EP3887805A1 - Dispositif de détection de gaz, et procédé servant à sa fabrication et à son fonctionnement - Google Patents

Dispositif de détection de gaz, et procédé servant à sa fabrication et à son fonctionnement

Info

Publication number
EP3887805A1
EP3887805A1 EP19808711.6A EP19808711A EP3887805A1 EP 3887805 A1 EP3887805 A1 EP 3887805A1 EP 19808711 A EP19808711 A EP 19808711A EP 3887805 A1 EP3887805 A1 EP 3887805A1
Authority
EP
European Patent Office
Prior art keywords
transducer
receptor
sensor device
gas sensor
pixels
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.)
Pending
Application number
EP19808711.6A
Other languages
German (de)
English (en)
Inventor
Philipp NOLTE
Maria Martinez Prada
Bernd Schumann
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 EP3887805A1 publication Critical patent/EP3887805A1/fr
Pending legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/128—Microapparatus
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
    • G01N27/227—Sensors changing capacitance upon adsorption or absorption of fluid components, e.g. electrolyte-insulator-semiconductor sensors, MOS capacitors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0031—General constructional details of gas analysers, e.g. portable test equipment concerning the detector comprising two or more sensors, e.g. a sensor array
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7793—Sensor comprising plural indicators

Definitions

  • Gas sensor device and method for its manufacture and its operation
  • the present invention relates to a gas sensor device.
  • the present invention also relates to a method for producing the
  • Gas sensor device and a method for operating the gas sensor device.
  • Gas sensors for odor detection are considered electronic
  • Substrate are provided. If different receptor materials are used for this purpose, the manufacturing effort increases with each type of material in thin-film processes, since it must be ensured that each material is applied and structured in the desired position.
  • the gas sensor device has a multi-transducer matrix
  • CCD camera chip charge-coupled device
  • Transducer pixels are read out individually, particularly in analog, amplified or digitized form.
  • the gas sensor device has receptor particles of different ones
  • Receptor types are understood to mean particles which are able to absorb or adsorb gas components.
  • Different types of receptors are understood to mean types of receptor particles which have a different absorption or adsorption behavior than the gas components, or whose physical properties are influenced differently by the same gas component. There are therefore several types of receptor particles, each of which can have different selectivities and sensitivities. These receptor particles can be applied to the transducer pixels in a different mixture.
  • the transducer pixels can be differentiated into first transducer pixels and second transducer pixels.
  • the first transducer pixels each have one or more receptor particles.
  • the second transducer pixels have no receptor particles. There are several in the multi-transducer matrix
  • Receptor particles arranged from each type of receptor are arranged from each type of receptor.
  • the gas sensor device is an integrated solution. It is therefore not necessary to combine many individual sensors with one another, which allows a small space requirement. By covering several transducer pixels with receptor particles of the same receptor type or the same mixture of different receptor types, redundancies result which can be used to increase the quality. If individual transducer pixels cannot be read or do not work, the Gas sensor device still have the desired function. Measured signals can also be averaged via the redundant receptor particle arrangements in order to increase the measurement quality.
  • the receptor particles are randomly distributed across the transducer pixels.
  • a random distribution enables a particularly simple production of the gas sensor device. This is especially true before
  • the gas sensor device preferably has more than 50 transducer pixels, particularly preferably more than 100 transducer pixels. Especially with such a high number of transducer pixels, there is a clear advantage of this integrated solution over an equal number of individual pixels.
  • the number of transducer pixels is at least ten times as large as the number of receptor types. It is particularly preferably at least twenty times as large. In this way it can be produced in such a way that it is highly likely that all types of receptors in the
  • receptor particles can be produced in one, two, three, four or even up to ten or more types of receptors if the number of transducer pixels is large enough to provide redundancies.
  • the multi-transducer matrix is arranged on an array that is set up around each
  • the array is an array, which uses the measurement of electrical, optical or thermal properties as an active principle of sensitivity and selectivity for the detection of one or more variables, in particular an electrical, an optical or a thermal array.
  • An electric one Array can determine the presence of a gas adsorbed on the receptor particles in particular via a resistance measurement, for example via
  • the receptor particles are preferably selected from metal oxide semiconductor particles, graphene and phthalocyanines.
