功能膜材料SXPHFA的合成及表征方法研究
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摘要
声表面波(surface acoustic wave,SAW)传感器是一类新兴检测化学毒气和爆炸物的传感器,因其独特的优越性,近年来受到广泛的关注。涂在SAW化学传感器上的聚合物敏感膜涂层与被测气体之间能发生可逆吸附作用,当涂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。
本文将研究Poly(methyl(3,5-bis(hexafluoroisopropanol)phenyl)siloxane)聚(甲基(3,5-二(六氟代异丙醇)苯基)硅氧烷)(SXPHFA)膜材料的合成工艺,通过阴离子聚合开环的方法合成不同分子量聚甲基苯基硅氧烷(PMPS),用红外光谱、GPC等方法进行表征。将PMPS与六氟丙酮气体在不同条件下反应,得到目标产物SXPHFA,并进行红外、氟元素、羟基含量的表征。用溶剂蒸发法和旋涂法将聚合物涂在SAW基片表面。装配配气系统,用甲基磷酸二甲酯(DMMP)为化学战剂模拟物进行检测,精确测试在一定气体含量下SAW化学传感器对模拟气体的响应值。
通过控制引发剂的加入量,可以得到在3500～35000范围内分子量不同且分布窄的PMPS。在合成SXPHFA过程中,考察了溶剂、反应时间、温度对产物的影响,根据表征结果对工艺条件进行筛选。确定以CS2为溶剂,0℃下反应10小时的最佳工艺条件。在吸附性检测中,讨论了溶液浓度及涂膜方法对响应值的影响。
Surface acoustic wave (SAW) sensor is a new kind of sensor to detect chemical poison gas and explosives. This sensor attracted considerable attention because of its many advantages. 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 concertration can be detected by the change of oscillation frequency.
The synthesis approachs of coating material, poly (methyl (3, 5-bis (hexafluoro- isopropanol) phenyl) siloxane) (SXPHFA), are studied in the paper. Poly (methylphenylsiloxane) (PMPS) with different molecular weights is synthesized by anionic ring-opening polymerization, characterized by infrared spectrum and GPC. The SXPHFA was synthesized from PMPS and hexafluoroaceton (HFA) and characterized by infrared spectrum, 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, dimethyl methyl phosphonate (DMMP) was used as simulation gas, and the responses of SAW sensor were tested at DMMP concertration of 500mg/m3.
PMPS with narrow molecular mass distribution of molecular weight between 3500 and 35000 was obtained by adding different amounts of initiator. In the synthesis of SXPHFA, the influences of reaction time, solvent, reaction temperature and catalyzer are investigated. By the result of Characterization, best process conditions were selected. The best condition for the reaction time is 10 hours, the solvent is CS2, and the best reaction temperature is 0℃. In the adsorption test, the influences of solution strength and coating methods on response are discussed.
本文将研究Poly(methyl(3,5-bis(hexafluoroisopropanol)phenyl)siloxane)聚(甲基(3,5-二(六氟代异丙醇)苯基)硅氧烷)(SXPHFA)膜材料的合成工艺,通过阴离子聚合开环的方法合成不同分子量聚甲基苯基硅氧烷(PMPS),用红外光谱、GPC等方法进行表征。将PMPS与六氟丙酮气体在不同条件下反应,得到目标产物SXPHFA,并进行红外、氟元素、羟基含量的表征。用溶剂蒸发法和旋涂法将聚合物涂在SAW基片表面。装配配气系统,用甲基磷酸二甲酯(DMMP)为化学战剂模拟物进行检测,精确测试在一定气体含量下SAW化学传感器对模拟气体的响应值。
通过控制引发剂的加入量,可以得到在3500～35000范围内分子量不同且分布窄的PMPS。在合成SXPHFA过程中,考察了溶剂、反应时间、温度对产物的影响,根据表征结果对工艺条件进行筛选。确定以CS2为溶剂,0℃下反应10小时的最佳工艺条件。在吸附性检测中,讨论了溶液浓度及涂膜方法对响应值的影响。
Surface acoustic wave (SAW) sensor is a new kind of sensor to detect chemical poison gas and explosives. This sensor attracted considerable attention because of its many advantages. 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 concertration can be detected by the change of oscillation frequency.
