摘要
声表面波化学传感器(SAW chemical sensor)是一种用于现场实时检测爆炸物的气敏传感器。涂在SAW化学传感器上的敏感膜涂层与被测气体之间能发生可逆吸附作用,当敏感膜与被测气体发生作用时,会引起膜密度和弹性等性质发生变化,从而使在压电晶体表面上传播的瑞利波速度随其表面沉积的质量而变化,导致振荡频率发生变化。通过检测振荡频率的变化,能获知是否存在某种气体和被吸附气体的浓度,具有灵敏度高、方便、快捷等诸多优点。
本论文以合成敏感膜材料为目的。首先采用无水解缩聚方法合成了环状硅氧烷,进一步合成了聚苯乙烯/聚甲基苯基硅氧烷嵌段共聚物(PS-b-PMPS),并用红外、核磁、凝胶色谱、乌氏粘度计方法进行表征。PS-b-PMPS与六氟丙酮(HFA)在不同条件下进行反应,进行六氟代异丙醇(HFIP)功能化,反应产物用红外、氟元素分析以及羟基分析等方法进行表征。然后采用溶剂蒸发法和旋涂法将聚合物敏感膜材料涂覆在SAW基片表面,通过装配配气系统,用二硝基甲苯(DNT)为爆炸物进行检测,精确测试了在一定气体浓度含量下SAW化学传感器的响应值,考察了羟基含量和嵌段比例对吸附性能的影响。
本文根据对各种反应条件下产物结构分析和吸附性检测,证实具有优良性能膜材料的最佳合成条件是:以二硫化碳为反应溶剂,反应时间为20小时,反应温度为25℃。此条件下HFIP功能化聚苯乙烯/聚甲基苯基硅氧烷嵌段共聚物具有最佳的氟元素和羟基含量,作为SAW膜材料检测爆炸物具有高的灵敏度和较好的脱附性能。
Surface acoustic wave (SAW) sensor is a kind of vapor sensor which has been utilized to detect and monitor explosive gases. The technology employs polymer coating on SAW sensor to collect and concentrate analyte(s) of interest. When the selective coating contacts analyte, the density and elasticity of film will be changed, so the spreading of Rayleigh wave on piezocrystal will be changed with the variety of sediment mass. The analyte(s) and its concentration can be detected by the change of oscillation frequency. It has high sensitive, convenient, fast, and many other advantages.
Ring siloxane was prepared by anhydrous concentration, further, synthesis poly(styrene-b-methylphenylsiloxane) (PS-b-PMPS). The PS-b-PMPS was characterized by FT-IR, NMR, GPC and Ubbelohde viscometer. The product was synthesized from PS-b-PMPS and hexafluoroacetone (HFA), then, was functionalized by hexafluoroisopropanol (HFIP), the functionalized product was characterized by FT-IR, ion chromatograph and hydroxyl analysis. The polymer was coated on the piezocrystal by two methods of solvent evaporation and spin coating. In the gas supply system, dinitrotoluene (DNT) was used as explosives, and the responses of SAW sensor were tested at DNT concentration of 750mg/m3. The factors to adsorption were also discussed in this paper.
The absorption of product will be better when it is prepared by HFA with PS-b-PMPS at 25℃in 20 hours, in carbon disulfide as solvent. It has high sensitivity with the best fluorin and hydroxyl as polymer coating on SAW sensor.
引文
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