WO1980001840A1 - Probe for measuring the partial pressure of oxygen in gases - Google Patents

Probe for measuring the partial pressure of oxygen in gases Download PDF

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Publication number
WO1980001840A1
WO1980001840A1 PCT/DE1980/000021 DE8000021W WO8001840A1 WO 1980001840 A1 WO1980001840 A1 WO 1980001840A1 DE 8000021 W DE8000021 W DE 8000021W WO 8001840 A1 WO8001840 A1 WO 8001840A1
Authority
WO
WIPO (PCT)
Prior art keywords
solid electrolyte
tablet
measuring
tube
gases
Prior art date
Application number
PCT/DE1980/000021
Other languages
German (de)
French (fr)
Inventor
F Baucke
T Frey
H Schaeffer
Original Assignee
Jenaer Glaswerk Schott & Gen
F Baucke
T Frey
H Schaeffer
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 Jenaer Glaswerk Schott & Gen, F Baucke, T Frey, H Schaeffer filed Critical Jenaer Glaswerk Schott & Gen
Publication of WO1980001840A1 publication Critical patent/WO1980001840A1/en

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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
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G01N27/4071—Cells and probes with solid electrolytes for investigating or analysing gases using sensor elements of laminated structure

Definitions

  • the invention relates to a novel measuring probe with which the oxygen partial pressure in gases, in particular hot gases, such as e.g. Exhaust gases can be determined easily and reliably.
  • gases in particular hot gases, such as e.g. Exhaust gases
  • Such probes consist of a tube which is closed on one side and consists of a solid electrolyte, e.g. Zirconium dioxide, in a solid-state electrode.
  • a solid electrolyte e.g. Zirconium dioxide
  • the aim of the present invention is a measuring probe which does not have the disadvantages described above.
  • the measuring principle is based on the ability of some ceramic ones
  • Conduct 2 materials e.g. stabilized ZrO ⁇ or ThO ⁇
  • Conduct 2 materials e.g. stabilized ZrO ⁇ or ThO ⁇
  • ne 2 partial pressures e.g P (1) in a reference gas on both sides of a solid ion conductor
  • the EMF is measured by means of a high-resistance voltmeter between two electrodes on both sides of the solid state electrolyte.
  • the electrodes are usually made of platinum.
  • the electrode on the reference side 5 is contacted via a porous Pt layer on the solid electrolyte surface.
  • the other electrode is contacted on the outside of the solid electrolyte.
  • the measuring chain therefore looks like this: Pt, 0 2 ( 0 ) / Zr0 2 (CaO) / Pt, 0 2 (P Q , x ).
  • the device according to the invention is produced by inserting a tablet made of an oxygen ion-conducting solid electrolyte into a metal tube in such a way that this tablet seals the lower end of this metal tube in a temperature-resistant and gas-tight manner.
  • the material can be made of a precious metal (e.g. platinum or platinum / rhodium) or e.g. are made of stainless steel.
  • a precious metal e.g. platinum or platinum / rhodium
  • stainless steel e.g. stainless steel
  • the solid electrolyte tablet is sintered onto the perforated bottom of the metal tube by hot pressing, the sintering pressure and temperature being able to be matched to one another.
  • the solid electrolyte is an oxygen-ion-conducting oxide, such as, for example, ZrO-, ThO_, HfO ⁇ or LaO-, which is optionally doped with a lower-valent oxide, such as CaO, MgO, Y 2 ° or Sc-, 0-.
  • the reference electrode is preferably contacted via a porous Pt layer on the surface of the tablet.
  • the Pt wire can be sintered onto the layer or simply pressed on (pressure contact).
  • a third possibility is to make a recess in the tablet and to sinter the electrode in it, which can be somewhat wound up at this point for better contact, with the aid of a powder at a maximum of 1500 ° C.
  • the reference electrode is preferably protected from electrical contact with the metallic outer tube by a single or multi-capillary tube made of an insulating refractory material (for example A1-.0-).
  • a thermocouple for measuring the temperature can be brought up to the solid electrolyte and reference gas can be passed through and finally, upon pressure contact, the pressure of the reference electrode, which is bent around the lower end of the capillary tube, is applied to the metallization surface.
  • the solid electrolyte tablet can also be attached to the bottom of the metal tube from the outside.
  • the probe according to the invention was in gases with the lower

Abstract

The new probe for measuring the partial pressure P02 in gases is provided with a measurement loop comprising a metal tube on the bottom of which is a pellet composed of a solid electrolyte oxide of which the anions have, at the ambient temperature, a transport member having the unit value. Inside the capsule there is provided a reference gas, outside the capsule is the gas object of the measurement. The electromotive force, resulting from the difference between partial pressures of oxygen, is measured on both sides of the solid electrolyte by means of two electrodes.

