CN203148883U - Carbon monoxide sensor - Google Patents
Carbon monoxide sensor Download PDFInfo
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- CN203148883U CN203148883U CN 201320014173 CN201320014173U CN203148883U CN 203148883 U CN203148883 U CN 203148883U CN 201320014173 CN201320014173 CN 201320014173 CN 201320014173 U CN201320014173 U CN 201320014173U CN 203148883 U CN203148883 U CN 203148883U
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Abstract
The utility model discloses a carbon monoxide sensor. The carbon monoxide sensor comprises a shell, a working electrode, a counter electrode, a reference electrode and acid electrolyte arranged in the shell, wherein the working electrode, the counter electrode and the referring electrode are contacted with the acid electrolyte; and each of the working electrode, the counter electrode and the referring electrode comprises a waterproof and breathable membrane and a noble metal catalyst layer arranged on the waterproof and breathable membrane. By using a selectivity carbon monoxide electrode as the working electrode of the carbon monoxide sensor, the goal of selectively detecting carbon monoxide is achieved, so that the response time of the sensor for the carbon monoxide is shortened by about 30%; the adsorption layer is not arranged; and the carbon monoxide sensor has the characteristics of simple structure, convenience in installation, quick response and stable and reliable property. The preparation method of the electrode of the carbon monoxide sensor can greatly reduce the consumption of the noble metal and is favorable for lowering the cost.
Description
Technical field
The utility model relates to the gas sensor based on electrochemical principle, relates in particular to a kind of carbon monoxide transducer.
Background technology
Carbon monoxide (CO) gas extensively is present in the daily productive life, and every year, a large amount of CO poisonings all can take place in the worldwide, were commonly called as gas poisoning.Because CO is colorless and odorless gas, be difficult for being discovered by the people, the human and animal is had height toxicity.CO is combined with haemoglobin after entering blood by breathing, forms carbonyl hemoglobin, thereby makes human body anoxia be subjected to major injury.In being the CO of 1600ppm, volume fraction treat will make in 20 minutes the people to feel headache, dizziness, and will be dead after 1 hour.Therefore, it is the important means that prevents that CO poisons that the CO alarm is installed, and the CO sensor is directly determining the performance of whole alarm as the core component of whole alarm.
The method that the detection of CO gas is used always is to adopt electrochemical gas sensor.Mostly present employed electrochemical gas sensor is with noble metal catalyst as active component, noble metal has certain wide spectrum catalytic performance, just can detect at noble metal catalyst generation chemical reaction by gas oxidized or reduction at normal temperatures.Though this has just caused electrochemical gas sensor that certain selectivity is arranged, the phenomenon that selectivity is not high.With regard to the detection of CO gas, the interference of gases such as the hydrogen that regular meeting is subjected to existing in the environment, sulphuric dioxide, sulfuretted hydrogen, alcohol.Be example with alcohol, disturb as the intersection of electrochemical gas sensor alcohol when detecting carbon monoxide of catalyzer with noble metal platinum to reach 110%.
In order to solve above-mentioned interference problem, generally adopt the mode of in gas sensor, adding the physics filtering layer to eliminate the influence of interference gas at present in the industry, commonly used is the interference of eliminating gases such as alcohol by the suction-operated of activated charcoal.But there are three defectives in this method: the one, because the influence of factors such as gas molecule polarity and size makes activated charcoal can not eliminate the influence of common interference gas fully; The 2nd, any adsorbent has saturated extent of adsorption, even without the adsorbance that reaches capacity, adsorption area available on the adsorbent also can have certain influence to eliminating effects of jamming, this has just determined that the influence at whole electrochemical sensor interference gas in the serviceable life process is not changeless, can cause and detect inaccurate phenomenon; The 3rd, add gas after the physics filtering layer and before arriving detecting unit will be have earlier so just prolonged gas by the physical filtering layer and arrive path that detecting unit need pass through and required time, caused the prolongation of sensor to gas response time, be example with city company 7 series sensor, added the response time of the 7E/F carbon monoxide transducer of physical filtering layer and grown about 20% than the response time of the 7E series of no filtering layer.
