CN105158312A - Preparation and application of electrochemical oxygen sensor sensitive material - Google Patents
Preparation and application of electrochemical oxygen sensor sensitive material Download PDFInfo
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- CN105158312A CN105158312A CN201510609442.0A CN201510609442A CN105158312A CN 105158312 A CN105158312 A CN 105158312A CN 201510609442 A CN201510609442 A CN 201510609442A CN 105158312 A CN105158312 A CN 105158312A
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Abstract
The invention discloses preparation and application of an electrochemical oxygen sensor sensitive material and belongs to the technical field of electrochemistry. The preparation include the following steps that firstly, a precious metal precursor salt solution and conductive carriers are taken, the conductive carriers are dispersed into the precious metal precursor salt solution, stirring is continuously performed, and meanwhile steeping liquor is added; secondly, under the condition of 15-30 DEG C, steeping liquor is added into mixed liquid obtained in the first step, meanwhile an alkaline solution is added, the PH value of the mixed solution is adjusted to 10-11, and a loaded precious metal matter static solution is obtained; thirdly, the loaded precious metal matter static solution obtained in the second step is centrifuged, washed and dried under the vacuum condition so that dried powder can be obtained, and then the electrochemical oxygen sensor sensitive material can be obtained. Under the condition of acidic electrolyte, the sensitive material which is novel in composition is combined with an oxygen gas diffusion electrode and thus has better activity, and the sensitive material is more stable and can provide detecting and warning signals.
Description
Technical field
The invention belongs to electrochemical material technical field, particularly relate to a kind of Synthesis and applications of electrochemical oxygen sensor material.
Background technology
The oxygen sensor of electrochemical principle has highly sensitive, that selectivity is good advantage, but the sensitive material of oxygen determines the performance of oxygen sensor, improving the efficiency of oxygen reduction, shortening the oxygen corresponding time as needed in industry and alarm for safety guard.And the long-term work in acidic electrolyte bath of most of sensitive material can be lost efficacy, cause the wrong report of oxygen sensor and misrepresent deliberately.
Noble metal is well-known in oxygen electro-catalysis field, particularly the eelctro-catalyst of platinum group is applied in oxygen gas diffusion electrode structure at large, and the commercialization being applied to acidic electrolyte bath has extremely important effect, but face this corrosive environment, the stability aspect of sensor has some limitations.Therefore need badly in the middle of prior art and want a kind of novel technical scheme to solve this problem.
Summary of the invention
Technical matters to be solved by this invention is: provide a kind of preparations and applicatio for electrochemical oxygen sensor sensitive material, under the condition of acidic electrolyte bath, the sensitive material of its novel composition is combined in oxygen gas diffusion electrode more has activity, and more stable, and detection, alerting signal can be provided.
For a preparation for electrochemical oxygen sensor sensitive material, it is characterized in that: comprise the following steps,
Step one, get 250ml noble metal precursor salt solusion, 400mg conductive carrier, the conductive carrier of 400mg is dispersed in the noble metal precursor salt solusion of 250ml, Keep agitation, and adds 100mg maceration extract;
Step 2, under the condition of 15 DEG C ~ 30 DEG C, in the mixed liquor of described step one, add 100mg maceration extract, the concentration of maceration extract is 10mg/m, adds alkaline solution simultaneously, and the pH value of solution is adjusted to 10 ~ 11, obtains the quiet solution of precious metals species of load;
Step 3, the quiet solution of precious metals species described step 2 being obtained load carry out centrifugal, and rotating speed is 4000rmp, adopts deionized water washing, washing to chlorine detection ion concentration is 0, and under the condition of vacuum, dry 4h, obtain dried powder, the i.e. sensitive material of electrochemical oxygen sensor.
A kind of application for electrochemical oxygen sensor sensitive material, it is characterized in that: a kind of electrochemical oxygen sensor sensitive material that is used for is applied to oxygen sensor, and described sensitive material comprises the adjuvant adding portion of noble metal sensitization material, inorganic additive and one or more metal oxides of one or more loads in conductive carbon; Described oxygen sensor comprises two or more electrodes contacted with acidic electrolysis bath.
Described noble metal precursor body salt solusion is gold chloride, chloroplatinic acid, palladium bichloride, iridium chloride, radium chloride, ruthenic chloride or silver nitrate.
