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WO2009083375A1 - Procédé pour la détermination d'une composition de gaz dans un espace de mesure de gaz, élément de détection et agencement de détection - Google Patents

Procédé pour la détermination d'une composition de gaz dans un espace de mesure de gaz, élément de détection et agencement de détection Download PDF

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Publication number
WO2009083375A1
WO2009083375A1 PCT/EP2008/066688 EP2008066688W WO2009083375A1 WO 2009083375 A1 WO2009083375 A1 WO 2009083375A1 EP 2008066688 W EP2008066688 W EP 2008066688W WO 2009083375 A1 WO2009083375 A1 WO 2009083375A1
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WIPO (PCT)
Prior art keywords
electrode
pumping
voltage
gas
sensor element
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.)
Ceased
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PCT/EP2008/066688
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German (de)
English (en)
Inventor
Bernd Schumann
Henrico Runge
Holger Reinshagen
Thomas Classen
Martin Le-Huu
Berndt Cramer
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Robert Bosch GmbH
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Robert Bosch GmbH
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Publication of WO2009083375A1 publication Critical patent/WO2009083375A1/fr
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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
    • G01N27/26—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
    • G01N27/4065—Circuit arrangements specially adapted therefor
    • 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
    • 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
    • G01N27/416—Systems
    • G01N27/417—Systems using cells, i.e. more than one cell and probes with solid electrolytes
    • G01N27/419—Measuring voltages or currents with a combination of oxygen pumping cells and oxygen concentration cells
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02D—CONTROLLING COMBUSTION ENGINES
    • F02D41/00—Electrical control of supply of combustible mixture or its constituents
    • F02D41/02—Circuit arrangements for generating control signals
    • F02D41/14—Introducing closed-loop corrections
    • F02D41/1438—Introducing closed-loop corrections using means for determining characteristics of the combustion gases; Sensors therefor
    • F02D41/1444—Introducing closed-loop corrections using means for determining characteristics of the combustion gases; Sensors therefor characterised by the characteristics of the combustion gases
    • F02D41/1454—Introducing closed-loop corrections using means for determining characteristics of the combustion gases; Sensors therefor characterised by the characteristics of the combustion gases the characteristics being an oxygen content or concentration or the air-fuel ratio
    • F02D41/1456—Introducing closed-loop corrections using means for determining characteristics of the combustion gases; Sensors therefor characterised by the characteristics of the combustion gases the characteristics being an oxygen content or concentration or the air-fuel ratio with sensor output signal being linear or quasi-linear with the concentration of oxygen

Definitions

  • PROCEDURE FOR DETERMINING A GAS COMPOSITION IN A MEASURING ROOM, SENSOR ELEMENT AND SENSOR ARRANGEMENT
  • the invention is based on known sensor elements which are based on electrolytic properties of certain solids, ie the ability of these solids to conduct certain ions.
  • sensor elements are used in particular in motor vehicles to measure air-fuel-gas mixture compositions, in which case these sensor elements are also known as "lambda sensors" and an essential role in the reduction of pollutants in exhaust gases, both in gasoline engines as well in diesel technology, play.
  • Such sensor elements are now known in numerous different embodiments.
  • One embodiment is the so-called "jump probe” whose measuring principle is based on the measurement of an electrochemical potential difference between a reference electrode exposed to a reference gas and a measuring electrode exposed to the gas mixture to be measured conductive properties usually doped zirconium dioxide (eg yttrium-stabilized ZrC ⁇ ) or similar Liche ceramics are used as solid electrolyte.
  • doped zirconium dioxide eg yttrium-stabilized ZrC ⁇
  • Liche ceramics similar Liche ceramics are used as solid electrolyte.
  • Various exemplary embodiments of such jump probes which are also referred to as "Nernst cells” are described, for example, in DE 10 2004 035 826 A1, DE 199 38 416 A1 and
  • pump cells are used in which an electrical “pumping voltage” is applied to two electrodes connected via the solid electrolyte, whereby the “pumping current” is measured by the pump cell
  • both electrodes are usually connected to the gas mixture to be measured, whereby one of the two electrodes is exposed directly to the gas mixture to be measured (usually via a permeable protective layer) can not get directly to this electrode, but must first penetrate a so-called “diffusion barrier” to get into a cavity adjacent to this second electrode.
  • the diffusion barrier used is usually a porous ceramic structure with specifically adjustable pore radii.
  • the sensor elements are usually operated in so-called limiting current operation, that is, in an operation in which the pumping voltage is selected such that the oxygen entering through the diffusion barrier is completely pumped to the counterelectrode.
  • the pumping current is approximately proportional to the partial pressure of the oxygen in the exhaust gas mixture, so that such sensor elements are often referred to as proportional sensors.
  • proportional sensors can be used as so-called broadband sensors over a comparatively wide range for the air ratio
  • the sensor principles described above are also combined, so that the sensor elements contain one or more sensors ("cells") operating according to the jump sensor principle and one or more proportional sensors Pump cell principle working "single cell” by adding a snap cell (Nernst cell) to a "double"
  • a snap cell Nel cell
  • the multicell sensor elements are used as amperometric gas sensors, gas sensors with three electrodes typically being used.
  • a pumping voltage is applied between an outer pumping electrode (APE), which is usually located under a protective layer, and an inner pumping electrode (IPE) arranged behind a diffusion barrier.
  • APE outer pumping electrode
  • IPE inner pumping electrode
  • RE reference electrode
  • the measured IPE-APE pumping current is a measure of the amount of oxygen in the exhaust gas.
  • water or carbon dioxide is decomposed at the APE and oxygen ions are pumped from there to the IPE (negative pumping voltage).
