环糊精—聚合物薄膜玻璃光波导传感元件的气敏性研究
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摘要
化学传感器是识别、检测化学物质，再转换成电信号的仪器。随着科学技术的发展，化学传感器在科学、工业及军事领域的应用越来越广泛。而气敏材料是传感器的核心部分。因此，具有气敏功能的聚合物复合材料的研究与开发由于具有广阔的应用前景和重要的理论研究意义而越来越受到人们的广泛关注。气敏材料种类很多，其中高分子材料由于成本低、易加工、物理或化学性能修饰比较简单等优点，在传感器的发展中具有举足轻重的作用。
光波导传感器（OWG）对敏感试剂的选择灵活，且具有灵敏度高、响应快、成本低等诸多特点。因此，在环境监测、生化监测等领域有着广泛应用前景。将光波导传感技术应用到气体的检测领域时，能发挥出更好的价值。
文章前言部分以超分子化合物及其在传感器领域中的应用及挥发性有机气体的危害性出发，讲述了超分子衍生物作为敏感试剂的各种传感器的检测对象和检测方法。同时介绍了光波导化学传感器在分析领域中的重要性，及其工作原理和特点。
本文以β-环糊精（β-cyclodextrin，简称为β-CD），聚乙烯吡咯烷酮（PVP），对叔丁基杯[6]芳烃（4-tert-butylcalix[6]arene），溴酚蓝等材料作为光波导传感元件主体敏感材料，设计并制作了光波导气体传感器，并考察了其对挥发性有机气体的响应。具体内容如下：
1.聚合物，高分子气敏材料具有成本低，易修饰等特点，被广泛使用在传感器领域当中。在第二章中，筛选β-环糊精作为敏感试剂，并将其固定在K~+交换玻璃光波导表面研制了β-环糊精薄膜光波导传感元件。同时筛选出制备光波导敏感元件的最佳条件（溶剂、敏感试剂浓度、匀胶机速度等）。将β-环糊精薄膜/K~+交换玻璃光波导元件固定在光波导气体传感检测系统中，检测了该传感元件对挥发性有机气体的气敏性。通过敏感膜光学特性变化来解释了敏感机理。研究结果表明，该元件能够检测出体积比为1×10~(-5)（43.3mg/m~3）的苯乙烯气体并具有一定的选择性响应。
2.第三章以第二章为基础，对β-环糊精薄膜进行了修饰。本章中筛选了不同百分含量的PVP和β-环糊精作为敏感试剂，并将其固定在K~+交换玻璃光波导表面研制了PVP-环糊精薄膜/K~+交换玻璃光波导元件，对不同挥发性有机气体进行了检测。实验结果表明，该元件能够检测到体积比为1×10~(-6)(4.33mg/m3)的苯乙烯气体。当气体浓度为1×10~(-3)时，该光波导元件对甲醇、乙醇和甲醛的响应较小。此外还对PVP-环糊精薄膜进行了红外光谱分析并研究了两者之间的相互作用。
3.第四章中，又对β-环糊精薄膜进行了修饰。本章中，先筛选出了溴酚蓝最佳含量，然后确定最佳制膜条件（匀胶机速度）。研制出了溴酚蓝-环糊精薄膜/K+交换玻璃光波导元件，并研究了其对挥发性有机气体的响应。同时，还研究了该元件对酸性气体的气敏性并分析其原理。实验结果表明，该传感元件对二甲苯具有较好的选择性响应，能够检测浓度为1×10~(-6)(4.41mg/m3)的二甲苯。该元件对SO_2和NH_3具有较明显的响应，但酸性气体的恢复较慢，不利于检测该传感元件对不同浓度酸性气体的传感响应，但此元件对NH3的恢复较好，能够成功地检测到浓度为1×10~(-5)(7.1mg/m~3)的NH_3气体。
4.传感器技术能够提供低成本的装置，可调整传感器敏感材料来实现新型材料在传感器领域中的应用。在第五章中，以对叔丁基杯[6]芳烃作为敏感试剂，通过旋转甩涂法在K~+交换玻璃光波导表面制备了对叔丁基杯[6]芳烃薄膜，研制出了对叔丁基杯[6]芳烃薄膜/K+交换玻璃光波导传感元件并对挥发性有机气体进行了检测。同时研究了其气敏性。实验结果表明，该元件对苯乙烯具有较好的选择性响应。能够检测到浓度为1×10~(-7)(0.43mg/m~3)的苯乙烯。此外还对氯苯和甲苯分别进行气敏性研究。
Chemical sensor is the instrument that can identify and detect the chemicalsubstance and then experiment consequent can replaced electric signal. With thedevelopment of science and technology, chemical sensors possess widespreadapplications in the area of scientific, industrial and military. However Gas-Sensingmaterial is a core part of the sensor device. Therefore, the research and developmentof the polymer composite materials has wide application prospects and importanttheoretical significance and researcher has been concerned. Gas-Sensing material hasmany different types. Among that, polymer materials due to be low cost, simplemodified of physical and chemical properties, so it plays a decisive role in thedevelopment of sensors.