Description

Beschreibung description
Meßsonde zur Bestimmung des Sauerstoff-Partialdruckes in GasenMeasuring probe for determining the oxygen partial pressure in gases
Die Erfindung betrifft eine neuartige Meßsonde, mit welcher der Sauerstoff-Partialdruck in Gasen, insbesondere heißen Gasen, wie z.B. Abgasen einfach und zuverlässig bestimmt werden kann.The invention relates to a novel measuring probe with which the oxygen partial pressure in gases, in particular hot gases, such as e.g. Exhaust gases can be determined easily and reliably.
Die Kenntnis des Sauerstoff-Partialdruckes (PQ ) in Gasen ist aus vielen Gründen von großer technischer Bedeutung, beispielsweise bei der Schaffung umweltfreundlicher Ab¬ gasanlagen.Knowledge of the oxygen partial pressure (P Q ) in gases is of great technical importance for many reasons, for example when creating environmentally friendly exhaust gas systems.
Man hat bereits versucht, zur Durchführung derartiger . Messungen Festkörperelektrolytsonden, die nach elektro¬ chemischen Prinzip arbeiten, einzusetzen. Derartige Sonden bestehen im Prinzip aus einem einseitig verschlossenen Rohr aus einem Festkörperelektrolyten, wie z.B. Zirkon- dioxid, in einer Festkörper-Meßkette.Attempts have already been made to implement such. To use measurements of solid-state electrolyte probes which operate on the electrochemical principle. In principle, such probes consist of a tube which is closed on one side and consists of a solid electrolyte, e.g. Zirconium dioxide, in a solid-state electrode.
Eine Anwendung dieser bekannten, aus einseitig ge¬ schlossenen Festkörperelektrolytrohren bestehenden Meß- sonden zur Messung von sehr heißen Gasen standen bisher folgende Nachteile entgegen:The use of these known measuring probes, consisting of solid electrolyte tubes closed on one side, for measuring very hot gases has hitherto had the following disadvantages:
OMPIOMPI
WIPO - - schlechte Temperaturwechselbeständigkeit,WIPO - - poor resistance to temperature changes,
- schlechte mechanische Stabilität,- poor mechanical stability,
- korrosiver Angriff der Gase und damit verbundene uner¬ wünschte Korrosionsprodukte,corrosive attack of the gases and associated undesired corrosion products,
5 - kurze Standzeit,5 - short service life,
- hoher Preis.- high price.
. Ziel der vorliegenden Erfindung ist eine Meßsonde, welche die vorstehend geschilderten Nachteile nicht aufweist.. The aim of the present invention is a measuring probe which does not have the disadvantages described above.
Dieses Ziel wird mit einer Meßsonde gemäß den Patentan- 0 Sprüchen erreicht.This goal is achieved with a measuring probe according to the patent claims.
Das Meßprinzip beruht auf der Fähigkeit einiger keramischerThe measuring principle is based on the ability of some ceramic ones
2 Materialien (z.B. stabilisiertes ZrO~ oder ThO~ ) 0 -Ionen bei erhöhten Temperaturen zu leiten. Befinden sich näm¬ lich auf beiden Seiten eines festen Ionenleiters verschiede- 5 ne 02-Partialdrücke (z.B. P (1) in einem Bezugsgas,Conduct 2 materials (e.g. stabilized ZrO ~ or ThO ~) 0 ions at elevated temperatures. If there are different ne 2 partial pressures (eg P (1) in a reference gas on both sides of a solid ion conductor,
Pn (2) in einem Abgas) so entsteht nach Nernst eine elektro motorische Kraft EMK der Größe:P n (2) in an exhaust gas), according to Nernst, there is an electromotive force EMF of the size:
RTRT
EMK = In (P (D/Pn (2) zF U2 U2EMF = In (P (D / P n (2) zF U 2 U 2
(z = Wertigkeitswechsel; hier = 4); F = Faradaykonst. ; Q E = Gaskonst.; T = abs. Temp.) .(z = change in value; here = 4); F = Faraday const. ; Q E = gas const .; T = abs. Temp.).
Die EMK wird mittels eines hochohmigen Vol eters zwischen zwei Elektroden auf beiden Seiten des Festkörperelektro¬ lyten gemessen. Die Elektroden bestehen in der Regel aus Platin. Dabei wird die Elektrode auf der Referenzseite 5 über eine poröse Pt-Schicht auf der Festkörperelektrolyt- Oberfläche kontaktiert. Die andere Elektrode wird außen am Festkörperelektrolyten kontaktiert.The EMF is measured by means of a high-resistance voltmeter between two electrodes on both sides of the solid state electrolyte. The electrodes are usually made of platinum. The electrode on the reference side 5 is contacted via a porous Pt layer on the solid electrolyte surface. The other electrode is contacted on the outside of the solid electrolyte.
Die Meßkette sieht demnach folgendermaßen aus: Pt, 02 ( 0 ) /Zr02 (CaO) /Pt , 02 (PQ , x) .The measuring chain therefore looks like this: Pt, 0 2 ( 0 ) / Zr0 2 (CaO) / Pt, 0 2 (P Q , x ).
