JPH053539B2 - - Google Patents
Info
- Publication number
- JPH053539B2 JPH053539B2 JP59069335A JP6933584A JPH053539B2 JP H053539 B2 JPH053539 B2 JP H053539B2 JP 59069335 A JP59069335 A JP 59069335A JP 6933584 A JP6933584 A JP 6933584A JP H053539 B2 JPH053539 B2 JP H053539B2
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen gas
- electrode
- film
- sensor
- palladium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 29
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 19
- 239000010408 film Substances 0.000 claims description 18
- 229910052763 palladium Inorganic materials 0.000 claims description 11
- 238000012856 packing Methods 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 3
- 238000007738 vacuum evaporation Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 7
- 230000035945 sensitivity Effects 0.000 description 7
- 239000012528 membrane Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000005574 cross-species transmission Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- -1 isobutane or propane Chemical compound 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、水素ガスの気体中に含有される量を
電気的信号として検出する水素ガスセンサーに関
する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a hydrogen gas sensor that detects the amount of hydrogen gas contained in the gas as an electrical signal.
従来例の構成とその問題点
最近、エネルギー需要の増大、環境汚染による
クリーンエネルギーの要望から、水素ガスをエネ
ルギー源に使用しようとする要求が高まつてい
る。一方、水素ガスは、引火点が低く危険性の高
いガスであることから、水素ガスのガス濡れを検
出するガスセンサーの要求も高まりつつある。Conventional configurations and their problems Recently, due to the increase in energy demand and the desire for clean energy due to environmental pollution, there has been an increasing demand for using hydrogen gas as an energy source. On the other hand, since hydrogen gas is a highly dangerous gas with a low flash point, there is an increasing demand for gas sensors that detect gas wetness of hydrogen gas.
従来、一般に使用されている水素ガスセンサー
は、加熱白金線において水素ガスを燃焼させるこ
とによる白金線の電気抵抗値変化を利用したもの
である。このようなセンサーにおいては、次の欠
点を有していた。すなわち、水素ガス以外のイソ
ブタン、プロパン等の可燃性のガスが共存する場
合にも、水素ガスと同様に感知してしまい誤動作
する。そのため水素ガスだけを感知できる信頼性
の高いセンサーが望まれていた。 Conventionally, commonly used hydrogen gas sensors utilize changes in the electrical resistance of a platinum wire caused by burning hydrogen gas in a heated platinum wire. Such a sensor had the following drawbacks. That is, even if a flammable gas other than hydrogen gas, such as isobutane or propane, coexists, it will be detected in the same way as hydrogen gas, resulting in malfunction. Therefore, there was a need for a highly reliable sensor that could only detect hydrogen gas.
従来より、酸化タングステン(WO3)が白金
等の触媒により水素と反応することが知られてい
る。その反応機構は、酸化タングステンと白金も
しくはパラジウム等の接触界面において、水素ガ
スが酸化タングステン中にInter calation
(Spill over現象とも言う)することであり、そ
の結果、生成したタングステンブロンズの電気抵
抗が、極端に低くなる。 It has been known that tungsten oxide (WO 3 ) reacts with hydrogen using a catalyst such as platinum. The reaction mechanism is that at the contact interface between tungsten oxide and platinum or palladium, hydrogen gas is intercalated into tungsten oxide.
(also called spill over phenomenon), and as a result, the electrical resistance of the produced tungsten bronze becomes extremely low.
このような現象を利用したものとして、例えば
特開昭57−74648号公報には、スパツタ蒸着によ
るWO3膜を利用したガスセンサーが記載されて
いる。しかし、このWO3膜は多結晶体であり、
水素ガスに対して感度の低いものであつた。 As a device that takes advantage of such a phenomenon, for example, Japanese Patent Application Laid-Open No. 57-74648 describes a gas sensor that uses a WO 3 film formed by sputter deposition. However, this WO 3 film is polycrystalline,
It had low sensitivity to hydrogen gas.
発明の目的
本発明は、このWO3膜を利用する水素ガスセ
ンサーを改良して、より感度を高くすることを目
的とする。Purpose of the Invention The purpose of the present invention is to improve the hydrogen gas sensor using this WO 3 membrane and to make it more sensitive.
