EP0647319A1 - Element detecteur permettant de determiner la concentration de composants gazeux - Google Patents

Element detecteur permettant de determiner la concentration de composants gazeux

Info

Publication number
EP0647319A1
EP0647319A1 EP94912450A EP94912450A EP0647319A1 EP 0647319 A1 EP0647319 A1 EP 0647319A1 EP 94912450 A EP94912450 A EP 94912450A EP 94912450 A EP94912450 A EP 94912450A EP 0647319 A1 EP0647319 A1 EP 0647319A1
Authority
EP
European Patent Office
Prior art keywords
diffusion channel
sensor element
measuring
gas
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Withdrawn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
EP94912450A
Other languages
German (de)
English (en)
Inventor
Karl-Hermann Friese
Werner Gruenwald
Roland Stahl
Claudio De La Prieta
Gerhard Schneider
Harald Neumann
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 EP0647319A1 publication Critical patent/EP0647319A1/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Withdrawn legal-status Critical Current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
    • G01N27/406—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 is based on a sensor with a diffusion channel according to the preamble of the main claim, for example for exhaust gas measurement of internal combustion engines in various embodiments, most often as a laminar or finger probe, which with different cavity systems d.
  • a further restriction is given for gas flows from the measuring gas space into the disk-shaped diffusion channel through the right-angled deflection of diffusing gas components, even in the case where w already assumes the multiple dimension of the diameter of the gas component.
  • Such a sensor element is constructed from a base body made of z. B. zirconia ceramic, which serves as a solid electrolyte.
  • a laminar design of the sensor is advantageous for economic reasons, but this is not the only design.
  • exhaust gas probes examples include EGOS (exhaust gas oxygen sensor), HEGOS (heated EGOS), PEGOS (proportional EGOS), UEGOS (universal EGOS) and TF-HEGOS (thin film HEGOS). Measurements are made in the electrochemical sensor element, including in a limit current probe, with at least two electrodes, one of which can come into contact with the reference gas, the other with the exhaust gas.
  • the gas component to be measured comes completely into contact with the porous electrode. In the event of the appearance of saturation on the electrode surface due to complete coverage with one or more gas components, this can lead to poisoning or overloading of the contact surface.
  • Such sensors work according to the polarographic measuring principle. A constant electrode voltage is applied between an anode and a cathode and a diffusion limit current is measured. However, the sensor could also use a different electrochemical measuring principle, e.g. B. the potentiometric measuring principle.
  • the diffusion limit current for example in the case of a limit current probe, is determined by ions after having overcome a diffusion barrier of the component of the measurement gas to be measured, the charges of which cause the current.
  • the design of the sample gas space in particular the diffusion channel in front of the electrodes, determines the diffusion resistance for the sample gas and influences the gradient of the concentration of the sample gas component to be measured. This affects the control position of the sensor.
  • measuring gas space will also include the diffusion channel and the electrode space, if these are not specifically mentioned.
  • a diffusion channel the part of the measuring gas space, for. B. is an exhaust gas probe, the gas mixture to be measured flows into the probe via the sample gas chamber supplied from the outside.
  • the measuring gas space should include every gas space that can house the gas component of the sensor to be measured.
  • the electrode space is the space that lies between the electrodes and contains the gas. It connects to the diffusion channel and is at least flooded by the gas component to be measured.
  • Diffusion channel tunnel dimensions or filled tunnels of the diffusion channel are known as mixed diffusion from Knudsen and gas phase diffusion, which can be the reason for the pressure dependence of the probe signals.
  • Sensor elements with diffusion channels which are designed according to the invention, have sufficient free path lengths for the measuring gas component. This means that gas phase diffusion essentially occurs for the measuring gas, without impacts against the wall or chemical reactions which could falsify this.
  • the diffusion coefficient of the sample gas component is then inversely proportional to the pressure in the sample gas space. Flow problems and tendencies to wall reactions of the gas component to be measured due to collisions of the molecules are largely avoided.
  • an average free path length of about 0.3 microns follows. From this, the minimum dimension of the diffusion channel is determined to be 30 micrometers, which corresponds to 100 times the mean free path of the oxygen anion. For functional reasons, a probe is limited in terms of its volume of the sample gas space and the diffusion channel for its inner channel system. The minimum expansion of the measuring gas space at any point in the interior of the sensor is known.
  • the minimal dimensions of the diffusion channel and measuring gas space gains advantages through a greater freedom of choice of the electrode geometry, for example in the electrode space.
  • Additional components for example support elements or channel expansion systems of the electrode space, can be attached at a suitable location.
  • FIG. 1 shows a cross section through the measuring gas space with a diffusion channel for a sensor
  • FIG. 2 shows a cross section through a sensor that was constructed from a pump and measuring cell
  • FIG. 5 shows a cross section through the measurement gas space of a sensor of FIG. 3 along the axis AB with the diffusion channel widened in a fan shape
