多孔硅基复合薄膜气敏传感器的研究
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摘要
多孔硅是一种新兴的室温气敏材料。由于其具有较高的比表面积，而且制备过程简单，近年来被广泛应用于气体检测及环境监视领域。本文主要针对大孔硅、大孔硅基氧化钨、介孔硅以及介孔硅基氧化钨气敏传感器的制备与性能进行分析和研究。
采用双槽电化学腐蚀法腐蚀P型单晶硅形成有序大孔硅。研究了不同的腐蚀时间对于大孔硅结构、孔隙率、电学和气敏特性的影响。研究发现：随着腐蚀时间的增加，大孔硅的腐蚀深度增加，孔隙率变大。大孔硅与电极之间形成了欧姆接触。腐蚀时间为5min的大孔硅气敏特性最好。其在室温下对50ppm的NH_3的灵敏度为4.2，响应/恢复时间为51s/242s，恢复特性良好。
以大孔硅为基底，在其上溅射淀积氧化钨薄膜，制备出了大孔硅基氧化钨气敏传感器。研究了大孔硅基氧化钨薄膜的形貌，晶体结构，成分以及气敏特性。通过SEM观察发现，氧化钨薄膜淀积在大孔硅表面。气敏特性实验表明：气敏特性最好的大孔硅基氧化钨气敏传感器对1ppm、10ppm、25ppm和50ppm的NO_2的灵敏度分别为1.40、5.01、9.01和14.4，明显好于大孔硅对NO_2的气敏特性。
使用双槽电化学腐蚀法在P型重掺杂单晶硅表面制备介孔硅。分析了不同腐蚀电流密度对于介孔硅的结构，深度，孔隙率，电学特性和气敏特性的影响。结果表明：随着腐蚀电流密度的增加，其表面孔洞增多，深度增加，孔隙率变大，电阻升高。腐蚀电流密度为80mA/cm~2的介孔硅的室温气敏性能最好。与大孔硅相比，介孔硅具有较高的气体灵敏度。大孔硅对NH_3具有较好的选择性，而介孔硅对NO_2具有较好的选择性。随后采用不同放置方法对介孔硅的气敏稳定性进行了研究。实验发现：采用真空放置的介孔硅气敏稳定性较好。
采用对向靶直流反应磁控溅射法在介孔硅上制备介孔硅基氧化钨气敏传感器，通过实验分析了溅射时间、溅射压强和氩氧比等各因素对介孔硅基氧化钨薄膜微观结构和气敏特性的影响，获得了制备介孔硅基氧化钨薄膜的各个溅射工艺条件的最佳参数。通过不同温度下介孔硅和介孔硅基氧化钨气敏传感器对于NO_2和NH_3灵敏度对比发现：介孔硅基氧化钨气敏传感器具有比介孔硅更好的气敏特性。在室温下，其对1ppm的NO_2的灵敏度为4.22，对50ppm的NH_3的灵敏度为18.3。并且响应速度较快，很大程度上缩短了响应时间。
Porous silicon (PS) is a new type gas sensor which operated at room temperature.As it has large specific surface and can be easily produced, it has been widely used inthe fields of gas detecting and environmental protection. In this paper, macro-PS,WO_3/macro-PS, meso-PS and WO_3/meso-PS were prepared. The gas sensingproperties of macro-PS, WO_3/macro-PS, meso-PS and WO_3/meso-PS werethoroughly analyzed and studied.
Ordered macro-PS was formed by electrochemical anodisation ofmonocrystalline p-type silicon wafer in a double-tank cell. The effect of etching timeon the structure, porosity, electrical characteristics and gas sensing properties ofmacro-PS were investigated. It is shown the depth and the porosity of the macro-PSget larger with that the increase of etching time. The electrical behavior exhibits thatthere is ohmic contact of between the macro-PS and Pt contact. The macro-PS withthe etching time of5min shows best gas sensing properties. The sensitivity of themacro-PS with the etching time of5min to50ppm NH_3is4.2. It has goodresponse-recovery characteristic. The response/recover time is51s/242s.