The synthesis approachs of coating material, poly (methyl (3, 5-bis (hexafluoro- isopropanol) phenyl) siloxane) (SXPHFA), are studied in the paper. Poly (methylphenylsiloxane) (PMPS) with different molecular weights is synthesized by anionic ring-opening polymerization, characterized by infrared spectrum and GPC. The SXPHFA was synthesized from PMPS and hexafluoroaceton (HFA) and characterized by infrared spectrum, 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, dimethyl methyl phosphonate (DMMP) was used as simulation gas, and the responses of SAW sensor were tested at DMMP concertration of 500mg/m3.
PMPS with narrow molecular mass distribution of molecular weight between 3500 and 35000 was obtained by adding different amounts of initiator. In the synthesis of SXPHFA, the influences of reaction time, solvent, reaction temperature and catalyzer are investigated. By the result of Characterization, best process conditions were selected. The best condition for the reaction time is 10 hours, the solvent is CS2, and the best reaction temperature is 0℃. In the adsorption test, the influences of solution strength and coating methods on response are discussed.
引文
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[2] 景小峰,城市地铁反恐解决方案,中国安防产品信息,2005, (3): 17~18
[3] 张南,美国联合毒剂探测器的 SAW 与 IMS 之争,国外防化科技动态, 2004,12:1~4
[4] Wohltjen H, Dessy R, Surface acoustic wave probe for chemical analysis. I. Introduction and instrument description, Anal Chem., 1979, 51(9): 1458~1464
[5] Kannan G K, Nimal A T, Mittal U et al. Adsorption studies of carbowax coated surface acoustic wave (SAW) sensor for 2,4-dinitro toluene (DNT) vapour detection, Sensors and Actuators B, 2004, 101(3): 328~334
[6] 张杨,孙伟民,于蕾等,荧光传感器应用综述,光电子技术与信息,2004,17(6): 104~104
[7] Yang J S, Swager T M, Porous shape persistent fluorescent polymer films: An approach to TNT sensory materials, J. Am.Chem. Soc., 1998, 120(21): 5321~5322
[8] Cumming C J, Aker C, Fisher M,et al. Using novel fluorescent polymers as sensory materials for above-ground sensing of chemical signature compounds emanating from buried landmines, IEEE Transactions on Geoscience and Remote Sensing, 2001, 39 (6): 1119~1128
[9] 许峰,王海龙,关亚风,离子迁移谱研究进展,化学进展,2005,17(3): 514~522
[10] Ewing R G, Miller C J,Detection of Volatile Vapors Emitted from Explosives with a Handheld Ion Mobility Spectrometer,Field Analytical Chemistry and Technology, 2001, 5(5): 215~221
[11] Vautz W, Zimmermann D, Hartmann M et al. Ion mobility spectrometry for food quality and safety, Food Additives and Contaminants, 2006, 23(11): 1064~1073
[12] 徐淑武,郑健,毕志毅等,离子迁移谱检测技术及其应用,物理,2003, 32(8): 539~542
[13] 姚守拙,化学与生物传感器,北京:化学工业出版社,2006,179~180
[14]Janata J, Chemical sensors, J. Anal. Chem., 1990, 62 (12): 33~44
[15] Caron J J, Haske11 R B, Benoit P, A surface acoustic wave mercury vapor sensor [J]. IEEE Tmnsactions on Ultrasonics, Ferroelectrlcs and Frequency Control, 1998, 45(5): 1393~1398
[16] Anisimkin V I, Verona E, New capabilities for optimizing SAW gas sesnsos[J], IEEE Transactions on Ultrasonics,Ferroelectrlc and Frequency Control,2001,48(5):1413~1418
[17] 陈显萼,姚海伦,声表面波传感器 SAWS 的进展,电子瞭望,1992, (8): 23~26
[18] 李晖,潘峰, 声表面波器件的研究进展, 真空科学与技术,2001,21(5):376~380
[19] 钱峰,声表面波传感器及其应用,自动化仪表,1992,13(2): 5~7
[20] 纪军,黄启斌,丁学全, 国外化学毒剂检测器技术与评价, 北京:国防工业出版社,2006,58~62
[21] Edmonson P J, Campbell C K, Selectable reflector arrays for SAW sensors and identification devices, United States Patent, 6967428, 2005-11-22
