气敏薄膜及气体传感器阵列的制备及特性研究
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摘要
利用具有不同选择性的多个气敏元件组成气体传感器阵列,可充分利用传感器阵列所提供的交叉敏,并运用人工神经网络的模式识别技术对其响应输出谱进行分析,就可以实现传感器的高选择性,并提高气体传感器的测量精度。军事和工程上有着广泛应用的电子鼻就是在此基础上发展起来的,它由气体传感器阵列、数据采集卡及模式识别算法三部分组成,它在食品、化工、环保、医疗诊断、毒品检验等方面有很重要的应用,其关键技术就是气体传感器阵列。
本论文以气敏薄膜及气体传感器阵列为研究对象,首先对气敏薄膜体系进行了系统研究:采用真空热蒸发工艺制备了WO_3薄膜、通过真空蒸发法和旋涂法制备了TCNQ薄膜和SnPc薄膜及它们与PMMA的复合薄膜、通过掺杂诱导自组装工艺制备了纳米金基底,并进一步制备了聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜。其次,率先设计了电子聚合物化学场效应管型气体传感器阵列结构,并针对基于聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜的气体传感器阵列的敏感特性进行系统的研究及分析。最后对气体传感器阵列测试算法进行了初期研究。所得到的主要结论及创新性结果可归纳如下:
1.采用真空热蒸发工艺及合适的热处理工艺,在微晶玻璃基片上得到了六方结构并且在<100>方向上择优取向的WO_3薄膜,得到了最佳成膜工艺条件。结果表明,WO_3薄膜是可以通过热处理晶化。研究表明,在退火处理温度为600℃,可以得到六方结构并且在<100>方向上择优取向的WO_3薄膜。对WO_3薄膜传感器NO_2敏感特性研究表明,其敏感特性很大程度上由蒸发时的工艺条件、热处理温度及工作温度决定。得到的最优条件为:热处理温度600℃、工作温度200℃。
2.采用掺杂诱导自组装与静电力自组装工艺相结合的方法制备了纳米金膜,在此基膜上进一步制备了聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜。研究表明,在胶体金的合成过程中,还原剂量越多,金纳米粒子的粒径越小且粒子为球形,粒度较均一,单分散性好;随着还原剂用量的减少,金纳米粒子的粒径变大,但其形状呈较明显的椭圆形。同时发现,与其他三种溶胶比较,使用乙醇溶剂胶体的自组装膜沉积粒子的分布比较均匀,平整度最好,达到纳米量级。XPS分析表明聚苯胺只在表面被部分掺杂,所制各自组装膜均匀、致密。研究表明,自组装的聚苯胺薄膜均匀牢固,与衬底的附着性较好。红外吸收谱分析表明,制备的聚苯胺薄膜在1683cm~(-1)处出现了一个新的峰值。气敏测试表明,聚苯胺薄膜对NO_2气体的灵敏度随膜层增加而增加,。
3.创新性地将TCNQ和SnPc小分子掺入PMMA中形成复合薄膜,并对掺杂前后薄膜的性能进行了系统研究。研究发现,真空蒸发制备的SnPc薄膜对于NO_2具有良好的敏感特性,但对NH_3敏感型很弱。同时发现,薄膜厚度控制在1200(?)敏感特性最好。研究发现,在PMMA/TCNQ的旋涂复合薄膜中,TCNQ晶体颗粒明显变小,分布比较均匀。旋涂制备的TCNQ薄膜对NH_3敏感性很好,但是响应和恢复随NH_3浓度的增加迅速增大,而TCNQ掺杂的PMMA旋涂薄膜的响应不稳定。旋涂制备的SnPc与PMMA复合薄膜对NO_2具有良好的敏感性,同时响应时间较快,达到10秒左右,具有实用价值,但恢复时间随NO_2浓度的增加而变长。纯SnPc的旋涂薄膜虽然有较好的灵敏度,但是响应时间相对较慢,而且恢复时间很长。
4.率先设计并研制出了化学场效应管型气体传感器阵列,并对其主要工艺参数进行了优化。气敏测试表明,本文设计的无栅结构气体传感器阵列器件的在一定浓度的气氛中重复性和响应时间(开关特性)均优于课题组初期设计的槽栅型化学场效应管器件。研究还表明,表明栅极绝缘层厚度对器件的灵敏度有很大影响,而增加金基底对NO_2气体响应输出灵敏度的提高有一定的改善。对阵列的气敏测试表明,低浓度下输出电流与气体浓度呈对数变化关系,且随膜层增大,器件输出响应在低浓度时灵敏度降低,在高浓度时灵敏度增加。气敏输出响应随气体浓度增大而指数增大,到一定浓度达到最大值,随后出现“中毒”现象。实验测试结果还发现,宽度相同的器件,一般情况下宽长比越大灵敏度越高。研究表明,气体传感器阵列对温湿度的响应成线性关系,因此,从本论文研制的气体传感器阵列中提取不同敏感量的特征响应向量,就可以实现环境介质如温度、湿度及气体浓度的检测,从而为研制检测温度、湿度及气体浓度的一体化环境介质传感器奠定了基础,这对国民生产和军事国防都有重要意义。
5.运用MATLAB设计了适用于线性系统与非线性系统的BP神经网络,得到了具有较大工程应用价值的阶段性成果。本论文运用BP算法与“提前停止”法相结合来处理非线性问题,加快了网络的训练速度,使网络的推广能力大大提高,为气体传感器阵列的实用化奠定了基础。研究表明,本论文设计的系统具有良好的非线性近似处理能力及很高的模式识别能力;
