EP2396650A1 - Elément détecteur d'un détecteur de gaz, et procédé permettant de le faire fonctionner - Google Patents

Elément détecteur d'un détecteur de gaz, et procédé permettant de le faire fonctionner

Info

Publication number
EP2396650A1
EP2396650A1 EP09801687A EP09801687A EP2396650A1 EP 2396650 A1 EP2396650 A1 EP 2396650A1 EP 09801687 A EP09801687 A EP 09801687A EP 09801687 A EP09801687 A EP 09801687A EP 2396650 A1 EP2396650 A1 EP 2396650A1
Authority
EP
European Patent Office
Prior art keywords
sensor element
protective cap
gas
ceramic
element according
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.)
Withdrawn
Application number
EP09801687A
Other languages
German (de)
English (en)
Inventor
Oliver Wolst
Stefan Henneck
Markus Widenmeyer
Alexander Martin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Robert Bosch GmbH
Original Assignee
Robert Bosch GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Robert Bosch GmbH filed Critical Robert Bosch GmbH
Publication of EP2396650A1 publication Critical patent/EP2396650A1/fr
Withdrawn legal-status Critical Current

Links

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
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
    • 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
    • G01N33/0011—Sample conditioning
    • G01N33/0013—Sample conditioning by a chemical reaction
    • 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
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
    • G01N27/4141—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS specially adapted for gases

