十六氯酞菁锌有机半导体材料的合成及其气敏性研究

Due to the difficulty in synthesizing perhalogenated metallophthalocyanine, the method of ammonium molybdate solid phase catalysis was introduced, and by using tetrachlorophthalic anhydride and urea as the raw materials, hexadecachloro zinc phthalocyanine （ZnPcCl16） was synthesized. Components of the composite were analyzed by energy spectrum, and its functional group structures and absorption peaks were characterized by IR and UV-vis spectroscopy. The thin films of gas sensors were prepared in a vacuum evaporation system and evaporated onto SiO2 substrates, where sensing electrodes were made by MEMS micromachining. The optimal conditions for the films are： substrate temperature of 150 ℃ evaporation current of 95 A and film thickness of 50 nm. The result showed that the sensors were ideally sensitive to Cl2 gas and could detect the minimum concentration of 0.3 ppm.     

酞菁钯-聚苯胺修饰声表面波传感器及含磷毒气的检测

针对含磷毒气快速检测问题,以自制的杂化酞菁钯.聚苯胺为敏感膜材料,设计了一种双信道声表面波(SAW)传感器.阐述了传感器的基本原理,推导出以有机膜作为信道中间介质时,差频输出△f由物理化学吸附两种机制叠加的数学模型.依据声波振荡条件,设计了146±5MHz振荡频率的信号采集电路;以钽酸锂晶体为压电基片,通过MEMS微加工技术形成叉指电极对和加热膜;以真空镀膜工艺将敏感膜材料成膜,修饰在SAW信道中间区域构成SAW传感器.测试结果表明:最优气敏性时的材料配比为PdPc0.35PANI0.65;芯片加热60～80℃可提高性能,响应时间≤30s;输出与测试气体浓度与数学模型一致,为线性变化率-110kHz(mg/m3)的N型线性关系;抗汽油、CO2等气体干扰;80天稳定性考核,△f≤±0.1kHz,满足实际使用要求.     

基于MEMS叠层微结构SO2毒气传感器的研究

针对新型有机半导体电导率偏低的技术难点,提出了一种多孔上电极的叠层微结构,以真空镀膜技术形成气敏膜,采用MEMS微加工制成气体传感器。依据等效电路和工艺边界条件,通过电导公式推导出传感器的输出电导可提高103倍,解决了有机半导体的信号采集问题。通过SEM微观形貌,确认蒸发电流100~120A、蒸发时间8~12s的电极成膜最佳条件;气敏膜表面呈现二次化学反应融合的200nm左右“米粒状” 活性颗粒状态,均匀一致,孔隙有序。测试结果表明：对SO2最佳灵敏度时,比例系数为0.15~0.35硫酸掺杂CuPcxPANI1-x,考虑到减少H2S气体干扰,选择CuPc0.35PANI0.65;加热电压VH为1~2.5V会提高灵敏度特性和响应恢复特性,响应时间30 s;传感器输出特性为单对数线性关系,可实现0~200×10-6之间检测范围;6个月的稳定性考核,输出阻抗漂移≤±5%,灵敏度漂移≤10%。     

纳米孔Al2 O3修饰Si基氨气传感器设计

针对Si基微结构气体传感器中Si基与敏感材料之间附着性较差的问题,提出在Si基与敏感材料之间引入纳米孔Al2 O3膜形成新型Si基微结构传感器,利用ANSYS分析软件对微结构进行热分析。采用薄膜工艺、光刻工艺、电化学阳极氧化工艺在Si衬底上制成Si基微结构,采用超声波的方法使聚苯胺敏感材料渗入纳米孔Al2 O3膜中制成气体传感器,并在室温下测试了传感器对氨气的检测特性。结果表明：将纳米孔Al2 O3膜移植到Si基上增加了敏感材料的附着性;传感器对响应时间约为40 s,恢复时间约为960 s,灵敏度随着氨气浓度的增加而增大,并且呈现出良好的线性关系。     

多孔型阳极氧化铝膜的制备及微观分析

在硫酸电解液、草酸和磷酸电解液中,采用阳极氧化方法制备多孔型氧化铝膜。通过扫描电子显微镜对多孔型氧化铝膜进行形貌表征。根据试验得到:当0.3mol/L硫酸中,恒压25V阳极氧化1h可得到孔径约为40～60nm多孔氧化铝膜。在电解液为10.0g/L草酸与3.0ml/L磷酸混合液中,恒压140V二次阳极氧化可得到孔径为160～190nm多孔氧化铝膜。讨论了高温退火及磷酸处理对多孔氧化铝膜的影响,并进行了机理分析。     