Described conductive carrier is carbon, carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri, and the conductance of conductive carrier is more than or equal to 5S/m, and surface area is more than or equal to 200m
2/ g ~ 350m
2/ g, metal and the adjuvant ratio charge capacity on conductive carrier is 10% ~ 30%.
Described maceration extract is strong reductant, and reduction potential is less than 0.13V/SHE.
The concentration of described maceration extract is 10mg/ml ~ 50mg/ml.
Described electrode comprises metal platinum Pt, ruthenium Ru, iridium Ir, golden Au, palladium Pd or silver-colored Ag, be selected from the metal oxide of platinum Pt, ruthenium Ru, iridium Ir, golden Au, palladium Pd or silver-colored Ag, and the potpourri of described metal and metal oxide, or carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri.
In described electrode, the content of the adjuvant of sensitive material is 10% ~ 15%.
The content of the adjuvant adding portion of one or more metal oxides described is 5% ~ 10%.
By above-mentioned design proposal, the present invention can bring following beneficial effect: a kind of preparations and applicatio for electrochemical oxygen sensor sensitive material, under the condition of acidic electrolyte bath, the sensitive material of its novel composition is combined in oxygen gas diffusion electrode more has activity, and more stable, and detection, alerting signal can be provided.Adopt carbon, carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri as conductive carrier, there is higher specific area, electric conductivity and suitable porosity.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated:
Fig. 1 is a kind of preparation method's schematic process flow diagram for electrochemical oxygen sensor sensitive material of the present invention.
Embodiment
For a preparation method for electrochemical oxygen sensor sensitive material, as shown in Figure 1, comprise the following steps,
Step one, get 250ml noble metal precursor salt solusion, 400mg conductive carrier, the conductive carrier of 400mg is dispersed in the noble metal precursor salt solusion of 250ml, Keep agitation, and adds 100mg maceration extract;
Step 2, under the condition of 15 DEG C ~ 30 DEG C, in the mixed liquor of described step one, add 100mg maceration extract, the concentration of maceration extract is 10mg/m, adds alkaline solution simultaneously, and the pH value of solution is adjusted to 10 ~ 11, obtains the quiet solution of precious metals species of load;
Step 3, the quiet solution of precious metals species described step 2 being obtained load carry out centrifugal, rotating speed is 4000rmp, employing deionized water washs, washing to chlorine detection ion concentration is 0, and under the condition of vacuum, dry 4h, obtains dried powder, namely obtains the sensitive material of electrochemical oxygen sensor.
A kind of electrochemical oxygen sensor sensitive material that is used for is applied to oxygen sensor, and described sensitive material comprises the adjuvant adding portion of noble metal sensitization material, inorganic additive and one or more metal oxides of one or more loads in conductive carbon; Described oxygen sensor comprises two or more electrodes contacted with acidic electrolysis bath.
Described conductive carrier is carbon, carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri; Described conductive carrier has higher electric conductivity; Described conductive carrier has suitable porosity.Described conductive carrier has higher specific surface area.Such as CabotCorpVulcanXC-72, is particularly suitable for this scope.
Described maceration extract is strong reductant, and reduction potential is less than 0.13V/SHE.As reductive agent, preferred sodium borohydride, but other reductive agents be applicable to comprise lithium borohydride, potassium borohydride, hydrazine, formaldehyde and metallic aluminium, zinc etc.
The concentration of described maceration extract is 10mg/ml ~ 50mg/ml.
In one aspect, the sensitive material of electrochemical oxygen sensor, comprising: described oxygen sensor such as can comprise at least two electrodes contacted with acidic electrolysis bath.
Comprise the sensitive material of at least one noble metal, described sensitive material comprises the noble metal sensitization material of at least one load in conductive carbon, at least comprises the adjuvant adding portion of inorganic additive or at least one metal oxide.
Described electrode such as can comprise the metal being selected from Pt, Ru, Ir, Au, Pd or Ag; Be selected from the oxide of the metal of Pt, Ru, Ir, Au, Pd or Ag; The potpourri of this metal and/or metal oxide; Or carbon, is selected from carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri.
Described additive for electrode part such as can exist with the amount of 0.1 to 15%.When it is present, the adjuvant of one or more burnings can exist with the amount of 0.05 to 10%.