Definitions

  • the channel current without exposure to the substance to be detected which corresponds to a so-called zero signal or offset, often orders of magnitude of usually IG 3 higher than the channel current change by the application of a substance to be detected.
  • This places high demands on the current measurement due to the poor signal-to-offset ratio.
  • the offset from outer Interference can be influenced.
  • External disturbances result, for example, from temperature changes or sensor degradation, which are not based on the presence of substances to be detected.
  • Due to the given signal-to-offset ratio the change in the kana current due to disturbances of the same magnitude or, in the worst case, may even be greater than the change which occurs due to the presence of the substance to be detected. Since interference can not be completely ruled out, the associated error of the measurement signal is large and prevents in the worst case, a sufficiently accurate determination of the substance to be detected.
  • gas sensors which are constructed, for example, on the basis of a Halbieitergassensors and having a porous ceramic layer as gastperrneables protective element to prevent the ingress of harmful gases.
  • the sensor element of the gas sensor for example, a
  • Protective cap which prevents direct access of the gas mixture to be determined to the surface of the sensor element and having a heating means, a glass former and / or an oxidation catalyst.
  • the claimed sensor element is used to determine the exhaust gases of internal combustion engines, appreciable concentrations of silicon compounds are still to be found in such exhaust gases. These lead in extreme cases to a glazing of the electrodes of the sensor element, so that they do not show sufficient sensitivity to the gas components to be determined.
  • the protective cap of the sensor element has, for example, a glass former as a coating or as a material component, then the said interfering substances are permanently bound by physical effects or by corresponding chemical reactions in the region of the protective cap due to the getter characteristic of the glass bead. Further advantageous Aussili ⁇ ngsformen the present invention are the subject of the dependent claims.
  • the protective cap is made of a ceramic and is fixed by means of a Giaslots on the sensor element. This embodiment ensures a high temperature resistance of the sensor element according to the invention and thus opens up the possibility of investigating
  • Combustion gases in terms of its composition Combustion gases in terms of its composition.
  • a titanate, a silicate, a borate or a phosphate is used as the glass binder.
  • the advantage of using these substances is that they are available on an industrial scale and can easily be applied to the protective cap by means of a corresponding impregnation process.
  • Sensitive element for example, to run on nitrogen oxides, since existing in a gas mixture oxidizable gas components such as hydrocarbons, hydrogen or nitrogen monoxide and dinitrogen monoxide are oxidized to carbon dioxide, water or nitrogen dioxide. In this way, only nitrogen dioxide is to be detected as a gas component in a sensitive
  • the sensor element according to the invention or the method for operating the same is advantageously suitable for the determination of gas components in exhaust gases of internal combustion engines, power plants or heaters.
  • an application for monitoring the functionality of NOX storage catalytic converters or SCR exhaust aftertreatment systems is also to be seen.
  • FIG. 1 shows a schematic process sequence during the production of a sensor element according to the invention.
  • Figure 2 is a plan view of a sensor element during the
  • FIG. 3 shows a plan view of a completed sensor element
  • FIG. 4 is a schematic representation of a section of the material of a protective cap of the sensor element according to a first embodiment
  • FIG. 5 the schematic illustration of a section of the material of a protective cap of the sensor element according to a second embodiment
  • Figure ⁇ is a schematic representation of a section of the material of a protective cap of the sensor element according to a third embodiment
  • Figure 7 is a schematic sectional view of a sensor element according to the invention.
  • FIGS. 1 and 2 show a sensor element on which the invention is based during its production.
  • the sensor element 10 comprises a substrate 12 on which, for example, at least one, preferably a plurality of gas-sensitive detection units 28 are provided.
  • the gas-sensitive detection units are preferably designed on the basis of a semiconductor structure and can thus be designed, for example, as a field-effect transistor in the form of a MOSFET or CHEMFET or, for example, as semiconductor diodes.
  • the gas-sensitive detection units arranged on the substrate 12 are connected, for example, via contacts 14, as well as conductor track structures 16 with a corresponding signal evaluation structure, which is not shown in the figures.
  • the contacts 14 serve, for example, the electrical contacting of the source or drain electrodes of the individual
  • each of the gas-sensitive detection units arranged on the substrate 12 preferably captures another one Gas component of a gas mixture to be determined or another group of gas components present in a gas mixture.
  • the substrate 12 is preferably completely protected against direct access of the gas mixture to be determined, for example with a ceramic protective cap 18.
  • the ceramic protective cap 18 is designed, for example, in the form of a cuboid open on a large surface.
  • the support member 20 is provided, for example, with a Giaslot 22 and the ceramic cap 18 with the open side over the substrate 12 and pressed with the support member 20 so pressed that the glass solder 22, the protective cap 18 with the support member 20th gastight connects and fixes.
  • Heat treatment process creates a permanent connection between the protective cap 18 and the support member 20 of the sensor element 10th
  • the sensor element 10 finished in this way is shown for example in FIG.
  • the same reference numerals designate the same Bautesl- grain components, as in Figures 1 and 2.
  • Protective cap 18 for example, made of a porous, especially open-porous material. In this way, the access of entrained in a gas mixture particles or aerosols can be prevented; the access to gas components to the gas-sensitive detection units of the sensor element 10 is guaranteed.
  • the protective cap 18 is designed so that the substrate 12 is as completely as possible enclosed by the protective cap 18 and the additionally enclosed volume of air between the substrate 12 and the Protective cap 18 is gehaiten as low as possible.
  • the gas volume enclosed between the protective cap 18 and the substrate 12 is 0.0001 ⁇ l to 1 ml, preferably 0.0005 to 10 ⁇ l and in particular 0.001 to 0.003 ⁇ l. It is furthermore advantageous if the wall thickness of the ceramic protective cap 18 is carried out in this way is that to be determined