  • the oxygen that is pumped in reacts with hydrogen and carbon monoxide, which in turn are limited in their secondary flow by the diffusion barrier.
  • the pumping current is a measure of the oxygen deficit in the exhaust gas even in the rich air range.
  • a disadvantage of the multicellular structures of the sensor elements is the complexity of such sensor elements.
  • the number of electrodes and / or the number of leads to these electrodes represents a significant cost factor, which should be reduced if possible.
  • single-cell arrangements with two electrodes exposed to the gas mixture have the problem that there is no clear relationship between the pumping current and the gas mixture composition.
  • a positive pumping current (lean pumping current) is generally measured at a fixed pumping voltage in a lean gas mixture.
  • a positive pumping current is usually also recorded, even if the applied pumping voltage (usually about 400 to 700 mV, for example, 500 mV) is well below the decomposition voltage of water (about 1, 23 V).
  • This positive pumping current in the rich rich is essentially attributable to the molecular hydrogen or other fuel gases contained in the gas mixture, which influences the electrochemical potential of the anode, since water can now be formed on the first electrode from the oxygen ions leaving the solid electrolyte instead of molecular oxygen. The energy released at the anode during H 2 O formation thus compensates for the H 2 O formation.
  • DE 10 2005 054 144 A1 therefore describes a gas sensor with an outer electrode and an inner electrode, which are each separated from a measuring space by diffusion barriers. In this case, the two diffusion barriers have different diffusion coefficients.
  • a circuit is provided which is arranged by reversing the polarity of the pumping voltage and comparing the pumping currents before and after the polarity reversal in order to distinguish rich air-frequency ranges from lean air-power ranges.
  • a method for determining at least one physical property of a gas in at least one measuring gas space, as well as a sensor element and a sensor arrangement, which are particularly suitable for implementing the described method and which at least largely avoid the disadvantages of known methods and devices.
  • a basic idea of the present invention is the recognition that limiting the speed of known reversing methods, such as, for example, the method described in DE 10 2005 054 144 A1, which is particularly due to the fact that it is to be reloaded Capacities (electrical capacitance of the electrodes and optionally double-layer capacitances) is limited, can be improved by suitable design of the sensor system and the method. For example, after a change in the polarity of the pumping voltage, it is necessary to wait until all the capacitors have been reloaded and a new, steady state has been established.
  • the present invention therefore describes an electronic method by means of which the time resolution can be increased to the extent that an application in a car is possible.
  • the method is comparatively flexible with regard to the sensor elements used and can be carried out, for example, using conventional broadband probes, simple single-cell constructions, the sensor structure described in DE 10 2005 054 144 A1 and with a special sensor element proposed according to the invention.
  • conventional broadband probes allows a cost-effective implementation of the method, since known and proven sensor geometries can be used.
  • the proposed method for determining at least one physical property of a gas in a measurement gas space can be used in particular for determining an oxygen concentration in the exhaust gas of an internal combustion engine, for example in the context of one or more of the lambda probes described above.
  • other types of physical properties of the gas are also measurable, for example gas concentrations of other gas components in the gas.
  • the proposed method uses a sensor element having at least one first electrode and at least one second electrode and at least one solid electrolyte connecting the first electrode and the second electrode.
  • the sensor element comprises at least one pumping cell.
  • the first electrode and the second electrode are connected to the measuring gas space in such a way that these two electrodes can be acted upon in each case with gas from the measuring gas space.
  • this application can be carried out, for example, directly and / or via a protective layer (for example a protective layer which protects the electrodes from contamination) and / or one or more diffusion barriers.
  • the proposed method is based on the basic idea described in DE 10 2005 054 144 A1, which consists in measuring different pump currents in the event of reversal of a pump voltage applied between the two electrodes due to inevitably existing (for example, component tolerances) and / or deliberately induced asymmetries which can be detected by reversing a pump voltage. Accordingly, at least a first pumping voltage is applied between the first electrode and the second electrode, so that the pumping cell with this first pumping voltage is applied. In this case (ie simultaneously or with a time delay), at least one first pumping current is measured between the first electrode and the second electrode.
  • At least one second pumping voltage is applied between the first electrode and the second electrode (ie, again to the pumping cell) and thereby (i.e., simultaneously and / or delayed) at least a second pumping current is measured through this pumping cell.
  • the second pumping voltage is selected such that it has a polarity reversed to the first pumping voltage (polarity reversal).
  • the second pumping voltage can be designed to be equal in magnitude to the first pumping voltage, although other types of a second pumping voltage are also possible.
  • a basic idea of the present invention consists in modifying the plausibility considerations mentioned in DE 10 2005 054 144 A1 in such a way that an unambiguous measured variable is formed from the measured pumping currents (i.e., directly from these pumping currents and / or from measured variables derived from these pumping currents).
  • This unique measure is to be chosen such that, in contrast to the pumping current itself, it substantially (i.e., for example, except for device-related fluctuations or noise) is unique, i. reversible, related to the physical property of the gas, for example a gas mixture composition, in particular an oxygen concentration (or another measurement gas concentration).
  • this can be a monotonic or strictly monotonic with the physical property of the gas, for example the oxygen concentration, increasing or decreasing, unambiguous measured variable, from which the physical property can be deduced.
  • the present invention proposes this, this unique
  • a linear combination of the minimum MIN and the maximum MAX of the two pump currents is a combination of the following type:
  • the coefficients a, b and c can be any numbers, for example real numbers, which in each case can also assume the value 0.
  • a, b and c are such Selects that the unique measurand ⁇ , as stated above, at each measurement point of a given range allows a clear inference to the physical property.
  • the coefficients a or b can also assume the value zero (but not simultaneously).
  • c can take the value zero.
  • a sum pumping current can also be formed from the maximum and the minimum and used as a linear combination ⁇ .
