多孔硅基氧化钨气敏传感器的研究
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摘要
随着工业和日常生活向空气中排放的污染气体越来越多,新型高性能低功耗的气敏传感器越来越受到人们的关注。本文主要针对多孔硅基氧化钨气敏薄膜以及传感器的电学特性和气敏特性进行了研究。
首先,通过双槽电化学腐蚀法制备介孔硅基底。选取40,60和80mA/cm~2三种腐蚀电流密度,得到不同孔隙结构参数的介孔硅样品,对样品进行了孔隙率、SEM、I-V特性等各种测试,分析了介孔硅的材料参数、微观形貌和电学特性等。用静态配气法对一定浓度的NH_3、C_2H_5OH和NO_2进行了气敏特性测试。结果显示:腐蚀电流密度为80mA/cm~2的介孔硅样品具有较好的气敏特性。
随后,在制备的介孔硅基底上溅射氧化钨薄膜以及Pt电极,形成介孔硅基氧化钨薄膜气敏传感器。通过对氧化钨薄膜溅射时间的选取,得到不同膜厚的样品,对样品进行了SEM、阻温特性等各种测试,分析了介孔硅基氧化钨薄膜的材料参数、微观形貌和电学特性等。用静态配气法对一定浓度的NH_3和NO_2进行了气敏特性测试。研究表明:溅射氧化钨薄膜的时间为5分钟的样品具有较好的气敏特性。虽然器件在常温下具有较高的灵敏度,但器件的响应较慢,迫切需求制备一种大孔硅基底,以制备更高性能的大孔硅基氧化钨薄膜气敏传感器。
最后,实验提出了大孔硅的制备方法,并对大孔硅的表面形貌,腐蚀深度,孔隙率和气敏特性进行了测试,并且测试了大孔硅基氧化钨气敏薄传感器的气敏特性,为下一步制备更高性能的多孔硅基氧化钨气敏传感器奠定了基础。
With more and more contaminated gas emissions from industry and daily life, novel high-performance and low-power gas sensors has attracted increasing attention. This paper mainly studies silicon electrical properties and gas sensitivity of the porous tungsten oxide gas sensors.
First of all, by the method of double-tank cell electrochemical corrosion meso-porous silicon substrate is fabricated, on whose surface tungsten oxide and metal electrodes thin film is deposited through the magnetron sputtering. With 80, 40 and 60 mA/cm~2 corrosion current density respectively, different parameters of pore structure of mesoporous silicon samples are attained. In addition, we tested the porosity of samples, SEM, IV and other characteristics and analyst material parameters. In a certain concentration of NH_3, C_2H_5OH and NO_2 made by static state analytical method,gas sensitive characteristics of the samples are tested. It is showed that: the sample prepared with 80mA/cm~2 corrosion current density has the best gas-sensing properties.
Subsequently, tungsten trioxide thin film is deposited on the samples through magnetron sputtering as the sensitive material of gas sensor. Depending on the different sputtering time, tungsten trioxide thin films were formed with different thickness. The properties of thin film were tested and analyst, including SEM, resistance-temperature characteristics, the material parameters, microstructure and electrical properties of tungsten trioxide thin-film based on mesoporous silicon substate. Similarly, in a certain concentration of NH_3, C_2H_5OH and NO_2 made by static state analytical method,gas sensitive characteristics of the samples are tested. The result shows that: tungsten trioxide thin film for 5 minutes sputtering time has the best gas-sensitive properties. Although the device at room temperature has high sensitivity, the responding time is long. there is an urgent demand for the preparation of a macroporous silicon substrate in order to prepare more high-performance macroporous silicon-based tungsten oxide thin film gas sensors.
Finally, the experiments put forward the fabrication method of macroporous silicon and test the samples for surface morphology, corrosion depth, porosity and gas sensitivity. At the same time, we carried out test for the gas sensitivity of WO3 thin film gas sensor based on macroporous silicon. These lay foundation for the next high-performance WO_3 thin film gas sensor based on macroporous silicon.
首先,通过双槽电化学腐蚀法制备介孔硅基底。选取40,60和80mA/cm~2三种腐蚀电流密度,得到不同孔隙结构参数的介孔硅样品,对样品进行了孔隙率、SEM、I-V特性等各种测试,分析了介孔硅的材料参数、微观形貌和电学特性等。用静态配气法对一定浓度的NH_3、C_2H_5OH和NO_2进行了气敏特性测试。结果显示:腐蚀电流密度为80mA/cm~2的介孔硅样品具有较好的气敏特性。
随后,在制备的介孔硅基底上溅射氧化钨薄膜以及Pt电极,形成介孔硅基氧化钨薄膜气敏传感器。通过对氧化钨薄膜溅射时间的选取,得到不同膜厚的样品,对样品进行了SEM、阻温特性等各种测试,分析了介孔硅基氧化钨薄膜的材料参数、微观形貌和电学特性等。用静态配气法对一定浓度的NH_3和NO_2进行了气敏特性测试。研究表明:溅射氧化钨薄膜的时间为5分钟的样品具有较好的气敏特性。虽然器件在常温下具有较高的灵敏度,但器件的响应较慢,迫切需求制备一种大孔硅基底,以制备更高性能的大孔硅基氧化钨薄膜气敏传感器。
最后,实验提出了大孔硅的制备方法,并对大孔硅的表面形貌,腐蚀深度,孔隙率和气敏特性进行了测试,并且测试了大孔硅基氧化钨气敏薄传感器的气敏特性,为下一步制备更高性能的多孔硅基氧化钨气敏传感器奠定了基础。
With more and more contaminated gas emissions from industry and daily life, novel high-performance and low-power gas sensors has attracted increasing attention. This paper mainly studies silicon electrical properties and gas sensitivity of the porous tungsten oxide gas sensors.
