聚苯胺基复合材料的制备及其气敏性能研究
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摘要
对于SnO_2、Fe_2O_3、ZnO等传统的无机金属氧化物气敏材料,自上世纪60年代以来广大科技工作者已进行了广泛而深入的研究,使气体传感器在民用和工业等方面的应用得到了很大发展。但到目前为止,半导体气敏元件仍然存在选择性差、功耗高、环境温湿度效应大等缺点,从而限制了气体传感器的发展和应用。针对目前半导体气敏元件中存在的问题,本文对聚苯胺基复合材料的合成、气敏性能和气敏机理等有关问题进行了较为系统的研究。主要研究内容如下:
采用化学氧化聚合法,以苯胺为单体,过硫酸铵为氧化剂,在HCl介质中合成了掺杂态聚苯胺,采用傅里叶红外光谱和紫外可见光光谱对聚苯胺掺杂前后的结构变化进行了分析,系统研究了单体浓度、氧化剂用量、酸浓度、聚合温度、聚合时间、工作温度、环境湿度等因素对聚苯胺气敏性能的影响。结果表明,经HCl掺杂后的聚苯胺在室温下对NH_3具有较好的灵敏度,对常见干扰气体具有较高的选择性,不同的制备条件和工作环境对材料的气敏性能影响较大。同时还对聚苯胺材料的响应恢复过程进行了分析,研究了聚苯胺材料与NH_3气体接触前后的结构变化以及材料与目标气体之间的相互作用机制,为进一步研究聚苯胺基复合材料的气敏机理奠定了一定基础。
针对HCl掺杂态聚苯胺易脱掺杂、环境稳定性差的缺点,以大分子有机磺酸对甲基苯磺酸、十二烷基苯磺酸和磺基水杨酸为掺杂剂,采用水溶液化学氧化法直接合成了不同磺酸掺杂的聚苯胺,元素分析的结果表明,所合成材料的掺杂率可达40%左右。采用TGA-DTA技术对不同掺杂态聚苯胺的热分解过程进行了研究,结果表明,掺杂剂的加入降低了聚苯胺分子链的分解温度,与HCl掺杂相比,有机磺酸掺杂的聚苯胺具有更好的热稳定性。对材料的气敏性能的研究结果表明,有机磺酸掺杂的聚苯胺比盐酸掺杂的聚苯胺的灵敏度有了很大提高,其中磺基水杨酸掺杂的聚苯胺在室温下对1000ppm NH_3的灵敏度达到了15.47,且元件的响应时间小于30s,恢复时间小于3min,响应恢复性能良好,同时还测试了不同酸掺杂聚苯胺灵敏度的长期稳定性,结合TGA-DTA的分析结果,表明有机磺酸掺杂的聚苯胺具有较好的环境稳定性,因而具有一定的实用价值。
针对单一的聚苯胺材料不易成膜、可加工性差的缺点,采用原位复合法分别合成了PAn-SSA/SnO_2和PAn-SSA/In_2O_3复合材料,红外光谱和X射线衍射(XRD)分析结果表明,纳米金属氧化物粒子与聚苯胺之间存在着相互作用;TGA-DTA的分析结果表明,无机纳米粒子的加入能够提高聚苯胺的链分解温度,改善聚苯胺的环境稳定性;研究还发现,复合材料的气敏性能受到纳米粒子的用量的影响,当纳米SnO_2和纳米In_2_3的用量分别为50%和30%时,复合材料的灵敏度达到最高,适量纳米粒子的加入不会对材料的选择性产生不利影响,且PAn/纳米In_2O_3复合材料能够在提高元件选择性的同时减少响应恢复时间,因而更具有实际应用前景。
将聚苯胺与传统的高分子材料进行复合是改善聚苯胺成膜和加工性能的又一方法,但是普通的聚苯胺/高分子复合材料在提高聚苯胺可加工性能的同时,往往会降低材料的气敏性能。针对这一问题,本文以十二烷基苯磺酸作为乳化剂和掺杂剂,在聚乙酸乙烯酯-聚乙烯醇复合乳液中采用乳液聚合法得到聚苯胺/聚乙酸乙烯酯-聚乙烯醇复合乳液,并采用高分子辅助倒相法制备出了聚苯胺/聚乙烯醇多孔复合材料。研究结果表明,抽提对复合膜中的聚苯胺结构影响不大,但复合膜的表面出现了明显的多孔性结构,使抽提后元件的灵敏度和响应恢复性能均有很大提高,连续使用50天后灵敏度未见明显变化,具有良好的环境稳定性。文章最后指出,如果能够控制元件表面的孔结构,将有可能在保持元件灵敏度和响应恢复性能的同时提高元件的选择性。
Since 1960,the conventional semiconductor gas-sensing materials(SnO_2,Fe_2O_3, ZnO,and so on,) have been extensively studied by many researchers,and the application of gas sensors has been developed in domestic and industrial fields.But the semiconductor gas sensors have some disadvantages such as poor sensitivity,high power consumption and large dependence of environmental temperature and humidity, thus the development and application of semiconductor gas sensor are limited.In order to upgrade the gas-sensing properties of semiconductor gas sensor,the preparation,gas-sensing properties,and sensing mechanism of gas-sensing materials based on polyaniline(PAn) have been investigated systemically in this thesis.The contents are listed below:
Aniline was oxidized by ammonium persulfate(APS) in HC1 for the synthesis of PAn.By means of FTIR spectra and UV-Vis spectra,the structural changes of intrinsic and doped PAn were measured.The influence of the reaction condition on the PAn sensitive properties have been investigated systemically such as the concentration of monomer,APS and HC1,the reaction temperature and reaction time, environmental temperature and humidity et al.The results reveal that gas sensors based on HC1 doped PAn have a high sensitive and selective properties to NH3 under the room temperature,but the gas-sensing properties of materials were influenced by synthesis and environmental conditions.In the same time,the response and recovery process has been analysised,the interaction mechanism of PAn and target gas was also investigated by measure the structural changes of HC1 doped PAn after it contact with NH3,which establish the base to investigate the gas-sensing mechanism of composites based on PAn.