発明の構成
本発明は、真空蒸着法によつて充填密度の低い
アモルフアスWO3膜が水素ガスに対して高感度
であることを見出したことに基づくもので、第1
の電極上にアモルフアスWO3膜を形成し、その
上に第2電極として白金またはパラジウムの薄膜
を設けたものである。Structure of the Invention The present invention is based on the discovery that an amorphous WO 3 film with a low packing density is highly sensitive to hydrogen gas by a vacuum evaporation method.
An amorphous WO 3 film is formed on the electrode, and a thin film of platinum or palladium is provided thereon as a second electrode.
本発明では、前記のように、触媒金属の白金ま
たはパラジウムが第2の電極を兼用しているの
で、素子構造を単純化することができる。 In the present invention, as described above, the catalytic metal platinum or palladium also serves as the second electrode, so the device structure can be simplified.
なお、WO3の充填密度は4.0〜6.0g/cm3、その
膜厚は100〜10000Åが好ましい。 Note that the packing density of WO 3 is preferably 4.0 to 6.0 g/cm 3 and the film thickness is preferably 100 to 10,000 Å.
実施例の説明
実施例 1
セラミツク・ガラス等の絶縁性基板上に、Pt、
Pd、Ni、Ti、Ta、Au、Ag、Al等の金属もしく
はIn2O3、SnO2等の半導体からなる第1の電極を
設け、その上に真空蒸着法の1つである抵抗加熱
法によつてアモルフアスWO3膜を形成し、さら
にその上にパラジウムを蒸着によつて積層し、第
2の電極を設けた。Description of Examples Example 1 Pt,
A first electrode made of a metal such as Pd, Ni, Ti, Ta, Au, Ag, Al, or a semiconductor such as In 2 O 3 or SnO 2 is provided, and then a resistance heating method, which is one of the vacuum evaporation methods, is applied. An amorphous WO 3 film was formed by this method, and palladium was further laminated thereon by vapor deposition to provide a second electrode.
第1図は上記のようにして構成した水素ガスセ
ンサーを示すもので、1は基板、2は第1の電
極、3はWO3膜、4は第2の電極である。WO3
の充填密度は5.4g/cm3、その膜厚は3000Åであ
り、第2の電極の膜厚は500Åであり、第1の電
極との対向面積は0.3cm2である。 FIG. 1 shows a hydrogen gas sensor constructed as described above, in which 1 is a substrate, 2 is a first electrode, 3 is a WO 3 film, and 4 is a second electrode. WO 3
The packing density of the electrode is 5.4 g/cm 3 , the thickness of the second electrode is 3000 Å, the thickness of the second electrode is 500 Å, and the area facing the first electrode is 0.3 cm 2 .
なお、5および6はそれぞれ第1および第2の
電極のリード、7は電気抵抗の検出器である。 Note that 5 and 6 are leads for the first and second electrodes, respectively, and 7 is an electrical resistance detector.
上記のセンサー部に一定濃度の水素ガスを吹き
つけると、第1電極と第2電極間の抵抗が大きく
変化する。水素ガス濃度と電極間の抵抗値の関係
を第2図に示す。同図よりH2濃度1000ppmに対
する100ppmの電気抵抗値の比は7.2倍である。こ
れに対してスパツタリング法で形成し、熱処理し
た結晶状態のセンサーの比は1.5倍で感度が低か
つた。 When a certain concentration of hydrogen gas is blown onto the sensor section, the resistance between the first electrode and the second electrode changes significantly. FIG. 2 shows the relationship between the hydrogen gas concentration and the resistance value between the electrodes. From the same figure, the ratio of the electrical resistance value at 100 ppm to the H 2 concentration of 1000 ppm is 7.2 times. On the other hand, the sensitivity of the crystalline sensor formed by sputtering and heat-treated was 1.5 times lower.
なお、電気抵抗値の測定は、±50mV、60Hzで
行なつた。測定値は水素ガス吹きつけ後3秒後の
値である。この後、センサー部に空気を吹きつけ
ると、5〜10秒以内に元の状態に回復した。 Note that the electrical resistance value was measured at ±50 mV and 60 Hz. The measured value is the value 3 seconds after spraying hydrogen gas. After this, when air was blown onto the sensor part, it returned to its original state within 5 to 10 seconds.
実施例 2
実施例1においてアモルフアスWO3膜の蒸着
時の真空度をかえて異なつた充填密度の膜を3000
Åの厚みに蒸着し、実施例1と同様のセンサーを
構成して試験した。Example 2 In Example 1, the degree of vacuum during vapor deposition of the amorphous WO 3 film was changed to produce films with different packing densities.