Optical waveguide sensor has the characteristics of flexibility, high sensitivity tothe choice of sensitive reagents, fast response, low cost and other many features.Therefore, it has wide application prospects in the field of environmental monitoring,chemical and biological monitoring. The optical waveguide sensor technology canplay a better value in the area of gas detection.
The article began by describing the poisoning effect of the human and theapplication of supramolecular compounds in the sensor field, we introduced thedetected object and detection methods of the supramolecular derivatives as a sensitivereagent. Meanwhile, we also introduced the importance of optical waveguidechemical sensors in the analysis of the field and its working principle andcharacteristics.
Here, β-cyclodextrin(β-CD), polyvinylpyrrolidone(PVP), tert-butylcalix[6]arene,bromophenol blue material as the waveguide main sensitive materials. Opticalwaveguide gas chemical sensors were designed and fabricated. And its response to thevolatile organic gases was studied. The main contents were listed below.
1. Polymer gas-sensing material has the important characteristics of low cost,easymodification, so they are widely used in the sensor field. In the second chapter,β-cyclodextrin was used as sensitive material, the β-cyclodextrin/K~+-exchanged optical waveguide sensor was fabricated. Meanwhile, the best condition tofabricate the sensing element was selected (solvent, the concentration ofsensitive reagent, the speed of spin-coating machine). The OWG sensor wasused to detect Volatile Organic Compounds gas. The sensing principle wasstudied by the change of optical characteristics of sensitive film. Theexperiment result indicated that the minimum concentration of detection tostyrene gas of sensor is1×10~(-5）(43.3mg/m3).
2. Chapter third is based on chapter second, the β-cyclodextrin thin film wasmodified. In this chapter, we first choice adequate PVP, and we choose certainamount of PVP and β-cyclodextrin as the sensitive reagents. And thePVP-cyclodextrin/K~+-exchanged OWG sensor was fabricated by spin-coatingmethod. And the sensitive characteristics of the sensor device was detected. Theexperiment results indicated that, the minimum concentration of detection tostyrene gas of sensor is1×10~(-6)(4.3mg/m~3).while the concentration of the gaseswas1×10~(-3), the response of sensor to methanol, ethanol and formaldehyde wassmall. In addition, the infrared spectroscopy of PVP-cyclodextrin film wasmeasured and the interaction between them was studied.
3. In the fourth chapter, the β-cyclodextrin film was modified. In this chapter, wefirst decided the certain amount of BPhB, and then chose the appropriate speedof spin-coating machine. The BPhB-cyclodextrin composite film/K~+-exchangedOWG sensor was fabricated by spin-coating method. And carried out theVolatile Organic Compounds gas detection. Meanwhile, the sensitiveperformance to acidity of sensor device was studied. The experiment resultsindicated that, the sensor device has high response to xylene and the minimumdetection concentration of1×10~(-6)(4.41mg/m3). Meantime, has good responseto SO2and NH3, but it has slow recovery time to acidic gases.
4. Sensor technology can provide low-cost device, therefore, an adjustable sensorsensitive material has wide application of new material in the sensor field. In thefifth chapter,4-tert-butylcalix[6]arene was selected as sensitive material. The4-tert-butylcalix[6]arene/K~+-exchanged OWG sensor was fabricated by spin-coating method. And the sensitive performance to VOC was detected andthe sensing principle was studied. The experiment results indicated that, thesensor device has good selective response to styrene and the minimum detectionconcentration was1×10~(-7)(0.43mg/m~3). In addition, the sensitive characteristicsof sensor device to chlorobenzene and toluene was researched.
