甲基膦酸二甲酯质量敏感型气体传感器的制备及特性研究
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摘要
20世纪化学恐怖事件的屡次发生,引起了世界各国的广泛关注,这也表明对能够快速检测化学战剂的传感器具有迫切需求,以保障民众的安全。本文研究了“质量敏感型压电化学传感器”这一广泛应用于化学战剂检测领域的热点问题。重点研究了聚合物薄膜作为敏感材料的该类传感器,深入研究了不同聚合物敏感材料的敏感特性,并进一步将不同聚合物材料应用于传感器阵列,以改善单一传感器在选择性和稳定性方面的性能,其主要内容包括以下几个方面:
1.首次采用了聚偏氟乙烯(PVDF)材料作为石英晶体微天平(QCM)传感器敏感材料,用于检测化学战剂模拟剂甲基膦酸二甲酯(DMMP),并详细研究了该敏感材料在各种条件下的气敏特性。在DMMP浓度为5～60ppm范围内,PVDF-QCM传感器具有良好的线性相关性(相关系数高于0.997);且传感器响应值与环境温度符合阿累尼乌斯(Arrhenius)方程负的温度依赖关系;而环境湿度的变化不会影响PVDF-QCM传感器的使用。同时对干扰气体的检测结果表明PVDF对DMMP有良好的选择性。将高度有序的LB成膜技术引入使用,成功制备了PVDF-QCM传感器并研究了其对DMMP的敏感特性。
2.根据需要检测的对象的不同性质选取传感器敏感薄膜,获得了良好的敏感特性:(1)对甲基-3,3,3-三氟丙基聚硅氧烷(PMTFPS)进行低温氧等离子体改性,并通过缔合酸性小分子化合物磺基水杨酸(SSA)获得了对DMMP具有较好响应特性的敏感薄膜,传感器的灵敏度从9.91 Hz/ppm提高到11.96Hz/ppm,响应时间从141s降低到112s。(2)对环境湿度的监测则采用在具碱性特性的聚吡咯烷酮(PVP)中加入SSA,在降低PVP和水蒸气之间氢键作用强度的同时提高了聚合物的稳定性,使传感器在性能上表现为响应速度快、可逆性能良好。
3.研究了实验室自行设计合成的聚硅氧烷类材料的敏感特性。在不同的膜厚下,将聚甲基[3-(2-羟基)苯基]丙基硅氧烷(PMPS)薄膜应用于QCM和声表面波(SAW)传感器,两者均表现出响应频率与DMMP气体浓度呈线性关系,且响应快速,具有非常好的重复性、一致性及选择性。PMPS-SAW对DMMP的响应幅度和BSP3-SAW相当,但稳定性相对稍差。将含不同氟原子数目的PMPS,聚甲基[3-(2-羟基-3-氟)苯基]丙基硅氧烷(PMFPS),聚甲基[3-(2-羟基-3,4-二氟)苯基]丙基硅氧烷(PMDFPS)三种聚硅氧烷材料应用于QCM和SAW传感器,实验得出一致结论:含单个氟原子的PMFPS对DMMP的敏感性能最差,而PMPS和PMDFPS则需要在响应时间和响应幅度之间综合考虑选择。
4.通过使用模式识别中的主成分分析以及聚类分析,从15种不同性质的聚合物材料中挑选出所需最少数目的敏感薄膜,用于构成检测化学战剂的QCM传感器阵列。根据主成份分析结果,结合聚类分析结果,由PVP、PVDF、聚异丁烯(PIB)和聚-2-甲氧基-5-辛氧基-对苯乙炔(PMOCOPV)作为敏感薄膜的传感器阵列能够最大程度保留信息。选用了DMMP、N,N-二甲基乙酰胺(DMA)、二氯乙烷(DCE)和二氯戊烷(DCP)分别作为有机磷神经性毒剂以及糜烂性毒剂的模拟剂进行验证实验,主成分分析结果清楚地显示了4种气体在主成分图上的不同位置,2个主成分之和就可以代表95.46%的信息,说明该传感器阵列能够完全地分辨上述4种气体。
5.分析了聚合物薄膜对DMMP的敏感机理。对实验中聚合物材料与不同DMMP气体浓度的关系进行了数据分析,结果表明QCM传感器的作用规律符合BET吸附模型,并由此计算出三种聚硅氧烷材料的吸附比表面积大小顺序为PMPS＞PMDFPS＞PMFPS,也与实验得到的传感器灵敏度相符。另外把化学传感器看成一个线性定常(linear time-invariant,LTI)系统,建立方程模拟其在单位浓度脉冲信号作用下的响应曲线,模拟结果与实际响应曲线有较好的一致性。结合气体响应的动力学过程以及线性溶剂化能关系,阐述气体分子对聚合物敏感膜的响应结果综合了其中的各作用力影响因素。
The frequently chemical terrorism cases in 20~(th) Century arose great attentions in the world, and these demonstrate that there is a critical need for detectors and sensors that are able to warn about imminent chemical warfare agents (CWA) danger, to enable people to safely leave a contaminated zone or to protect themselves. The dissertation focused on the mass-sensitive piezoelectric sensors, which have been widely used as detections of CWA. Especially, a great deal investigations have been done on the polymers as sensitive materials and sensitivity characteristics towards CWA. Furthermore, the application of kinds of polymers in a sensor array to improve the selective performance of single sensor was also described. The main research results were as follows:
1. Quartz crystal microbalance (QCM) sensors coated with poly (vinylidene fluoride) (PVDF) were fabricated for the first time, and the sensitive characteristics were investigated in detail. It was found that the frequency shifts were linear to the concentrations of dimethyl methyl phosphonate (DMMP), a simulant of nerve agents, in the range of 5-60 ppm with a correlation coefficient of above 0.997, and the absolute frequency responses of the sensor all exhibited negative Arrhenius temperature dependencies at different concentrations. The results also showed that the sensitivity to DMMP vapor was almost identical in various humidity circumstances, and the sensitivity to DMMP was absolutely greater than to the interferences. Lanmuir-Blodgett (LB) method was introduced to prepare the PVDF film, and besides successfully preparation of the QCM sensor with PVDF LB film, the sensing properties to DMMP were also studied.
