CN101435790B - Method for preparing multiple-electrode electrochemical gas sensor - Google Patents
Method for preparing multiple-electrode electrochemical gas sensor Download PDFInfo
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- CN101435790B CN101435790B CN2008100516467A CN200810051646A CN101435790B CN 101435790 B CN101435790 B CN 101435790B CN 2008100516467 A CN2008100516467 A CN 2008100516467A CN 200810051646 A CN200810051646 A CN 200810051646A CN 101435790 B CN101435790 B CN 101435790B
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Abstract
The invention belongs to a method for producing a multi-electrode electrochemical gas sensor, which consists of two working electrodes, two auxiliary electrodes and a reference electrode, wherein the two working electrodes are a platinum air electrode and a gold air electrode respectively, and the reference electrode and the auxiliary electrodes are all platinum air electrodes. The assembly of the sensor is as follows: the electrodes adopt laminated placement and have a sandwich structure and the integrated gold and platinum working electrodes, the reference electrode and the two auxiliary electrodes are arranged from the top down respectively. When the sensor tests mixed gas of carbon monoxide and hydrogen sulfide, a total response signal of the two gas is generated on the platinum working electrode, and a response signal of hydrogen sulfide gas is generated on the gold working electrode, thus the response signals of the thereby simplifying a test method and also greatly reducing actual application cost.
Description
Technical field
The present invention is a kind of preparation method of multiple-electrode electrochemical gas sensor.
Background technology
Electrochemical gas sensor has that the detected gas kind is many, and concentration range is wide, and volume is little; Low in energy consumption, can be used for advantages such as field monitoring, therefore; This sensor is widely used at industrial or agricultural monitoring, detection range; But, therefore there is in the actual monitoring process cross interference problem of gas with various because the base attribute of multiple poison gas is consistent.Especially in industries such as petrochemical industry, smelting iron and steels; The phenomenon that carbon monoxide and sulfuretted hydrogen occur and deposit through regular meeting, and have the problem of cross interference in the three-electrode electro Chemical carbon monoxide that industrial transmitter adopts, these hydrogen sulfide gas sensor practical application, promptly all there is response signal in carbon monoxide transducer to carbon monoxide, hydrogen sulfide gas; Also all there is response signal in hydrogen sulfide sensor to carbon monoxide, sulfuretted hydrogen simultaneously; Therefore when two kinds of gas coexistences, the bigger error of the actual test signal existence of sensor, and during the actual installation monitoring instrument; Need two cover sensor unit, increased the O&M cost.
The traditional electrical chemical sensor adopts two electrodes or three-electrode structure design basically.Chinese patent CN2456165 discloses a kind of " galvanochemistry carbon monoxide transducer "; This sensor is liquid chamber in a housing; Place bottom electrode sheet and following induction electrode, intermediate insulation separation layer, last induction electrode and the pole piece that powers on, outer cover on it; Following induction electrode upper surface scribbles catalyst film conduct counter electrode down, and last induction electrode lower surface scribbles catalyst film as last counter electrode, and the bottom electrode sheet has the liquid permeability hole; The pole piece that powers on has air admission hole, is the gas filtration chamber in the outer cover.Chinese patent 01252229.5 discloses a kind of " solid polymer electrolyte carbon monoxide transducer "; It mainly is made up of sensor chip, ventilative dividing plate, spilehole, appearance air chamber, sensor outer housing; Wherein sensor chip be with solid polymer as electrolyte, with noble metal powder with the bonding waterproof catalyst film of bonding agent as working electrode, auxiliary electrode, contrast electrode and solid polymer dielectric film and electrode through the sinter integrator.These Design of Sensor all adopt two electrodes and three electrode design, can only measure single gas.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of multiple-electrode electrochemical gas sensor.
Sensor of the present invention utilizes the ultimate principle of galvanochemistry CONTROLLED POTENTIAL electrolysis, through the operate outside circuit; With the contrast electrode is benchmark; Working electrode is constant under selected current potential; Make tested gas on working electrode, produce oxidation or reduction reaction, on to electrode, produce corresponding electrochemical reaction, and in the loop, produce oxidation or reduction current.This electric current is directly proportional with gas concentration, so can be quantitative.
Sensor of the present invention adopts two working electrodes, two auxiliary electrodes and a slice contrast electrode to form; Wherein two working electrodes adopt platinum air electrode and golden air electrode respectively; Reference and auxiliary electrode all adopt the platinum air electrode; Five plate electrodes adopt the lamination placement to be sandwiched type structure, from top to bottom are respectively gold, platinum one working electrode, contrast electrode, two auxiliary electrodes.