  • Metal oxide semiconductors are preferably selected from the group consisting of tin (IV) oxide, tungsten (VI) oxide, zinc (II) oxide, tin (IV) oxide, copper (II) oxide or mixtures of these materials.
  • An optical array measures the change in the color and / or the brightness of the receptor particles when gas components are absorbed or adsorbed.
  • it can have diodes or a camera chip. If the array is an optical array, then the receptor particles are
  • chemochromic materials preferably selected from chemochromic materials, organometallic networks, quantum dots and materials which are gas-dependent
  • a thermal array can preferably be implemented by bimetallic contacts and the measurement of the thermal voltage.
  • Thermal voltage can be caused by the heat of reaction of a chemical reaction taking place on receptor particles. Therefore, if the array is a thermal array, then the receptor particles are
  • catalytically active particles in particular around metal particles which have at least one of the metals nickel, palladium, platinum, silver or gold.
  • the transducer pixels are designed as troughs. Due to the presence and size of the troughs, the arrangement of the
  • Receptor particles in terms of their position to match the location of the
  • Transducer pixels are aligned. For example, a
  • Access receptor particles if this lies exactly in the middle between two metal fingers of an interdigital electrode.
  • each well is so large that it can receive a receptor particle. This ensures that each transducer pixel has only one type of receptor and that the receptor particle of this type of receptor is precisely positioned.
  • each well is so large that it can accommodate several receptor particles.
  • Receptor particles In this way, different types of receptor particles can also be located in one well, so that different gas selectivities can be realized on a single transducer pixel or one transducer pixel is then sensitive to several gases to be detected.
  • the troughs can also have different sizes.
  • the transducer pixels each have a plurality of depressions, which are then together from the transducer element of the
  • Transducerpixels can be measured. If its array is designed, for example, as an electrical array, then several troughs can be located between the electrode fingers of an interdigital electrode, so that the electrical resistance between the electrode fingers is created by applying several
  • Receptor particles can be reduced.
  • the troughs can be realized by depressions. However, structuring should also be understood as wells that are caused by chemical
  • auxiliary materials such as a structured intermediate layer locally improve the adhesion of receptor particles on the substrate of the transducer pixels.
  • the method for manufacturing the gas sensor device comprises a
  • a multi-transducer matrix with transducer pixels Provide a multi-transducer matrix with transducer pixels.
  • a mixture is applied to these, which contains receptor particles from different receptor types and / or precursors of these receptor particles. These are then converted to sensitive receptor particles on the sensor by heating or another treatment.
  • the mixture is a suspension such as an ink or a paste, which is dropped onto the multitransducer matrix and then dried. This allows a random distribution of the
  • Receptor particles can be reached on the transducer pixels.
  • the method for operating the gas sensor device comprises a calibration step in which the
  • Gas sensor device is exposed to a reference atmosphere.
  • Reference atmosphere contains gas components that are known to interact with the receptor particles of the gas sensor device. If transducer pixels behave in the same way in the reference atmosphere, it is concluded that they are coated with receptor particles of the same receptor type.
  • the calibration step is preferably used to:
  • transducer pixels that are not occupied by at least one receptor particle. These second transducer pixels are then determined to be invalid and are no longer activated or read out in later measuring steps carried out by means of the gas device.
  • transducer pixels can also be determined in the calibration step which do not function properly because, for example, several receptor particles undesirably touch and occupy the same transducer pixel or because a receptor particle does not lie optimally on a transducer pixel. If, however, for the
  • the gas sensor device provides that touching receptor particles of different compositions may be arranged in a group of receptors on a transducer pixel
  • the composition of the receptor particle group is stored on the transducer pixel. This can be done, for example, in a computer with a data memory, the composition then being processed in a computer program.
  • the assignment between transducer pixels and receptor type is also saved for all other transducer pixels.
  • the calibration step can in particular provide for the transducer pixels to be subdivided into a group of selective or sensitive transducer pixels and into a group of nonsensitive or non-selective transducer pixels.
  • the group of selective or sensitive transducer pixels is then preferably used in measurement steps for the analysis of a gas mixture, while the non-sensitive or non-selective ones
  • Transducer pixels can be used for self-diagnosis of the measurement process.
  • the gas sensor device can be trained in a manner that is also used for known nasal devices.