In the 21~(st) IT era, sensor plays a important role in our life, and more and more attention has been paid on this research topic. In order to detect more components using small and compact sensor unit, sensor array is one of the best choices to be realized. As each sensor responds to a class of gases rather than to a specific one (which is also called as over-lapping sensitivity), gas sensor arrays can make use of such over-lapping sensitivity. To process such a partial overlapping response, pattern recognition techniques are generally employed. Based on this principle, an electronic nose has been developed, which is conventionally made up of gas sensor array, data collecting card and pattern recognition, and has been widely used in many areas such as food, aerospace, environment, etc.
This dissertation mainly focused on gas sensing thin films and gas sensor array. Firstly, a few gas sensing thin films such as WO_3 thin films, TCNQ and SnPc thin films and their composite films with PMMA, and PANi/PSSA thin films were studied. Then, ChemFET gas sensor array was designed and investigated. Finally, testing algorithms were designed and simulated. The main conclusions and original results are summarized as follows.
1. WO_3 thin films were deposited on glass ceramics substrates with a pair of interdigitated Au-film electrodes by vacuum thermal evaporation, and then annealed at temperature between 300-600℃. It shows that crystallite phase and mean grain size varied significantly with the change of annealing temperature. As the annealing temperature increased, the general crystallite size considerably increased, and WO3 amorphous thin films began to crystallize. And finally we got WO3 thin films with hexagonal structure, which grew preferentially on the direction <100>. Annealing conditions and working temperatures play an important role in its sensitive characteristics to NO_2 The optimum conditions are as follows: annealing temperature 600℃and working temperature 200℃.
2. Gold nanoparticulate thin films were built up using the electrostatic self-assembly method. And self-assembled polyaniline (PANi) composite films with poly (styrenesulfonic acid) were fabricated based on doping-induced deposition effect above aurum. The gold colloid was a monodispersive suspension and had more uniform micro-particle with more sodium citrate or NaBH_4. The colloid synthesized using NaBH_4 with ethanol has the highest performance and has a micro-particle diameter of 1.7 nm. The self-assembled PAN films above the aurum were uniform and highly adhesive to the substrates. And there was a new infrared absorbance spectrum at 1683cm~(-1). It was also found out that the sensitivity of PANi/PSSA thin films increased with the number of film layer.