A sensor similar to that of Example 1 was constructed and tested.
その結果、充填密度が低くなる膜ほど水素ガス
に対する感度が高くなつた。しかし、充填密度が
低くなるとWO3膜自身が脆くなり、安定性に欠
けることが判かつた。安定で、かつ高感度の
WO3膜としては、充填密度4.0〜6.0g/cm3の範囲
のものが好ましかつた。 As a result, the lower the packing density of the membrane, the higher the sensitivity to hydrogen gas. However, it was found that when the packing density became low, the WO 3 film itself became brittle and lacked stability. Stable and sensitive
The WO 3 membrane preferably had a packing density in the range of 4.0 to 6.0 g/cm 3 .
さらに、WO3膜の充填密度を5.4g/cm3と一定に
して蒸着膜厚を変化させて検討した結果、薄い状
態の膜ほど高い感度を示した。好ましい膜厚は
100〜10000Åの範囲であつた。 Furthermore, as a result of an investigation while keeping the packing density of the WO 3 film constant at 5.4 g/cm 3 and varying the thickness of the deposited film, it was found that the thinner the film, the higher the sensitivity. The preferred film thickness is
It was in the range of 100 to 10,000 Å.
実施例 3
実施例1において、第2電極のパラジウムにか
えて、白金を用いたセンサーを作成し、水素ガス
に対する感度を測定した結果、実施例1とほぼ同
程度の感度が得られた。Example 3 In Example 1, a sensor was fabricated using platinum instead of palladium for the second electrode, and the sensitivity to hydrogen gas was measured. As a result, almost the same sensitivity as in Example 1 was obtained.
実施例 4
実施例1において、第2電極のパラジウムの蒸
着膜厚の異なるセンサーを作成した。パラジウム
膜厚が薄い程WO3への水素ガスのインターカレ
ーシヨン反応は速くなるが、電極自身の電気抵抗
が高くなる。パラジウム膜厚は100〜1000Åが好
ましいものであつた。白金についても同様であつ
た。Example 4 In Example 1, sensors were created in which the thickness of the palladium vapor deposition film of the second electrode was different. The thinner the palladium film is, the faster the intercalation reaction of hydrogen gas into WO 3 becomes, but the electrical resistance of the electrode itself becomes higher. The palladium film thickness was preferably 100 to 1000 Å. The same was true for platinum.
なお、実施例においては真空蒸着法として抵抗
加熱法について説明したが、これに代えてEB(電
子線)加熱法を用いても同様の効果が得られた。 In addition, in the examples, a resistance heating method was explained as a vacuum evaporation method, but the same effect was obtained even if an EB (electron beam) heating method was used instead.
発明の効果
以上のように、本発明によれば、構造が簡単で
高感度の安定した水素ガスセンサーが得られる。
また、このセンサーは、他の可燃性ガスに応答す
ることがないので、信頼性の高いものである。Effects of the Invention As described above, according to the present invention, a hydrogen gas sensor having a simple structure, high sensitivity, and stability can be obtained.
Additionally, this sensor is highly reliable as it does not respond to other combustible gases.
第1図は本発明の水素ガスセンサーの実施例を
示す要部を断面にした図、第2図は水素ガス濃度
とセンサーの電気抵抗値の関係を示す図である。
1……基板、2……第1の電極、3……WO3
膜、4……第2の電極。
FIG. 1 is a cross-sectional view of the main part of a hydrogen gas sensor according to an embodiment of the present invention, and FIG. 2 is a diagram showing the relationship between the hydrogen gas concentration and the electrical resistance value of the sensor. 1...Substrate, 2...First electrode, 3...WO 3
Membrane, 4... second electrode.