The utility model content
The technical problems to be solved in the utility model is, at the above-mentioned defective of prior art, provides a kind of selectivity that realizes to detect the carbon monoxide transducer of carbon monoxide.
The technical scheme that its technical matters that solves the utility model adopts is: a kind of carbon monoxide transducer is provided, comprise housing, be arranged at working electrode in the described housing, to electrode, contrast electrode and acidic electrolysis bath, described working electrode, electrode and contrast electrode are all contacted with acidic electrolysis bath, described working electrode, electrode and contrast electrode are included waterproof ventilated membrane and be located at noble metal catalyst layer on the described waterproof ventilated membrane.
Described working electrode is selectivity carbon monoxide electrode.
Described housing comprises base and is covered on lid on it, described working electrode, electrode, contrast electrode and acidic electrolysis bath all is contained between described base and the lid; Be connected with corresponding described working electrode respectively on the described base, to the contact conductor of electrode and contrast electrode; Described electrode, contrast electrode and working electrode below are respectively equipped with electrode diaphragm, described electrode, contrast electrode are connected with described corresponding contact conductor by corresponding electrode diaphragm with working electrode.
Also be provided with pole cup between described base and the lid, described acidic electrolysis bath is loaded in the described pole cup; Described to electrode, contrast electrode and working electrode respectively with its noble metal catalyst layer down, be set in turn on the described pole cup by back up pad.
Described lid is provided with the gas regulation film enters described housing with adjusting gas content; Be provided with O type packing ring between described working electrode and the loam cake.
Described acidic electrolysis bath is the acidic electrolysis bath of sulfuric acid or phosphoric acid, and wherein the content of sulfuric acid or phosphoric acid is 10 ~ 90%.
Described waterproof ventilated membrane is polytetrafluoroethylene (PTFE), gathered one or more the combination in fluorothene (PVDF), teflon/hexafluoroethylene multipolymer (PFEP), teflon/perfluor third vinyl ether copolymers (PFA), tygon/TFE copolymer (PFTFE), silicon rubber (SR) and the silicon fluoride rubber (FSR); In the described noble metal catalyst layer, bullion content is 10 ~ 90wt%, and noble metal is as active component, and it is in platinum (Pt), ruthenium (Ru), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh) and the silver (Ag) one or more.
In the described noble metal catalyst layer, described noble metal is supported on the conductive carbon particle, and described conductive carbon is carbon black, carbon nano-tube or activated charcoal.
Described working electrode, identical or different to the active component in the noble metal catalyst layer of electrode and contrast electrode.
Carbon monoxide transducer of the present utility model, by using selectivity carbon monoxide electrode to be working electrode, realized that selectivity detects the purpose of carbon monoxide, with the response time shortening about 30% of described sensor to carbon monoxide, need not to arrange adsorbed layer, characteristics such as have simple in structure, easy for installation, response rapidly and stable and reliable for performance; The preparation method of electrode of the present utility model can greatly reduce the consumption of noble metal, favourable reducing cost.
Description of drawings
The utility model is described in further detail below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the decomposition texture synoptic diagram of the utility model carbon monoxide transducer;
Fig. 2 is the unitized construction synoptic diagram of carbon monoxide transducer shown in Figure 1;
Fig. 3 is the synoptic diagram when adopting bitubular roll squeezer to prepare electrode in the utility model;
Carbon monoxide transducer was to the response curve of 500PPM carbon monoxide and 500PPM alcohol gas when Fig. 4 was to use the working electrode of broad spectrum activity noble metal catalyst preparation;
Carbon monoxide transducer was to the response curve of 500PPM carbon monoxide and 500PPM alcohol gas when Fig. 5 was to use selectivity carbon monoxide electrode to be working electrode.
Embodiment
Understand for technical characterictic of the present utility model, purpose and effect being had more clearly, now contrast accompanying drawing and describe embodiment of the present utility model in detail.
As shown in Figures 1 and 2, carbon monoxide transducer of the present utility model, comprise housing 10, be arranged at working electrode 20 in the housing 10, contrast electrode 30, to electrode 40 and acidic electrolysis bath (not shown), working electrode 20, contrast electrode 30 and electrode 40 is all contacted with acidic electrolysis bath.
