CN1033717C - 常温co气体传感器的制造方法 - Google Patents

常温co气体传感器的制造方法 Download PDF

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CN1033717C
CN1033717C CN94101843.1A CN94101843A CN1033717C CN 1033717 C CN1033717 C CN 1033717C CN 94101843 A CN94101843 A CN 94101843A CN 1033717 C CN1033717 C CN 1033717C
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李文范
刘秀英
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Changchun Institute of Applied Chemistry of CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004—CO or CO2

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Abstract

本发明属于常温CO气体传感器的制造方法。本发明以SnO2为基准材料，加入Pt黑、La2O3、Y2O3、Cr、Al2O3经配料、研磨、烧结、老化等步骤，制备出在常温下对25～600PPmCO的定量和选择性检测的传感器。本发明由于加入高纯Cr，加速了对气体的吸附和脱附，使传感器的响应时间小于10秒，恢复时间小于15秒。

Description

本发明属于常温CO气体传感器的制造方法。
中科院长春应用化学研究所CN92110578.9公开一种“常温一氧化碳气敏元件的制备方法”，该技术是以SnOx为基质材料，以Al2O3、MgO、Pt、Pd、ThO2、为添加剂，其SnOx之X值在1.0～1.6之间，是非化学剂量比。该方法制造的CO传感器可以实现在室温下检测CO。传感器表面温度低、本质安全、功耗小、应用电路简单。
中科院长春应用化学研究所CN89102921.4公开了一种“常温氧化物半导体气体传感器”。该气体传感器主要检测煤气、液化石油气。其原料配比为： SnCl4/SnO2＝0.5～1.5倍(重量比)、稀土氧化物/SnO2＝0.5～1倍(重量比)，但其稀土氧化物只选择了LaO2和CeO2。
本发明的目的是选择以SnO2为基质材料，掺杂Y2O3、LaO3、Al2O3、Cr和Pt黑，制备CO气体传感器。
本发明选择的原料配方为：以SnO2为基准(按重量比)，Pt黑量为SnO2的0.0003～0.018倍，高纯LaO3量为SnO2的0.0002～0.05倍，高纯Y2O3量为SnO2的0.0003～0.02倍，高纯Cr量为SnO2的0.00015～0.04倍，高纯Al2O3量为SnO20.0003～0.05倍。
制备方法为：把上述原料放入玛脑乳钵中，加入去离子水2.5～5ml研磨，使其呈浆糊状。用φ0.03～0.05mmPt丝做成螺旋电极，螺旋长0.8～1.4mm，大直径为0.6～1mm，小直径为0.3～0.6mm，将料涂在电极上，把小电极放入大电极中，制成球状传感器。在780～900℃下在空气中烧结80～130分钟，冷却到室温取出，老化168小时以上。
本发明制备的传感器能定量和有选择性地检测CO。对500ppm甲烷、500ppm丙烷、400ppm丁烷、200ppm乙醇、400ppm乙酸乙酯等任何一种气体产生的信号均小于60ppmCO的信号，对检测100ppmCO无干扰。在25～600ppmCO之间与灵敏度ΔI成线性关系。
本发明气体传感器灵敏度为ΔI＝Imax-Imin。Imax为传感器在气体中的最大电流，Imin为最小电流。
本发明由于加入高纯Cr，加速了对气体的吸附和脱附，缩短了响应时间和恢复时间，响应时间小于10秒，恢复时间小于15秒，并增加了传感器的稳定性。选择Y2O3在高温下与SnO2等生成复合氧化物，在室温下使吸附在SnO2表面上的氧以O2 -状态存在，这种O2 -对CO敏感.因此传感器能在室温下，低功率下检测CO。
本发明提供的实施例如下：
实施例1：
称取SnO22g，Pt黑0.006g，La2O30.0004g，Y2O30.0006g，Cr0.0003g，Al2O30.0006g。放到玛脑乳钵中，加入去离子水研磨，呈浆糊状。用φ0。03mmPt丝做成螺施状电极，将料涂在电极上，制成球状传感器。在空气中，在780℃下烧结130分钟，冷却到室温取出，老化168小时。该传感器响应时间小于10秒，恢复时间小于15秒，在25～600ppmCO之间与ΔI成线性关系。
以下8个实施例的制造方法同实施例1。气敏性能也相同。9个实施例结果列在表1中。
实施例2：
SnO22g，Pt黑0.036g，La2O30.1g，Y2O30.04g，Cr0.08g，Al2O30.1g。900 ℃烧结80分钟。
实施例3：
SnO22g，Pt黑0.00065g，La2O30.0008g，Y2O30.0013g，Cr0.0009g，Al2O30.0095g。850℃烧结100分钟。
实施例4：
SnO22g，Pt黑0.0093g，La2O30.0019g，Y2O30.0035g，Cr0.0025g，Al2O30.012g。800℃烧结120分钟。
实施例5：
SnO22g，Pt黑0.0099g，La2O30.0033g，Y2O30.0056g，Cr0.0043g，Al2O30.034g。 820℃烧结110分钟。
实施例6：
SnO22g，Pt黑0.018g，La2O30.0057g，Y2O30.01g，Cr0.0085g，Al2O30.085g，Al2O30.0065g。810℃烧结120分钟。
实施例7：
SnO22g，Pt黑0.025g，La2O30.009g，Y2O30.037g，Cr0.029g，Al2O30.081g。850℃烧结100分钟。
实施例8：
SnO22g，Pt黑0.031g，La2O30.015g，Y2O30.036g，Cr0.013g，Al2O30.094g。 900℃烧结90分钟。
实施例9：
SnO22g，Pt黑    0.0072g，La2O30.083g，Y2O30.005g，Cr0.055g，Al2O30.068g。900℃烧结100分钟。
9个实施例结果列在表1中。表lCO浓度与ΔI的关系
    CO(ppm)ΔI(mA)实施例 25 50 100 200 300 400 500 600
    1     1.1     2.1     4.0     8.2     12.5     15.9     20.0     23.8
    2     1.0     2.0     3.9     8.0     11.5     15.3     19.2     24
    3     1.2     2.1     4.3     8.4     12.7     16.8     20.5     25.4
    4     1.4     2.3     4.5     8.9     13.5     17.6     22.1     26.6
    5     1.3     2.2     4.2     8.1     12.5     16.3     21.0     24.9
    6     0.9     2.0     4.0     7.8     11.9     15.8     19.7     23.9
    7     1.1     1.9     3.9     7.7     11.7     15.3     19.5     23.1
    8     1.5     2.7     5.2     10.1     15.6     20.5     25.8     30.0
    9     1.2     2.2     4.3     8.1     12.0     17.2     21.6     26.1

