CN107293759A - A kind of preparation method of fuel cell oxygen reduction electrocatalyst - Google Patents
A kind of preparation method of fuel cell oxygen reduction electrocatalyst Download PDFInfo
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- CN107293759A CN107293759A CN201710740602.4A CN201710740602A CN107293759A CN 107293759 A CN107293759 A CN 107293759A CN 201710740602 A CN201710740602 A CN 201710740602A CN 107293759 A CN107293759 A CN 107293759A
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- fuel cell
- oxygen reduction
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- cell oxygen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a kind of preparation method of fuel cell oxygen reduction electrocatalyst, by 2 amino 1,3,5 triazines 4,6 two mercaptan and quality are done to be well mixed wiring solution-forming through ultrasonic disperse with deionized water for 37% formalin, add manganese chloride and be uniformly mixed and obtain suspension, obtained suspension is transferred in autoclave and sealed, 6 h are reacted in 160 DEG C, reaction naturally cools to room temperature after terminating, obtained product is washed with deionized up to filtrate becomes colorless, puts into vacuum drying chamber and is dried in 80 DEG C to constant weight, then in N23h is calcined in 800 DEG C obtain double-deck ghost spherical structure sulphur, nitrogen, manganese codoped carbon material i.e. fuel cell oxygen reduction electrocatalyst under atmosphere.Sulphur that the present invention is provided, nitrogen, manganese codoped carbon material show prominent electro catalytic activity to oxygen reduction reaction, and preparation method is simple, and cost of material is low, is expected to extensive use in a fuel cell.
Description
Technical field
The invention belongs to the preparing technical field of fuel-cell catalyst, and in particular to a kind of fuel cell oxygen reduction electricity is urged
The preparation method of agent.
Background technology
Fuel cell is a kind of cleaning, efficient novel energy, is acknowledged as preferable energy conversion system.But combustion
The high cost of material battery constrains its commercialization process, is one of most important key issue of this area research.Fuel
Cell cathode oxygen reduction reaction speed is slow, generally requires to load more platinum carbon catalyst, causes fuel cell cost very high.
Therefore, the research tendency about fuel cell oxygen reduction electrocatalyst is that its catalysis is lived around reduction catalyst cost and raising
Property.Doping carbon-supported catalysts have the features such as oxygen reduction catalytic activity is high, stability is good, and with low in raw material price, come
The advantages of source is extensive.Therefore, doping carbon-supported catalysts very likely replace platinum based catalyst, there is good application prospect.
Nano material with shell structurre shows huge application potential in every field, such as Shell Materials have
Higher specific surface area, its abundant hole can also promote mass transfer and electro transfer, be advantageous to improve catalyst
Activity.It is template to synthesize shell structurre nano material most common method, i.e., carve by the manufacture of template and optionally
Template is lost, so as to produce desired hollow-core construction, this method is related to tediously long step, and combined coefficient is relatively low.So setting
Meter is simple, green, the method without template have very big challenge to synthesize the shell nano material of special composition.
The content of the invention
Present invention solves the technical problem that there is provided a kind of simple and with low cost fuel cell oxygen reduction electricity of technique
The preparation method of catalyst, effectively increases the performance of fuel cell oxygen reduction electrocatalyst.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, a kind of fuel cell oxygen reduction electrocatalyst
Preparation method, it is characterised in that concretely comprise the following steps：The mercaptan of 2- amino -1,3,5- triazines -4,6- two and quality are done to the first for 37%
Aldehyde solution is well mixed wiring solution-forming with deionized water through ultrasonic disperse, adds manganese chloride and is uniformly mixed and obtains suspended
Liquid, obtained suspension is transferred in autoclave and sealed, and 6 h are reacted in 160 DEG C, and reaction naturally cools to room after terminating
Temperature, obtained product is washed with deionized up to filtrate becomes colorless, puts into vacuum drying chamber and is dried in 80 DEG C to perseverance
Weight, then in N23h is calcined in 800 DEG C obtain double-deck ghost spherical structure sulphur, nitrogen, manganese codoped carbon material i.e. fuel under atmosphere
Battery oxygen reduction electro-catalyst.
Further preferably, the 2- amino-mercaptan of 1,3,5-triazines -4,6- bis-, mass concentration for 37% formalin with
The mass ratio that feeds intake of manganese chloride is 1:6:10.
