碳纳米管气/湿敏传感器的制备及特性研究
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摘要
神经毒剂自其出现以来，用于战争和恐怖袭击事件时有发生，因此，发展和研制神经毒剂传感器，对国家和公共安全都有重要意义。碳纳米管以其极高的长宽比和比表面积，以及强的气体吸附能力，成为气体传感器中一种非常理想的敏感材料。本文分别采用气喷、丝网印刷、化学气相沉积、电泳和自组装工艺制备碳纳米管薄膜，并运用多种方法进行了表征和分析；制备了平面叉指电容型和平板电容器型传感器，测试和研究了碳纳米管传感器对甲基磷酸二甲酯（DMMP）蒸气的气体敏感特性。其主要内容包括以下几个方面：
1.采用气喷工艺制备单壁碳纳米管平面叉指电容型传感器，在暴露到DMMP蒸气中时，电容迅速减小，电容响应幅度随着DMMP蒸气浓度的增加而增大，对12mg/m3DMMP蒸气的电容响应达到12.43%。传感器具有良好的重复性和选择性。同时也测试了传感器的电阻变化，电阻响应随DMMP蒸气浓度的增加而增加，其响应幅度比电容小约一个数量级。气喷多壁碳纳米管传感器、单壁碳纳米管和聚甲基-{3-[2-羟基-3,5-二(三氟甲基)]苯基}-丙基硅氧烷（DKAP）复合薄膜传感器与单壁碳纳米管传感器有类似的电容响应特性，但其电容响应都显著变小，对12mg/m3DMMP蒸气的电容响应分别为1.39%和0.54%。复合薄膜中DKAP缠绕和包裹了单壁碳纳米管，减小了碳纳米管的有效表面积，使其电容响应明显小于相应的单壁碳纳米管传感器。实验还发现，具有较大初始电容和损耗角正切的传感器，薄膜更为稠密，形成的微孔尺寸较小，用于吸附的有效表面积较大，具有的电容响应更大。
2.采用丝网印刷工艺制备单壁碳纳米管传感器，对50ppm (250mg/m3) DMMP蒸气的电阻响应为16.4×10-3。由于丝网印刷碳纳米管膜中残留有乙基纤维素等原料，所以其电阻响应幅度远低于气喷工艺所制碳纳米管传感器。该传感器具有很好的重复性和长期稳定性，但是其电阻恢复较慢，特别是在高浓度下较为明显。传感器对空气中存在的水、氧气和二氧化碳等气体选择性较好，但对NH3等强氧化还原性气体和醇、芳烃等有机蒸气的选择性很差。因为这些气体与残留的乙基纤维素有较好的吸附作用。丝网印刷单壁碳纳米管传感器上下板极之间形成的平板电容对DMMP蒸气也有响应，当暴露到20mg/m3DMMP蒸气中时，其电容响应仅为0.028%，低于电阻的响应。
3.采用自组装工艺在QCM上制备了单壁碳纳米管气体传感器，由聚电解质聚二烯丙基二甲基氯化铵（PDDA）和单壁碳纳米管层交替组装而成，发现传感器对湿度的响应明显大于DMMP蒸气的响应。并对比了含有-COOH和不含-COOH的碳纳米管原料对传感器湿敏的影响。结果发现，当湿度从20.9%变化到80.2%时，自组装PDDA/SWNT-COOH传感器和PDDA/SWNT QCM传感器的频率相对变化分别为16.64%和13.84%，前者相对于后者灵敏度提高了20.23%，而且选择性更好，响应时间更短，而恢复时间则更长，相应的湿滞也从3.9%增大到8.0%。这是因为含羧基的单壁碳纳米管在氧化处理后其π-π*转变结构和相应含氧官能团的含量高于经氧化处理的普通单壁碳纳米管。但是，两个传感器对60%饱和蒸气浓度DMMP蒸气的灵敏度却只有2.06%-2.17%。
Since the appearance of nerve agents, they are frequently used in war and terroristattacks. Therefore, the manufacture and development of nerve agent sensors are of greatsignificance for national and public security. Because of the high aspect ratio andspecific surface area, as well as the strong gas adsorption capacity, carbon nanotubes(CNTs) are ideal sensitive materals in gas sensors. In this dissertation, CNT thin filmswere prepared by airbrush, screen printing, chemical vapor deposition (CVD),electrophoresis and layer-by-layer self-assembly techniques, which were characterizedand analyzed with different methods. The planar interdigital capacitor and platecapacitor were fabricated, and the dimethyl methylphosphonate (DMMP) gas-sensingproperties of these CNT sensors were carried out and studied. The main research resultswere as follows:
1. Single-walled carbon nanotubes (SWNTs) were deposited on interdigitalelectrodes (IDTs) by airbrush method, and it formed interdigital capacitive sensor. Thecapacitance of this sensor decreased rapidly when exposed to DMMP. The capacitanceresponse increased with the increase of DMMP concentration and was12.43%to12mg/m3DMMP. The sensor had a good reproducibility and selectivity. Meanwhile, theresistance response of airbrush SWNT sensor was also studied. The resistance of thissensor increased immediately when exposed to DMMP and the response increased withthe increase of DMMP concentration, but the resistance response was smaller than thecapacitance response by one order in magnitude. The capacitance responses of airbrushmulti-walled carbon nanotube (MWNT) sensor and SWNT/DKAP (poly{methyl[3-(2-hydroxyl,3,5-bistrifluoromethyl)phenyl]propylsiloxane}) composite film sensor weresimilar to the response of airbrush SWNT sensor, but their responses were sigmificatelysmaller and were1.39%and0.54%to12mg/m3DMMP, respectively. The DKAPtwined and wrapped SWNTs in the composite film, reducing the effective surface areaof CNTs and causing the capacitance response significately smaller than thecorresponding SWNT sensor. It is also found that when the airbrush CNT sensor withlarger initial capacitance and loss tangent, the CNT film was denser, the average pore size was smaller and the effective surface area for gas adsorption was larger, leading tohigher capacitance response.
