最强;当Mn掺杂ZnO的中Zr的掺杂量为3%时,在室温下经沉淀反应生成氢氧化物后,再经过150℃水热处理0.5h,所制备的Mn掺杂ZnO样品的紫外线屏蔽性能最强。为了避免表面活性剂对产物性能的影响,以上三种产物在经过水热处理后都经过去离子水和无水乙醇冲洗,以清除产物中的表面活性剂。
将所制备的复合粉体材料采用机械搅拌与超声波分散方法相结合的复合分散手段,制得复合材料的分散液,将此分散液添加到含量为9.1%的聚乙烯醇(PVA)溶胶里,制成PVA薄膜,采用紫外分光光度仪,对不同样品的紫外屏蔽性能进行了测量,分析得出:添加微量复合材料粉体的薄膜与添加纯ZnO粉体相比,对可见光透光性方面没有差别,但是对紫外线的屏蔽性有明显增强,说明通过掺杂和复合的方法可以提高材料的紫外线屏蔽的性能。
The Zr doped zinc oxide, Zn-Ce composite oxide and Mn doped zinc oxide were synthesized by combining co-precipitation and hydrothermal method under mild condition from zinc nitrate. The effects of the amount of Zr(CeO2 and Mn)in composite material, hydrothermal temperature, hydrothermal time and prepared method on composite material were systematically studied. And the prepared inorganic material were characterized by some kinds of means. The UV-Shielding property of prepared material was tested with a coating method. The results are as follows:
For Zr doped zinc oxide, the optimal amount of doped Zr is 3.5%, and the optimal process is as follows: under the effect of surfactant(CTAB), zinc nitrate and zirconium oxychloride were suffered precipitation under room temperature and then hydrothermal treatment with 150℃and 0.5h respectively; For Zn-Ce composite oxide, the optimal amount of CeO2 is 12.5%, and the optimal process is as follows: under the effect of surfactant, zinc nitrate and cerous nitrate were suffered precipitation under room temperature and then hydrothermal treatment with 120℃and 1h respectively; For Mn doped oxide, the optimal amount of Mn is 3%, and the optimal process is as follows: under the effect of surfactant, zinc nitrate and manganese nitrate were suffered precipitation under room temperature and then hydrothermal treatment with 150℃and 0.5h respectively. In order to avoid the effect of surfactant on the property of UV-Shielding, the above three kind of inorganic material were all washed by de-ionized water and ethanol.
The prepared inorganic composite material were dispersed by ultrasonic dispersion and mechanic dispersion to form dispersing agent. The thin films were prepared by adding the above dispersing agent into hydrosol of polymer binder. The UV-Shieding property of the films was tested by UV-3010 ultraviolet spectrophotometer. As the result revealed: compared with pure ZnO, these composite material has the almost same transmittance for visible light but the transmittance of ultraviolet is lower than that of ZnO. That means doping some other element(s) and compound other semiconductor can strengthen the UV-Shielding property of ZnO.
引文
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