  • the concentration of gas components in reference gases is compared with the sensor response and the sensor response for gas mixtures that correspond to certain human perceptions, such as a good or bad smell, is recorded.
  • the result of the training can be stored in a computer unit using characteristic maps and used to output the measurement result in an HMI (Human Machine Interface) such as a display.
  • HMI Human Machine Interface
  • the gas sensor device is exposed to a measuring atmosphere and the transducer pixels that are not found to be invalid are read out electrically, optically or thermally.
  • the type of reading depends on the array of the multi-transducer matrix. It is further preferred that the transducer pixels are optically and / or thermally modulated in the measuring step.
  • the gas sensor device can be excited in particular by light in a suitable wavelength range in order to achieve a predetermined balance between adsorption and
  • regeneration can take place in a regeneration step in which the gas components are also excited optically or thermally.
  • the wavelength range or temperature are selected so that the gas components are desorbed or oxidized.
  • Figure 1 shows a multi-transducer matrix of a gas sensor device according to an embodiment of the invention.
  • FIG. 2 shows a multi-transducer matrix of a gas sensor device according to another exemplary embodiment of the invention.
  • Figure 3 shows a plan view of a trough of a gas sensor device according to an embodiment of the invention.
  • Figure 4 shows a sectional view of the trough according to Figure 3 along the line IV-IV.
  • Figure 5 shows a plan view of a trough of a gas sensor device according to another embodiment of the invention.
  • a multi-transducer matrix 10a with 16x16 transducer pixels in 20 is shown in FIG. In the present case, these have an electrical array
  • a suspension of receptor particles 30 is dropped onto the transducer matrix 10a consist of five different types of receptors 1 to 5.
  • the receptor types are tin (IV) oxide (receptor type 1), tungsten (VI) oxide (receptor type 2), zinc (II) oxide (receptor type 3), tin (II) oxide (receptor type 4) ) and copper (II) oxide (receptor type 5).
  • the receptor particles 30 are suspended in a volatile organic solvent. After its evaporation, the random arrangement of the receptor particles 30 results, which is shown in FIG. 1.
  • the suspension contains the same types of receptors 1 to 5. Their concentration in the suspension was chosen such that it was to be expected that after evaporation of the solvent every second transducer pixel 20 would be coated with a receptor particle 30. This results in the expected values listed in Table 1 for the assignment of the 256 transducer pixels 20. Furthermore, the random distribution actually achieved is on the
  • the arrangement of the receptor particles 30 in the transducer pixels 20 is shown in Figures 3 and 4.
  • the transducer pixels 20 are designed such that the electrode fingers 41, 42 of the interdigital electrode of each transducer pixel 20 each form a trough 51 which can receive exactly one receptor particle.
  • the receptor particles 30 of all receptor types 1 to 5 have an essentially identical number-average particle size. This design of the wells 51 ensures that each transducer pixel 20 has only one
  • Receptor particles 30 can accommodate a type of receptor.
  • Figure 5 shows the execution of a trough 52 in a second
  • Embodiment of the gas sensor device This well is so large that it can hold several receptor particles 30 of the different receptor types 1 to 5. This means that one transducer pixel 20 can have several
  • the gas sensor device After the gas sensor device has been manufactured, it is first calibrated. For this purpose, it is exposed to a reference atmosphere, the gas components of which are adsorbed on the receptor particles 30 and thus change their electrical resistance. This change in resistance can be measured for each transducer pixel 20 by means of the interdigital electrodes 41, 42. Transducer pixels 20 which have no change in resistance in the reference atmosphere are not covered with receptor particles 30 and are found to be invalid. If an unfavorable positioning of a receptor particle 30 on the
  • Interdigital electrodes 41, 42 gives a measured value that is outside of a
  • the respective transducer pixel 20 is also determined to be invalid. All other transducer pixels 20 are divided into five groups, each with the same change in resistance, which is the five
  • the gas sensor device is then trained using the transducer pixels 20 which are not found to be invalid
  • Transducer pixels 20 of the same group each form the basis for the generation of a redundant measurement signal.
  • the gas sensor device If the gas sensor device has been trained, it is exposed to a measuring atmosphere in a measuring operation and, based on the electrical response of the transducer pixels 20, it is concluded which gas components in the each sample gas are included.
  • the temperature of the transducer pixels 20 can be modulated in each case in order to obtain a plurality of measuring points for the measuring gas at each transducer pixel 20. This takes advantage of the fact that different gases desorb from the receptor particles 30 at different temperatures, which can be measured as an electrical resistance change.
  • the multi-transducer matrix 10a, 10b is then heated to such an extent that any eventual adsorb on the receptor particles 30