In order to upgrade the environmental stability of gas sensors based on PAn, organic sulfonic acid such as TSA,DBSA and SSA were used as doped acids to synthesis PAn.The thermal decomposition process of different acids doped PAn were investigated by means of TGA-DTA.It can be found that the dopants reduced the decomposed temperature of the molecule chain of PAn,organic sulfonic acid doped PAn has better thermal stability than HC1 doped PAn.Sensitive properties of organic sulfonic acid doped PAn have also been investigated,the results reveal that the gas sensors based on organic sulfonic acid doped PAn have better sensitive and response-recovery properties than HC1 doped PAn,especially the sensitivity of PAn-SSA to 1000ppm NH_3 reached 15.47,the response time less than 30S,recovery time less than 3min.Long-term stability of different acid doped PAn were also investigated,combine with the analysis result of TGA-DTA,it can be concluded that organic sulfonic acid doped PAn have better environmental stability.
In order to improve the processability of PAn,PAn-SSA/nano-SnO_2 and PAn-SSA/nano-In_2O_3 composites were synthesized respectively by in situ polymerization.Interaction of PAn and inorganic nano-particles were confirmed by FTIR and XRD.The thermal stability of the two composites was investigated by TGA-DTA.The results suggest that the thermal stability of the two composites is higher than that of the PAn.Sensitive properties of the composites were influenced by the contents of inorganic nano-particles,sensitivity of the two composites reached highest when the content of nano-SnO_2 and nano-In_2O_3 reached 50%and 30% respectively.PAn-SSA/nano-In_2O_3 composites are more suitable as practical sensor materials because it can improve the sensitivity and selectivity of composites simultaneousely.
The synthesis of its blends with ordinary polymers was the other way to improve the processability of PAn,but the ordinary PAn/polymer composites usually harmed the sensitive properties of PAn.In this thesis,PAn were synthesized in the composite emulsion system of PVA-PVAc,DBSA was used as dopants and emulsifier.Polymer assisted phase inversion(PAPI) process was used first to get PAn/PVA porous composite gas sensitive material.The FTIR and SEM indicates that the extraction has little effect on the structure of PAn in the composite membrane but the porous structure was formed on the composite film after extracting by acetone,which can improve the sensitive and response-recovery properties of the composites.The environmental stability is perfect because its sensitivity varieties in a narrow range during 50 days.The selective property of the composite membrane should also be improved if the pore structure can be controlled.
