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WO2020138591A1 - Capteur de gaz électrochimique possédant une structure d'électrode de détection double - Google Patents

Capteur de gaz électrochimique possédant une structure d'électrode de détection double Download PDF

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Publication number
WO2020138591A1
WO2020138591A1 PCT/KR2019/003090 KR2019003090W WO2020138591A1 WO 2020138591 A1 WO2020138591 A1 WO 2020138591A1 KR 2019003090 W KR2019003090 W KR 2019003090W WO 2020138591 A1 WO2020138591 A1 WO 2020138591A1
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WO
WIPO (PCT)
Prior art keywords
gas
working electrode
electrode
sensor
gas inlet
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Ceased
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PCT/KR2019/003090
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English (en)
Korean (ko)
Inventor
정병길
하승철
김형태
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Senko Co Ltd
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Senko Co Ltd
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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
    • G01N27/407—Cells and probes with solid electrolytes for investigating or 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
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • 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
    • 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
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/0044—Sulphides, e.g. H2S

Definitions

  • the present invention relates to an electrochemical gas sensor, and more particularly, to an electrochemical gas sensor having a double action electrode.
  • the electrochemical gas sensor when used for continuous gas concentration detection monitoring, the sensor output without the detection gas due to changes in the external environment (temperature, humidity, etc.) may vary from tens of ppb to hundreds of ppb depending on the sensor type. It will change within range. Accordingly, the electrochemical gas sensor has a disadvantage of displaying an abnormal gas concentration value in response to changes in the external environment when measuring the gas concentration at the ppb level, and a separate baseline out correction algorithm must be applied for accurate gas concentration measurement. to be.
  • the baseline output due to changes in the external environment is changed by various factors such as the wet state of the electrode and electrolyte interface and the size of the gas diffusion inlet, and the external environment changes in a state where the sensitivity required by the electrochemical gas sensor is secured. It is a difficult situation to minimize the change of the baseline output. Therefore, it is necessary to develop an electrochemical gas sensor capable of more stably detecting the gas concentration in a change in the external environment in order to measure the gas concentration of the environmental pollutant at the ppb level.
  • the present invention has been proposed to solve such a conventional problem, and the working electrode is composed of a working electrode that causes an oxidation reaction of the sensing gas and a working electrode that represents a baseline out according to changes in the external environment, and thus an electrochemical gas. It is an object of the present invention to provide an electrochemical gas sensor having a dual action electrode structure capable of stably detecting a gas concentration of ppb level by removing external environmental change factors within the sensor itself.
  • an embodiment of an electrochemical gas sensor having a double electrode structure includes a housing in which a first gas inlet and a second gas inlet are formed; A first working electrode disposed below the first gas inlet in the housing and reacting with gas introduced through the first gas inlet; A second working electrode disposed under the second gas inlet in the housing and reacting with gas introduced through the second gas inlet; A filter for removing detection gas disposed between the second gas inlet and the second working electrode, and filtering in which the sensing gas to be sensed flows into the second working electrode; A reference electrode disposed below the first working electrode and the second working electrode; And a counter electrode disposed under the reference electrode.
  • a working electrode supporting member disposed in the housing is further provided, and the first working electrode and the second working electrode are disposed on the working electrode supporting member. Can.
  • the first working electrode and the second working electrode are each formed in a semicircular shape, and the first working electrode and the second working electrode face each other. Can be placed to see.
  • the filter for removing the detection gas is at least one of activated carbon, silica (SiO 2 ), manganese oxide (MnO), PTFE (Polytetrafluoroethylene) powder, and Nafion. It can be made including one.
  • the sensing gas is hydrogen sulfide (H 2 S), and the filter for removing the sensing gas may be activated carbon.
  • the electrochemical gas sensor according to the present invention has a double structure of the working electrode and one of the working electrodes shows a baseline out according to the change in the external environment, so it is possible to remove the external environment change factor within the gas sensor itself, and thus the ppb level It is possible to stably detect the gas concentration of.