Embodiment 1:
By the CabotCorpVulcanXC-72 activated charcoal of 400mg, be distributed to 250mL chloroplatinic acid, under stirring, add sodium borohydride 100mg, make the concentration of sodium borohydride in deionized water be 10mg/mL.Temperature of reaction system controls in room temperature.The pH value of solution is adjusted to the scope of 10 ~ 11 by ammoniacal liquor.Finally, product is centrifugal, washing, vacuum drying 4h i.e. obtained sensitive material.Mean grain size is 20nm.
Embodiment 2:
By the CabotCorpVulcanXC-72 activated charcoal of 400mg, be distributed in 250mL ruthenic chloride solution, under stirring, add sodium borohydride 100mg, make the concentration of sodium borohydride in deionized water be 10mg/mL.Temperature of reaction system controls in room temperature.The pH value of solution is adjusted to the scope of 10 ~ 11 by ammoniacal liquor.Finally, product is centrifugal, washing, vacuum drying 4h, powder mull is even, is placed on surface plate, is placed in muffle furnace, 300 degree of calcinings 12 hours.Namely the ruthenium-oxide of load is obtained.Above-mentioned ground material is distributed to sensitive material.Be distributed to 250mL chloroplatinic acid, under stirring, add sodium borohydride 100mg, make the concentration of sodium borohydride in deionized water be 10mg/mL.Temperature of reaction system controls in room temperature.The pH value of solution is adjusted to the scope of 10 ~ 11 by ammoniacal liquor.Finally, product is centrifugal, washing, vacuum drying 4h i.e. obtained sensitive material.
Embodiment 3:
By the multiple-wall carbon nanotube of 400mg, be distributed in 250mL ruthenic chloride solution, under stirring, add sodium borohydride 250mg, make the concentration of sodium borohydride in deionized water be 25mg/mL.Temperature of reaction system controls in room temperature.The pH value of solution is adjusted to the scope of 10 ~ 11 by ammoniacal liquor.Finally, product is centrifugal, washing, vacuum drying 4h, powder mull is even, is placed on surface plate, is placed in muffle furnace, 300 degree of calcinings 12 hours.Namely the ruthenium-oxide of load is obtained.Above-mentioned ground material is distributed to sensitive material.Be distributed to 250mL chloroplatinic acid, under stirring, add sodium borohydride 100mg, make the concentration of sodium borohydride in deionized water be 10mg/mL.Temperature of reaction system controls in room temperature.The pH value of solution is adjusted to the scope of 10 ~ 11 by ammoniacal liquor.Finally, product is centrifugal, washing, vacuum drying 4h i.e. obtained sensitive material.
The sensitive material that a kind of preparation method for electrochemical oxygen sensor sensitive material of the present invention obtains can be the metal of Pt, Ru, Ir, Au, Pd or Ag, or be selected from the oxide of metal of Pt, Ru, Ir, Au, Pd or Ag, and the potpourri of this metal or metal oxide.Sensitive material is optionally dispersed on the surface of carbon-based material activated metal and oxide addition thereof, and what obtain is the catalyzer of carbon-based material load.It is characterized in that the carrying capacity reducing noble metal.
Claims (9)
1. for a preparation for electrochemical oxygen sensor sensitive material, it is characterized in that: comprise the following steps,
Step one, get 250ml noble metal precursor salt solusion, 400mg conductive carrier, the conductive carrier of 400mg is dispersed in the noble metal precursor salt solusion of 250ml, Keep agitation, and adds 100mg maceration extract;
Step 2, under the condition of 15 DEG C ~ 30 DEG C, in the mixed liquor of described step one, add 100mg maceration extract, the concentration of maceration extract is 10mg/m, adds alkaline solution simultaneously, and the pH value of solution is adjusted to 10 ~ 11, obtains the quiet solution of precious metals species of load;
Step 3, the quiet solution of precious metals species described step 2 being obtained load carry out centrifugal, rotating speed is 4000rmp, employing deionized water washs, washing to chlorine detection ion concentration is 0, and under the condition of vacuum, dry 4h, obtains dried powder, namely obtains the sensitive material of electrochemical oxygen sensor.