  • the maximum and the minimum for the implementation of the method according to the invention need not be explicitly determined, but it is also possible to determine directly, for example, a linear combination of this minimum and this maximum. Further embodiments of this idea will be further elaborated below.
  • the method described can be implemented in particular by means of a sensor arrangement which has at least one drive device.
  • This electrical control device makes it possible to quickly generate and / or determine the partial measured values (for example the first pumping current and the second pumping current) necessary for the method and to assemble these partial measured values into the unambiguous measured variable.
  • this results in a sensor operating mode for a sensor element, which shows a clear characteristic over a wide range of physical size, in particular over a wide lambda range, which is largely independent of the sensor geometry.
  • sensor elements with only two electrodes in various possible geometries and / or conventional sensor elements can also be used.
  • the operation of the sensor element can be done with high dynamics.
  • the switching between the first pumping voltage and the second pumping voltage in addition to a simple voltage-controlled mode, can take place in a current-controlled mode in order to further reduce the switching time.
  • the voltage pulse can be selected to be higher than the second pumping voltage by at least a factor of 1.5, in particular by at least a factor of 2 and particularly preferably by at least a factor of 3.
  • the voltage pulse may have a length between 2 and 100 microseconds, and preferably between 20 microseconds and 50 microseconds.
  • other types of voltage pulses or voltage pulse combinations are conceivable.
  • the switching between the first pumping voltage and the second pumping voltage can be repeated periodically, in which case the first pumping voltage and the second pumping voltage exchange the rollers and the method according to the invention is repeated analogously.
  • a voltage pulse can be used, which is then connected upstream in this case the first pumping voltage.
  • the proposed method is based in particular on an asymmetry between the first electrode and the second electrode, which is naturally present in most sensor elements.
  • this asymmetry can also be brought about artificially, which is particularly preferred in the context of the present invention.
  • the first electrode and the second electrode can each be connected via a first or second connection to the sample gas space.
  • These connections can be configured, for example, in the form of bores, openings or the like.
  • one or both of the electrodes may be exposed directly to the measuring gas space, that is to say have a free surface towards this measuring gas space, or a surface covered only by a protective layer or thin diffusion barrier.
  • first connection and the second connection have an asymmetry, so that the first electrode and the second electrode have different limiting currents. It is particularly preferred if these limit currents differ by at least 10%, but higher differences, for example by a factor of 20, are also possible.
  • the limiting current of an electrode is defined as the saturation pumping current, ie the maximum pumping current for the pure oxygen decomposition (or measuring gas decomposition), which can be achieved when the pumping voltage between the at least two electrodes is increased.
  • This limiting current can be defined, for example, for oxygen and oxygen ion transport through the solid electrolyte as the current which is achieved when all of the oxygen molecules which reach the cathode-operated electrode are completely transported through the solid electrolyte to the anode.
  • the pumping current is approximately proportional to the gas molecule concentration, the limiting current of the opposite electrode, which previously operated as the anode was accordingly determined experimentally by polarity reversal, so that now the former anode is operated as a cathode.
  • the setting of the different limiting currents of the two electrodes or of the two connections, in combination with the electrodes, can be achieved in particular by providing diffusion barriers in one or both of these connections.
  • This at least one diffusion barrier has a diffusion resistance.
  • the diffusion barriers are preferably selected such that the diffusion resistances of the two diffusion barriers of the two compounds differ by a factor of at least 1.1, preferably by a factor between 1.5 and 3 (or by the inverse of these numbers).
  • the diffusion resistance is that resistance which a diffusion barrier opposes to a concentration difference ⁇ c between both sides of the diffusion barrier of length 1 and of cross-section A and which thus hinders diffusion (current I gas ):
  • the diffusion coefficient D is composed (inverse additive) of the diffusion coefficients for the gas phase diffusion and for the Knudsendiffusion, both of which have different temperature dependencies.
  • the temperature dependence of the flow thus depends on the proportions of the individual types of diffusion.
  • the flux changes by about 4% when the temperature changes by 100 ° C.
  • a diffusion barrier is to be understood as meaning in general a porous element, for example a ceramic porous element which has a diffusion resistance
  • the term diffusion barrier may also include other types of elements which provide resistance to diffusion
  • porous covering layers, channels (in particular channels with a reduced cross-section), combinations of channels or similar elements or combinations of elements should be mentioned. Possibilities are also arbitrarily combinable to set a desired diffusion resistance.
  • the same diffusion medium eg a porous material
  • the two diffusion barriers can be used for the two diffusion barriers, but in different layer thicknesses, so that, for example, a higher layer thickness is used in front of the at least one first electrode than in front of the at least one second electrode .
  • an adjustment of the surface of the diffusion barriers can also take place.
  • the limiting current increases at least approximately proportionally with the cross-sectional area available for the diffusion, and inversely proportional to the length or layer thickness of the diffusion barriers.
  • a sensor element may be used in which the first electrode and the second electrode are separated from the measurement gas space by at least one cover layer.
  • the first compound and the second compound may each include one or more gas access holes, which are preferably formed at least partially separated for the first compound and the second compound and which penetrate the at least one cover layer.
  • a layer structure can be used in which the first electrode and the second electrode are arranged in the same layer plane of the layer structure, ie side by side, in contrast to the stacked embodiment according to DE 10 2005 054 144 A2. In this way, layer planes can be saved, and the entire sensor structure can be greatly simplified.
  • other types of sensor elements may be used.
  • FIG. 1 shows an embodiment of a sensor arrangement with a sensor element according to the prior art and a drive device
  • FIG. 2 shows an inventive sensor element which is alternative to the sensor element in FIG.
  • Figure 3 is a perspective view of a sensor element according to the invention.