2. Different kinds of polymers were choosed due to various analyte compounds, and thus good sensitivities were reached. (1) Poly (methyl-3, 3, 3- trifluoropropyl-siloxane) (PMTFPS) was oxygen plasma treated and then grafted with sulfosalicylic acid (SSA). After that, the sensitivity of this material to DMMP was found to be enhanced from 9.91 Hz/ppm to 11.96 Hz/ppm, and the response time was reduced from 141s to 112s. (2) Poly (vinyl pyrrolidone) (PVP) with hydrogen-bond basicity was used as humidity sensitive coating. PVP complexed with SSA depressed the hydrogen-bond ability between PVP and water, and so that both the reversibility and response time of this sensor were improved.
3. A series of polysiloxane materials synthesized in our group were analysed. The frequency shifts behaved linear to the concentrations of analyte in various film thicknesses, whether the poly methyl [3-(2-hydroxyl)phenyl] propyl siloxane (PMPS) film fabricated on QCM or surface acoustic wave (SAW) sensors, and they showed rapid response, good repeatability, and favorable selectivity. The capability of PMPS-SAW was corresponded with BSP3-SAW, although the stability was a little worse. Compared three polysiloxane materials with different amount of fluorin atom in QCM and SAW sensors, which were PMPS, poly methyl [3-(2-hydroxyl-3-fluoro) phenyl] propyl siloxane (PMFPS) and poly methyl [3-(2-hydroxyl-3, 4-difluoro) phenyl] propyl siloxane (PMDFPS), the results both indicated that PMPS, which only had single fluorin atom, had the least sensitivity to DMMP vapor, and the selection of PMPS and PMDFPS needed compromising between response time and magnitude.
4. Pattern recognition techniques, both principal component analysis (PCA) and hierarchical cluster, were applied to frequency shift data obtained from 15 piezoelectric sensors, to obtain the least number of sensors composed an array for CWA detection. Combined with hierarchical cluster method, the results of PCA indicated that the four-sensor array providing the greatest degree of discrimination would consist of sensors coated with PVP, PVDF, poly(isobutylene) (PIB) and poly (2-methoxy-5-octyloxy)-1, 4-phenylene vinylene (PMOCOPV). DMMP, N, N- dimethylacetamide (DMA), 1, 5-dichloropentane (DCP) and dichloroethane (DCE), used as the simulants of organophosphorus nerve agents and vesicant agents, were tested by the above sensor array. It can be observed that DMMP, DMA, DCP and DCE can be clearly distinguished, and 95.46% information can be preserved with only two principal components, which indicated the successful distinguishability of the four vapors with this sensor array.
5. The gas-sensing mechanism of polymers to DMMP was investigated. The response of each QCM sensor to different DMMP concentration was modeled with BET adsorption isotherms, and results showed that the affinities of different sensors to vapor can be described well with the BET parameters. The ordinal magnitudes of the adsorbent specific surface areaes of the three polysiloxane materials were calculated out as PMPS>PMDFPS>PMFPS, which were consistent with the experimental results. We treated the chemical sensor as a linear time-invariant (LTI) system, and equations were established to simulate the response curves caused by an impulse signal of analyte concentration. The model was validated by comparing its predictions to experimental data. Both the kinetic process and the linear salvation energy relationship (LSER) were regarded to explain that the responses between analytes and sensing materials were integrated all the ingredients of interaction.