  • FIG. 1 shows a cross section through the measuring gas space with a diffusion channel for a sensor
  • FIG. 2 shows a cross section through a sensor that was constructed from a pump and measuring cell
  • FIG. 6 shows the hatched area The area of the electrode coating using the example of a partially coated circular sector, ie a ring electrode coating
  • FIG. 8 shows a pump current-pump voltage diagram to represent the pressure Dependency of a sensor
  • Figure 9 shows the middle free path length for a selection of different gases depending on the gas pressure of a measuring gas and the channel dimensions resulting at 20 degrees Celsius
  • Figure 10 shows the operation of a non-regulated heating element of an exhaust gas probe and the pressure-sensitive position of the working point of the exhaust gas probe.
  • the porous anode 15 is covered with a cover layer 16.
  • the minimum dimension is indicated by a drawn ball with the diameter w, which can be moved freely.
  • the porous electrodes 15 and 13 are made of platinum or a platinum alloy.
  • w> 30 microns may filler material 17, for example, A l porous be 3 ° **** introduced n ⁇ s diffusion channel. It is conceivable that the measurement gas 20 flows into the diffusion channel 12 of the measurement gas chamber 18 from several sides. In the direction of the third dimension, the exhaust gas probe 21 can also be in a non-planar form be executed. Due to tests with more complex sensors, the w: L ratio could also be maintained for other sensors.
  • the cathode 13 can be coated with a porous protective layer or a plurality of porous protective layers in order to prevent the effects of corrosion and poisoning of its surface, as well as the removal of its material, or to avoid damage and / or impairments caused by components of the measurement gas 20.
  • a diffusion channel bent at its ends could be of more fluid design.
  • FIG. 2 shows a largely pressure-independent exhaust gas probe 21, consisting of a measuring cell 22 and a pump cell 23. Not all electrodes were tempered, e.g. B. the cathode 13 and the first electrode 24 are exposed.
  • measuring gas 20 enters the electrode space 24, 31 via the diffusion channel 12, it comes into contact with the first electrode 24 of the measuring cell 22, the potential of which changes relative to the second electrode 31.
  • the first electrode 24 and the second electrode 31 are separated by means of an intermediate layer 32 which conducts oxygen ions.
  • the potential difference is detected and used to regulate the potential between cathode 13 and anode 15 of the pump cell 23.
  • the oxygen concentration to be measured is measured after connecting the electrodes to an electrical network.
  • the measuring principle is described in more detail, for example, in EP-A 0 194 082.
  • the electrodes of the measuring cell 22 could also be arranged centrally below the electrodes of the pump cell 23.
  • the number of diffusion channels 12, their topography and their cross-sectional dimensions relative to one another are decisive for their position.
  • a distance is conceivable for the exhaust gas, the oxygen gas concentration of which is measured at several points in order to achieve better regulation of the inflowing gases, that is to say a supply regulation via several electrode pairs used for the measurement.
  • an electrode space 25 is spread out like a fan.
  • the measuring gas 20 flows into this electrode space 25 via a cylindrical measuring gas space 18, which can also be a partial volume of the measuring gas space, via the diffusion channel 12.
  • the electrode surfaces 26 and 27 are well suited as a covered anode surface 26 and a covered cathode surface 27 for contacting the electrodes.
  • the electrodes are designed as sector-shaped sections, as shown in FIG. 4.
  • the opening angle ⁇ is 60 degrees.
  • the manufacturing possibilities of the electrode contacts are expanded.
  • very thin layers of different material thickness and different local composition for contacting can be realized with great freedom for the choice of material and thus good electrical and mechanical contact stability and freedom from noise.
  • the active electrode area and a contact-dispensing means for coupling the leads to the electrode to an external electrical network lie in separate areas, which is why a double function at a geometrical location does not lead to compromises for the electrode and forcing contact.
  • the covered electrode surfaces 26, 27 directly adjoin the uncovered active electrode surfaces 28, 29, as shown in FIG. 6. It would be possible to choose the opening angle on one or both sides differently for the covered and effective electrode surface, so that there are interruptions in the conductor track or are knotted.
  • a circular disk coating in a corresponding modification according to FIG. 6 is conceivable.
  • FIG. 4 shows a section A-B, in which the effective electrode surface 28 directly adjoins the edge of the rectangular, columnar diffusion channel 12.
  • the opening angle ß is 45 degrees.
  • FIG. 5 shows a section A-B, in which the effective electrode surface 29 does not directly adjoin the edge of the rectangular, column-shaped diffusion channel 12 but only comprises one ring section.
  • the diffusion channel 12 is also expanded in a fan shape.
  • the opening angle ⁇ can be chosen up to 90 degrees for those in FIGS. 4 and 5, depending on how many electrode spaces are connected to one another via a plurality of diffusion channels. It would be conceivable to design the anode surface like the cathode surface. Another geometry of the electric field for measurement with non-homogeneous fields can also be produced.
  • FIG. 7 shows an example of a cross section through the diffusion and electrode space of an exhaust gas probe with an internal structure.
  • the column-shaped pillars, that is, cavity supports 30 serve to regulate the flow of measurement gas to the electrode surface.
  • the aperture function of the columns protects the electrodes from oversaturation and contamination. Furthermore, the structure becomes mechanically more stable and easier to shrink.