  • the wall thickness of the ceramic protective cap 18 is, for example, 2 ⁇ m to 5 mm, preferably between 10 and 200 ⁇ m and in particular between 20 and 80 ⁇ m.
  • the protective cap 18 is made, for example, of the same ceramic material as the carrier element 20 on which the substrate 12 is positioned. In this way, in Ternperatur pizzabe screw strictungen a largely comparable thermal expansion behavior of ceramic protective cap 18 and support member 20 can be observed. This also allows the use of a glass solder or other Kerarnikkleber for connecting the ceramic cap 18 with the support member 20. In principle, however, ceramic materials can be used with different composition, as long as they have a comparable thermal expansion behavior or comparable thermal expansion coefficient as the ceramic material of the carrier element 20. Thus, for example, zirconium dioxide, which can be used in an expensive or fully stabilized manner, is suitable as a ceramic material for the protective cap 18 or the carrier element 20. As an alternative ceramic materials of the cap 18 are also Low Temperature Cofired
  • the production of the protective cap 18 takes place, for example, by processing corresponding green sheets of the ceramic material by laminating a plurality of layers and then milling out the desired trough-shaped geometry to form a ceramic green body.
  • the green body is sintered, for example, below a sintering sintering temperature of the ceramic for a prolonged period of, for example, one hour, whereby a open porosity of, for example, 30 to 38, in particular 34 vol.% Can be achieved.
  • Is used as a ceramic material for example, zirconium dioxide, the temperature during the heat treatment 1150-1200 0 C, whereas a dense sintering is only to be expected at a temperature from 1380 to 1400 ° C. Furthermore, an open-porous structure of the sintered ceramic can be ensured by additionally enriching the material of the green body with organic, for example pulverulent, materials which are burned out during the heat treatment and into a porous one
  • the substrate 12 which may be made of zirconia, mounted, for example.
  • the positioned gas-sensitive detection units are contacted, for example, by using the fiap-cip technique or via bonding wire connections, and finally the protective cap 18 is placed on a ring of a glass solder previously positioned on the carrier element 20.
  • a drying of the glass solder paste and preferably a heat treatment which leads to the melting of the glass and in this way ensures a firm connection of the ceramic protective cap 18 on the ceramic support member 20. It is advantageous if GSaslot a glass is used, at least partially during the
  • an electrical resistance structure may for example comprise a meander-shaped resistance conductor track, which leads to a heating of the protective cap 18 when a corresponding heating voltage is applied.
  • the meander-shaped resistor track 24 the surface of the ceramic cap 18 at least partially or cover the entire surface.
  • the heating of the ceramic protective cap 18 can be carried out for example, regularly for a predetermined period of time.
  • the heating of the resistor track can be carried out for example, regularly for a predetermined period of time.
  • the time delay between the occurrence of a change in concentration of a gas component to be detected and the time of detection of this change in concentration can be used.
  • an artificially increased proportion of ammonia within the gas mixture to be determined for determining the time difference between the occurrence of the ammonia within the gas mixture to be determined and the detection of ammonia the sensor element 10 can be used to control the loading of the ceramic protective cap 18 with undesired constituents.
  • Halides, carbonates or acetates occur.
  • substances acting as oxidation catalyst can also be applied in the form of a washcoat suspension, for example by brushing, dipping, suction, etc. onto the porous protective cap 18 in the form of an additional layer.
  • the thickness of the layer is, for example, 1 .mu.m to 5 mm, preferably between 10 and 1000 .mu.m.
  • a drying step at, for example, 50 to 500 0 C is provided and then followed by a heat treatment process at a temperature of for example 350 to 700 ° C.
  • a suitably selected calcination atmosphere such as a hydrogen / nitrogen atmosphere.
  • the catalyst precursor compounds are converted into a catalytically active, for example elemental form. If the catalytically active substances are applied in the form of a washcoat formulation, sintering of the ceramic particles to the material of the porous protective cap 18 is ensured in this way.
  • the process sequence of impregnation, drying and calcining can also be repeated nacheina ⁇ der be performed until a loading of the ceramic material of the protective cap 18 with, for example, 0.1 to 50 weight percent, preferably 2 to 20 weight percent is reached.
  • kataiytisch active acting as Qxidationskatalysatoren substances, for example, noble metals such as platinum, palladium or rhodium or mixtures thereof are used.
  • the material of the ceramic protective cap 18 alternatively or additionally comprises a so-called getter material. This serves in general form of the impurization of undesirable substances which may be part of the gas mixture to be determined, but which leads to an inactivation of the gas-sensitive
  • Detection units of SensoreSement 10 can lead. These are, for example, alkaline or erdalkaii restroom substances that may result, for example, from road salt, or to magnesium or iron-containing compounds that may result from the abrasion of the piston or the engine block of a corresponding internal combustion engine.
  • mineral impurities are aluminum and silicon-containing compounds, which can be formed, for example, from impurities with engine oil.
  • getter materials are used in the context of the present invention, for example, Giastruckner. These can for example be added to the material of the green body used in the production of the ceramic protective cap 18 as a doping.
  • another possibility is to introduce corresponding Glasbüdner after completion of the protective cap 18 via an impregnation process, as already described for the introduction of catalytically active substances acting as oxidation catalysts.
  • the additional layer 26 is present as a substantially crack-free, porous layer.
  • lanthanum oxides or based on perovskites are suitable as oxygen-storing compounds and can thus supportively intervene in the oxidative removal of combustible impurities of the protective cap 18.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Molecular Biology (AREA)
  • Electrochemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (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)