3. TCNQ and SnPc thin films were prepared by thermal vacuum evaporation. The effects of substrate temperature on the surface morphology and the conductance of the thin film have been investigated. The results show that TCNQ is sensitive to both NO_2 and NH_3, but the response and recovery rate are not fast. SnPc is sensitive to NO_2 but insensitive to NH_3.Then, TCNQ and SnPc films as well as their composite films with poly(metheyl methacrylate) (PMMA) were prepared by spin coating method. And we found that the crystalline grain of TCNQ in TCNQ/PMMA composite film became smaller than that of the pure TCNQ thin film. Results show that TCNQ film is highly sensitive to NH_3. The SnPc/PMMA composite film is also highly sensitive to NO_2 with fast response rate, but the recovery time becomes longer with the increase of gas concentration. The results show that TCNQ particles in TCNQ/PMMA composite film become smaller and disperse more uniform, but the response to NH_3 is unstable. TCNQ film is highly sensitive to NH_3 whereas the response and recovery time are much longer.
4. Based on conventional MOSFET, a novel kind of chemical field-effect transistor (ChemFET) gas sensor array have been designed and fabricated. The sensor consists of self-assembled PAN composite films with polymeric acids deposited on the gate area of MOSFET replacing metallic material. The gas-sensing property and mechanism of the ChemFET array was investigated. And the effect of temperature and humidity on the gas sensors array was also studied. The results show that the output of the array also changes with the temperature and humidity, which suggests that one-bodied sensor detecting temperature, humidity, and gas concentrations based on this kind of sensor array can be got.
5. BP algorithms in ANN used in linear and nolinear systems were designed to process gas sensor array signal. The simulation of gas sensor array has been made using computer simulation method, and BP artificial neural network has been designed by using MATLAB neural network toolbox to process and verify the simulation data. By combining BP algorithms with "early stopping" method, we found that the drilling time of this new method becomes shorter than common BP algorithm. The results also show that the algorithms designed in this work have good non-linear, approximation ability and high discrimination ratio.
In summary, the work in this dissertation is helpful for the development of gas sensor array, and high performance device can be anticipated based on this study.