Also be provided with pole cup 50 between base 11 and the lid 12, be used for storing acidic electrolysis bath, and give because the acidic electrolysis bath volume change that temperature variation causes provides certain space, prevent acidic electrolysis bath expansion seepage.Pole cup 50 is provided with through hole 51 for the injection of acidic electrolysis baths wherein, base 11 and the lid 12 corresponding hole portions 110,120 that can be communicated with through hole 51 that are provided with.
Working electrode 20, to electrode 40 and contrast electrode 30 core as whole sensor, be used for redox reaction takes place, the carbon monoxide gas body burden in the environment is directly changed into the signal that can detect.This working electrode 20, electrode 40 and contrast electrode 30 are included waterproof ventilated membrane and be located at noble metal catalyst layer on the waterproof ventilated membrane.Be set in turn in pole cup 50 tops by back up pad 60 to electrode 40, contrast electrode 30 and working electrode 20 respectively with its noble metal catalyst layer down.Wherein, electrode 40, contrast electrode 30 and working electrode 20 belows are respectively equipped with electrode diaphragm 42,32,22, electrode 40, contrast electrode 30 and working electrode 20 are passed through corresponding electrode diaphragm 42,32,22 be connected with corresponding contact conductor.Further be provided with O type packing ring 70 between working electrode 20 and the loam cake 12, can prevent direct contact the between working electrode 20 and the loam cake 12, can also provide certain gas collection zone for the gases (as carbon monoxide) that enter in the housing 10.
Described waterproof ventilated membrane is polytetrafluoroethylene (PTFE), gathered one or more the combination in fluorothene (PVDF), teflon/hexafluoroethylene multipolymer (PFEP), teflon/perfluor third vinyl ether copolymers (PFA), tygon/TFE copolymer (PFTFE), silicon rubber (SR) and the silicon fluoride rubber (FSR).In the noble metal catalyst layer, noble metal is as active component, content is 10 ~ 90%, and noble metal can be one or more in platinum (Pt), ruthenium (Ru), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh) and the silver (Ag), namely can be the alloy that simple substance also can be multiple noble metal.Can be identical or different to the active component (being noble metal) in the noble metal catalyst layer of electrode 40, contrast electrode 30 and working electrode 20.In order to realize optionally detecting carbon monoxide, working electrode 20, to adopting different noble metals in the noble metal catalyst layer of electrode 40 and contrast electrode 30, wherein working electrode 20 is selectivity carbon monoxide electrode, noble metal in its noble metal catalyst layer adopts one or more in platinum (Pt), ruthenium (Ru), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh) and the silver (Ag), and wherein the content of rhodium is 10 ~ 90%; Be the porous gas diffusive electrode of broad spectrum activity to electrode 40 with contrast electrode 30, noble metal in its noble metal catalyst layer adopts one or more in platinum (Pt), ruthenium (Ru), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh) and the silver (Ag) equally, and wherein the content of platinum is 10 ~ 90%.
In the noble metal catalyst, noble metal can directly be incorporated into wherein by its powder morphology, also can support on the conductive carbon particle (carbon carrier) by its powder morphology, form carbon supported noble metal catalyst, the two can reach identical catalytic performance, the preferred mode that adopts noble metal powder to support on the conductive carbon particle forms the noble metal catalyst layer, this mode can be so that noble metal powder be distributed on the active surface of whole conductive carbon particle equably, thereby can greatly reduce the consumption of noble metal powder, favourable reducing cost.Described conductive carbon particle adopts carbon black, carbon nano-tube or activated charcoal etc. to have the material of high-specific surface area.
Described acidic electrolysis bath mainly plays protolysis, can be the acidic electrolysis bath that has the specified moisture value under specified temp of sulfuric acid or phosphoric acid etc., and wherein the content of sulfuric acid or phosphoric acid is 10 ~ 90%.In the present embodiment, acidic electrolysis bath dress exists in the pole cup 50 and places in the housing 10.