  • the electrochemical gas sensor according to the present invention it is possible to secure a more stable operation by excluding errors in the sensor output value caused by changes in the external environment (temperature, humidity, etc.), and stable gas concentration as low as ppb. As it can be detected, it can be stably used in applications such as odor and exhalation gas measurement.
  • FIG. 1 is a view schematically showing a cross section of an embodiment of an electrochemical gas sensor according to the present invention.
  • FIG. 2 is a view of FIG. 1 as viewed from the top, showing the gas inlets formed in the upper housing.
  • FIG. 3 is a view of FIG. 1 viewed from the bottom, and is a view showing sensor pins formed in the lower housing.
  • FIG. 4 to 6 is a view showing the shape of the electrodes provided in one embodiment of the electrochemical gas sensor according to the present invention
  • Figure 4 is a view showing two working electrodes
  • Figure 5 is a view showing a reference electrode
  • Figure 6 is a view showing a corresponding electrode.
  • FIGS. 7 to 10 are views for explaining the effect of the electrochemical gas sensor according to the present invention
  • FIG. 7 is a view showing changes in external temperature and humidity over time
  • FIGS. 8A and 8B are diagrams of FIG. 7 A diagram showing a sensor output measured by an electrochemical gas sensor according to the present invention according to changes in the external environment
  • FIG. 9 is detected based on the output of the first working electrode among the sensor outputs of FIGS. 8A and 8B.
  • FIG. 10 is a diagram in which the detected gas concentration is calculated based on both the sensor outputs of FIGS. 8A and 8B.
  • FIG. 1 is a view schematically showing a cross-section of one embodiment of an electrochemical gas sensor according to the present invention
  • FIG. 2 is a view seen from the top of FIG. 1, showing the gas inlets formed in the upper housing
  • FIG. 3 is a view seen from the bottom of FIG. 1, showing the sensor pins formed in the lower housing.
  • the electrochemical gas sensor 100 includes housings 10A and 10B, a dust filter 11, a working electrode support member 51, and a working electrode (Sensing) Electrode) 31A, 31B, reference electrode support member 52, reference electrode 32, counter electrode support member 53, counter electrode 33, and electrolyte carrier 40 , It has a detection gas removal filter 14 and sensor pins (20A, 20B, 20C, 20D).
  • the housings 10A and 10B are provided with an upper housing 10A and a lower housing 10B, and the lower housing 10B is formed with a receiving portion therein, so that the working electrode support member 51 is formed inside the lower housing 10B, The working electrodes 31A and 31B, the reference electrode supporting member 52, the reference electrode 32, the corresponding electrode supporting member 53, the corresponding electrode 33, the electrolyte support member 40, and the like are accommodated.
  • the lower housing 10B is formed in an open top, and the open upper part of the lower housing 10B is closed by being coupled with the upper housing 10A.
  • the upper housing (10A) and the lower housing (10B) can be coupled by pressing using an ultrasonic welding machine, and the components accommodated inside the housing (10A, 10B) are coupled to be completely sealed so as not to leak to the outside.
  • two gas inlets 12 and 13 through which gas is introduced are formed.
  • the two gas inlets 12 and 13 are divided into a first gas inlet 12 and a second gas inlet 13.
  • the external gas is introduced into the housings 10A and 10B through the gas inlets 12 and 13. All external gases are introduced into the housings 10A and 10B through the first gas inlet 12, and the gas introduced through the first gas inlet 12 reaches the first working electrode 31A.
  • the gas introduced through the second gas inlet 13 is supplied to the second working electrode 31B in a state in which the sensing gas is filtered by the detection gas removal filter 14 disposed below the second gas inlet 13. To reach.
  • the gas inlets 12 and 13 are holes having a diameter of about 1.0 to 5.0 mm, and may be formed by drilling with a drill. Depending on the type of sensing gas to be detected through the gas sensor 100, the sizes of the gas inlets 12 and 13 may be different to secure an efficient sensing capability. For example, when the sensing gas is hydrogen sulfide (H 2 S), when the diameters of the gas inlets 12 and 13 are 3.0 to 4.0 mm, a sensing capability of 600 to 800 nA/ppm can be secured. When the two gas inlets 12 and 13 are the same diameter, effective performance can be expected.
  • H 2 S hydrogen sulfide
  • the dust filter 11 is arranged to cover the two gas inlets 12 and 13 at the top of the upper housing 10A to prevent dust and moisture from entering the housings 10A and 10B from outside.
  • the dust filter 11 is made of a porous PTFE (Polytetrafluoroethylene) having a porosity of about 30 to 50%, and a structure in the form of a mesh of plastic material such as PE (polyethylene) on the surface to increase mechanical strength. It is made of a glued material.
  • the detection gas removal filter 14 is disposed between the second gas inlet 13 and the second working electrode 31B, adsorbs and removes the detection gas from the gas flowing through the second gas inlet 13 to remove the second gas. Filtering is performed so that the sensing gas does not reach the working electrode 31B.