The present invention has the advantages that compared with prior art：
1st, the present invention successfully synthesizes sulphur, nitrogen, manganese codoped carbon material with double-deck ghost spherical structure, the hollow knot first
Structure can provide three-phase for electrode reaction（Solid-liquid-gas）Area, provides passage, and then improve catalyst for the transmission of electrolyte
Specific surface area, increases the catalytic activity of elctro-catalyst；
2nd, the present invention is designed by simple method and synthesized using cheap, wide material sources transistion metal compounds as raw material
Elctro-catalyst with special nanometer package assembly, and method therefor of the present invention is simple and easy to do, is suitable for the scale of catalyst
Metaplasia is produced；
3rd, new fuel cell oxygen reduction electro-catalyst produced by the present invention, should compared with the nanocarbon catalyst of only N doping
Class catalyst has higher activity, and the catalysis material surface that is doped to of sulphur atom creates more positively charged sites, increases
It is strong that oxygen molecule is adsorbed, the pi-electron enriched in carbon conjugated system is activated, nitrogen, sulphur, manganese have been played to the good of carbon material together
Good cooperative effect.
Brief description of the drawings
Fig. 1 is the TEM figures that fuel cell oxygen reduction electrocatalyst is made in embodiment 1；
Fig. 2 is that the oxygen reduction reaction polarization of catalyst in embodiment 1 and comparative example 1, comparative example 2, comparative example 3 and comparative example 4 is bent
Line.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
Formalin and 40mL by the mercaptan of 0.01g 2- amino -1,3,5- triazines -4,6- two and 0.06g mass concentrations for 37%
Deionized water is well mixed wiring solution-forming through ultrasonic disperse, adds 0.1g manganese chlorides and is uniformly mixed and obtains suspension；
Obtained suspension is transferred in autoclave and sealed, 6h is reacted in 160 DEG C, reaction naturally cools to room temperature after terminating；
Obtained product is washed with deionized up to filtrate becomes colorless, puts into vacuum drying chamber and is dried in 80 DEG C to constant weight,
Then in N23h is calcined in 800 DEG C obtain sulphur, nitrogen, manganese codoped carbon material i.e. fuel cell oxygen reduction electrocatalyst under atmosphere.
Sulphur, nitrogen, manganese codoped carbon material made from the present embodiment are double-deck ghost spherical structure as seen from Figure 1, this
The special material composition of kind and appearance structure provide passage for the transmission of electrolyte, and then improve the specific surface area of catalyst, have
The catalytic activity of effect increase elctro-catalyst.
Electro-chemical test uses Solartron 1287（Solartron Analytical, England）The electrode body of type three
The half-cell of system is carried out.It is respectively 1cm to electrode and reference electrode to scribble the glass-carbon electrode of catalyst as working electrode2's
The saturated calomel electrode of platinized platinum and Ag/AgCl, electrolyte is the 0.1M KOH aqueous solution, to make catalyst be attached to glass-carbon electrode
On, clean glass-carbon electrode using secondary water and be dried at room temperature for.The preparation process of thin layer catalyst is as follows on electrode：Take 5mg
The perfluorinated sulfonic acid that catalyst adds 0.5mL ethanol and 50 μ L mass concentrations are 5%（PFSA）Solution, ultrasonic disperse about 10min, with micro-
Amount injector takes 15 μ L to be coated onto through the uniform suspension of ultrasonic disperse on bright and clean glass-carbon electrode, can be surveyed after being dried at room temperature for
Examination, electric performance test result is as shown in Figure 2.
Comparative example 1
0.01g melamines and 0.05g mass concentrations are mixed for 37% formalin with 40mL deionized waters through ultrasonic disperse
Uniform wiring solution-forming, adds 0.1g manganese chlorides and is uniformly mixing to obtain suspension；Obtained suspension is transferred to high pressure anti-
Answer in kettle and seal, 6h is reacted in 180 DEG C, reaction naturally cools to room temperature after terminating；Obtained product is washed with deionized
Until filtrate becomes colorless, put into vacuum drying chamber and dried in 80 DEG C to constant weight, then in N2Under atmosphere 2h is calcined in 800 DEG C
Obtain nitrogen, manganese codoped carbon material i.e. fuel-cell catalyst.
Electro-chemical test uses Solartron 1287（Solartron Analytical, England）The electrode body of type three
The half-cell of system is carried out.It is respectively 1cm to electrode and reference electrode to scribble the glass-carbon electrode of catalyst as working electrode2's
The saturated calomel electrode of platinized platinum and Ag/AgCl, electrolyte is the 0.1M KOH aqueous solution, to make catalyst be attached to glass-carbon electrode
On, clean glass-carbon electrode using secondary water and be dried at room temperature for.The preparation process of thin layer catalyst is as follows on electrode：Take 5mg
The perfluorinated sulfonic acid that catalyst adds 0.5mL ethanol and 50 μ L mass concentrations are 5%（PFSA）Solution, ultrasonic disperse about 10min, with micro-
Amount injector takes 15 μ L to be coated onto through the uniform suspension of ultrasonic disperse on bright and clean glass-carbon electrode, can be surveyed after being dried at room temperature for
Examination, electric performance test result is as shown in Figure 2.