First of all, by the method of double-tank cell electrochemical corrosion meso-porous silicon substrate is fabricated, on whose surface tungsten oxide and metal electrodes thin film is deposited through the magnetron sputtering. With 80, 40 and 60 mA/cm~2 corrosion current density respectively, different parameters of pore structure of mesoporous silicon samples are attained. In addition, we tested the porosity of samples, SEM, IV and other characteristics and analyst material parameters. In a certain concentration of NH_3, C_2H_5OH and NO_2 made by static state analytical method,gas sensitive characteristics of the samples are tested. It is showed that: the sample prepared with 80mA/cm~2 corrosion current density has the best gas-sensing properties.
Subsequently, tungsten trioxide thin film is deposited on the samples through magnetron sputtering as the sensitive material of gas sensor. Depending on the different sputtering time, tungsten trioxide thin films were formed with different thickness. The properties of thin film were tested and analyst, including SEM, resistance-temperature characteristics, the material parameters, microstructure and electrical properties of tungsten trioxide thin-film based on mesoporous silicon substate. Similarly, in a certain concentration of NH_3, C_2H_5OH and NO_2 made by static state analytical method,gas sensitive characteristics of the samples are tested. The result shows that: tungsten trioxide thin film for 5 minutes sputtering time has the best gas-sensitive properties. Although the device at room temperature has high sensitivity, the responding time is long. there is an urgent demand for the preparation of a macroporous silicon substrate in order to prepare more high-performance macroporous silicon-based tungsten oxide thin film gas sensors.
Finally, the experiments put forward the fabrication method of macroporous silicon and test the samples for surface morphology, corrosion depth, porosity and gas sensitivity. At the same time, we carried out test for the gas sensitivity of WO3 thin film gas sensor based on macroporous silicon. These lay foundation for the next high-performance WO_3 thin film gas sensor based on macroporous silicon.
引文
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[46] G. Garcia Salgado, T. Diaz Becerril, H. Juarez Santiesteban, et al. Porous silicon organic vapor sensor．Optical Materials, 2006, 29, 51–55．
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[2]彭军，传感器与检测技术，西安：西安电子科技大学出版社，2003
[3]李平,余萍,肖定全.气敏传感器的近期进展.功能材料,1999,30（2）:126-128．
[4]P.M.Woodward. A.W.Sleight.FerroelectrictungstenTrioxide. SolidStateChem, 1997, 131(1): 9—17.
[5] M.Bedahan, R.Boulmani, Characterization of ozone sensors based on WO3 reactively sputtered films: influence of O2 concentration in the sputtering gas, and working temperature Sensors and Actuators, 2004, B100: 323-327
[6] X.L.He, J.P.Li et.al, NO2 sensing characteristics of WO3 thin film microgas sensor, Sensors and Actuators, 2003, B93: 463-467
[7] J.Tamaki et al, Detection of dilute nitrogen dioxide and thickness effect of tungsten oxide thin film sensors Sensors and Actuators, 2003, B95: 111-115
[8] T.S.Kim, Y.B. Kim,et.al, Sensing characteristics of dc reactive sputtered WO3 thin films as an NOx gas sensor Sensors and Actuators, 2000, B62: 102-108
[9] K.S.Yoo, Y.J. Oh, et.al, Korean Phys.Soc. 1999, 35: 420
[10] A.H.Jayatissa et al, Annealing effect on the formation of nanocrystals in thermally evaporated tungsten oxide thin films, Materials Science and Engineering, 2004, B109: 269-275
[11]金宝富,戚金清，等.云南大学学报(自然科学版) 1997, 19(2): 117-120
[12] M.Penza, C. Martucci,G. Cassano, NOx gas sensing characteristics of WO3 thin films activated by noble metals (Pd, Pt, Au) layers Sensors and Actuators, 1998 B56: 52-59
[13] Uhlir A, Electrolytic shaping of germanium and silicon, The Bell System Technical Journal, 1956, 35:333～347
[14] Steiner P, Lang W, Micromachining applications of porous silicon, Thin Solid Films, 1995, 255(1-2):52～58
[15] Smith R L, Collins S D, Porous silicon formation mechanisms, Journal of Applied Physics, 1992, 71(8):R1～R22
[16]Smith R L, Collins S D, Porous silicon formation mechanisms, Journal ofApplied Physics, 1992, 71(8):R1～R22
[17]Lehmann V, Gosele U, Porous silicon formation: A quantum wire effect, Applied Physics Letters, 1991, 58(8):856～858
[18]Dücso C S, Vázsonyié, Adám M, et al. Porous silicon bulk micromachining for thermally isolated membrane formation, Sensors and Actuators A, 1997, 60(1-3):235～239
[19]Kronast W, MülleR B, Siedel W, et al. Single-chip condenser microphone using porous silicon as sacrificial layer for the air gap. Sensors and Actuators A, 2001, 87(3):188～193.