The preparation process of electrode is following: at first the film to preliminary election cleans, dries, and the electrode film thickness of selection is at the 0.05-0.2 millimeter, and smooth being fixed on the screen printing apparatus; Printing stencil is fixed on the film upper surface that is printed; Preparation printed catalyst slurry; According to mass ratio 1-3: 9-7 weighing bonding agent and catalyzer with bonding agent and catalyst mix, are uniformly dispersed through ultrasonic disperser; Scattered slurry is printed on the teflon waterproof and breathable diaphragm through knife coating, and the carrying capacity of catalyzer is controlled at 2 milligrams of-20 milligrams/cm
2, the area of electrode is at 0.5-5cm
2, working electrode is made up of two semicircular electrodes in the shape of electrode, and a side semicircular electrode is the Au catalyst electrode, and a side semicircular electrode is the platinum catalyst electrode, and auxiliary electrode and contrast electrode are the annular membrane structure.Afterwards, electrode is cleaned once more, the electrode after cleaning was carried out in 100-240 ℃ of temperature conditions sintering 30-60 minute under the high pure nitrogen protection.Working electrode, contrast electrode are consistent with two auxiliary electrode preparation technologies.
It is only responsive to hydrogen sulfide gas that electrode is made in wherein semi-circular metal working; And semicircle platinum working electrode all has response signal to hydrogen sulfide and CO gas; When this sensor test carbon monoxide and hydrogen sulfide mist, be the overall response signal of two kinds of mists on the platinum working electrode like this, and metal working to do on the electrode be the response signal of hydrogen sulfide gas; Calculate by difference like this; Just can on this sensor, obtain the response signal of two kinds of gases synchronously, not only simplify method of testing, also greatly reduce the practical application cost.
Embodiment
Embodiment 1: prepares 5 electrode electro Chemical sensors, the film of preliminary election cleaned, dries, and smooth being fixed on the screen printing apparatus; Printing stencil is fixed on the film upper surface that is printed; According to mass ratio is 2: 8 ratio weighing bonding agents and catalyzer; Catalyzer is mixed with bonding agent, be uniformly dispersed through ultrasonic disperser; Scattered slurry is printed on the teflon waterproof and breathable diaphragm through knife coating, and wherein the working electrode film thickness is 0.05 millimeter, and catalyzer is made up of two semicircular electrodes on the film, and wherein a side is the platinum working electrode, 2 milligrams/cm of catalyst loading
2, an other side is that electrode is made in metal working, 2 milligrams/cm of catalyst loading
2, electrode area is 1cm
2, contrast electrode and two auxiliary electrode electrode areas are 2cm
2, catalyst loading is 2 milligrams/cm
2Electrode is cleaned once more; Electrode after cleaning was carried out sintering 60 minutes in 100 ℃ of temperature conditions under the high pure nitrogen protection, the assembling of sensor, the electrodes use lamination is placed and is sandwiched type structure; From top to bottom be respectively gold, platinum one working electrode, contrast electrode, two auxiliary electrodes.
Embodiment 2: prepare 5 electrode electro Chemical sensors, preparation process is with embodiment 1, and wherein the mass ratio of bonding agent and catalyzer is 1: 9; The working electrode film thickness is 0.2 millimeter; Catalyzer is made up of two semicircular electrodes on the film, and wherein a side is the platinum working electrode, 20 milligrams/cm of catalyst loading
2, an other side is that electrode is made in metal working, 20 milligrams/cm of catalyst loading
2, electrode area is 2cm
2, contrast electrode and two auxiliary electrode electrode areas are 4cm
2, catalyst loading is 20 milligrams/cm
2, electrode is cleaned once more, the electrode after cleaning was carried out sintering 40 minutes in 180 ℃ of temperature conditions under the high pure nitrogen protection.
Embodiment 3: prepare 5 electrode electro Chemical sensors, preparation process is with embodiment 1, and wherein the mass ratio of bonding agent and catalyzer is 3: 7; The working electrode film thickness is 0.1 millimeter; Catalyzer is made up of two semicircular electrodes on the film, and wherein a side is the platinum working electrode, 10 milligrams/cm of catalyst loading
2, an other side is that electrode is made in metal working, 10 milligrams/cm of catalyst loading
2, electrode area is 2cm
2, contrast electrode and two auxiliary electrode electrode areas are 4cm
2, catalyst loading is 10 milligrams/cm
2, electrode is cleaned once more, the electrode after cleaning was carried out sintering 30 minutes in 240 ℃ of temperature conditions under the high pure nitrogen protection.