Abstract

L'invention concerne un élément détecteur d'un détecteur de gaz, pour la détermination de composants gazeux dans des mélanges gazeux, comprenant un transistor à effet de champ et/ou une diode qui, lors d'un contact avec un gaz à détecter, présentent une conduction de courant variable, et qui sont positionnés, protégés par une coiffe de protection, vis-à-vis d'une arrivée directe du mélange gazeux. L'invention est caractérisée en ce que la coiffe de protection (18) présente un moyen de chauffage (24), une matière vitrifiable (34) et/ou un catalyseur d'oxydation (32).
EP09801687A 2009-02-12 2009-12-15 Elément détecteur d'un détecteur de gaz, et procédé permettant de le faire fonctionner Withdrawn EP2396650A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102009000820A DE102009000820A1 (de) 2009-02-12 2009-02-12 Sensorelement eines Gassensors und Verfahren zum Betrieb desselben
PCT/EP2009/067160 WO2010091761A1 (fr) 2009-02-12 2009-12-15 Elément détecteur d'un détecteur de gaz, et procédé permettant de le faire fonctionner

Publications (1)

Publication Number Publication Date
EP2396650A1 true EP2396650A1 (fr) 2011-12-21

Family

ID=42077702

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09801687A Withdrawn EP2396650A1 (fr) 2009-02-12 2009-12-15 Elément détecteur d'un détecteur de gaz, et procédé permettant de le faire fonctionner

Country Status (6)

Country Link
US (1) US8833141B2 (fr)
EP (1) EP2396650A1 (fr)
JP (1) JP2012517600A (fr)
CN (1) CN102317767B (fr)
DE (1) DE102009000820A1 (fr)
WO (1) WO2010091761A1 (fr)

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DE102013204469A1 (de) * 2013-03-14 2014-09-18 Robert Bosch Gmbh Mikroelektrochemischer Sensor und Verfahren zum Betreiben eines mikroelektrochemischen Sensors
CN105900236B (zh) * 2013-10-30 2020-03-17 罗伯特·博世有限公司 金属氧化物半导体传感器和使用原子层沉积形成金属氧化物半导体传感器的方法
CN105445420B (zh) * 2014-09-24 2019-12-06 普因特工程有限公司 微加热器和微传感器及其制造方法
DE102014223778A1 (de) 2014-11-21 2016-05-25 Robert Bosch Gmbh Vorrichtung zum Erfassen zumindest eines gasförmigen Analyten und Verfahren zum Herstellen derselben
US10363514B2 (en) 2015-03-27 2019-07-30 Koninklijke Philips N.V. Protecting an optical particle sensor from particulate desposits by thermophoresis
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JP6553587B2 (ja) * 2016-12-20 2019-07-31 Ｎｉｓｓｈａ株式会社 ガスセンサモジュール及びその製造方法
CN107966531A (zh) * 2017-11-24 2018-04-27 岑溪市辰运生态农业开发有限公司 一种砂糖橘厂制作用气体检测装置
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Also Published As

Publication number Publication date
WO2010091761A1 (fr) 2010-08-19
JP2012517600A (ja) 2012-08-02
US20120017665A1 (en) 2012-01-26
US8833141B2 (en) 2014-09-16
CN102317767A (zh) 2012-01-11
CN102317767B (zh) 2015-03-25
DE102009000820A1 (de) 2010-08-19

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