Claims (1)
アス酸化タングステン層を設け、さらにその上に
第2電極として白金またはパラジウムの薄膜層を
積層したことを特徴とする水素ガスセンサー。 2 アモルフアス酸化タングステン層が、充填密
度4.0〜6.0g/cm3で、かつ膜厚100〜10000Åであ
る特許請求の範囲第1項記載の水素ガスセンサ
ー。 3 白金またはパラジウムの薄膜層の膜厚が100
〜1000Åである特許請求の範囲第1項記載の水素
ガスセンサー。[Claims] 1. A hydrogen gas characterized in that an amorphous tungsten oxide layer is provided on a first electrode by vacuum evaporation, and a thin film layer of platinum or palladium is further laminated thereon as a second electrode. sensor. 2. The hydrogen gas sensor according to claim 1, wherein the amorphous tungsten oxide layer has a packing density of 4.0 to 6.0 g/cm 3 and a film thickness of 100 to 10,000 Å. 3 The thickness of the platinum or palladium thin film layer is 100
10. The hydrogen gas sensor according to claim 1, wherein the hydrogen gas sensor is 1000 Å.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6933584A JPS60211347A (en) | 1984-04-06 | 1984-04-06 | Gaseous hydrogen sensor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6933584A JPS60211347A (en) | 1984-04-06 | 1984-04-06 | Gaseous hydrogen sensor |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS60211347A JPS60211347A (en) | 1985-10-23 |
JPH053539B2 true JPH053539B2 (en) | 1993-01-18 |
Family
ID=13399574
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP6933584A Granted JPS60211347A (en) | 1984-04-06 | 1984-04-06 | Gaseous hydrogen sensor |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS60211347A (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4440572C2 (en) * | 1994-11-14 | 1997-05-07 | Fraunhofer Ges Forschung | Glazing element with variable transmission |
JP2007071866A (en) * | 2005-08-10 | 2007-03-22 | Tokyo Univ Of Science | Film for gas sensor, element for gas sensor and method for manufacturing the element for gas sensor |
JP5422281B2 (en) * | 2009-07-13 | 2014-02-19 | 株式会社アルバック | Hydrogen gas sensor and method for manufacturing hydrogen gas sensor |
US9134270B2 (en) * | 2010-03-25 | 2015-09-15 | Stichting Imec Nederland | Amorphous thin film for sensing |
JP6738749B2 (en) | 2016-03-25 | 2020-08-12 | パナソニックセミコンダクターソリューションズ株式会社 | Gas sensor, hydrogen detection method, and fuel cell vehicle |
WO2018123673A1 (en) * | 2016-12-28 | 2018-07-05 | パナソニックIpマネジメント株式会社 | Gas detection device, gas detection system, fuel cell vehicle, and gas detection method |
JP6865234B2 (en) * | 2016-12-28 | 2021-04-28 | ヌヴォトンテクノロジージャパン株式会社 | Gas detectors, gas sensor systems, fuel cell vehicles, and hydrogen detection methods |
JP7195766B2 (en) * | 2018-05-14 | 2022-12-26 | キヤノン株式会社 | Reducing gas detection material and reducing gas detection sensor |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53141098A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS53141096A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS53141097A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS55124058A (en) * | 1979-03-09 | 1980-09-24 | Gen Motors Corp | Titanium dioxide exhaust sensor |
JPS5690250A (en) * | 1979-12-22 | 1981-07-22 | Matsushita Electric Works Ltd | Detection element of combustible gas |
JPS5774648A (en) * | 1980-08-28 | 1982-05-10 | Siemens Ag | Selective thin film gas sensor and manufacture thereof |
JPS5857702A (en) * | 1981-09-30 | 1983-04-06 | 三洋電機株式会社 | Moisture sensor |
JPS58182545A (en) * | 1982-04-21 | 1983-10-25 | Hitachi Ltd | Detecting element of gaseous carbon monoxide |
-
1984
- 1984-04-06 JP JP6933584A patent/JPS60211347A/en active Granted
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53141098A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS53141096A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS53141097A (en) * | 1977-05-16 | 1978-12-08 | Toshiba Corp | Gas sensing element |
JPS55124058A (en) * | 1979-03-09 | 1980-09-24 | Gen Motors Corp | Titanium dioxide exhaust sensor |
JPS5690250A (en) * | 1979-12-22 | 1981-07-22 | Matsushita Electric Works Ltd | Detection element of combustible gas |
JPS5774648A (en) * | 1980-08-28 | 1982-05-10 | Siemens Ag | Selective thin film gas sensor and manufacture thereof |
JPS5857702A (en) * | 1981-09-30 | 1983-04-06 | 三洋電機株式会社 | Moisture sensor |
JPS58182545A (en) * | 1982-04-21 | 1983-10-25 | Hitachi Ltd | Detecting element of gaseous carbon monoxide |
Also Published As
Publication number | Publication date |
---|---|
JPS60211347A (en) | 1985-10-23 |
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