In-Nb复合半导体氧化物Cl2敏感特性的研究

以检测Cl2为目标,采用恒温化学共沉积法合成了In-Nb复合半导体氧化物,并研究了其气体传感器的制作方法,分析了In-Nb气敏材料的微观特性和敏感特性,探讨了气敏机理。实验证明,In-Nb材料具有良好的Cl2敏感特性。     

酞菁钯-聚苯胺修饰声表面波传感器及含磷毒气的检测

针对含磷毒气快速检测问题,以自制的杂化酞菁钯.聚苯胺为敏感膜材料,设计了一种双信道声表面波(SAW)传感器.阐述了传感器的基本原理,推导出以有机膜作为信道中间介质时,差频输出△f由物理化学吸附两种机制叠加的数学模型.依据声波振荡条件,设计了146±5MHz振荡频率的信号采集电路;以钽酸锂晶体为压电基片,通过MEMS微加工技术形成叉指电极对和加热膜;以真空镀膜工艺将敏感膜材料成膜,修饰在SAW信道中间区域构成SAW传感器.测试结果表明:最优气敏性时的材料配比为PdPc0.35PANI0.65;芯片加热60～80℃可提高性能,响应时间≤30s;输出与测试气体浓度与数学模型一致,为线性变化率-110kHz(mg/m3)的N型线性关系;抗汽油、CO2等气体干扰;80天稳定性考核,△f≤±0.1kHz,满足实际使用要求.     

基于MEMS叠层微结构的SO2毒气传感器

利用多孔上电极叠层微结构,以真空镀膜技术形成气敏膜,采用MEMS微加工技术研制了气体传感器.依据等效电路和工艺边界条件,通过电导公式推导出传感器的输出电导提高了103倍,解决了有机半导体的信号采集问题.通过SEM微观形貌,确认蒸发电流100～120 A、蒸发时间8～12 s为电极成膜最佳条件;气敏膜表面呈现二次化学反应融合的200 nm左右"米粒状" 活性颗粒状态,均匀一致,孔隙有序.测试结果表明:比例系数为0.15～0.35的硫酸掺杂CuPcxPANI 1-x对SO2有最佳的灵敏度;考虑到减少H2S气体干扰,选择CuPc0.35PANI0.65为气敏材料,在加热电压VH为1～2.5 V时提高了传感器的灵敏度特性和响应恢复特性,响应时间为30 s;传感器输出特性为单对数线性关系,检测范围为0～200×10-6;经6个月的稳定性考核,其输出阻抗漂移≤±5%,灵敏度漂移≤10%.     

In基复合半导体氧化物Cl2敏感特性的研究

Aiming at detecting Cl2 gas, this study was made on how to make In-based compound semiconductor oxide gas sensor. The micro-property and sensitivity of In-based gas sensing material were analyzed and its gas sensitive mechanism was also discussed. Adopting constant temperature chemical coprecipitation, the compound oxides such as In-Nb, In-Cd and In-Mg were synthesized, respectively. The products were sintered at 600 ℃ and characterized by the Scanning Electron Microscope （SEM）, showing the grain size almost about 50-60 nm. The test results show that the sensitivities of In-Nb, In-Cd and In-Mg materials under the concentration of 50 × 10^-6 in Cl2 gas are above 100 times, 4 times and 10 times, respectively. The response time of In-Nb, In-Cd and In-Mg materials is about 30, 60 and 30 s, and the recovery time less than 2, 10 and 2 min, respectively. Among them, the In-Nb material was found to have a relatively high conductivity and ideal sensitivity to Cl2 gas, which showed rather good selectivity and stability, and could detect the minimum concentration of 0.5 × 10^-6 with the sensitivity of 2.2, and the upper limit concentration of 500 × 10^-6. The power loss of the device is around 220 mW under the heating voltage of 3 V.     

基于MSP430的高压开关柜火灾预警系统的研制

采用红外热电堆为温度传感器,设计了一种基于MSP430单片机的高压开关柜火灾预警系统,该系统由温度传感器,信号调理电路,单片机,RS485网络和上位机组成。系统能实现对多个开关柜内接点进行温度实时测量,并具有温度预警功能,其测量误差不超过1℃。通过RS485网络,该系统能够与变电站综合自动化系统相连,实现远程监测。该系统为高压开关柜提供了超温预警,有效地预防了电气火灾的发生。