  • a measuring gas space with three diffusion channels inclined at 60 degrees to one another can also form a star with adjoining electrode spaces.
  • the oxygen content is measured at a pressure between 0.1 and 10 bar for the examples.
  • FIG. 9 contains examples of channel design for the gases a H, b air, c CO, and shows the mean free path length on the vertical axes on the left and the channel dimensions w on the right.
  • the horizontal axis corresponds to the gas pressure.
  • An example of the pressure insensitivity of a probe, e.g. B. the probe of Figure 2 is shown in Figure 10. If a heating element is attached to the lower substrate of the exhaust gas probe, the probe can be heated.
  • FIG. 10 illustrates for two exhaust gas probes A and B designed in this way, with electrode spaces corresponding to FIG. 4 and FIG. 5, the ratio of the limit currents with different temperature stability, which is set by the heating power.
  • the electrode spaces corresponding to those in FIGS. 4 and 5, respectively, are recorded in FIG. 10, the ratio of the limit currents of these probes at a gas pressure in the vicinity of 1 bar, or an increased gas pressure of 2 bar. Hatched areas denote variable temperatures for the gas, light areas denote constant temperatures. The dashed lines indicate no overlap of the measuring fields for constant and changeable temperatures in the case of the probe of FIG. 4 and therefore a somewhat higher temperature sensitivity of this layout for measuring the exhaust gas of the oxygen concentration.
  • the best embodiment of a probe is in FIG. 10 for probe B, in the case of small rectangular areas of FIG. 10 which are symmetrical about the limit current ratio at a setpoint of 1 for the limit current ratio at different pressures.
  • the parameter d is a measure of the missing overlap of the working point of the exhaust gas probes A or B).
  • the invention relates generally to sensors in which a reaction electrode is preceded by a diffusion barrier.
  • a technique for producing an exhaust gas probe is screen pressing e.g. B. a crackable organic form-forming layer, the form-forming agent, or a body part of this material on a substrate 11 or generally on another layer.
  • the cavity of the measuring gas chamber 18 is determined in shape and dimensions, that is to say also the w / L ratio.
  • This screen-printed layer forms, for example, the diffusion channel volume.
  • the measuring gas space 18 is later decomposed, evaporated or burned out during sintering.
  • the superimposition can include, for example, ceramic, matching, electrode, catalyst, line, cover or ceramic layers of the exhaust gas probe and can optionally be carried out by machine.
  • the ceramic layers are often between 0.3 and 2 millimeters thick.
  • a manufacturing process by sintering the diffusion barrier requires the minimum height of the channel of 30 micrometers.
  • the shrinkage for a 20 volume percent shrinkage when using theobromine as the shape-forming material is then chosen to be 42 micrometers and the laminar structure is sintered at at least 1000 degrees Celsius.
  • ZrO with 4 mol percent Y.0 was used as the ceramic
  • the electrodes 28/29 for the cathode and / or the corresponding anode of the sensor preferably consist of a metal from the platinum group, in particular platinum, or from alloys from the platinum group or alloys from metals from the platinum group with other substances, as is described, inter alia, in DE PS 41 00 106 is described. If necessary, you will receive a ceramic yttrium-stabilized zirconium oxide support framework material, for example in the form of a YSZ powder, with a volume fraction of preferably about 40 volume percent. They are porous and as thin as possible. They preferably have a thickness of 8 to 15 micrometers.
  • the conductor tracks belonging to the electrodes preferably also consist of platinum or a platinum alloy of the type described. They can also be produced from a paste based on a precious metal cermet.
  • the solid electrolyte layer (intermediate layer) 14 or 26 consists of one of the known, for the production of divalent negative
  • Oxygen conducting solid electrolytes used oxides such as in particular ZrO ", CeO .., HfO" and ThO "with a content
  • the layer can be about 80 to 97 mole percent ZrO, CeO, HfO or ThO and 3 to 20
  • Mole percent consist of MgO, CaO, SrO and / or rare earth oxides and / or in particular Y, 0.
  • the layer advantageously consists of ZrO stabilized with ⁇ .0. Sc 0 can be used as a full or partial replacement for Y-0.
  • the thickness of the layer can advantageously be 10 to 200 micrometers, in particular 15 to 50 micrometers.
  • the diffusion channel can have a filling made of coarsely porous sintering material, for example based on Al 0 or ZrO,
  • Thermal soot powder, graphite, plastics, for example based on polyurethane, salts, for example ammonium carbonate, and other organic substances, such as theobromine, were used as pore-forming agents or shape-forming agents for the design of the measuring gas space 18 and / or the diffusion channel 12 and / or the electrode space 24, 25 and indanthrene blue are used.
  • Unsupported structures also change their shape at sintering temperatures that are above a threshold temperature of around 300 degrees Celsius, which, for example when using theobromine, results in structural deformations because theobromine has already been completely removed from the cavity structure.
  • a solidification that is to say a shape that is true to shape, can only be obtained at temperatures above about 700 degrees Celsius. Further advantages arise when different shape-forming agents are used together, in that the volumes of individual cavities which are burned out are produced by joining, for example gluing together individual shape-forming partial volumes. Spacers can also be made from glass ceramic. Example 7 was made using picein.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Measuring Oxygen Concentration In Cells (AREA)