  • the filter for removing the detection gas 14 is made of a material having a large capacity to adsorb the detection gas, among activated carbon, silica (SiO 2 ), manganese oxide (MnO), PTFE (Polytetrafluoroethylene) powder, and Nafion It may include at least one.
  • the sensing gas is a gas to be measured by the electrochemical gas sensor 100 of this embodiment, and may be hydrogen sulfide (H 2 S), carbon monoxide (CO), hydrogen (H 2 ), sulfur dioxide (SO 2 ), etc. Is not limited to the type of sensing gas.
  • the detection gas removal filter 14 may be made of different materials depending on the detection gas. For example, when the sensing gas to be filtered is hydrogen sulfide, activated carbon may be used. At this time, the activated carbon has a surface area of 900 to 1,500 m 2 /g, and a granular or fibrous form may be used.
  • the working electrodes 31A and 31B are electrodes in which an oxidation reaction of the sensing gas occurs, and are disposed below the two gas inlets 12 and 13 and supported by the working electrode supporting member 51.
  • the working electrodes 31A and 31B are formed by being separated into two, and as shown in FIG. 4, each of the two working electrodes 31A and 31B is formed in a semi-circular shape to support the working electrodes so as to face each other. It is arranged on the member 51.
  • the first working electrode 31A is disposed below the first gas inlet 12, and there is no separate filter between the first gas inlet 12 and the first working electrode 31A, All gases flowing through the first gas inlet 12 reach the first working electrode 31A.
  • the second working electrode 31B is disposed below the second gas inlet 13, and by the filter 14 for removing the detection gas disposed between the second gas inlet 13 and the second working electrode 31B.
  • the gas from which the sensing gas is filtered reaches the second working electrode 31B.
  • the working electrode support member 51 may be made of a porous PTFE material having a pore size of 0.3 to 0.5 ⁇ m and a thickness of 100 to 300 ⁇ m, and the working electrodes 31A and 31B may promote the oxidation reaction of the sensing gas. It may be made of a catalyst material such as platinum (Pt), gold (Au), platinum-ruthenium (Pt-Ru), silver (Ag), palladium (Pd), carbon (Carbon).
  • the working electrode support member 51 is coupled to the upper housing 10A by heat sealing.
  • the reference electrode 32 is an electrode that maintains a constant potential to the working electrodes 31A and 31B, and is disposed below the working electrodes 31A and 31B, and is supported by the reference electrode supporting member 52.
  • the reference electrode 32 and the reference electrode support member 52 are formed in a disk shape in which holes are formed in the center portion, as shown in FIG. 5.
  • the electrolyte supported on the electrolyte carrier 40 moves through the holes in the center portion of the reference electrode 32 and the reference electrode support member 52, wherein the holes have a diameter of about 5 to 7 mm.
  • the reference electrode support member 52 may be made of a porous PTFE material. When the diameter of the hole is smaller than 5 mm, the long-term stability of the sensor is greatly reduced.
  • the counter electrode 33 is an electrode that causes a reduction reaction in proportion to the oxidation reaction of the sensing gas at the working electrodes 31A and 31B, and is disposed below the reference electrode 32 and is provided by the counter electrode support member 53. Is supported.
  • the counter electrode 33 and the counter electrode support member 53 are formed in a disk shape with holes formed in the center portion, as shown in FIG. 6.
  • the electrolyte supported on the electrolyte carrier 40 moves through the holes in the center portion of the counter electrode 33 and the counter electrode support member 53, wherein the holes have a diameter of about 5 to 7 mm.
  • the corresponding electrode support member 53 may be made of a porous PTFE material. When the diameter of the hole is smaller than 5 mm, the long-term stability of the sensor is greatly reduced.
  • the electrolyte carrier 40 is accommodated in the receiving portion of the lower housing 10B, and is generally disposed under the corresponding electrode 33.
  • the electrolyte support 40 is to support the electrolyte, and is made of a material having excellent chemical resistance and high absorption rate of the electrolyte, such as boron silicate glass mat and polyester fiber mat.
  • hydrogen ions generated by the oxidation reaction in the working electrodes 31A and 31B are transferred to the corresponding electrode 33 through the electrolyte to cause a reduction reaction. In this way, holes are formed in the central portion of the reference electrode 32 and the corresponding electrode 33 so that hydrogen ions can easily move through the electrolyte.
  • the electrolyte support member 40 on which the electrolyte solution is supported is supplied with the electrolyte solution smoothly to each of the electrodes 31A, 31B, 32, and 33 to maintain an equilibrium state, and the electricity between each electrode 31A, 31B, 32, 33 is maintained. It serves to prevent short circuits.