  • FIG. 4 shows a pumping current characteristic as a function of a gas partial pressure
  • FIG. 5 shows pump current characteristics analogous to FIG. 4 with and without reversing the polarity of the pump voltage
  • FIG. 6 shows the pumping current characteristic according to FIG. 5 with additionally a sum pump current characteristic
  • FIG. 7 shows pump current characteristics for sensor elements with virtually unhindered gas access to an electrode
  • FIG. 8 shows pumping currents when the pumping voltage is reversed
  • FIG. 9 shows pumping currents when switching over with an additional voltage pulse
  • FIG. 10 shows a further embodiment of a sensor element according to the invention.
  • FIG. 11 an exemplary embodiment of a circuit of the sensor element according to FIG. 10;
  • FIG. 12 shows a pump voltage curve at the electrodes of the sensor element according to FIG. 10 for explaining a method according to the invention.
  • FIG. 1 shows an exemplary embodiment of a sensor arrangement 110 according to the present invention.
  • the sensor arrangement 110 comprises, in addition to a drive device 112, which can provide pumping voltages and / or pumping currents, take over measuring functions or perform similar tasks, a sensor element 114.
  • the drive device 112 can contain, for example, at least one of the following devices: a power source, a voltage source, a current measuring device, in particular for measuring a pumping current, a Voltage measuring device, in particular for measuring a pump voltage and / or for measuring a reference voltage, one or more control devices and other functions, such as logic functions, memory functions or the like.
  • the drive device 112 may also comprise one or more data processing devices, for example one or more microcomputers.
  • the control device 112 can be centralized, ie accommodated in one piece and / or housed in a single housing, configured or decentralized, ie distributed, for example, distributed in several separate components.
  • the at least one microcomputer can be set up, for example, in terms of programming, in order to control or completely or partially implement the method proposed above in one or more of the described embodiments.
  • the control device 112 is connected to the sensor element 114 via control lines 116.
  • the sensor element 114 corresponds to a sensor element known from the prior art. However, this sensor element 114 can be replaced by other types of sensor elements, for example, against the sensor elements described in subsequent embodiments.
  • the sensor element 114 shown in Figure 1 is a commercially available broadband sensor element, whose operation is described for example in Robert Bosch GmbH: Sensors in the motor vehicle, 2001, pages 116-117.
  • the sensor element 114 comprises a pumping cell 118 having a first electrode 120, a solid electrolyte 122 and a second electrode 126, which is in two parts in this exemplary embodiment and is arranged in an electrode cavity 124.
  • a second connection 134 is provided, which in this embodiment comprises a gas inlet hole 136, the electrode cavity 124 and a second connection 134 arranged between the electrode cavity 124 and the gas inlet hole 136 Diffusion barrier 138 includes.
  • the gas inlet hole 136 is disposed perpendicular to the layer structure shown in FIG. 1 and penetrates the solid electrolyte 122.
  • the sensor element 114 designed as a broadband probe comprises a reference air channel 140 with a reference electrode 142, as well as a heating element 144.
  • the functions of the reference electrode 142 and of the Heating element 144 will not be discussed in more detail below, but reference is made in this regard to the description of the sensor elements 114 known from the prior art.
  • the first electrode 120 which in this embodiment is designed as an outer electrode, is also referred to as APE (outer potential electrode or outer pumping electrode), the second electrode 126 as IPE (inner potential electrode or inner pumping electrode) and the reference electrode 142 as RE.
  • FIGS. 2 and 3 show possible alternative embodiments of the sensor element 114, wherein a possibly additionally present control device 112 has been dispensed with in this illustration.
  • the first electrode 120 has been separated from the sample gas chamber 132 only by a protective layer 130
  • the first connection 128 via which the first electrode 120 also has gas can be acted upon from the sample gas space 132, a first diffusion barrier 146.
  • a first electrode cavity 148 is provided, which, together with the first diffusion barrier 146, forms the first connection 128.
  • the second electrode 126 has a second electrode cavity 150 which corresponds to the electrode cavity 124 according to FIG. 1 and which, together with the second diffusion barrier 138, forms the second connection 134 between the second electrode 126 and the measurement gas space 132.
  • a heating element 144 is provided.
  • Electrodes 120, 126 are formed in this embodiment as two-part electrodes and arranged in a first or second electrode cavity 148, 150 and contactable by electrode leads 116, plated-through holes 154 and electrode contacts 156.
  • a heating element 144 with insulating foils 158 and heating resistors 160 is again provided.
  • connections 128, 134 are again provided.
  • These compounds which may also be wholly or partly filled with a gas-permeable, porous material, include, in addition to the electrode cavities 148, 150 a first gas inlet hole 162 and a second gas inlet hole 164 and a first diffusion barrier 146 and a second diffusion barrier 138.
  • the electrodes 120 and 126 are also arranged in the same layer plane of the layer structure of Figure 3, which is an introduction of additional layers, as criz- For example, in DE 10 2005 054 144 Al shown, avoidable makes.
  • the sensor element described in this document is basically used in the context of the present invention.
  • the present method is based on asymmetry effects between the two electrodes 120, 126 or the pump cell 118 formed from these electrodes and the solid electrolyte 122.
  • Previous designs have generally been optimized in such a way that the characteristic of the pump current is unambiguous in lean operation is, so that usually no pumping current in rich operation is measurable.
  • the pumping cells 118 are configured such that both electrodes 120, 126 experience a connection to the sample gas chamber 132. The result of this design is a V-shaped characteristic.
  • limiting currents are now measured for the fatty gas reaction at the anode (H 2 O decomposition at the cathode). Which of the electrodes 120, 126 functions as the anode and which as the cathode depends on the sonication. Limit currents in rich operation and in lean operation are positive, whereby the characteristic is not unique.