Die erfindungsgemäße Vorrichtung wird hergestellt, indem eine Tablette aus einem sauerstoffionenleitenden Fest¬ körperelektrolyten in ein Metallrohr derart eingesetzt wird, daß diese Tablette das untere Ende dieses Metallrohres temperaturbeständig und gasdicht abschließt.The device according to the invention is produced by inserting a tablet made of an oxygen ion-conducting solid electrolyte into a metal tube in such a way that this tablet seals the lower end of this metal tube in a temperature-resistant and gas-tight manner.
Das Material kann aus einem Edelmetall (z.B. Platin oder Platin/Rhodium) oder z.B. aus Edelstahl bestehen.The material can be made of a precious metal (e.g. platinum or platinum / rhodium) or e.g. are made of stainless steel.
Gemäß einer bevorzugten Ausführungsform der Erfindung wird die Festkörperelektrolyttablette durch Heißpressen auf den durchbohrten Boden des Metallrohres aufgesintert, wobei Sinterdruck und -temperatur einander angepaßt werden können. Der Festkörperelektrolyt ist ein sauerstoffionen¬ leitendes Oxid, wie z.B. ZrO-, ThO_, HfO~ oder LaO-,, der gegebenenfalls mit einem niedrigerwertigen Oxid, wie CaO, MgO, Y2° oder Sc-,0-, dotiert ist.According to a preferred embodiment of the invention, the solid electrolyte tablet is sintered onto the perforated bottom of the metal tube by hot pressing, the sintering pressure and temperature being able to be matched to one another. The solid electrolyte is an oxygen-ion-conducting oxide, such as, for example, ZrO-, ThO_, HfO ~ or LaO-, which is optionally doped with a lower-valent oxide, such as CaO, MgO, Y 2 ° or Sc-, 0-.
Vorzugsweise wird die Bezugselektrode über eine poröse Pt- Schicht auf der Oberfläche der Tablette kontaktiert. Da¬ bei kann der Pt-Draht auf die Schicht aufgesintert oder einfach nur aufgedrückt (Druckkontakt) werden. Eine dritte Möglichkeit besteht darin, in der Tablette eine Ver¬ tiefung anzubringen und in ihr die Elektrode, die an dieser Stelle zum besseren Kontakt etwas aufgewickelt sein kann, mit Hilfe eines Pulvers bei maximal 1500°C einzu- sintern.The reference electrode is preferably contacted via a porous Pt layer on the surface of the tablet. The Pt wire can be sintered onto the layer or simply pressed on (pressure contact). A third possibility is to make a recess in the tablet and to sinter the electrode in it, which can be somewhat wound up at this point for better contact, with the aid of a powder at a maximum of 1500 ° C.
Vorzugsweise wird die Bezugselektrode durch ein Ein- bzw. Mehrkapillarenrohr aus einem isolierenden Feuerfest- Material (z.B. A1-.0-) vor elektrischem Kontakt zum metallischen Außenrohr geschützt. Mit seiner Hilfe kann auch ein Thermoelement zur Messung der Temperatur bis an den Festelektrolyten herangeführt, Bezugsgas durchgeleitet und schließlich bei Druckkontakt der Druck der Bezugselek¬ trode, die um das untere Ende des Kapillarenrohres ge¬ bogen ist, auf die Metallisierungsfläche aufgebracht werden.The reference electrode is preferably protected from electrical contact with the metallic outer tube by a single or multi-capillary tube made of an insulating refractory material (for example A1-.0-). With its help, a thermocouple for measuring the temperature can be brought up to the solid electrolyte and reference gas can be passed through and finally, upon pressure contact, the pressure of the reference electrode, which is bent around the lower end of the capillary tube, is applied to the metallization surface.
Die Festkörperelektrolyt-Tablette kann auch von außen am Boden des Metallrohres befestigt werden.The solid electrolyte tablet can also be attached to the bottom of the metal tube from the outside.
Weitere Vorteile dieser neuen Hochtemperatur-Festkörper- meßkette bestehen darin, daß dieselbe auch als Meßsonde zur Bestimmung des Sauerstoff-Partialdruckes in Schmelzen mit dem gleichen Erfolg wie oben angegeben verwendet wer¬ den kann.Further advantages of this new high-temperature solid-state measuring chain are that it can also be used as a measuring probe for determining the oxygen partial pressure in melts with the same success as stated above.
Die erfindungsgemäße Sonde wurde in Gasen mit den unter-The probe according to the invention was in gases with the lower
-12 schiedlichsten Sauerstoff-Partialdrücken (1 atm - 10 at ) in einem Temperaturbereich von 700 bis 1500°C getes- tet. In allen Fällen erfüllte sie die Nernst-Gleichung bis auf + 2 % genau.-12 different oxygen partial pressures (1 atm - 10 at) tested in a temperature range from 700 to 1500 ° C. In all cases, it met the Nernst equation with an accuracy of + 2%.
OMPI OMPI