  • the sensor pins 20A, 20B, 20C, and 20D are installed on the lower portion of the lower housing 10B, as shown in FIG. 3, and transmit electrical signals generated from the respective electrodes 31A, 31B, 32, 33. It is an output terminal.
  • the sensor pins 20A, 20B, 20C, and 20D are applied by applying an epoxy 21 having chemical resistance to prevent corrosion by the electrolyte supported on the electrolyte carrier 40.
  • the sensor pins 20A, 20B, 20C, and 20D are manufactured by processing a metal made of brass and plating the surface with gold.
  • the sensor pins 20A, 20B, 20C, and 20D are electrically connected to the electrodes 31A, 31B, 32, 33 through wires (not shown).
  • the wire is made of precious metal materials such as platinum (Pt), gold (Au), and tantalum (Ta) having a diameter of 0.01 to 0.03 mm, and the wire and sensor pins (20A, 20B, 20C, 20D) are spot welded. ).
  • precious metal materials such as platinum (Pt), gold (Au), and tantalum (Ta) having a diameter of 0.01 to 0.03 mm, and the wire and sensor pins (20A, 20B, 20C, 20D) are spot welded. ).
  • the first sensor pin 20A is electrically connected to the reference electrode 32 to transmit an electrical signal generated from the reference electrode 32 to an external circuit
  • the second sensor pin 20B is the first working electrode 31A And is electrically connected to transmit an electrical signal generated from the first working electrode 31A to an external circuit
  • the third sensor pin 20C is electrically connected to the counter electrode 33 and generated from the counter electrode 33 The electrical signal is transmitted to the external circuit
  • the fourth sensor pin 20D is electrically connected to the second working electrode 31B to transmit the electrical signal generated from the second working electrode 31B to the external circuit.
  • the electrochemical gas sensor 100 described above is connected to the second working electrode 31B through the filter 14 for detecting gas removal disposed between the second gas inlet 13 and the second working electrode 31B. Since the detected gas reaches the filtered gas, the signal output by the second working electrode 31B is a signal from which the output by the sensing gas is excluded, and corresponds to a signal that can indicate a baseline out according to changes in the external environment. That is, changes in the external environment can be measured through the second working electrode 31B.
  • the first working electrode 31A is an output signal by the sensing gas
  • the output signal of the second working electrode 31B is excluded from the output signal of the first working electrode 31A, an error caused by an external environment change Since it can be excluded, it is possible to secure a more stable sensor operation. Therefore, since the gas concentration can be stably detected at a low concentration of ppb, it can be stably used in applications such as odor and exhalation gas measurement.
  • the detection gas was hydrogen sulfide
  • the filter 14 for removing the detection gas used activated carbon and the results measured by the electrochemical gas sensor according to the present invention were shown for about 2 days.
  • FIG. 7 is a view showing changes in external temperature and humidity over time
  • FIGS. 8A and 8B are sensor outputs measured by an electrochemical gas sensor according to the present invention according to changes in the external environment of FIG. 7.
  • FIG. 9 is a diagram illustrating the detection gas concentration based on the output of the first working electrode among the sensor outputs of FIGS. 8A and 8B
  • FIG. 10 is detected based on both the sensor outputs of FIGS. 8A and 8B. It is the figure which calculated the gas concentration.
  • FIG. 7 it can be seen that the temperature and the humidity greatly changed during the measured 2 days, and the outputs output from the two working electrodes 31A and 31B as shown in FIGS. 8A and 8B are also shown. You can see that it changes greatly.
  • the graph shown in FIG. 8A is an output value of the first working electrode 31A, and corresponds to a value output by an oxidation reaction of hydrogen sulfide as a sensing gas.
  • the graph illustrated in FIG. 8B is an output value of the second working electrode 31B, and corresponds to a value output by a change in the external environment.
  • FIG. 9 is a diagram in which the concentration of the detection gas is calculated based on the output value of the first working electrode 31A, and the concentration of the detection gas shown in FIG. 9 corresponds to the concentration of the detection gas when the external environment change is not excluded.
  • do. 10 is a diagram of the output value of the first working electrode 31A calculated as the concentration of the sensing gas excluding the output value of the second working electrode 31B corresponding to a change in the external environment. The concentration corresponds to the concentration of the sensing gas when the external environmental change is excluded. 9 and 10, if the external environment change is not excluded, the concentration of the sensing gas changes significantly according to the external environment change such as temperature and humidity (see FIG.
  • the concentration of the sensing gas is stably measured within about 20 ppb. That is, when the sensing gas is measured using the electrochemical gas sensor according to the present invention, it is possible to stably secure a very low sensing gas concentration of ppb level even in an external environment change.