  • FIG. 4 An exemplary embodiment of various pump current characteristics is shown in FIG. 4 for the sensor element 114 shown in FIG.
  • the first electrode 120 in FIG. 3 is connected as the anode, and the second electrode 126 as the cathode.
  • the pump currents I p (shown in arbitrary units in FIG. 4 and provided with an offset) were measured by the pump cell 118 for various sensor elements 114.
  • the ratio of the diffusion resistances or flow resistances of the connections 128 and 134 in FIG. 3 was varied. This occurs, for example, in that the distance between the first gas inlet hole 162 and the first electrode 120, denoted by d in FIG. 3, ie the length the first diffusion barrier 146 was varied. The numerical values given represent this distance d in mm. It can be seen that all the sensor elements 114 in the lean region, which is denoted by reference numeral 166 in FIG. 4, have an almost identical characteristic, since it is essentially not for this lean region 166 to the length of the first diffusion barrier 146 of the first electrode 120 acting as the anode arrives. In the rich region, which is denoted symbolically by the reference numeral 168 in FIG.
  • the characteristic curves of the sensor elements 114 differ greatly. Depending on how large the diffusion resistance in front of the anode 120, now limit currents for the fat gas oxidation at this anode 120 (H 2 O decomposition at the cathode) are measured. This shows that the slope of the fat branch of the characteristic curve in FIG. 4 can be influenced in a targeted manner by varying the diffusion resistance of the connection (in this case the first connection 128 in front of the anode-connected first electrode 120), so that the characteristic curve runs in the lean region 166 ("Lean load”) and the characteristic curve in the rich area 168 (“Fettast”) can be set differently.
  • the diffusion resistance of the connection in this case the first connection 128 in front of the anode-connected first electrode 120
  • fat operation and lean operation can be distinguished and the limit currents assigned accordingly.
  • the different gradients of the fat and lean load form a "tilted V" with different rising arms and thus allow the evaluation of both branches when quickly switching the pump voltage.
  • the limiting currents of the connections 128, 134, in particular of the diffusion barriers 146, 138, should differ by at least 10%. There are also differences by a factor of 20 possible. All in all, these signals can be used to measure plausible signals by means of a suitable control device 112, which contains a corresponding evaluation circuit. The aim is in particular a factor between 1.5 and 3 in the diffusion resistance of the diffusion barrier 146, 138. However, larger or smaller differences in the diffusion resistance are in principle possible.
  • the measuring range for the limiting currents can be, for example, in the range between 1 mA and 20 mA. An optimum range is usually between 1.5 mA and 6.0 mA.
  • the limiting currents (the pump currents IP in FIG.
  • FIG. 5 shows further pump current characteristics, by means of which the measuring principle, which is based on the asymmetry between lean and rich load, will be explained in more detail. The illustration is in principle the same as that shown in FIG.
  • first characteristic curve 170 is plotted which corresponds to the measured values in FIG.
  • This first characteristic 170 was recorded with the above-described wiring in which the first electrode 120 acts as a building electrode and the second electrode 126 acts as a built-in electrode.
  • the pumping voltage at the pumping cell 118 was chosen to be -500 mV for this first characteristic 170 (the sign results from the cited circuit).
  • the pumping current of the first characteristic 170 is determined by the second diffusion barrier 138 in the second connection 134 toward the second electrode 126 (labeled DB1 in FIG. 5), whereas in the rich region 168 the first diffusion barrier 146 is the deciding factor for the pumping current (denoted by DB2 in FIG. 5). Furthermore, a second characteristic curve 172 is plotted in FIG. 5, which results from the fact that the pumping voltage U p at the pumping cell 118 was reversed. The pump voltage in this case is for example +500 V, the sign in turn resulting from the wiring.
  • the first electrode 120 is connected as a built-in electrode, and the second electrode 126 as an expanding electrode.
  • the influences of the two diffusion barriers 146, 138 have reversed, since the roles of installing and removing electrode or diffusion barrier have interchanged.
  • the first characteristic curve 170 and the second characteristic curve 172 each differ at least approximately by a point reflection at the zero point.
  • the proposed method is based on a "trial-and-error" method as to whether the gas mixture in the sample gas chamber 132 is in the lean region 166 or in the rich region 168, which is unsatisfactory and not necessarily expedient in the proposed method described above
  • a characteristic curve of a definite measured variable is formed, by means of which not only an unambiguous assignment of the pumping currents I p to an air region is possible but which under certain circumstances can also be performed faster than a method in which periodically switched between a positive and a negative pump voltage U p .
  • the described method which is to be described with reference to FIG. 6, is composed of several sub-steps.
  • the starting point are the characteristic curves 170 and 172, as they have already been plotted in FIG.
  • the representation in FIG. 6 is essentially identical to the representation according to FIG. 5, whereby in turn the pumping current I p is plotted in arbitrary units against the partial pressure of oxygen p in%.
  • a further, third characteristic 173 is shown, which represents a definite measured variable.
  • the third characteristic curve 173 represents a linear combination of the two characteristic curves 170, 172, which, for example, can be predetermined and stored in the control device 112 numerically, analytically, as a table, as a function or in another known manner. In the exemplary embodiment illustrated in FIG. 6, a simple sum of the two characteristic curves 170, 172 is selected as the linear combination.
  • This third characteristic curve 173, which is monotonic or even strictly monotone increasing, is even at least approximately linear in the exemplary embodiment shown.