With reference to shown in Figure 1, during the utility model assembling, earlier three pins 21,41,31 on base 11 burn-on respectively the working electrode lead-in wire, to contact conductor and contrast electrode lead-in wire, pole cup 50 is placed on the base 11 by assigned direction, place back up pad 60 again; One electrode diaphragm 42 is placed on the back up pad 60, will be connected on this electrode diaphragm 42 contact conductor, will be to electrode 40 with its noble metal catalyst layer towards contact conductor being placed on this electrode diaphragm 42; Then on to electrode 40, place an electrode diaphragm 32 again, the contrast electrode lead-in wire is connected on this electrode diaphragm 32, contrast electrode 30 is placed on this electrode diaphragm 32 towards the contrast electrode lead-in wire with its precious metal catalyst layer; In kind place working electrode 20 again in contrast electrode 30 tops, thereby electrode 40, contrast electrode 30 and working electrode 20 are placed on back up pad 60 tops successively; Place O type packing ring 70 at working electrode 20 at last, cover lid 12, the hole portion 110 of base 11 and lid 12,120 with the through hole 51 of pole cup 50 over against being communicated with, acidic electrolysis bath by the hole that is communicated with injection certain volume in the pole cup 50, adopt hot melting mode again with through hole 51 or reach hole portion 110,120 to seal, thereby be assembled into whole carbon monoxide transducer.
Working electrode described in the utility model 20, all can adopt following method to make to electrode 40 and contrast electrode 30, said method comprising the steps of:
(1), place an amount of spreading agent fully to disperse in the noble metal catalyst powder, obtain suspension.
Spreading agent comprises isopropyl alcohol, also can comprise one or more combinations in water, methyl alcohol, the ethanol equal solvent, and wherein the content of isopropyl alcohol is greater than 50%, and the content of water is less than 50%.The mass ratio of spreading agent and noble metal catalyst is 1:15 ~ 1:50.Process for dispersing can be the conventional process for dispersing that divides such as mechanical raking, sonic oscillation, and the temperature of dispersion is room temperature.
(2), add an amount of hydrophober in the suspension, fully mix, obtain mixed liquor.
It is 20 ~ 60wt% that hydrophober can be PTFE content, and the PTFE particle diameter is 0.02 ~ 1 micron PTFE emulsion, the PTFE30 emulsion that typically has E.I.Du Pont Company to produce.In the gained mixed liquor, the mass ratio of PTFE and noble metal catalyst is 1:1 ~ 1:10.
(3), mixed liquor is stirred the bulk adherent coatings of formation down in heating.
Mixed liquor is reunited adding under the thermal agitation, and the bulk coating of the catalyzer/hydrophober that is formed for being coated with is described adherent coatings.Heating-up temperature is 80 ~ 130 ℃, and the time is 5 ~ 20 minutes.
(4), adherent coatings is evenly coated on the hydrophobic carbon paper.
Wherein, the hydrophobic carbon paper mainly adopts carbon fibre or graphitized fibre to make, and it is 50 ~ 200g/m that the hydrophobic carbon paper can adopt weight per unit area
2, bulk density is 0.2 ~ 0.6g/cm
3Porosity is 20 ~ 80%, interface resistance is less than 1 ohmcm, aspect resistance is less than the carbon paper of 0.1 ohmcm, hydrophober content is 5% ~ 85% in this hydrophobic carbon paper, and hydrophober can be in the fluorinated polymers such as multipolymer of teflon, Kynoar, PEP one or more combination.Coating method can adopt the mode of blade coating, and the thickness of control adherent coatings is 0.2 ~ 1mm, and catalyst consumption is 0.5 ~ 3mg on every square centimeter of carbon paper.
(5), utilizing the adherent coatings that is coated with on the hydrophobic carbon paper that the hydrophobic carbon paper is suppressed with waterproof ventilated membrane bonds, makes electrode.
The hydrophobic carbon paper is coated with one of adherent coatings faces down and be placed on the waterproof ventilated membrane, and method is bonded together the two by adopting roll-in or roll etc., the pressure that applies is 1 ~ 15N/cm
2, the time of exerting pressure is 2 ~ 10 minutes.
Also comprise (6), with the thermal treatment under vacuum state of gained electrode, to remove the impurity that hydrophober is brought.In this step, can adopt vacuum drying oven to carry out, heating-up temperature is 50 ~ 180 ℃, and be 0.5 ~ 3 hour heat time heating time.