采用化学氧化聚合法,以苯胺为单体,过硫酸铵为氧化剂,在HCl介质中合成了掺杂态聚苯胺,采用傅里叶红外光谱和紫外可见光光谱对聚苯胺掺杂前后的结构变化进行了分析,系统研究了单体浓度、氧化剂用量、酸浓度、聚合温度、聚合时间、工作温度、环境湿度等因素对聚苯胺气敏性能的影响。结果表明,经HCl掺杂后的聚苯胺在室温下对NH_3具有较好的灵敏度,对常见干扰气体具有较高的选择性,不同的制备条件和工作环境对材料的气敏性能影响较大。同时还对聚苯胺材料的响应恢复过程进行了分析,研究了聚苯胺材料与NH_3气体接触前后的结构变化以及材料与目标气体之间的相互作用机制,为进一步研究聚苯胺基复合材料的气敏机理奠定了一定基础。
针对HCl掺杂态聚苯胺易脱掺杂、环境稳定性差的缺点,以大分子有机磺酸对甲基苯磺酸、十二烷基苯磺酸和磺基水杨酸为掺杂剂,采用水溶液化学氧化法直接合成了不同磺酸掺杂的聚苯胺,元素分析的结果表明,所合成材料的掺杂率可达40%左右。采用TGA-DTA技术对不同掺杂态聚苯胺的热分解过程进行了研究,结果表明,掺杂剂的加入降低了聚苯胺分子链的分解温度,与HCl掺杂相比,有机磺酸掺杂的聚苯胺具有更好的热稳定性。对材料的气敏性能的研究结果表明,有机磺酸掺杂的聚苯胺比盐酸掺杂的聚苯胺的灵敏度有了很大提高,其中磺基水杨酸掺杂的聚苯胺在室温下对1000ppm NH_3的灵敏度达到了15.47,且元件的响应时间小于30s,恢复时间小于3min,响应恢复性能良好,同时还测试了不同酸掺杂聚苯胺灵敏度的长期稳定性,结合TGA-DTA的分析结果,表明有机磺酸掺杂的聚苯胺具有较好的环境稳定性,因而具有一定的实用价值。
针对单一的聚苯胺材料不易成膜、可加工性差的缺点,采用原位复合法分别合成了PAn-SSA/SnO_2和PAn-SSA/In_2O_3复合材料,红外光谱和X射线衍射(XRD)分析结果表明,纳米金属氧化物粒子与聚苯胺之间存在着相互作用;TGA-DTA的分析结果表明,无机纳米粒子的加入能够提高聚苯胺的链分解温度,改善聚苯胺的环境稳定性;研究还发现,复合材料的气敏性能受到纳米粒子的用量的影响,当纳米SnO_2和纳米In_2_3的用量分别为50%和30%时,复合材料的灵敏度达到最高,适量纳米粒子的加入不会对材料的选择性产生不利影响,且PAn/纳米In_2O_3复合材料能够在提高元件选择性的同时减少响应恢复时间,因而更具有实际应用前景。
将聚苯胺与传统的高分子材料进行复合是改善聚苯胺成膜和加工性能的又一方法,但是普通的聚苯胺/高分子复合材料在提高聚苯胺可加工性能的同时,往往会降低材料的气敏性能。针对这一问题,本文以十二烷基苯磺酸作为乳化剂和掺杂剂,在聚乙酸乙烯酯-聚乙烯醇复合乳液中采用乳液聚合法得到聚苯胺/聚乙酸乙烯酯-聚乙烯醇复合乳液,并采用高分子辅助倒相法制备出了聚苯胺/聚乙烯醇多孔复合材料。研究结果表明,抽提对复合膜中的聚苯胺结构影响不大,但复合膜的表面出现了明显的多孔性结构,使抽提后元件的灵敏度和响应恢复性能均有很大提高,连续使用50天后灵敏度未见明显变化,具有良好的环境稳定性。文章最后指出,如果能够控制元件表面的孔结构,将有可能在保持元件灵敏度和响应恢复性能的同时提高元件的选择性。
Since 1960,the conventional semiconductor gas-sensing materials(SnO_2,Fe_2O_3, ZnO,and so on,) have been extensively studied by many researchers,and the application of gas sensors has been developed in domestic and industrial fields.But the semiconductor gas sensors have some disadvantages such as poor sensitivity,high power consumption and large dependence of environmental temperature and humidity, thus the development and application of semiconductor gas sensor are limited.In order to upgrade the gas-sensing properties of semiconductor gas sensor,the preparation,gas-sensing properties,and sensing mechanism of gas-sensing materials based on polyaniline(PAn) have been investigated systemically in this thesis.The contents are listed below:
Aniline was oxidized by ammonium persulfate(APS) in HC1 for the synthesis of PAn.By means of FTIR spectra and UV-Vis spectra,the structural changes of intrinsic and doped PAn were measured.The influence of the reaction condition on the PAn sensitive properties have been investigated systemically such as the concentration of monomer,APS and HC1,the reaction temperature and reaction time, environmental temperature and humidity et al.The results reveal that gas sensors based on HC1 doped PAn have a high sensitive and selective properties to NH3 under the room temperature,but the gas-sensing properties of materials were influenced by synthesis and environmental conditions.In the same time,the response and recovery process has been analysised,the interaction mechanism of PAn and target gas was also investigated by measure the structural changes of HC1 doped PAn after it contact with NH3,which establish the base to investigate the gas-sensing mechanism of composites based on PAn.