本论文以气敏薄膜及气体传感器阵列为研究对象,首先对气敏薄膜体系进行了系统研究:采用真空热蒸发工艺制备了WO_3薄膜、通过真空蒸发法和旋涂法制备了TCNQ薄膜和SnPc薄膜及它们与PMMA的复合薄膜、通过掺杂诱导自组装工艺制备了纳米金基底,并进一步制备了聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜。其次,率先设计了电子聚合物化学场效应管型气体传感器阵列结构,并针对基于聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜的气体传感器阵列的敏感特性进行系统的研究及分析。最后对气体传感器阵列测试算法进行了初期研究。所得到的主要结论及创新性结果可归纳如下:
1.采用真空热蒸发工艺及合适的热处理工艺,在微晶玻璃基片上得到了六方结构并且在<100>方向上择优取向的WO_3薄膜,得到了最佳成膜工艺条件。结果表明,WO_3薄膜是可以通过热处理晶化。研究表明,在退火处理温度为600℃,可以得到六方结构并且在<100>方向上择优取向的WO_3薄膜。对WO_3薄膜传感器NO_2敏感特性研究表明,其敏感特性很大程度上由蒸发时的工艺条件、热处理温度及工作温度决定。得到的最优条件为:热处理温度600℃、工作温度200℃。
2.采用掺杂诱导自组装与静电力自组装工艺相结合的方法制备了纳米金膜,在此基膜上进一步制备了聚苯胺/聚苯乙烯磺酸掺杂自组装复合膜。研究表明,在胶体金的合成过程中,还原剂量越多,金纳米粒子的粒径越小且粒子为球形,粒度较均一,单分散性好;随着还原剂用量的减少,金纳米粒子的粒径变大,但其形状呈较明显的椭圆形。同时发现,与其他三种溶胶比较,使用乙醇溶剂胶体的自组装膜沉积粒子的分布比较均匀,平整度最好,达到纳米量级。XPS分析表明聚苯胺只在表面被部分掺杂,所制各自组装膜均匀、致密。研究表明,自组装的聚苯胺薄膜均匀牢固,与衬底的附着性较好。红外吸收谱分析表明,制备的聚苯胺薄膜在1683cm~(-1)处出现了一个新的峰值。气敏测试表明,聚苯胺薄膜对NO_2气体的灵敏度随膜层增加而增加,。
3.创新性地将TCNQ和SnPc小分子掺入PMMA中形成复合薄膜,并对掺杂前后薄膜的性能进行了系统研究。研究发现,真空蒸发制备的SnPc薄膜对于NO_2具有良好的敏感特性,但对NH_3敏感型很弱。同时发现,薄膜厚度控制在1200(?)敏感特性最好。研究发现,在PMMA/TCNQ的旋涂复合薄膜中,TCNQ晶体颗粒明显变小,分布比较均匀。旋涂制备的TCNQ薄膜对NH_3敏感性很好,但是响应和恢复随NH_3浓度的增加迅速增大,而TCNQ掺杂的PMMA旋涂薄膜的响应不稳定。旋涂制备的SnPc与PMMA复合薄膜对NO_2具有良好的敏感性,同时响应时间较快,达到10秒左右,具有实用价值,但恢复时间随NO_2浓度的增加而变长。纯SnPc的旋涂薄膜虽然有较好的灵敏度,但是响应时间相对较慢,而且恢复时间很长。
4.率先设计并研制出了化学场效应管型气体传感器阵列,并对其主要工艺参数进行了优化。气敏测试表明,本文设计的无栅结构气体传感器阵列器件的在一定浓度的气氛中重复性和响应时间(开关特性)均优于课题组初期设计的槽栅型化学场效应管器件。研究还表明,表明栅极绝缘层厚度对器件的灵敏度有很大影响,而增加金基底对NO_2气体响应输出灵敏度的提高有一定的改善。对阵列的气敏测试表明,低浓度下输出电流与气体浓度呈对数变化关系,且随膜层增大,器件输出响应在低浓度时灵敏度降低,在高浓度时灵敏度增加。气敏输出响应随气体浓度增大而指数增大,到一定浓度达到最大值,随后出现“中毒”现象。实验测试结果还发现,宽度相同的器件,一般情况下宽长比越大灵敏度越高。研究表明,气体传感器阵列对温湿度的响应成线性关系,因此,从本论文研制的气体传感器阵列中提取不同敏感量的特征响应向量,就可以实现环境介质如温度、湿度及气体浓度的检测,从而为研制检测温度、湿度及气体浓度的一体化环境介质传感器奠定了基础,这对国民生产和军事国防都有重要意义。
5.运用MATLAB设计了适用于线性系统与非线性系统的BP神经网络,得到了具有较大工程应用价值的阶段性成果。本论文运用BP算法与“提前停止”法相结合来处理非线性问题,加快了网络的训练速度,使网络的推广能力大大提高,为气体传感器阵列的实用化奠定了基础。研究表明,本论文设计的系统具有良好的非线性近似处理能力及很高的模式识别能力;
In the 21~(st) IT era, sensor plays a important role in our life, and more and more attention has been paid on this research topic. In order to detect more components using small and compact sensor unit, sensor array is one of the best choices to be realized. As each sensor responds to a class of gases rather than to a specific one (which is also called as over-lapping sensitivity), gas sensor arrays can make use of such over-lapping sensitivity. To process such a partial overlapping response, pattern recognition techniques are generally employed. Based on this principle, an electronic nose has been developed, which is conventionally made up of gas sensor array, data collecting card and pattern recognition, and has been widely used in many areas such as food, aerospace, environment, etc.