  • a first pumping current having a first polarity of the pumping voltage U p is first measured at the pumping cell 118, and this first pumping current is temporarily stored as an intermediate value, for example. Subsequently, the polarity of the pumping voltage is reversed and a second pumping current is measured. From the current and stored last measured value is thus obtained directly by summation, the unique measure of the characteristic curve 173. If this polarity reversal, so each of the previous reading can be cached, for example by means of a sample-and-hold method or the like.
  • the gas composition or the oxygen partial pressure p can be directly deduced, for example by comparison with stored curves, tables, analytical functions or the like.
  • a particular advantage of this method is that the effective measuring frequency is twice as high as the switching frequency of the polarity reversal of the pumping voltage U p .
  • each voltage change of the pump voltage U P (thus, for example, an From +500 mV to -500 mV) first a transloading of the capacitance of the sensor element 114 entails.
  • Relevant for this are, in particular, electrical double-layer capacitances as well as the electrical capacitance of the electrodes 120, 126 or similar capacitances.
  • One possibility for further increasing the measurement frequency consists in optimizing the geometry of the sensor element 114, in particular the electrodes 120, 126 and / or electrode cavities 148, 150.
  • a further possibility consists in a reduction of the lead electrolyte resistance.
  • One possibility, which can be used alternatively or additionally to a component optimization, is an electronic acceleration of the transhipment and thus an increased measuring frequency.
  • the polarity reversal between positive and negative pump voltages U p can be done, for example, by means of a periodic or non-periodic square-wave voltage. In this case, a square-wave voltage is applied and the measurement waits for the end of the exponentially decaying transhipment.
  • the voltage or current curve can also be chosen so that the transhipment is completed as quickly as possible. Then, for a short time, a measured current value at a known set voltage or a voltage value at a set current is measured, and then preferably directly poled again in the reverse direction with a suitable course.
  • this can be done by a current-controlled operation, for example, an operation in which the charge flow during polarity reversal a predetermined current profile is impressed.
  • a current-controlled operation for example, an operation in which the charge flow during polarity reversal a predetermined current profile is impressed.
  • this can be done by recharging in a constant current mode (CC, uniform current) instead of a constant voltage mode (CV, uniform voltage).
  • CC constant current mode
  • CV uniform voltage
  • FIG. 8 shows an example of a polarity reversal of the pumping voltage under different conditions.
  • the curve 174 shows the pump voltage curve, which is designed in this case rectangular periodically with the same residence time on positive and negative pumping voltage.
  • the two curves 176 and 178 denote the current response (ie the pumping current) at 3% oxygen (curve 176) or at -6% oxygen (curve 178).
  • the pump current is shown in arbitrary units on the I p axis.
  • the point 180 in FIG. 8 designates the state at which the current profile has settled, and to which a meaningful pump current measurement of the pumping current I p through the pumping cell 118 is thus possible.
  • this time period can be calculated, for example (for example, from the known R and C values) or determined empirically from empirical values.
  • this time period can be calculated, for example (for example, from the known R and C values) or determined empirically from empirical values.
  • the steady state is reached approximately 200 ms after the switchover.
  • a voltage-controlled transhipment with a suitable temporal voltage curve can be used.
  • a particular simple embodiment of such a voltage-controlled switching with a suitable temporal voltage curve is the abovementioned embodiment of an upstream voltage pulse.
  • a voltage pulse having a significantly increased voltage for example, a voltage increased by a factor of 3 may first precede the actual pumping voltage Uo. This is shown by way of example in FIG. Again, curve 174 represents the pump voltage curve, which in turn is plotted here in seconds, as in FIG.
  • this voltage pulse has a duration of approximately 50 ms and an amount of approximately 1.5 V.
  • the current response to the voltage waveform shown is represented by curves 176 (current response at 3% oxygen) and 178 (current response at -6% oxygen), respectively.
  • the pump current is shown in arbitrary units on the I p axis. It can be seen that a steady state 180 is achieved by this sounding as a whole already after 100 ms instead of the 200 ms in FIG. This allows the effective measuring frequency to be doubled again. Other adapted voltage curves may allow even higher speed increases.
  • the method according to the invention has hitherto been explained on a sensor element 114 with two diffusion barriers 146, 138.
  • the method described can in principle be used for different types of sensor elements 114, for example also for a sensor element 114 according to the embodiment in FIG. 1.
  • the diffusion restricting element is attached.
  • a diffusion barrier 138 exists in front of the second electrode 126 formed as an inner potential electrode.
  • a standard broadband lambda probe according to the sensor element 114 in FIG. 1 thus already fulfills the requirements for a sensor element 114 which can be used for the method according to the invention.
  • the first characteristic curve 170 is a characteristic of polarity of the sensor element 114 (this time, for example, according to the exemplary embodiment in FIG. 1), in which the first electrode 120 is used as the expansion electrode, and the second electrode 126 as the mounting electrode.
  • the second characteristic curve 172 again corresponds to a reverse polarity of the pumping voltage U p .
  • the first characteristic curve 170 in the lean air-fuel ratio range 166 increases substantially linearly.
  • the first characteristic curve 170 increases abruptly with decreasing oxygen concentration, that is to say as the fuel gas excess increases, since the diffusion resistance of the protective layer 130, which now acts as a diffusion barrier, is extremely low.
  • this sudden increase is limited by the fact that, starting from a certain pumping current, other limiting factors, such as, for example, subsequent delivery of gases through the diffusion barrier 138, which in theory is not limiting, become effective.
  • the first characteristic 170 goes into saturation.
  • the second characteristic curve 172 behaves in the lean air frequency range 166.
  • This fourth characteristic curve 184 in turn increases substantially strictly monotonically and, for example, in turn, again exhibits an approximately linear course.
  • two measured values are again measured by reversing polarity, for example by a voltage curve according to FIG. 8 or FIG. 9.
  • each measured value can be compared with the previously measured and buffered measured value of the reversed polarity and the smaller of these values can be used in each case.