In order to upgrade the environmental stability of gas sensors based on PAn, organic sulfonic acid such as TSA,DBSA and SSA were used as doped acids to synthesis PAn.The thermal decomposition process of different acids doped PAn were investigated by means of TGA-DTA.It can be found that the dopants reduced the decomposed temperature of the molecule chain of PAn,organic sulfonic acid doped PAn has better thermal stability than HC1 doped PAn.Sensitive properties of organic sulfonic acid doped PAn have also been investigated,the results reveal that the gas sensors based on organic sulfonic acid doped PAn have better sensitive and response-recovery properties than HC1 doped PAn,especially the sensitivity of PAn-SSA to 1000ppm NH_3 reached 15.47,the response time less than 30S,recovery time less than 3min.Long-term stability of different acid doped PAn were also investigated,combine with the analysis result of TGA-DTA,it can be concluded that organic sulfonic acid doped PAn have better environmental stability.
In order to improve the processability of PAn,PAn-SSA/nano-SnO_2 and PAn-SSA/nano-In_2O_3 composites were synthesized respectively by in situ polymerization.Interaction of PAn and inorganic nano-particles were confirmed by FTIR and XRD.The thermal stability of the two composites was investigated by TGA-DTA.The results suggest that the thermal stability of the two composites is higher than that of the PAn.Sensitive properties of the composites were influenced by the contents of inorganic nano-particles,sensitivity of the two composites reached highest when the content of nano-SnO_2 and nano-In_2O_3 reached 50%and 30% respectively.PAn-SSA/nano-In_2O_3 composites are more suitable as practical sensor materials because it can improve the sensitivity and selectivity of composites simultaneousely.
The synthesis of its blends with ordinary polymers was the other way to improve the processability of PAn,but the ordinary PAn/polymer composites usually harmed the sensitive properties of PAn.In this thesis,PAn were synthesized in the composite emulsion system of PVA-PVAc,DBSA was used as dopants and emulsifier.Polymer assisted phase inversion(PAPI) process was used first to get PAn/PVA porous composite gas sensitive material.The FTIR and SEM indicates that the extraction has little effect on the structure of PAn in the composite membrane but the porous structure was formed on the composite film after extracting by acetone,which can improve the sensitive and response-recovery properties of the composites.The environmental stability is perfect because its sensitivity varieties in a narrow range during 50 days.The selective property of the composite membrane should also be improved if the pore structure can be controlled.
引文
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