By the electrode that said method makes, its noble metal catalyst layer is smooth evenly, free from flaw, bonding firmly and respond goodly, can be directly used in the assembling carbon monoxide transducer.
As shown in Figure 3, can adopt bitubular roll squeezer 100 to prepare electrode of the present utility model, wherein the gap between roller 101 and the roller 102 is adjustable, so that handling the electrode support 120(of different-thickness is the hydrophobic carbon paper), after in the gap, putting into electrode, roll squeezer roller 101,103 controls of 102 torsional moment are at 0 ~ 4NM, and adherent coatings layer 130 directly contact with roller 101, but passes through waterproof ventilated membrane 140 between roller 101,102.The hydrophobic carbon paper 120 that will be coated with adherent coatings 130 by roller 101,102 roll-in is bonded together with waterproof ventilated membrane 140 compactings.
Prepare the porous gas diffusive electrode that uses in the carbon monoxide transducer by the following method:
The noble metal catalyst powder that the platinum content that 135mg is made by the electronation mode is 12%, carbon carrier is VULACAN XC-72 carbon black joins in the 5ml aqueous isopropanol, and mechanical raking was disperseed in 30 minutes; Add the PTFE30 emulsion that 300 microlitre E.I.Du Pont Company produce then, mechanical raking 30 minutes; The above-mentioned potpourri that stirs is reunited under 100 ℃, when the solid-liquid two-phase obviously separates in the potpourri, go the supernatant liquid part namely to get bulk adherent coatings.
Be 33% carbon paper with hydrophober content, cut into the disk that diameter is 18mm, the bulk adherent coatings of gained is applied on 50 described carbon paper disks uniformly.
With facing down of scribbling bulk adherent coatings, when adherent coatings is still moistening, the PTFE waterproof ventilated membrane of itself and diameter 25mm is bondd, with running roller at 4N/cm
2Roll-in is 3 minutes under the pressure, namely gets electrode.
50 plate electrodes of above-mentioned preparation are put into vacuum drying oven,, take out cooling and namely get galvanochemistry carbon monoxide transducer broad spectrum activity electrode after 30 minutes 150 ℃ of following thermal treatments.
The preparation method of selectivity carbon monoxide electrode is same as described above, just noble metal platinum is changed into the Noble Metal Rhodium of same amount.
The test of gas response performance:
Comparative example
The carbon monoxide transducer of employing structure shown in Fig. 1 is used for the test of gas response performance.Test condition is at ambient temperature, and operation steps: import cleaned air earlier, import 500PPM alcohol gas and 500PPM CO gas more successively respectively, (GAMRY reference600) carries out the test of gas response performance with electrochemical workstation.
Test findings is seen shown in Figure 4, Fig. 4 is the response condition when adopting the working electrode of broad spectrum activity noble metal catalyst preparation, as seen from Figure 4 when importing cleaned air the signal of sensor close to 0, the situation of change of sensor response signal is about 93uA when importing the 500PPM alcohol gas, and the changing value of the response signal of sensor is 82uA when importing the 500PPM CO gas, and the response time is 15 seconds.Therefore ethanol can have a strong impact on the detection of CO gas as seen from Figure 4, the intersection of carbon monoxide is disturbed can reach 110%.
Embodiment
Still adopt the carbon monoxide transducer of structure shown in Figure 1, working electrode adopts selectivity carbon monoxide electrode, the same comparative example of method of testing, test result such as Fig. 5, as seen from Figure 5 when using selectivity carbon monoxide electrode when working electrode, the response signal changing value of sensor is zero substantially when importing the 500PPM alcohol gas, the changing value of sensor response is 83uA when importing the 500PPM CO gas, response time is 14 seconds, as seen from Figure 5 when using selectivity carbon monoxide electrode, it is 0 that ethanol disturbs the intersection of carbon monoxide, and corresponding sensor has good selectivity to carbon monoxide.
Claims (7)
1. carbon monoxide transducer, it is characterized in that, comprise housing, be arranged at working electrode in the described housing, to electrode, contrast electrode and acidic electrolysis bath, described working electrode, electrode and contrast electrode are all contacted with acidic electrolysis bath, described working electrode, electrode and contrast electrode are included waterproof ventilated membrane and be located at noble metal catalyst layer on the described waterproof ventilated membrane.