2. the application for electrochemical oxygen sensor sensitive material, it is characterized in that: a kind of electrochemical oxygen sensor sensitive material that is used for is applied to oxygen sensor, and described sensitive material comprises the adjuvant adding portion of noble metal sensitization material, inorganic additive and one or more metal oxides of one or more loads in conductive carbon; Described oxygen sensor comprises two or more electrodes contacted with acidic electrolysis bath.
3. a kind of preparation for electrochemical oxygen sensor sensitive material according to claim 1, is characterized in that: described noble metal precursor body salt solusion is gold chloride, chloroplatinic acid, palladium bichloride, iridium chloride, radium chloride, ruthenic chloride or silver nitrate.
4. a kind of preparation for electrochemical oxygen sensor sensitive material according to claim 1, it is characterized in that: described conductive carrier is carbon, carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri, and the conductance of conductive carrier is more than or equal to 5S/m, surface area is more than or equal to 200m
2/ g ~ 350m
2/ g, metal and the adjuvant ratio charge capacity on conductive carrier is 10% ~ 30%.
5. a kind of preparation for electrochemical oxygen sensor sensitive material according to claim 1, is characterized in that: described maceration extract is strong reductant, and reduction potential is less than 0.13V/SHE.
6. a kind of preparation for electrochemical oxygen sensor sensitive material according to claim 1, is characterized in that: the concentration of described maceration extract is 10mg/ml ~ 50mg/ml.
7. a kind of application for electrochemical oxygen sensor sensitive material according to claim 2, it is characterized in that: described electrode comprises metal platinum Pt, ruthenium Ru, iridium Ir, golden Au, palladium Pd or silver-colored Ag, be selected from the metal oxide of platinum Pt, ruthenium Ru, iridium Ir, golden Au, palladium Pd or silver-colored Ag, and the potpourri of described metal and metal oxide, or carbon black, graphite, carbon nano-tube, carbon fiber, activated charcoal and their potpourri.
8. a kind of application for electrochemical oxygen sensor sensitive material according to claim 2, is characterized in that: in described electrode, the content of the adjuvant of sensitive material is 10% ~ 15%.
9. a kind of application for electrochemical oxygen sensor sensitive material according to claim 2, is characterized in that: the content of the adjuvant adding portion of one or more metal oxides described is 5% ~ 10%.
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| CN201510609442.0A CN105158312A (en) | 2015-09-22 | 2015-09-22 | Preparation and application of electrochemical oxygen sensor sensitive material |
| CN201710575753.9A CN107290408A (en) | 2015-09-22 | 2015-09-22 | A kind of application of electrochemical oxygen sensor sensitive material |
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| CN114994132B (en) * | 2022-08-01 | 2022-11-01 | 成都工业学院 | Method for testing regulation and control of Rh-N4-graphene hydrogen evolution performance by stress |
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| CN101116817B (en) * | 2007-05-10 | 2011-04-06 | 南京大学 | Method for preparing carbon nitride nanotubes load platinum ruthenium nanometer particle electrode catalyst |
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| CN102353702A (en) * | 2011-07-22 | 2012-02-15 | 李学中 | Oxide semiconductor normal temperature oxygen sensor |
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Non-Patent Citations (5)
| Title |
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| CHENG, YUANHANG ET. AL: "Ag Nanoparticles on Boron Doped Multi-walled Carbon Nanotubes as a Synergistic Catalysts for Oxygen Reduction Reaction in Alkaline Media", 《ELECTROCHIMICA ACTA》 * |
| HOSSEINI, M. G. ET.AL: "Electrocatalytical study of carbon supported Pt, Ru and bimetallic Pt-Ru nanoparticles for oxygen reduction reaction in alkaline media", 《APPLIED SURFACE SCIENCE》 * |
| RAMASWAMY, NAGAPPAN ET.AL: "Electrochemical Kinetics and X-ray Absorption Spectroscopic Investigations of Oxygen Reduction on Chalcogen-Modified Ruthenium Catalysts in Alkaline Media", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| YI, QINGFENG ET.AL: "Carbon nanotube-supported binary silver-based nanocatalysts for oxygen reduction reaction in alkaline media", 《JOURNAL OF ELECTROANALYTICAL CHEMISTRY》 * |
| 邱永峰: "Pt@CNTs纳米复合结构的制备及其气体传感性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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