2. SWNT sensor was prepared on SiO2/Si substrate by screen printing, and theresistance response of this sensor to50ppm (250mg/m3) DMMP was16.4×10-3.Because there was residual ethyl cellu, etc. in the screen printed SWNT film, theresistance response was far less than the corresponding airbrush SWNT sensor. Thesensor had a very good reproducibility and long-term stability, but its resistancerecovered very slowly, which was more obvious at high concentration of DMMP. Thesensor had a good selectivity to the gases which were present in the air, such as water,oxygen and carbon dioxide. But the selectivity to the gases with redox, such as NH3,etc., and organic vapors, such as alcohols and aromatics, was very poor due to thestrong adsorption between these gases and the residual ethyl cellu. The capacitor formedby the two plates of the screen printed SWNT sensor had response to DMMP. Whenexposed to20mg/m3DMMP, the capacitance response was only0.028%, which wassmaller than the resistance response.
3. SWNT gas sensors were fabricated on quartz crystal microbalance (QCM) bylayer-by-layer self-assmbly of polyelectrolyte poly(diallyldimethylammonium chloride)(PDDA) and SWNTs. It was found that the sensors had a significantly greater responseto humidity than to DMMP. The effect of raw SWNT materials with and withoutcarboxyl (-COOH) on the humidity sensing properties of these SWNT composite thinfilm sensors was studied and compared. The results showed that when the relativehumidity was changed from20.9%to80.2%, the relative frequency shifts of thePDDA/SWNT-COOH QCM sensor and PDDA/SWNT QCM sensor were16.64%and13.84%, respectively. The former had a sensitivity enhanced by20.03%, a betterselectivity and a shorter response time, but the recovery time was longer and thehysteresis was increased from3.9%to8.0%. It was attributed to that the relative contentof π-π*transition structures and the corresponding functional groups in modifiedSWNTs-COOH was much higher than that in modified SWNTs. However, thesensitivities of the two sensors to60%saturated vapor pressure concentration of DMMPwere only2.06%-2.17%.
1.采用气喷工艺制备单壁碳纳米管平面叉指电容型传感器，在暴露到DMMP蒸气中时，电容迅速减小，电容响应幅度随着DMMP蒸气浓度的增加而增大，对12mg/m3DMMP蒸气的电容响应达到12.43%。传感器具有良好的重复性和选择性。同时也测试了传感器的电阻变化，电阻响应随DMMP蒸气浓度的增加而增加，其响应幅度比电容小约一个数量级。气喷多壁碳纳米管传感器、单壁碳纳米管和聚甲基-{3-[2-羟基-3,5-二(三氟甲基)]苯基}-丙基硅氧烷（DKAP）复合薄膜传感器与单壁碳纳米管传感器有类似的电容响应特性，但其电容响应都显著变小，对12mg/m3DMMP蒸气的电容响应分别为1.39%和0.54%。复合薄膜中DKAP缠绕和包裹了单壁碳纳米管，减小了碳纳米管的有效表面积，使其电容响应明显小于相应的单壁碳纳米管传感器。实验还发现，具有较大初始电容和损耗角正切的传感器，薄膜更为稠密，形成的微孔尺寸较小，用于吸附的有效表面积较大，具有的电容响应更大。
2.采用丝网印刷工艺制备单壁碳纳米管传感器，对50ppm (250mg/m3) DMMP蒸气的电阻响应为16.4×10-3。由于丝网印刷碳纳米管膜中残留有乙基纤维素等原料，所以其电阻响应幅度远低于气喷工艺所制碳纳米管传感器。该传感器具有很好的重复性和长期稳定性，但是其电阻恢复较慢，特别是在高浓度下较为明显。传感器对空气中存在的水、氧气和二氧化碳等气体选择性较好，但对NH3等强氧化还原性气体和醇、芳烃等有机蒸气的选择性很差。因为这些气体与残留的乙基纤维素有较好的吸附作用。丝网印刷单壁碳纳米管传感器上下板极之间形成的平板电容对DMMP蒸气也有响应，当暴露到20mg/m3DMMP蒸气中时，其电容响应仅为0.028%，低于电阻的响应。
3.采用自组装工艺在QCM上制备了单壁碳纳米管气体传感器，由聚电解质聚二烯丙基二甲基氯化铵（PDDA）和单壁碳纳米管层交替组装而成，发现传感器对湿度的响应明显大于DMMP蒸气的响应。并对比了含有-COOH和不含-COOH的碳纳米管原料对传感器湿敏的影响。结果发现，当湿度从20.9%变化到80.2%时，自组装PDDA/SWNT-COOH传感器和PDDA/SWNT QCM传感器的频率相对变化分别为16.64%和13.84%，前者相对于后者灵敏度提高了20.23%，而且选择性更好，响应时间更短，而恢复时间则更长，相应的湿滞也从3.9%增大到8.0%。这是因为含羧基的单壁碳纳米管在氧化处理后其π-π*转变结构和相应含氧官能团的含量高于经氧化处理的普通单壁碳纳米管。但是，两个传感器对60%饱和蒸气浓度DMMP蒸气的灵敏度却只有2.06%-2.17%。
Since the appearance of nerve agents, they are frequently used in war and terroristattacks. Therefore, the manufacture and development of nerve agent sensors are of greatsignificance for national and public security. Because of the high aspect ratio andspecific surface area, as well as the strong gas adsorption capacity, carbon nanotubes(CNTs) are ideal sensitive materals in gas sensors. In this dissertation, CNT thin filmswere prepared by airbrush, screen printing, chemical vapor deposition (CVD),electrophoresis and layer-by-layer self-assembly techniques, which were characterizedand analyzed with different methods. The planar interdigital capacitor and platecapacitor were fabricated, and the dimethyl methylphosphonate (DMMP) gas-sensingproperties of these CNT sensors were carried out and studied. The main research resultswere as follows:
1. Single-walled carbon nanotubes (SWNTs) were deposited on interdigitalelectrodes (IDTs) by airbrush method, and it formed interdigital capacitive sensor. Thecapacitance of this sensor decreased rapidly when exposed to DMMP. The capacitanceresponse increased with the increase of DMMP concentration and was12.43%to12mg/m3DMMP. The sensor had a good reproducibility and selectivity. Meanwhile, theresistance response of airbrush SWNT sensor was also studied. The resistance of thissensor increased immediately when exposed to DMMP and the response increased withthe increase of DMMP concentration, but the resistance response was smaller than thecapacitance response by one order in magnitude. The capacitance responses of airbrushmulti-walled carbon nanotube (MWNT) sensor and SWNT/DKAP (poly{methyl[3-(2-hydroxyl,3,5-bistrifluoromethyl)phenyl]propylsiloxane}) composite film sensor weresimilar to the response of airbrush SWNT sensor, but their responses were sigmificatelysmaller and were1.39%and0.54%to12mg/m3DMMP, respectively. The DKAPtwined and wrapped SWNTs in the composite film, reducing the effective surface areaof CNTs and causing the capacitance response significately smaller than thecorresponding SWNT sensor. It is also found that when the airbrush CNT sensor withlarger initial capacitance and loss tangent, the CNT film was denser, the average pore size was smaller and the effective surface area for gas adsorption was larger, leading tohigher capacitance response.
2. SWNT sensor was prepared on SiO2/Si substrate by screen printing, and theresistance response of this sensor to50ppm (250mg/m3) DMMP was16.4×10-3.Because there was residual ethyl cellu, etc. in the screen printed SWNT film, theresistance response was far less than the corresponding airbrush SWNT sensor. Thesensor had a very good reproducibility and long-term stability, but its resistancerecovered very slowly, which was more obvious at high concentration of DMMP. Thesensor had a good selectivity to the gases which were present in the air, such as water,oxygen and carbon dioxide. But the selectivity to the gases with redox, such as NH3,etc., and organic vapors, such as alcohols and aromatics, was very poor due to thestrong adsorption between these gases and the residual ethyl cellu. The capacitor formedby the two plates of the screen printed SWNT sensor had response to DMMP. Whenexposed to20mg/m3DMMP, the capacitance response was only0.028%, which wassmaller than the resistance response.
3. SWNT gas sensors were fabricated on quartz crystal microbalance (QCM) bylayer-by-layer self-assmbly of polyelectrolyte poly(diallyldimethylammonium chloride)(PDDA) and SWNTs. It was found that the sensors had a significantly greater responseto humidity than to DMMP. The effect of raw SWNT materials with and withoutcarboxyl (-COOH) on the humidity sensing properties of these SWNT composite thinfilm sensors was studied and compared. The results showed that when the relativehumidity was changed from20.9%to80.2%, the relative frequency shifts of thePDDA/SWNT-COOH QCM sensor and PDDA/SWNT QCM sensor were16.64%and13.84%, respectively. The former had a sensitivity enhanced by20.03%, a betterselectivity and a shorter response time, but the recovery time was longer and thehysteresis was increased from3.9%to8.0%. It was attributed to that the relative contentof π-π*transition structures and the corresponding functional groups in modifiedSWNTs-COOH was much higher than that in modified SWNTs. However, thesensitivities of the two sensors to60%saturated vapor pressure concentration of DMMPwere only2.06%-2.17%.
引文
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