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Power Engineering (AREA)
  • Plasma & Fusion (AREA)
  • Nanotechnology (AREA)
  • Combustion & Propulsion (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)

Abstract

L'invention concerne un dispositif de détection de gaz. Celui-ci comporte une matrice à multiples transducteurs (10a) comprenant des pixels transducteurs (20), lesquels comportent des particules (30) de récepteur de différents types de récepteurs (1 - 5). Des premiers pixels transducteurs (20) comportent respectivement une ou plusieurs particules (30) de récepteur et des deuxièmes pixels transducteurs (20) ne comportent respectivement aucune particule (30) de récepteur. La matrice à multiples transducteurs (10a) comporte plusieurs particules (30) de récepteur de chaque type de récepteur. L'invention concerne également un procédé de fabrication du dispositif de détection de gaz, qui comprend les étapes consistant à fournir une matrice (10a) à multiples transducteurs comprenant des pixels transducteurs (20) et à appliquer un mélange sur la matrice (10a) à multiples transducteurs, lequel contient des particules (30) de récepteur de différents types de récepteurs (1 - 5) et/ou leurs précurseurs. L'invention concerne un procédé servant à faire fonctionner le dispositif de détection de gaz, qui comprend une étape d'étalonnage, dans laquelle le dispositif de détection de gaz est exposé à une atmosphère de référence et il est conclu que des pixels transducteurs (20) présentant un comportement identique sont dotés de particules (30) de récepteur des types de récepteurs (1 - 5) identiques.
EP19808711.6A 2018-11-29 2019-11-14 Dispositif de détection de gaz, et procédé servant à sa fabrication et à son fonctionnement Pending EP3887805A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102018220607.4A DE102018220607A1 (de) 2018-11-29 2018-11-29 Gassensorvorrichtung sowie Verfahren zu ihrer Herstellung und zu ihrem Betrieb
PCT/EP2019/081258 WO2020109008A1 (fr) 2018-11-29 2019-11-14 Dispositif de détection de gaz, et procédé servant à sa fabrication et à son fonctionnement

Publications (1)

Publication Number Publication Date
EP3887805A1 true EP3887805A1 (fr) 2021-10-06

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP19808711.6A Pending EP3887805A1 (fr) 2018-11-29 2019-11-14 Dispositif de détection de gaz, et procédé servant à sa fabrication et à son fonctionnement

Country Status (3)

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EP (1) EP3887805A1 (fr)
DE (1) DE102018220607A1 (fr)
WO (1) WO2020109008A1 (fr)

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CN112014439B (zh) * 2020-08-31 2022-05-31 南京信息工程大学 一种基于石墨烯量子点功能化的复合纳米薄膜材料及气敏传感元件

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DE202013005433U1 (de) 2013-06-14 2014-09-15 Sony Corporation Elektronische Nasenvorrichtung
US9857243B2 (en) * 2014-03-18 2018-01-02 Matrix Sensors, Inc. Self-correcting chemical sensor
CN107966478A (zh) * 2016-10-19 2018-04-27 华邦电子股份有限公司 感测器阵列、其制造方法及感测方法
AT519492B1 (de) * 2016-12-22 2019-03-15 Mat Center Leoben Forschung Gmbh Sensoranordnung zur Bestimmung und gegebenenfalls Messung einer Konzentration von mehreren Gasen und Verfahren zur Herstellung einer Sensoranordnung

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Publication number Publication date
DE102018220607A1 (de) 2020-06-04
WO2020109008A1 (fr) 2020-06-04

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