光波导传感器（OWG）对敏感试剂的选择灵活，且具有灵敏度高、响应快、成本低等诸多特点。因此，在环境监测、生化监测等领域有着广泛应用前景。将光波导传感技术应用到气体的检测领域时，能发挥出更好的价值。
文章前言部分以超分子化合物及其在传感器领域中的应用及挥发性有机气体的危害性出发，讲述了超分子衍生物作为敏感试剂的各种传感器的检测对象和检测方法。同时介绍了光波导化学传感器在分析领域中的重要性，及其工作原理和特点。
本文以β-环糊精（β-cyclodextrin，简称为β-CD），聚乙烯吡咯烷酮（PVP），对叔丁基杯[6]芳烃（4-tert-butylcalix[6]arene），溴酚蓝等材料作为光波导传感元件主体敏感材料，设计并制作了光波导气体传感器，并考察了其对挥发性有机气体的响应。具体内容如下：
1.聚合物，高分子气敏材料具有成本低，易修饰等特点，被广泛使用在传感器领域当中。在第二章中，筛选β-环糊精作为敏感试剂，并将其固定在K~+交换玻璃光波导表面研制了β-环糊精薄膜光波导传感元件。同时筛选出制备光波导敏感元件的最佳条件（溶剂、敏感试剂浓度、匀胶机速度等）。将β-环糊精薄膜/K~+交换玻璃光波导元件固定在光波导气体传感检测系统中，检测了该传感元件对挥发性有机气体的气敏性。通过敏感膜光学特性变化来解释了敏感机理。研究结果表明，该元件能够检测出体积比为1×10~(-5)（43.3mg/m~3）的苯乙烯气体并具有一定的选择性响应。
2.第三章以第二章为基础，对β-环糊精薄膜进行了修饰。本章中筛选了不同百分含量的PVP和β-环糊精作为敏感试剂，并将其固定在K~+交换玻璃光波导表面研制了PVP-环糊精薄膜/K~+交换玻璃光波导元件，对不同挥发性有机气体进行了检测。实验结果表明，该元件能够检测到体积比为1×10~(-6)(4.33mg/m3)的苯乙烯气体。当气体浓度为1×10~(-3)时，该光波导元件对甲醇、乙醇和甲醛的响应较小。此外还对PVP-环糊精薄膜进行了红外光谱分析并研究了两者之间的相互作用。
3.第四章中，又对β-环糊精薄膜进行了修饰。本章中，先筛选出了溴酚蓝最佳含量，然后确定最佳制膜条件（匀胶机速度）。研制出了溴酚蓝-环糊精薄膜/K+交换玻璃光波导元件，并研究了其对挥发性有机气体的响应。同时，还研究了该元件对酸性气体的气敏性并分析其原理。实验结果表明，该传感元件对二甲苯具有较好的选择性响应，能够检测浓度为1×10~(-6)(4.41mg/m3)的二甲苯。该元件对SO_2和NH_3具有较明显的响应，但酸性气体的恢复较慢，不利于检测该传感元件对不同浓度酸性气体的传感响应，但此元件对NH3的恢复较好，能够成功地检测到浓度为1×10~(-5)(7.1mg/m~3)的NH_3气体。
4.传感器技术能够提供低成本的装置，可调整传感器敏感材料来实现新型材料在传感器领域中的应用。在第五章中，以对叔丁基杯[6]芳烃作为敏感试剂，通过旋转甩涂法在K~+交换玻璃光波导表面制备了对叔丁基杯[6]芳烃薄膜，研制出了对叔丁基杯[6]芳烃薄膜/K+交换玻璃光波导传感元件并对挥发性有机气体进行了检测。同时研究了其气敏性。实验结果表明，该元件对苯乙烯具有较好的选择性响应。能够检测到浓度为1×10~(-7)(0.43mg/m~3)的苯乙烯。此外还对氯苯和甲苯分别进行气敏性研究。
Chemical sensor is the instrument that can identify and detect the chemicalsubstance and then experiment consequent can replaced electric signal. With thedevelopment of science and technology, chemical sensors possess widespreadapplications in the area of scientific, industrial and military. However Gas-Sensingmaterial is a core part of the sensor device. Therefore, the research and developmentof the polymer composite materials has wide application prospects and importanttheoretical significance and researcher has been concerned. Gas-Sensing material hasmany different types. Among that, polymer materials due to be low cost, simplemodified of physical and chemical properties, so it plays a decisive role in thedevelopment of sensors.