Claims (3)
1. the preparation method of a multiple-electrode electrochemical gas sensor is characterized in that adopting working electrode, two auxiliary electrodes and a slice contrast electrode to form, and working electrode adopts gold, platinum one working electrode, and reference and auxiliary electrode all adopt the platinum air electrode; The preparation process of electrode is following: at first the film to preliminary election cleans, dries; The electrode film thickness of selecting is at the 0.05-0.2 millimeter, and smooth being fixed on the screen printing apparatus, printing stencil is fixed on the film upper surface that is printed; Preparation printed catalyst slurry; According to mass ratio 1-3: 9-7 weighing bonding agent and catalyzer with bonding agent and catalyst mix, are uniformly dispersed through ultrasonic disperser; Scattered slurry is printed on the teflon waterproof and breathable diaphragm through knife coating, and the carrying capacity of catalyzer is controlled at 2 milligrams of-20 milligrams/cm
2, the area of electrode is at 0.5-5cm
2Afterwards, electrode is cleaned once more, the electrode after cleaning was carried out in 100-240 ℃ of temperature conditions sintering 30-60 minute under the high pure nitrogen protection; The assembling of sensor; The electrodes use lamination is placed and is sandwiched type structure, from top to bottom is respectively gold, platinum one working electrode, contrast electrode, two auxiliary electrodes.
2. the preparation method of a kind of multiple-electrode electrochemical gas sensor as claimed in claim 1; It is characterized in that the gold, the platinum one working electrode that adopt be made up of two semicircular electrodes; A slice working electrode is semicircle Au catalyst electrode, and a slice working electrode is semicircle platinum catalyst electrode.
3. the preparation method of a kind of multiple-electrode electrochemical gas sensor as claimed in claim 1 is characterized in that auxiliary electrode and contrast electrode are the annular membrane structure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100516467A CN101435790B (en) | 2008-12-22 | 2008-12-22 | Method for preparing multiple-electrode electrochemical gas sensor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100516467A CN101435790B (en) | 2008-12-22 | 2008-12-22 | Method for preparing multiple-electrode electrochemical gas sensor |
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| Publication Number | Publication Date |
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| CN101435790A CN101435790A (en) | 2009-05-20 |
| CN101435790B true CN101435790B (en) | 2012-06-27 |
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| CN2008100516467A Expired - Fee Related CN101435790B (en) | 2008-12-22 | 2008-12-22 | Method for preparing multiple-electrode electrochemical gas sensor |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8342007B2 (en) * | 2010-02-10 | 2013-01-01 | Dionex Corporation | Electrochemical detection cell for liquid chromatography system |
| CN102279210B (en) * | 2011-07-29 | 2013-02-20 | 吉林大学 | Double-sensitive-layer gas sensor based on nano fiber and particle adhesion layer and preparation method of double-sensitive-layer gas sensor |
| CN102621205B (en) * | 2012-03-28 | 2016-05-04 | 华瑞科学仪器(上海)有限公司 | Hydrogen sulfide sensor |
| CN103336041B (en) * | 2013-06-09 | 2016-03-30 | 华瑞科学仪器(上海)有限公司 | A kind of HCN electrochemical sensor |
| CN104391025B (en) * | 2014-11-19 | 2017-01-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrochemical carbon oxide gas sensor electrode |
| CN105241934A (en) * | 2015-10-28 | 2016-01-13 | 胡丽春 | Power plant and implementation method thereof |
| CN110045428B (en) * | 2019-03-26 | 2021-01-05 | 中国地质大学（武汉） | Deep sea pressure resistant solid nonpolarized electrode and preparation method thereof |
| CN113552194B (en) * | 2021-07-20 | 2024-05-28 | 上海松柏传感技术有限公司 | Preparation method of electrochemical gas sensor electrode and electrochemical gas sensor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040866A (en) * | 1988-09-01 | 1990-03-28 | 中国人民解放军防化研究院第三所 | Detect the sensor of sulfuretted hydrogen in the atmosphere |
| US5306414A (en) * | 1993-05-17 | 1994-04-26 | Regents Of The University Of California | Corrosion sensor |
| US5716506A (en) * | 1995-10-06 | 1998-02-10 | Board Of Trustees Of The University Of Illinois | Electrochemical sensors for gas detection |
| CN2456165Y (en) * | 2000-12-09 | 2001-10-24 | 林荣 | Electrochemical carbon oxide sensor |
-
2008
- 2008-12-22 CN CN2008100516467A patent/CN101435790B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040866A (en) * | 1988-09-01 | 1990-03-28 | 中国人民解放军防化研究院第三所 | Detect the sensor of sulfuretted hydrogen in the atmosphere |
| US5306414A (en) * | 1993-05-17 | 1994-04-26 | Regents Of The University Of California | Corrosion sensor |
| US5716506A (en) * | 1995-10-06 | 1998-02-10 | Board Of Trustees Of The University Of Illinois | Electrochemical sensors for gas detection |
| CN2456165Y (en) * | 2000-12-09 | 2001-10-24 | 林荣 | Electrochemical carbon oxide sensor |
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