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Abstract

La présente invention concerne un capteur de gaz électrochimique, et plus précisément un capteur de gaz électrochimique possédant une électrode à double action. Selon un mode de réalisation de la présente invention, le capteur de gaz électrochimique possédant une structure à double électrode comprend : un boîtier dans lequel une première entrée de gaz et une seconde entrée de gaz sont formées ; une première électrode de détection disposée au-dessous de la première entrée de gaz dans le boîtier et réagissant avec le gaz introduit par la première entrée de gaz ; une seconde électrode de détection disposée au-dessous de la seconde entrée de gaz dans le boîtier et réagissant avec le gaz introduit par la seconde entrée de gaz ; un filtre d'élimination de gaz de détection disposé entre la seconde entrée de gaz et la seconde électrode de détection et filtrant l'entrée de gaz de détection à détecter dans la seconde électrode de détection ; une électrode de référence disposée au-dessous de la première électrode de détection et de la seconde électrode de détection ; et une contre-électrode disposée au-dessous de l'électrode de référence.
PCT/KR2019/003090 2018-12-27 2019-03-18 Capteur de gaz électrochimique possédant une structure d'électrode de détection double Ceased WO2020138591A1 (fr)

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KR10-2018-0170394 2018-12-27
KR1020180170394A KR20200081579A (ko) 2018-12-27 2018-12-27 이중 작용 전극 구조의 전기화학식 가스 센서

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KR102434912B1 (ko) 2022-01-24 2022-08-23 주식회사 하이 신경언어장애를 개선하는 방법 및 장치
KR102839774B1 (ko) 2023-03-28 2025-07-29 대구가톨릭대학교산학협력단 상온에서 작동하는 포름알데히드 가스센서 및 측정시스템

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060069677A (ko) * 2004-12-18 2006-06-22 (주)센코 전기화학식 일산화탄소 가스 센서
KR20110012258A (ko) * 2009-07-30 2011-02-09 (주)센코 전기화학 수소 가스 센서
EP2494347B1 (fr) * 2009-10-30 2016-05-25 MSA Technology, LLC Capteurs électrochimiques comprenant des électrodes dotées de barrières de diffusion
JP2016211958A (ja) * 2015-05-08 2016-12-15 新コスモス電機株式会社 電気化学式ガスセンサ
US20170276634A1 (en) * 2016-03-22 2017-09-28 Alphasense Limited Electrochemical gas sensor, filter and methods

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060069677A (ko) * 2004-12-18 2006-06-22 (주)센코 전기화학식 일산화탄소 가스 센서
KR20110012258A (ko) * 2009-07-30 2011-02-09 (주)센코 전기화학 수소 가스 센서
EP2494347B1 (fr) * 2009-10-30 2016-05-25 MSA Technology, LLC Capteurs électrochimiques comprenant des électrodes dotées de barrières de diffusion
JP2016211958A (ja) * 2015-05-08 2016-12-15 新コスモス電機株式会社 電気化学式ガスセンサ
US20170276634A1 (en) * 2016-03-22 2017-09-28 Alphasense Limited Electrochemical gas sensor, filter and methods

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