2. carbon monoxide transducer according to claim 1 is characterized in that, described working electrode is selectivity carbon monoxide electrode.
3. according to each described carbon monoxide transducer of claim 1-2, it is characterized in that, described housing comprises base and is covered on lid on it, described working electrode, electrode, contrast electrode and acidic electrolysis bath all is contained between described base and the lid; Be connected with corresponding described working electrode respectively on the described base, to the contact conductor of electrode and contrast electrode; Described electrode, contrast electrode and working electrode below are respectively equipped with electrode diaphragm, described electrode, contrast electrode are connected with described corresponding contact conductor by corresponding electrode diaphragm with working electrode.
4. carbon monoxide transducer according to claim 3 is characterized in that, also is provided with pole cup between described base and the lid, and described acidic electrolysis bath is loaded in the described pole cup; Described to electrode, contrast electrode and working electrode respectively with its noble metal catalyst layer down, be set in turn on the described pole cup by back up pad.
5. carbon monoxide transducer according to claim 4 is characterized in that, described lid is provided with the gas regulation film enters described housing with adjusting gas content; Be provided with O type packing ring between described working electrode and the loam cake.
6. carbon monoxide transducer according to claim 1 is characterized in that, described acidic electrolysis bath is the acidic electrolysis bath of sulfuric acid or phosphoric acid.
7. carbon monoxide transducer according to claim 1 is characterized in that, in the described noble metal catalyst layer, described noble metal is supported on the conductive carbon particle, and described conductive carbon is carbon black, carbon nano-tube or activated charcoal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320014173 CN203148883U (en) | 2013-01-11 | 2013-01-11 | Carbon monoxide sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320014173 CN203148883U (en) | 2013-01-11 | 2013-01-11 | Carbon monoxide sensor |
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| CN203148883U true CN203148883U (en) | 2013-08-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926277A (en) * | 2013-01-11 | 2014-07-16 | 深圳市深安旭传感技术有限公司 | Carbon monoxide sensor and carbon monoxide sensor electrode production method |
| CN105242006A (en) * | 2015-09-17 | 2016-01-13 | 浙江工商大学 | Detection apparatus for carbon monoxide in laboratory environment and detection method |
| CN107817212A (en) * | 2017-10-31 | 2018-03-20 | 中国航空综合技术研究所 | A kind of micro- liquid film ion concentration sensor |
| CN114577866A (en) * | 2022-01-27 | 2022-06-03 | 广州奥松电子股份有限公司 | Gas sensor |
| CN114594143A (en) * | 2022-01-26 | 2022-06-07 | 广州奥松电子股份有限公司 | Inner core of gas sensor module and sensor module |
-
2013
- 2013-01-11 CN CN 201320014173 patent/CN203148883U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926277A (en) * | 2013-01-11 | 2014-07-16 | 深圳市深安旭传感技术有限公司 | Carbon monoxide sensor and carbon monoxide sensor electrode production method |
| CN103926277B (en) * | 2013-01-11 | 2017-02-15 | 深圳市深安旭传感技术有限公司 | Carbon monoxide sensor and carbon monoxide sensor electrode production method |
| CN105242006A (en) * | 2015-09-17 | 2016-01-13 | 浙江工商大学 | Detection apparatus for carbon monoxide in laboratory environment and detection method |
| CN107817212A (en) * | 2017-10-31 | 2018-03-20 | 中国航空综合技术研究所 | A kind of micro- liquid film ion concentration sensor |
| CN107817212B (en) * | 2017-10-31 | 2019-10-29 | 中国航空综合技术研究所 | A kind of micro- liquid film ion concentration sensor |
| CN114594143A (en) * | 2022-01-26 | 2022-06-07 | 广州奥松电子股份有限公司 | Inner core of gas sensor module and sensor module |
| CN114577866A (en) * | 2022-01-27 | 2022-06-03 | 广州奥松电子股份有限公司 | Gas sensor |
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Granted publication date: 20130821 Termination date: 20180111 |
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| CF01 | Termination of patent right due to non-payment of annual fee |