Abstract

L'invention concerne un élément détecteur (21) permettant de déterminer la concentration d'un des composants d'un mélange gazeux, qui comporte un canal de diffusion (12) qui mène à une chambre (18) destinée au gaz à analyser et jouxte une chambre à électrodes (24, 25). Chacune des dimensions (w) du canal de diffusion de la chambre (18) destinée au gaz, du détecteur (21), est un multiple de la longueur moyenne de parcours libre. On choisit une chambre à électrodes (25) qui jouxte le canal de diffusion (12). Ce procédé permet d'éviter que le système d'électrodes (13, 15) ne soit sursaturé par une configuration comportant des supports supplémentaires.
EP94912450A 1993-04-23 1994-04-13 Element detecteur permettant de determiner la concentration de composants gazeux Withdrawn EP0647319A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4313251A DE4313251C2 (de) 1993-04-23 1993-04-23 Sensorelement zur Bestimmung der Gaskomponentenkonzentration
DE4313251 1993-04-23
PCT/DE1994/000407 WO1994025864A1 (fr) 1993-04-23 1994-04-13 Element detecteur permettant de determiner la concentration de composants gazeux

Publications (1)

Publication Number Publication Date
EP0647319A1 true EP0647319A1 (fr) 1995-04-12

Family

ID=6486150

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94912450A Withdrawn EP0647319A1 (fr) 1993-04-23 1994-04-13 Element detecteur permettant de determiner la concentration de composants gazeux