Optical waveguide sensor has the characteristics of flexibility, high sensitivity tothe choice of sensitive reagents, fast response, low cost and other many features.Therefore, it has wide application prospects in the field of environmental monitoring,chemical and biological monitoring. The optical waveguide sensor technology canplay a better value in the area of gas detection.
The article began by describing the poisoning effect of the human and theapplication of supramolecular compounds in the sensor field, we introduced thedetected object and detection methods of the supramolecular derivatives as a sensitivereagent. Meanwhile, we also introduced the importance of optical waveguidechemical sensors in the analysis of the field and its working principle andcharacteristics.
Here, β-cyclodextrin(β-CD), polyvinylpyrrolidone(PVP), tert-butylcalix[6]arene,bromophenol blue material as the waveguide main sensitive materials. Opticalwaveguide gas chemical sensors were designed and fabricated. And its response to thevolatile organic gases was studied. The main contents were listed below.
1. Polymer gas-sensing material has the important characteristics of low cost,easymodification, so they are widely used in the sensor field. In the second chapter,β-cyclodextrin was used as sensitive material, the β-cyclodextrin/K~+-exchanged optical waveguide sensor was fabricated. Meanwhile, the best condition tofabricate the sensing element was selected (solvent, the concentration ofsensitive reagent, the speed of spin-coating machine). The OWG sensor wasused to detect Volatile Organic Compounds gas. The sensing principle wasstudied by the change of optical characteristics of sensitive film. Theexperiment result indicated that the minimum concentration of detection tostyrene gas of sensor is1×10~(-5）(43.3mg/m3).
2. Chapter third is based on chapter second, the β-cyclodextrin thin film wasmodified. In this chapter, we first choice adequate PVP, and we choose certainamount of PVP and β-cyclodextrin as the sensitive reagents. And thePVP-cyclodextrin/K~+-exchanged OWG sensor was fabricated by spin-coatingmethod. And the sensitive characteristics of the sensor device was detected. Theexperiment results indicated that, the minimum concentration of detection tostyrene gas of sensor is1×10~(-6)(4.3mg/m~3).while the concentration of the gaseswas1×10~(-3), the response of sensor to methanol, ethanol and formaldehyde wassmall. In addition, the infrared spectroscopy of PVP-cyclodextrin film wasmeasured and the interaction between them was studied.
3. In the fourth chapter, the β-cyclodextrin film was modified. In this chapter, wefirst decided the certain amount of BPhB, and then chose the appropriate speedof spin-coating machine. The BPhB-cyclodextrin composite film/K~+-exchangedOWG sensor was fabricated by spin-coating method. And carried out theVolatile Organic Compounds gas detection. Meanwhile, the sensitiveperformance to acidity of sensor device was studied. The experiment resultsindicated that, the sensor device has high response to xylene and the minimumdetection concentration of1×10~(-6)(4.41mg/m3). Meantime, has good responseto SO2and NH3, but it has slow recovery time to acidic gases.
4. Sensor technology can provide low-cost device, therefore, an adjustable sensorsensitive material has wide application of new material in the sensor field. In thefifth chapter,4-tert-butylcalix[6]arene was selected as sensitive material. The4-tert-butylcalix[6]arene/K~+-exchanged OWG sensor was fabricated by spin-coating method. And the sensitive performance to VOC was detected andthe sensing principle was studied. The experiment results indicated that, thesensor device has good selective response to styrene and the minimum detectionconcentration was1×10~(-7)(0.43mg/m~3). In addition, the sensitive characteristicsof sensor device to chlorobenzene and toluene was researched.
引文
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