This dissertation mainly focused on gas sensing thin films and gas sensor array. Firstly, a few gas sensing thin films such as WO_3 thin films, TCNQ and SnPc thin films and their composite films with PMMA, and PANi/PSSA thin films were studied. Then, ChemFET gas sensor array was designed and investigated. Finally, testing algorithms were designed and simulated. The main conclusions and original results are summarized as follows.
1. WO_3 thin films were deposited on glass ceramics substrates with a pair of interdigitated Au-film electrodes by vacuum thermal evaporation, and then annealed at temperature between 300-600℃. It shows that crystallite phase and mean grain size varied significantly with the change of annealing temperature. As the annealing temperature increased, the general crystallite size considerably increased, and WO3 amorphous thin films began to crystallize. And finally we got WO3 thin films with hexagonal structure, which grew preferentially on the direction <100>. Annealing conditions and working temperatures play an important role in its sensitive characteristics to NO_2 The optimum conditions are as follows: annealing temperature 600℃and working temperature 200℃.
2. Gold nanoparticulate thin films were built up using the electrostatic self-assembly method. And self-assembled polyaniline (PANi) composite films with poly (styrenesulfonic acid) were fabricated based on doping-induced deposition effect above aurum. The gold colloid was a monodispersive suspension and had more uniform micro-particle with more sodium citrate or NaBH_4. The colloid synthesized using NaBH_4 with ethanol has the highest performance and has a micro-particle diameter of 1.7 nm. The self-assembled PAN films above the aurum were uniform and highly adhesive to the substrates. And there was a new infrared absorbance spectrum at 1683cm~(-1). It was also found out that the sensitivity of PANi/PSSA thin films increased with the number of film layer.
3. TCNQ and SnPc thin films were prepared by thermal vacuum evaporation. The effects of substrate temperature on the surface morphology and the conductance of the thin film have been investigated. The results show that TCNQ is sensitive to both NO_2 and NH_3, but the response and recovery rate are not fast. SnPc is sensitive to NO_2 but insensitive to NH_3.Then, TCNQ and SnPc films as well as their composite films with poly(metheyl methacrylate) (PMMA) were prepared by spin coating method. And we found that the crystalline grain of TCNQ in TCNQ/PMMA composite film became smaller than that of the pure TCNQ thin film. Results show that TCNQ film is highly sensitive to NH_3. The SnPc/PMMA composite film is also highly sensitive to NO_2 with fast response rate, but the recovery time becomes longer with the increase of gas concentration. The results show that TCNQ particles in TCNQ/PMMA composite film become smaller and disperse more uniform, but the response to NH_3 is unstable. TCNQ film is highly sensitive to NH_3 whereas the response and recovery time are much longer.
4. Based on conventional MOSFET, a novel kind of chemical field-effect transistor (ChemFET) gas sensor array have been designed and fabricated. The sensor consists of self-assembled PAN composite films with polymeric acids deposited on the gate area of MOSFET replacing metallic material. The gas-sensing property and mechanism of the ChemFET array was investigated. And the effect of temperature and humidity on the gas sensors array was also studied. The results show that the output of the array also changes with the temperature and humidity, which suggests that one-bodied sensor detecting temperature, humidity, and gas concentrations based on this kind of sensor array can be got.
5. BP algorithms in ANN used in linear and nolinear systems were designed to process gas sensor array signal. The simulation of gas sensor array has been made using computer simulation method, and BP artificial neural network has been designed by using MATLAB neural network toolbox to process and verify the simulation data. By combining BP algorithms with "early stopping" method, we found that the drilling time of this new method becomes shorter than common BP algorithm. The results also show that the algorithms designed in this work have good non-linear, approximation ability and high discrimination ratio.
In summary, the work in this dissertation is helpful for the development of gas sensor array, and high performance device can be anticipated based on this study.
引文
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