1.首次采用了聚偏氟乙烯(PVDF)材料作为石英晶体微天平(QCM)传感器敏感材料,用于检测化学战剂模拟剂甲基膦酸二甲酯(DMMP),并详细研究了该敏感材料在各种条件下的气敏特性。在DMMP浓度为5～60ppm范围内,PVDF-QCM传感器具有良好的线性相关性(相关系数高于0.997);且传感器响应值与环境温度符合阿累尼乌斯(Arrhenius)方程负的温度依赖关系;而环境湿度的变化不会影响PVDF-QCM传感器的使用。同时对干扰气体的检测结果表明PVDF对DMMP有良好的选择性。将高度有序的LB成膜技术引入使用,成功制备了PVDF-QCM传感器并研究了其对DMMP的敏感特性。
2.根据需要检测的对象的不同性质选取传感器敏感薄膜,获得了良好的敏感特性:(1)对甲基-3,3,3-三氟丙基聚硅氧烷(PMTFPS)进行低温氧等离子体改性,并通过缔合酸性小分子化合物磺基水杨酸(SSA)获得了对DMMP具有较好响应特性的敏感薄膜,传感器的灵敏度从9.91 Hz/ppm提高到11.96Hz/ppm,响应时间从141s降低到112s。(2)对环境湿度的监测则采用在具碱性特性的聚吡咯烷酮(PVP)中加入SSA,在降低PVP和水蒸气之间氢键作用强度的同时提高了聚合物的稳定性,使传感器在性能上表现为响应速度快、可逆性能良好。
3.研究了实验室自行设计合成的聚硅氧烷类材料的敏感特性。在不同的膜厚下,将聚甲基[3-(2-羟基)苯基]丙基硅氧烷(PMPS)薄膜应用于QCM和声表面波(SAW)传感器,两者均表现出响应频率与DMMP气体浓度呈线性关系,且响应快速,具有非常好的重复性、一致性及选择性。PMPS-SAW对DMMP的响应幅度和BSP3-SAW相当,但稳定性相对稍差。将含不同氟原子数目的PMPS,聚甲基[3-(2-羟基-3-氟)苯基]丙基硅氧烷(PMFPS),聚甲基[3-(2-羟基-3,4-二氟)苯基]丙基硅氧烷(PMDFPS)三种聚硅氧烷材料应用于QCM和SAW传感器,实验得出一致结论:含单个氟原子的PMFPS对DMMP的敏感性能最差,而PMPS和PMDFPS则需要在响应时间和响应幅度之间综合考虑选择。
4.通过使用模式识别中的主成分分析以及聚类分析,从15种不同性质的聚合物材料中挑选出所需最少数目的敏感薄膜,用于构成检测化学战剂的QCM传感器阵列。根据主成份分析结果,结合聚类分析结果,由PVP、PVDF、聚异丁烯(PIB)和聚-2-甲氧基-5-辛氧基-对苯乙炔(PMOCOPV)作为敏感薄膜的传感器阵列能够最大程度保留信息。选用了DMMP、N,N-二甲基乙酰胺(DMA)、二氯乙烷(DCE)和二氯戊烷(DCP)分别作为有机磷神经性毒剂以及糜烂性毒剂的模拟剂进行验证实验,主成分分析结果清楚地显示了4种气体在主成分图上的不同位置,2个主成分之和就可以代表95.46%的信息,说明该传感器阵列能够完全地分辨上述4种气体。
5.分析了聚合物薄膜对DMMP的敏感机理。对实验中聚合物材料与不同DMMP气体浓度的关系进行了数据分析,结果表明QCM传感器的作用规律符合BET吸附模型,并由此计算出三种聚硅氧烷材料的吸附比表面积大小顺序为PMPS＞PMDFPS＞PMFPS,也与实验得到的传感器灵敏度相符。另外把化学传感器看成一个线性定常(linear time-invariant,LTI)系统,建立方程模拟其在单位浓度脉冲信号作用下的响应曲线,模拟结果与实际响应曲线有较好的一致性。结合气体响应的动力学过程以及线性溶剂化能关系,阐述气体分子对聚合物敏感膜的响应结果综合了其中的各作用力影响因素。
The frequently chemical terrorism cases in 20~(th) Century arose great attentions in the world, and these demonstrate that there is a critical need for detectors and sensors that are able to warn about imminent chemical warfare agents (CWA) danger, to enable people to safely leave a contaminated zone or to protect themselves. The dissertation focused on the mass-sensitive piezoelectric sensors, which have been widely used as detections of CWA. Especially, a great deal investigations have been done on the polymers as sensitive materials and sensitivity characteristics towards CWA. Furthermore, the application of kinds of polymers in a sensor array to improve the selective performance of single sensor was also described. The main research results were as follows:
1. Quartz crystal microbalance (QCM) sensors coated with poly (vinylidene fluoride) (PVDF) were fabricated for the first time, and the sensitive characteristics were investigated in detail. It was found that the frequency shifts were linear to the concentrations of dimethyl methyl phosphonate (DMMP), a simulant of nerve agents, in the range of 5-60 ppm with a correlation coefficient of above 0.997, and the absolute frequency responses of the sensor all exhibited negative Arrhenius temperature dependencies at different concentrations. The results also showed that the sensitivity to DMMP vapor was almost identical in various humidity circumstances, and the sensitivity to DMMP was absolutely greater than to the interferences. Lanmuir-Blodgett (LB) method was introduced to prepare the PVDF film, and besides successfully preparation of the QCM sensor with PVDF LB film, the sensing properties to DMMP were also studied.