[22] 刘雪梅, 邢婉丽, 聚合物在化学传感器的应用, 化学传感器, 1999, 19(3): 1~10
[23] 邹小红,郭成海,史瑞雪, 声表面波气体传感器的设计,化学传感器, 2000, 20(3): 6~11
[24] Thompson C H, Hu J, Kaganove S N, etal. Hydrogen-bond acidic hyperbranched polymers for Surface Acoustic Wave (SAW) sensors, Chem. Mater., 2004, 16(25): 5357~5364
[25] 刘卫卫,于建华,潘勇 等. SAW 聚环氧氯丙烷传感器检测芥子气的研究,化学传感器, 2005, 25(1): 57~60
[26] Grate J W, Patrash S J, Selective vapor sorption by polymers and cavitands on acoustic wave sensors: Is this molecular recognition, J. Anal. Chem., 1996, 68(5): 913~917
[27] Zimmermann C, Mazein P, Rebière D et al. Detection of GB and DMMP vapors by love wave acoustic sensors using strong acidic fluoride polymers IEEE Sensors J., 2004, 4(4): 479~487
[28] Grate J W, M Klusty, McGill R A et al. The predominant role of swelling-induced modulus changes of the sorbent phase in determining the responses of polymer-coated surface acoustic wave vapor sensors, J. Anal. Chem., 1992, 64(6): 610~624
[29] Grate J W, Zellers E T,The fractional free volume of the sorbed vapor in modeling the viscoelastic contribution to polymer-coated surface acoustic wave vapor sensor responses, J. Anal. Chem., 2000, 72(13): 2861~2868.
[30] Abraham M H, Scales of solute hydrogen-bonding: Their construction and application to physicochemical and biochemical processes, Chem. Soc. Rev., 1993, 22(2): 73~83
[31] McGill R A, Mlsna T E, Chung R,et al. Design of functionalized silicone polymers for chemical sensor detection of nitroaromatic compounds,Sensors and Actuators B, 2000, 65(1): 5~9
[32] Houser E J, Mlsna T E, Nguyen V K et al. Rational materials design of sorbent coatings for explosives: Applications with chemical sensors Talanta, 2001, 54: 469~485
[33] Abraham M H, Andonian-Haftvan J, Du C M et al. Hydrogen bonding. Part 29. Characterization of 14 sorbent coatings for chemical microsensors using a new solvation equation, J. Chem. Soc., Perkin Trans. 2, 1995, (2): 369~378
[34] McGill R A, Mlsna T E, Chung R et al. Sorbent Coatings for Nitroaromatic Vapors: Applications with Chemical Sensors, SPIE, 1998, 3392: 384~389.
[35] Grate J W, Acoustic wave microsensor arrays for vapor sensing, Chem. Rev., 2000, 100(7): 2627~2648.
[36] Grate J W, Patrash S J, Method for estimating polymer-coated acoustic wave vapor sensor responses, Anal. Chem., 1995, 67(13): 2162~2169
[37] Grate J W, Patrash S J, Kaganove S N, Hydrogen bond acidic polymers for surface acoustic wave vapor sensors and arrays, Anal. Chem., 1999, 71(5): 1033~1040
[38] McGill R A, Abraham M H, Grate J W, Choosing polymer coatings for chemical sensors, Chemtech., 1994, 24(9): 27~37
[39] 夏德意,90 年代国外神经性毒剂毒理学研究进展,解放军医学情报,1994,(8): 233~235
[40] Susan L, Rose-Pehrsson, Grate J W, Detection of hazardous vapors including mixtures using pattern recognition analysis of responses from surface acoustic wave devices, Anal. Chem., 1988, 60(24): 2801~2811
[41] 陈献新,何慧,贾德民等,聚硅氧烷的研究进展,绝缘材料,2006,39(1):59~63
[42] 李光亮,有机硅高分子化学,北京:科学出版社,1998,2~3
[43] 佀庆法，范晓东，功能性有机聚硅氧烷的研究进展，高分子通报，2004,(1):21~29
[44] 冯圣玉,张洁,李美江,有机硅高分子及其应用,北京:化学工业出版社,2004,16~19
[45] Speier J L, Zimmerman R, Webster J, The addition of silicon hydrides to olefinic double bonds. Part I. The use of phenylsilane, diphenylsilane, Phenylmethy- lsilane, Amylsilane and Tribromosilane, Am. Chem. Soc., 1956, 78(10): 2278~2281
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