[20]Chang C C, Chen L C, A new process for the fabrication of silicon-on-insulator structures by using porous silicon, Materials Letters, 1997, 32(4):287～290
[21]Rocchia M A, Garrone E, Geobaldo F, et al. Sensing CO2 in a chemically modified porous silicon film, Physica Status Solidi A, 2003, 197(2):365～369
[22]Massera E, Nasti I, Quercia L, et al. Improvement of stability and recovery time in porous-silicon-based NO2 sensor, Sensors and Actuators B, 2004, 102(2):195～197
[23]Irajizad A, Rahimi F, Chavoshi M, et al. Characterization of porous poly-silicon as a gas sensor, Sensors and Actuators B, 2004, 100(3):341～346
[24]Grigoris K, Athanase A, Nassiopoulos, Characterization of a silicon thermal gas-flow sensor with porous silicon thermal isolation, IEEE Sensor Journal, 2002, 2(5):463～475
[25]Tsamis C, Tserepi A, Nassiopoulou A G, Fabrication of suspended porous silicon micro-hotplates for thermal sensor applications, Physica Status Solidi A, 2003, 197(2):539～543
[26] Roussel Ph, Lysenko V, Remaki B, et al. Thick oxidized porous silicon layers for the design of a biomedical thermal conductivity microsensor, Sensors and Actuators A, 1999, 74:101～103
[27] O. Meskini, A. Abdelghani, et al. Porous silicon as functionalized material for immunosensor application, Talanta,2007, 71(3): 1430~1433
[28]周甫方,黄远明.多孔硅薄膜微结构的分形特征[J].微纳电子技术,2007,4：182—185．
[29] Kim S J, Lee S H, Lee C J, et a1．Organic vapour sensing by currentresponse of porous silicon layer, Journal of Physics D:Applied Physics,2001,34(24)：3505—3509．
[30] Baratto C, Faglia G, Sberveglieri G, Multiparametric porous silicon sensors, Sensors, 2002, 2(3):121～126
[31] N. Gabouze, N. Benzekkour, Be Mahmoudi et al. Study and applications of plasma-modified Si and porous Si surfaces, Applied Surface Science，2008，254（12）：3648-3652
[32] Arakelyana V M, Galstyana V E, Martirosyana K S, et al. Hydrogen sensitive gas sensor based on porous silicon/TiO2-x structure, Physica E, 2007, 38:219～221
[33] Pancheri L, Oton C J, Gaburro Z, et a1. Very sensitive porous silicon NO2 sensor, Sensors and Actuators B, 2003, 89(3):237～239
[34]Witten T A, Sander L M, Difusion-limited aggregation, Physical Review B, 1983, 27(9):5686～5697
[35]Lim P, Brock J R, Traehtenberg I, Laser-induced etching of silicon in hydrofluoric acid, Applied Physics Letters, 1992, 60(4):486～488
[36]Laiho R, Pavlov A, Preparation of porous silicon films by laser ablation, Thin solid films, 1995, 255:9～11
[37]陈乾旺,李新建,朱警生,多孔硅研究的新进展,电子显微学报, 1997, 16(4):493～496
[38]Saadoun M, Ezzaouia H, Bessais B, et al. Formation of porous silicon for large-area silicon solar cells: a new method, Solar Energy Materials and Solar Cells, 1999, 59(4):377～385
[39]Saadoun M, Mliki N, Kaabi H, Vapour-etching-based porous silicon: a new approach, Thin solid films, 2002, 405(1-2):29～34
[40]胡明,田斌,王兴,化学刻蚀法制备多孔硅的表面形貌研究,功能材料, 2004, 35(2):223～224
[41]汪开源,刘柯林,唐洁影,多孔硅的光致发光谱,电子器件, 1994, 17(2):47～53
[42]王清涛，李清山，多孔硅及其应用研究展望，辽宁大学学报：自然科学版，2001，28（4）：301-304,317
[43] Beale M I J, An experimental and theoretical study of the formation and microstructure of porous silicon, Crys Growth.1985,73(6):622~632
[44]林军,张丽珠,陈志坚等.多孔硅蓝光发射与发光机制,物理学报, 1996, 45(1):121～125
[45]K. N. Ali，M. R .Hashim，A. Abdul Aziz. Effects of surface passivation in porous silicon as H2 gas sensor. Solid-State Electronics 2008, 52, 1071–1074.
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