WO_3thin films were deposited on macro-PSsubstrate by the facing targets directcurrent reactive magnetron sputtering method. The morphology, crystallization,valence of the W and gas sensing properties of the WO_3/macro-PS were characterized,respectively. It can be concluded by the SEM that the WO_3nano-particles form asemi-continuous thin film on the surface of macro-PS layer. The sensitivity of theWO_3/macro-PS gas sensor upon exposure to1,10,25and50ppm NO_2are1.40,5.01,9.01and14.4, respectively. The WO_3/macro-PS gas sensor has higher sensitivity thanthat of the Macro-PS gas sensor in each NO_2gas concentration.
Meso-PS was formed by electrochemical anodisation of monocrystalline p+-typesilicon wafer in a double-tank cell. The effect of etching current density on thestructure, porosity, electrical characteristics and gas sensing properties of meso-PSwere investigated. It can be concluded that the depth, porosity and resistance value ofthe meso-PS get larger with the increase of etching time. The meso-PS with theetching current density of80mA/cm~2shows best gas sensing properties. It was shownthat meso-PS had much higher sensitivity and good selectivity to NO_2, whilemacro-PS showed a good response–recovery characteristic and good selectivity to NH_3. The stability of gas sensing properties of the meso-PS by different storagemethod was also studied. It can be concluded that the meso-PS stored in the vacuumhas better stability.
Then, WO_3thin films were deposited on meso-PS layers using dc reactivemagnetron sputtering method. The effects of sputtering time, working pressure andAr/O2ratio on the microstructure and gas sensing properties of WO_3/meso-PS weresystemically analyzed by orthogonal trial experiment method. The optimal depositionparameters for WO_3thin films based on meso-PSsubstrate were obtained. It can beconcluded that the gas sensing properties of WO_3/meso-PS to NO_2and NH_3werebetter than of those of PS. The sensitivity of the WO_3/meso-PS to1ppm NO_2was4.22and that to50ppm NH_3was18.3. The response time of WO_3/meso-PS was shorterthan that of meso-PS.
采用双槽电化学腐蚀法腐蚀P型单晶硅形成有序大孔硅。研究了不同的腐蚀时间对于大孔硅结构、孔隙率、电学和气敏特性的影响。研究发现：随着腐蚀时间的增加，大孔硅的腐蚀深度增加，孔隙率变大。大孔硅与电极之间形成了欧姆接触。腐蚀时间为5min的大孔硅气敏特性最好。其在室温下对50ppm的NH_3的灵敏度为4.2，响应/恢复时间为51s/242s，恢复特性良好。
以大孔硅为基底，在其上溅射淀积氧化钨薄膜，制备出了大孔硅基氧化钨气敏传感器。研究了大孔硅基氧化钨薄膜的形貌，晶体结构，成分以及气敏特性。通过SEM观察发现，氧化钨薄膜淀积在大孔硅表面。气敏特性实验表明：气敏特性最好的大孔硅基氧化钨气敏传感器对1ppm、10ppm、25ppm和50ppm的NO_2的灵敏度分别为1.40、5.01、9.01和14.4，明显好于大孔硅对NO_2的气敏特性。
使用双槽电化学腐蚀法在P型重掺杂单晶硅表面制备介孔硅。分析了不同腐蚀电流密度对于介孔硅的结构，深度，孔隙率，电学特性和气敏特性的影响。结果表明：随着腐蚀电流密度的增加，其表面孔洞增多，深度增加，孔隙率变大，电阻升高。腐蚀电流密度为80mA/cm~2的介孔硅的室温气敏性能最好。与大孔硅相比，介孔硅具有较高的气体灵敏度。大孔硅对NH_3具有较好的选择性，而介孔硅对NO_2具有较好的选择性。随后采用不同放置方法对介孔硅的气敏稳定性进行了研究。实验发现：采用真空放置的介孔硅气敏稳定性较好。
采用对向靶直流反应磁控溅射法在介孔硅上制备介孔硅基氧化钨气敏传感器，通过实验分析了溅射时间、溅射压强和氩氧比等各因素对介孔硅基氧化钨薄膜微观结构和气敏特性的影响，获得了制备介孔硅基氧化钨薄膜的各个溅射工艺条件的最佳参数。通过不同温度下介孔硅和介孔硅基氧化钨气敏传感器对于NO_2和NH_3灵敏度对比发现：介孔硅基氧化钨气敏传感器具有比介孔硅更好的气敏特性。在室温下，其对1ppm的NO_2的灵敏度为4.22，对50ppm的NH_3的灵敏度为18.3。并且响应速度较快，很大程度上缩短了响应时间。