Claims (1)

1.一种常温CO气体传感器制造方法，用于制造以SnO2为基质材料并掺杂稀土氧化物成分的传感器，包括以下工艺步骤：
1)把原料按一定配比放入玛脑乳体中，加入去离子水研磨呈浆糊状；
2)将浆糊状料涂在电极上，把小电极放入大电极中，制成球状传感器；
3)晾干后在空气中780～900℃烧结80～130分钟，冷却，取出老化168小时；
其特征在于，构成传感器的原料配比是：以SnO2为基准量(重量比)
Pt黑量为SnO2的0.003～0.018倍，
La2O3量为SnO2的0.0002～0.05倍，
Y2O3量为SnO2的0.0003～0.02倍，
Cr量为SnO2的0.0015～0.04倍，
Al2O2量为SnO2的0.0003～0.05倍。
CN94101843.1A 1994-03-17 1994-03-17 常温co气体传感器的制造方法 Expired - Fee Related CN1033717C (zh)

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US08/358,217 US5589046A (en) 1994-03-17 1994-12-16 Room temperature carbon monoxide gas sensor and the process for preparing the same

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US6319473B1 (en) * 1998-06-16 2001-11-20 Figaro Engineering, Inc. Co sensor and its fabrication
AU2001269546A1 (en) * 2000-06-29 2002-01-08 Jae-Ho Pyee Novel transgenic tobacco restraining activity of harmful materials thereof
AU2001267926A1 (en) * 2000-06-30 2002-01-14 Nam-In Hyung Anticancer transgenic tomato
CN101329294B (zh) * 2007-06-22 2012-05-23 郑州炜盛电子科技有限公司 一种抗干扰性强的气体传感器
CN101329293B (zh) * 2007-06-22 2012-05-23 郑州炜盛电子科技有限公司 一种用于酒精蒸汽和呼气酒精检测的半导体气体传感器
US20090101501A1 (en) * 2007-10-17 2009-04-23 Tao Xiao-Ming Room temperature gas sensors
US8114675B2 (en) * 2009-03-30 2012-02-14 The Ohio State University Research Foundation Room temperature CO sensor and method of making same
CN104820068B (zh) * 2015-04-22 2016-06-29 上海纳米技术及应用国家工程研究中心有限公司 氧化锡氧化铝基低浓度丙酮气体传感器及其制备方法
CN108107084A (zh) * 2017-12-11 2018-06-01 梁金凤 一种基于三元纳米材料的气体检测单元

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GB1596623A (en) * 1976-12-13 1981-08-26 Nat Res Dev Catalytic gas detectors
JPS5439197A (en) * 1977-09-02 1979-03-26 Shibaura Denshi Seisakushiyo K Method of making gas detector
CN1023509C (zh) * 1989-04-28 1994-01-12 里希尔国际有限公司 阀组件
JP2708915B2 (ja) * 1989-11-25 1998-02-04 日本特殊陶業株式会社 ガス検出センサ
US5226309A (en) * 1992-06-18 1993-07-13 Illinois Institute Of Technology Halogenated compounds sensor
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