Claims

Patentansprüche: Claims:
1. Vorrichtung zur Bestimmung des Sauerstoff-Partialdruckes in Gasen, bestehend aus einer Hochtemperatur-Festkörper¬ meßkette, bei welcher eine Edelmetall-Meßelektrode von einer Edelmetall-Bezugselektrode durch einen Festkörper¬ elektrolyten getrennt ist, dadurch gekennzeichnet, daß - der Festkörperelektrolyt eine am Boden eines Metallrohres angebrachte Tablette aus einem oxidischen Festkörperelek¬ trolyten ist, dessen Sauerstoffionen-Überführungszahl den Wert 1 hat.1. Device for determining the oxygen partial pressure in gases, consisting of a high-temperature solid measuring chain, in which a noble metal measuring electrode is separated from a noble metal reference electrode by a solid electrolyte, characterized in that - the solid electrolyte is at the bottom a tablet made of an oxidic solid electrolyte, the oxygen ion transfer number of which is 1.
2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, daß die Tablette aus einem Festkörper besteht, der durch Dotierung mit einem anderen Oxid Sauerstoffionenleitend wird.2. Device according to claim 1, characterized in that the tablet consists of a solid which becomes oxygen ion conductive by doping with another oxide.
3. Vorrichtung nach Anspruch 3, dadurch gekennzeichnet, daß der Festkörperelektrolyt ZrO-, oder ThO- oder HfO- öder LaO.- und das Dotierungsmittel CaO oder MgO oder Y-0-. oder Sc^O-, ist.4.3. Apparatus according to claim 3, characterized in that the solid electrolyte ZrO-, or ThO- or HfO- or LaO.- and the dopant CaO or MgO or Y-0-. or Sc ^ O-, is 4.
4. Vorrichtung nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Tablette aus dem Festkörperelek- trolyten an das Ende des Metallrohres angesintert ist.4. Device according to one of claims 1 to 3, characterized in that the tablet is sintered from the solid electrolyte to the end of the metal tube.
5. Vorrichtung nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß dieses Rohr aus Edelmetall besteht.5. Device according to one of claims 1 to 4, characterized in that this tube consists of precious metal.
6. Vorrichtung nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Bezugselektrode in oder an der6. Device according to one of claims 1 to 5, characterized in that the reference electrode in or on the
Festkörperelektrolyttablette festgesintert ist.Solid electrolyte tablet is sintered.
7. Vorrichtung nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß die Festkörperelektrolyttablette von außen am Ende des Rohres angesintert ist. 7. Device according to one of claims 1 to 6, characterized in that the solid electrolyte tablet is sintered from the outside at the end of the tube.
8. Vorrichtung nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß die Bezugselektrode von einem elek¬ trisch isolierenden Rohr umgeben ist.8. Device according to one of claims 1 to 8, characterized in that the reference electrode is surrounded by an electrically insulating tube.
9. Vorrichtung nach einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß dieses Rohr zugleich die Meßelektrode ist.9. Device according to one of claims 1 to 9, characterized in that this tube is also the measuring electrode.
O PI WIPO O PI WIPO
PCT/DE1980/000021 1979-03-03 1980-02-29 Probe for measuring the partial pressure of oxygen in gases WO1980001840A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19792908308 DE2908308A1 (en) 1979-03-03 1979-03-03 MEASURING PROBE FOR DETERMINING OXYGEN PARTIAL PRESSURE IN GASES
DE2908308 1979-03-03