Country Status (5)

Country Link
US (1) US5545301A (fr)
EP (1) EP0647319A1 (fr)
JP (1) JPH07508353A (fr)
DE (1) DE4313251C2 (fr)
WO (1) WO1994025864A1 (fr)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19815700B4 (de) 1998-04-08 2004-01-29 Robert Bosch Gmbh Elektrochemisches Sensorelement mit porösem Referenzgasspeicher
US5887240A (en) * 1998-05-11 1999-03-23 General Motors Corporation Method of manufacturing a platinum electrode
US6310398B1 (en) 1998-12-03 2001-10-30 Walter M. Katz Routable high-density interfaces for integrated circuit devices
DE19857471A1 (de) * 1998-12-14 2000-06-15 Bosch Gmbh Robert Sensorelement für Grenzstromsonden zur Bestimmung des Lambda-Wertes von Gasgemischen und Verfahren zu dessen Herstellung
US7750446B2 (en) 2002-04-29 2010-07-06 Interconnect Portfolio Llc IC package structures having separate circuit interconnection structures and assemblies constructed thereof
CN1659810B (zh) * 2002-04-29 2012-04-25 三星电子株式会社 直接连接信号传送系统
US6891272B1 (en) 2002-07-31 2005-05-10 Silicon Pipe, Inc. Multi-path via interconnection structures and methods for manufacturing the same
US7014472B2 (en) * 2003-01-13 2006-03-21 Siliconpipe, Inc. System for making high-speed connections to board-mounted modules
DE102004063084A1 (de) * 2004-12-28 2006-07-06 Robert Bosch Gmbh Sensorelement für einen Gassensor
DE102006061955A1 (de) * 2006-12-29 2008-07-03 Robert Bosch Gmbh Sensorelement mit brenngassensitiver Anode
DE102006062056A1 (de) * 2006-12-29 2008-07-03 Robert Bosch Gmbh Sensorelement mit unterdrückter Fettgasreaktion
JP5519596B2 (ja) * 2011-08-08 2014-06-11 日本特殊陶業株式会社 ガスセンサ装置およびガスセンサを用いた濃度測定方法

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JPS58153155A (ja) * 1982-03-09 1983-09-12 Ngk Spark Plug Co Ltd 酸素センサ
JPS59178354A (ja) * 1983-03-29 1984-10-09 Ngk Spark Plug Co Ltd 酸素センサ
JPH0612354B2 (ja) * 1983-11-28 1994-02-16 株式会社日立製作所 酸素濃度測定装置の製造方法
JPS61147155A (ja) * 1984-12-20 1986-07-04 Ngk Insulators Ltd 電気化学的装置
US4645572A (en) * 1985-02-23 1987-02-24 Ngk Insulators, Ltd. Method of determining concentration of a component in gases and electrochemical device suitable for practicing the method
JPH065222B2 (ja) * 1985-05-09 1994-01-19 日本碍子株式会社 電気化学的素子
DE3728289C1 (de) * 1987-08-25 1988-08-04 Bosch Gmbh Robert Nach dem polarographischen Messprinzip arbeitende Grenzstromsonde
JP2659793B2 (ja) * 1988-04-01 1997-09-30 日本特殊陶業株式会社 空燃比検出素子
US5106482A (en) * 1989-04-24 1992-04-21 Ephraim S. Greenberg High speed oxygen sensor
JP2744088B2 (ja) * 1989-10-13 1998-04-28 日本特殊陶業株式会社 空燃比センサ
DE4007856A1 (de) * 1990-03-13 1991-09-19 Bosch Gmbh Robert Sensorelement fuer eine sauerstoffgrenzstromsonde zur bestimmung des (lambda)-wertes von gasgemischen
JP2989961B2 (ja) * 1991-05-27 1999-12-13 株式会社デンソー 吸気管内用酸素濃度検出器

Non-Patent Citations (1)

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Title
See references of WO9425864A1 *

Also Published As

Publication number Publication date
DE4313251C2 (de) 2003-03-27
US5545301A (en) 1996-08-13
JPH07508353A (ja) 1995-09-14
WO1994025864A1 (fr) 1994-11-10
DE4313251A1 (de) 1994-10-27

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