摘要
近年来,绿色化学己成为人们广为关注的新兴课题。根据绿色化学原理,本文针对石英晶体微天平敏感膜的要求,设计了一种低温无模板的水热合成新方法。通过对反应条件的控制和优化,使水热温度最高不超过120℃,反应时间缩短至3小时。与传统水热法最高250℃水热温度和24小时以上的水热时间相比,此法更加节能环保。在元素周期表中均匀选取了五种金属元素,即Sn, Fe, Zr,La和Mg。用新法成功合成了相应的纳米氧化物,即SnO2, Fe2O3, ZrO2, La2O3和MgO纳米材料。随后对这五种材料进行了X射线衍射和扫描隧道显微镜的表征实验。结果表明,它们均具有良好的比表面积和形貌特性。
以此五种材料,常温制作了基于石英晶体微天平技术的甲基膦酸二甲脂室温传感器,并成功获取了传感器的重复性,灵敏度和选择性等重要参数。甲基膦酸二甲脂是一种常见的阻燃剂,由于其分子结构相似于战争毒气沙林,因此经常被用作沙林的模拟气体加以检测研究。本文实验结果对沙林传感器的研制具有一定的指导意义,同时也能给未来基于不同材料敏感膜的甲基膦酸二甲脂阵列型传感器的研发提供数据支持。
另外,本文针对五种材料的合成及其相应的传感器特性,进行了一系列有意义的对比实验。分析对比实验结果,也得到了部分有益的结论。
Nowadays, the issue of Green Chemisty has been wildly concerned. According to the principle of Green Chemisty and the demand of Quartz Crystal Microbalance (QCM) technology, a kind of low temperature and template free hydrothermal method has been created. The highest hydrothermal temperature can be controlled as lower as120℃and reaction time not more than3hours by reaction conditions adjusting. Comparing to the traditional hydrothermal method, which often has as highest as about250℃hydrothermal temperature and above24hours reaction time, it's a both energy saving and environment friendly method. Five sorts of elements, Sn, Fe, Zr, La and Mg, have been choosed because of their average locations in Element Periodic Table. Their five relative nano-oxides, SnO2,Fe2O3, ZrO2, La2O3and MgO, have been synthesized by the novel hydrothermal method. Then the X Ray Diffraction (XRD) and Scanning Electron Microscope (SEM) technologys have been applied to characterize them. The conclusion shows that the products have good rate surface area and promised morphology.
Based on the QCM technology, the five kinds of nano-oxides were used as the sensing film materials and Dimethyl Methyl Phosphonate (DMMP) sensors were fabricated for the room temperature detection. The crucial parameters of the sensors, such as repeated response, sensive degree and selectivity, have been obtained. DMMP is a kind of fire proof reagent and is sdudied as a simulatent of warfare gas sarin usually because of their similar molecule structure. The experimental results of our work can give some significant advices to the sarin sensor and also can provide basic data support for the future sensor array of DMMP with the different materials as the sensing films.
In addition, comparing experiments of synthsis and sensor sdudy to the five main nano-oxides have performed too. Some useful conclusions have been acquired from the analysis of their experimental data.
引文
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