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WO1980001840A1 true WO1980001840A1 (en) 1980-09-04

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JP (1) JPS56500270A (en)
DE (1) DE2908308A1 (en)
FR (1) FR2451030A1 (en)
WO (1) WO1980001840A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2797306B2 (en) * 1987-03-13 1998-09-17 三菱自動車工業株式会社 Oxygen sensor and air-fuel ratio control device for internal combustion engine using the sensor

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2118666A6 (en) * 1970-12-15 1972-07-28 Kernforschung Gmbh Ges Fuer
US3752753A (en) * 1971-04-30 1973-08-14 G Fitterer Method of fabricating a sensor for the determination of the oxygen content of liquid metals
US3768259A (en) * 1971-07-06 1973-10-30 Universal Oil Prod Co Control for an engine system
US3776831A (en) * 1972-11-15 1973-12-04 Atomic Energy Commission Device for measuring oxygen activity in liquid sodium
US3791954A (en) * 1970-08-06 1974-02-12 Ngk Insulators Ltd Device for measuring oxygen concentration of molten metal
US3819500A (en) * 1972-02-21 1974-06-25 Philips Corp Measuring cell for determining oxygen concentrations in a gas mixture
DE2304075A1 (en) * 1973-01-27 1974-08-08 Bosch Gmbh Robert Electrochemical measuring probe - for monitoring the oxygen content of exhaust gases after catalytic treatment
US3909385A (en) * 1973-09-04 1975-09-30 Universal Oil Prod Co Oxygen sensor for automotive use
DE2625040A1 (en) * 1975-06-03 1977-01-13 Nissan Motor OXYGEN SENSOR DEVICE
DE2650850A1 (en) * 1976-11-06 1978-05-11 Rosenthal Ag Analysis method using solid electrolytes - with different electrolytes in tandem and unity ion transport number
FR2390727A1 (en) * 1977-05-11 1978-12-08 Renault Oxygen concn. detection cell - has hollow cylindrical sample chamber containing reference and measurement electrodes, latter is made of oxide of zirconium

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3791954A (en) * 1970-08-06 1974-02-12 Ngk Insulators Ltd Device for measuring oxygen concentration of molten metal
FR2118666A6 (en) * 1970-12-15 1972-07-28 Kernforschung Gmbh Ges Fuer
US3752753A (en) * 1971-04-30 1973-08-14 G Fitterer Method of fabricating a sensor for the determination of the oxygen content of liquid metals
US3768259A (en) * 1971-07-06 1973-10-30 Universal Oil Prod Co Control for an engine system
US3819500A (en) * 1972-02-21 1974-06-25 Philips Corp Measuring cell for determining oxygen concentrations in a gas mixture
US3776831A (en) * 1972-11-15 1973-12-04 Atomic Energy Commission Device for measuring oxygen activity in liquid sodium
DE2304075A1 (en) * 1973-01-27 1974-08-08 Bosch Gmbh Robert Electrochemical measuring probe - for monitoring the oxygen content of exhaust gases after catalytic treatment
US3909385A (en) * 1973-09-04 1975-09-30 Universal Oil Prod Co Oxygen sensor for automotive use
DE2625040A1 (en) * 1975-06-03 1977-01-13 Nissan Motor OXYGEN SENSOR DEVICE
DE2650850A1 (en) * 1976-11-06 1978-05-11 Rosenthal Ag Analysis method using solid electrolytes - with different electrolytes in tandem and unity ion transport number
FR2390727A1 (en) * 1977-05-11 1978-12-08 Renault Oxygen concn. detection cell - has hollow cylindrical sample chamber containing reference and measurement electrodes, latter is made of oxide of zirconium

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DE2908308A1 (en) 1980-09-04
FR2451030A1 (en) 1980-10-03
JPS56500270A (en) 1981-03-05
FR2451030B1 (en) 1984-07-06

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