Porous silicon (PS) is a new type gas sensor which operated at room temperature.As it has large specific surface and can be easily produced, it has been widely used inthe fields of gas detecting and environmental protection. In this paper, macro-PS,WO_3/macro-PS, meso-PS and WO_3/meso-PS were prepared. The gas sensingproperties of macro-PS, WO_3/macro-PS, meso-PS and WO_3/meso-PS werethoroughly analyzed and studied.
Ordered macro-PS was formed by electrochemical anodisation ofmonocrystalline p-type silicon wafer in a double-tank cell. The effect of etching timeon the structure, porosity, electrical characteristics and gas sensing properties ofmacro-PS were investigated. It is shown the depth and the porosity of the macro-PSget larger with that the increase of etching time. The electrical behavior exhibits thatthere is ohmic contact of between the macro-PS and Pt contact. The macro-PS withthe etching time of5min shows best gas sensing properties. The sensitivity of themacro-PS with the etching time of5min to50ppm NH_3is4.2. It has goodresponse-recovery characteristic. The response/recover time is51s/242s.
WO_3thin films were deposited on macro-PSsubstrate by the facing targets directcurrent reactive magnetron sputtering method. The morphology, crystallization,valence of the W and gas sensing properties of the WO_3/macro-PS were characterized,respectively. It can be concluded by the SEM that the WO_3nano-particles form asemi-continuous thin film on the surface of macro-PS layer. The sensitivity of theWO_3/macro-PS gas sensor upon exposure to1,10,25and50ppm NO_2are1.40,5.01,9.01and14.4, respectively. The WO_3/macro-PS gas sensor has higher sensitivity thanthat of the Macro-PS gas sensor in each NO_2gas concentration.
Meso-PS was formed by electrochemical anodisation of monocrystalline p+-typesilicon wafer in a double-tank cell. The effect of etching current density on thestructure, porosity, electrical characteristics and gas sensing properties of meso-PSwere investigated. It can be concluded that the depth, porosity and resistance value ofthe meso-PS get larger with the increase of etching time. The meso-PS with theetching current density of80mA/cm~2shows best gas sensing properties. It was shownthat meso-PS had much higher sensitivity and good selectivity to NO_2, whilemacro-PS showed a good response–recovery characteristic and good selectivity to NH_3. The stability of gas sensing properties of the meso-PS by different storagemethod was also studied. It can be concluded that the meso-PS stored in the vacuumhas better stability.
Then, WO_3thin films were deposited on meso-PS layers using dc reactivemagnetron sputtering method. The effects of sputtering time, working pressure andAr/O2ratio on the microstructure and gas sensing properties of WO_3/meso-PS weresystemically analyzed by orthogonal trial experiment method. The optimal depositionparameters for WO_3thin films based on meso-PSsubstrate were obtained. It can beconcluded that the gas sensing properties of WO_3/meso-PS to NO_2and NH_3werebetter than of those of PS. The sensitivity of the WO_3/meso-PS to1ppm NO_2was4.22and that to50ppm NH_3was18.3. The response time of WO_3/meso-PS was shorterthan that of meso-PS.
引文
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