  • the measured value in the pumping direction in which the electrode with the thick diffusion barrier 138 functions as a removing electrode, whereas in the lean air-number region 166, the opposite direction.
  • thick is meant in general a diffusion barrier with high diffusion resistance, wherein, alternatively or in addition to an increase in thickness, for example also a compaction or pore reduction, a reduction of the cross-section or similar measures can be used in that, under certain circumstances, the first electrode 122, which functions as an external potential electrode, can be equipped with a smaller electrode area, since a thick diffusion barrier is dispensed with in this first electrode 120. Such a reduced electrode area leads to a lower system capacity and thus to an accelerated transhipment Capacities at the Umpolen.
  • the determination of the minimum and the maximum of the two pump current measured values can be carried out in various ways, for example, as described above, by a direct comparison of these two measured values. Alternatively or additionally, however, this determination of the minimum can also take place by means of a plausibility analysis, for example by rejecting measured values which lie above a predetermined plausibility threshold or treating them separately. This can in turn be explained using the example of FIG.
  • the above-described measuring method of the minimum determination can be replaced by an even faster variant, which consists in pumping continuously in a pumping direction until the pumping current signal becomes higher than a predetermined limit value.
  • this threshold is chosen to reflect a pumping current above the highest oxygen value encountered in operation (eg,> 21%), or in the reverse pumping direction beyond the most realistic oxygen demand gas.
  • the limiting factor for the pole reversal frequency is the transhipment of the capacitances connected to the electrodes 120, 126. These may be for example a double-layer capacity, a cavity gas capacity or similar capacities involved.
  • FIG. 10 shows a further exemplary embodiment of a sensor element 114 which can be used in the context of the present invention (for example in a sensor arrangement 110 according to FIG. 1) and which can manage almost completely without recharging the electrodes 120, 126.
  • the sensor element 114 is fundamentally configured similar to the sensor elements 114 shown in FIGS. 2 and 3, so that reference may be made, for example, to the description of the sensor element 114 according to FIG.
  • the first electrode 120 and the second electrode 126 are each formed in several parts and each have first partial electrodes 186 and 188 and second partial electrodes 190 and 192, respectively. These sub-electrodes 186, 188, 190, 192 are each contactable by separate leads 116.
  • the first sub-electrodes 186, 188 can be used for a measurement in a first direction and the second sub-electrodes 190, 192 for a measurement with pump voltage in the reverse direction.
  • a suitable transient sound for example, with a square wave
  • a faster operation can be achieved, since now no reloading of the electrodes 120, 126 and their sub-electrodes is required more.
  • it is alternately pumped, for example, from the first part electrode 186 to the first part electrode 188 and then from the second part electrode 192 to the second part electrode 190.
  • the sensor element 114 according to the exemplary embodiment in FIG. 10 requires four drive lines 116 for contacting the sub-electrodes.
  • this increased complexity can be reduced by using a suitable wiring of the sub-electrodes, in which the sub-electrodes of an electrode are each contacted by a single control line 116, wherein diodes are used in a suitable manner, which ensure that always the "right An example of such a circuit is shown in Figure 11.
  • This circuitry may be included, for example, in the sensor element 114 and / or in the drive device 112, although the former is preferred for reducing the manufacturing outlay.
  • diodes 194 are accommodated in each of the control lines 116. In this case, in the drive line 116 to the first sub-electrode 186 of the first
  • Electrode 120 the diode 194 poled such that the forward direction corresponds to a current to the partial electrode 186.
  • a diode 194 is connected in the reverse direction.
  • a diode 194 is accommodated in the drive line 116, the forward direction of which corresponds to a current direction away from the first partial electrode 188.
  • a diode 194 is added with reverse polarity.
  • the drive lines 116 of the sub-electrodes 186, 190 and 188, 192 of each of the two electrodes 120, 126 are then combined to form two overall lines 196.
  • These diodes 194 cause positive voltages to be pumped only between the electrodes 190 and 192 while blocking the pumping path between the electrodes 186, 188 while preventing their discharge. At negative voltages however, only the pumping path between the sub-electrodes 186, 188 is active, while the pumping path between the sub-electrodes 190, 192 is blocked by the diode circuit.
  • the electrode pairs 186, 188 and 190, 192 thus always retain their polarity, although the polarity on the overall lines 196 constantly changes. This is shown symbolically in FIG. 12, in which the pumping voltage U p is plotted against time. In the periods indicated by 198 in FIG.
  • the pumping through the pumping cell is via the second sub-electrodes 190, 192, whereas in the periods indicated by the reference numeral 200, the pumping is through the first sub-electrodes 186, 188 ,
  • the change in the polarity of a pair of electrodes is always accompanied by the reloading of the capacitance of the electrodes.
  • the diodes 194 may be applied to the sensor element 114 by screen printing, for example, whereby the sensor element 114 has only two contacts of the overall lines 196 for pumping, plus one or two contacts for the heating element 144.
  • the diodes can also be integrated in the sensor housing or in a connector housing, for example in the control device 112. As a result, the sensor element 114 has four contacts, but the sensor has only four connections on the cable (three connections when a heater line and an electrode line are combined).
  • the diodes produced by means of screen printing can be constructed, for example, from doped SiC. Such diodes can be sintered, for example, at temperatures up to about 1400 0 C with the sensor element.
  • Silicon carbide-based diodes can be operated at temperatures of up to 650 ° C.
  • suitable design of the sensor element and appropriate arrangement of the sensor in the exhaust system can be achieved that occur in the rear part of the sensor element during operation no temperatures above 650 0 C. There, screen-mounted diodes should be placed.