2. Different kinds of polymers were choosed due to various analyte compounds, and thus good sensitivities were reached. (1) Poly (methyl-3, 3, 3- trifluoropropyl-siloxane) (PMTFPS) was oxygen plasma treated and then grafted with sulfosalicylic acid (SSA). After that, the sensitivity of this material to DMMP was found to be enhanced from 9.91 Hz/ppm to 11.96 Hz/ppm, and the response time was reduced from 141s to 112s. (2) Poly (vinyl pyrrolidone) (PVP) with hydrogen-bond basicity was used as humidity sensitive coating. PVP complexed with SSA depressed the hydrogen-bond ability between PVP and water, and so that both the reversibility and response time of this sensor were improved.
3. A series of polysiloxane materials synthesized in our group were analysed. The frequency shifts behaved linear to the concentrations of analyte in various film thicknesses, whether the poly methyl [3-(2-hydroxyl)phenyl] propyl siloxane (PMPS) film fabricated on QCM or surface acoustic wave (SAW) sensors, and they showed rapid response, good repeatability, and favorable selectivity. The capability of PMPS-SAW was corresponded with BSP3-SAW, although the stability was a little worse. Compared three polysiloxane materials with different amount of fluorin atom in QCM and SAW sensors, which were PMPS, poly methyl [3-(2-hydroxyl-3-fluoro) phenyl] propyl siloxane (PMFPS) and poly methyl [3-(2-hydroxyl-3, 4-difluoro) phenyl] propyl siloxane (PMDFPS), the results both indicated that PMPS, which only had single fluorin atom, had the least sensitivity to DMMP vapor, and the selection of PMPS and PMDFPS needed compromising between response time and magnitude.
4. Pattern recognition techniques, both principal component analysis (PCA) and hierarchical cluster, were applied to frequency shift data obtained from 15 piezoelectric sensors, to obtain the least number of sensors composed an array for CWA detection. Combined with hierarchical cluster method, the results of PCA indicated that the four-sensor array providing the greatest degree of discrimination would consist of sensors coated with PVP, PVDF, poly(isobutylene) (PIB) and poly (2-methoxy-5-octyloxy)-1, 4-phenylene vinylene (PMOCOPV). DMMP, N, N- dimethylacetamide (DMA), 1, 5-dichloropentane (DCP) and dichloroethane (DCE), used as the simulants of organophosphorus nerve agents and vesicant agents, were tested by the above sensor array. It can be observed that DMMP, DMA, DCP and DCE can be clearly distinguished, and 95.46% information can be preserved with only two principal components, which indicated the successful distinguishability of the four vapors with this sensor array.
5. The gas-sensing mechanism of polymers to DMMP was investigated. The response of each QCM sensor to different DMMP concentration was modeled with BET adsorption isotherms, and results showed that the affinities of different sensors to vapor can be described well with the BET parameters. The ordinal magnitudes of the adsorbent specific surface areaes of the three polysiloxane materials were calculated out as PMPS>PMDFPS>PMFPS, which were consistent with the experimental results. We treated the chemical sensor as a linear time-invariant (LTI) system, and equations were established to simulate the response curves caused by an impulse signal of analyte concentration. The model was validated by comparing its predictions to experimental data. Both the kinetic process and the linear salvation energy relationship (LSER) were regarded to explain that the responses between analytes and sensing materials were integrated all the ingredients of interaction.
引文
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