  • the diodes 194 In an alternative attachment of the diodes 194 in the cable or connector are much lower demands on the temperature resistance to make. For this purpose, for example, a temperature resistance up to 200 0 C should be sufficient, as it is also met by simple, cheap diodes 194.
  • the diodes 194 can be mounted directly in this plug as the beginning of the sensor feed line.
  • the electrical control can be done by alternating positive and negative pump voltages. The magnitude and duration of these pump voltage pulses may vary, as in the other embodiments of the invention.
  • the device shown in FIG. 11 can be modified by interchanging the two lower sub-electrodes 190, 192, so that pumping takes place between the sub-electrodes 188 and 190 or 186 and 192.
  • an additional line piece without its own external contacting is provided in the electrolyte material above the sub-electrodes 186, 188 and / or below the sub-electrodes 190, 192.
  • FIG. 13 Another variant of the sensor element 114 is shown in FIG.
  • the supply lines can be combined to form two sub-electrodes, in particular a first sub-electrode and a second sub-electrode of different electrodes.
  • these are the drive lines of the first subelectrode 186 of the first electrode 120 and the second subelectrode 192 of the second electrode 126.
  • the electrodes 188 and 190 could also be combined, for example.
  • an electrode remains constantly at the same voltage in each pair of electrodes.
  • the number of sensor connection contacts thus corresponds to that of a standard broadband probe (three electrode connections), whereby one or two connections for the heating element 144 can additionally be added. These connections for the heating element 144 are not shown in FIG.
  • the sensor element 114 in FIG. 10 represents only one of several possibilities for designing the electrodes 120, 126 in each case in whole or in part in several parts.
  • the described sonicates in FIGS. 11 and 13, which are based on the idea of providing diodes in the leads to these sub-electrodes, in order to use different sub-electrodes at different polarities of the pumping voltage, are only some of the possibilities of a sonication of this arrangement.
  • a further variant of the multi-part design of the electrodes 120, 126 according to FIG. 10 would be, for example, designing the electrodes or sub-electrodes 120, 126, 186, 188, 190, 122 (or the further, additional electrodes) next to or behind one another.
  • the sonicating in FIGS. 11 and 13 could be used, or alternatively also alternative sonicating, which makes it possible to use only a few of the partial electrodes for one polarity in each case.

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  • Health & Medical Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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Abstract

La présente invention a pour objet un procédé pour la détermination d'au moins une propriété physique d'un gaz dans au moins un espace de mesure de gaz (132), en particulier pour la détermination d'une concentration en oxygène dans les gaz d'échappement d'un moteur à combustion interne. A cet effet, on utilise un élément de détection (114) qui comprend au moins une première électrode (120), au moins une seconde électrode (126), et au moins un électrolyte solide (122) reliant la première électrode (120) et la seconde électrode (126). La première électrode (120) et la seconde électrode (126) sont en liaison avec l'espace de mesure de gaz (132) de telle sorte qu'elles puissent être alimentées en gaz provenant de l'espace de mesure de gaz (132). Le procédé comprend les étapes suivantes : - au moins une première tension de pompage est établie entre la première électrode (120) et la seconde électrode (126) et au moins un premier courant de pompage est mesuré entre la première électrode (120) et la seconde électrode (126) ; - au moins une seconde tension de pompage est établie entre la première électrode (120) et la seconde électrode (126) et au moins un second courant de pompage est mesuré entre la première électrode (120) et la seconde électrode (126), la seconde tension de pompage présentant une polarité inverse de celle de la première tension de pompage. Au moyen d'au moins une combinaison linéaire d'un maximum du premier courant de pompage et du second courant de pompage avec un minimum du premier courant de pompage et du second courant de pompage, on établit une valeur de mesure claire à partir de laquelle on statue sur la propriété physique.
PCT/EP2008/066688 2007-12-27 2008-12-03 Procédé pour la détermination d'une composition de gaz dans un espace de mesure de gaz, élément de détection et agencement de détection Ceased WO2009083375A1 (fr)

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CN112384795A (zh) * 2018-05-02 2021-02-19 罗伯特·博世有限公司 用于运行用于证明测量气体中的具有结合的氧的测量气体组分的至少一个份额的传感器的方法
CN116242897A (zh) * 2022-12-29 2023-06-09 中国有研科技集团有限公司 一种NOx传感器陶瓷芯片进气口流导的调控方法

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DE102009029415A1 (de) * 2009-09-14 2011-03-24 Robert Bosch Gmbh Sensorelement mit mehrteiliger Diffusionsbarriere
DE102011007447B4 (de) * 2011-04-15 2026-02-05 Robert Bosch Gmbh Verfahren zum Erkennen des Sensortyps eines Sensorelements eines Abgassensors
EP3783355A1 (fr) * 2019-08-21 2021-02-24 Siemens Aktiengesellschaft Procédé et dispositif de capteur pour la détermination de la pression partielle du gaz

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KR20170018328A (ko) * 2014-06-13 2017-02-17 로베르트 보쉬 게엠베하 센서 장치의 작동 방법
KR102383817B1 (ko) 2014-06-13 2022-04-08 로베르트 보쉬 게엠베하 센서 장치의 작동 방법
CN112384795A (zh) * 2018-05-02 2021-02-19 罗伯特·博世有限公司 用于运行用于证明测量气体中的具有结合的氧的测量气体组分的至少一个份额的传感器的方法
CN112384795B (zh) * 2018-05-02 2023-11-21 罗伯特·博世有限公司 用于运行用于证明测量气体中的具有结合的氧的测量气体组分的至少一个份额的传感器的方法
CN116242897A (zh) * 2022-12-29 2023-06-09 中国有研科技集团有限公司 一种NOx传感器陶瓷芯片进气口流导的调控方法

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