Comparative example 2
Formalin and 40 mL by the mercaptan of 0.01g 2- amino -1,3,5- triazines -4,6- two and 0.06g mass concentrations for 37%
Deionized water is well mixed wiring solution-forming through ultrasonic disperse, and obtained solution is transferred in autoclave and sealed, in 160 DEG C
6h is reacted, reaction naturally cools to room temperature after terminating；Obtained product is washed with deionized up to filtrate becomes colorless, put
Dried into vacuum drying chamber in 80 DEG C to constant weight, then in N23h is calcined in 800 DEG C obtain sulphur, nitrogen co-doped carbon materials under atmosphere
Material is fuel-cell catalyst.
Electro-chemical test uses Solartron 1287（Solartron Analytical, England）The electrode body of type three
The half-cell of system is carried out.It is respectively 1cm to electrode and reference electrode to scribble the glass-carbon electrode of catalyst as working electrode2's
The saturated calomel electrode of platinized platinum and Ag/AgCl, electrolyte is the 0.1M KOH aqueous solution, to make catalyst be attached to glass-carbon electrode
On, clean glass-carbon electrode using secondary water and be dried at room temperature for.The preparation process of thin layer catalyst is as follows on electrode：Take 5mg
The perfluorinated sulfonic acid that catalyst adds 0.5mL ethanol and 50 μ L mass concentrations are 5%（PFSA）Solution, ultrasonic disperse about 10min, with micro-
Amount injector takes 15 μ L to be coated onto through the uniform suspension of ultrasonic disperse on bright and clean glass-carbon electrode, can be surveyed after being dried at room temperature for
Examination, electric performance test result is as shown in Figure 2.
Comparative example 3
Formalin and 40mL by the mercaptan of 0.01g 2- amino -1,3,5- triazines -4,6- two and 0.06g mass concentrations for 37%
Deionized water is well mixed wiring solution-forming through ultrasonic disperse, adds 0.1g iron chloride and is uniformly mixing to obtain suspension；Will
To suspension be transferred in autoclave seal, in 160 DEG C react 6h, reaction terminate after naturally cool to room temperature；Will
To product be washed with deionized until filtrate becomes colorless, put into vacuum drying chamber and dried in 80 DEG C to constant weight, then
In N23h is calcined in 800 DEG C obtain sulphur, nitrogen, iron codope carbon material i.e. fuel-cell catalyst under atmosphere.
Electro-chemical test uses Solartron 1287（Solartron Analytical, England）The electrode body of type three
The half-cell of system is carried out.It is respectively 1cm to electrode and reference electrode to scribble the glass-carbon electrode of catalyst as working electrode2's
The saturated calomel electrode of platinized platinum and Ag/AgCl, electrolyte is the 0.1M KOH aqueous solution.To make catalyst be attached to glass-carbon electrode
On, clean glass-carbon electrode using secondary water and be dried at room temperature for.The preparation process of thin layer catalyst is as follows on electrode：Take 5mg
The perfluorinated sulfonic acid that catalyst adds 0.5mL ethanol and 50 μ L mass concentrations are 5%（PFSA）Solution, ultrasonic disperse about 10min, with micro-
Amount injector takes 15 μ L to be coated onto through the uniform suspension of ultrasonic disperse on bright and clean glass-carbon electrode, can be surveyed after being dried at room temperature for
Examination, electric performance test result is as shown in Figure 2.
Comparative example 4
Take 20% Pt/Xc-72 of JM companies of the business platinum catalyst U.S..
Electro-chemical test uses Solartron 1287（Solartron Analytical, England）The electrode body of type three
The half-cell of system is carried out.It is respectively 1cm to electrode and reference electrode to scribble the glass-carbon electrode of catalyst as working electrode2's
The saturated calomel electrode of platinized platinum and Ag/AgCl, electrolyte is the 0.1M KOH aqueous solution.To make catalyst be attached to glass-carbon electrode
On, clean glass-carbon electrode using secondary water and be dried at room temperature for.The preparation process of thin layer catalyst is as follows on electrode：Take 5mg
The perfluorinated sulfonic acid that catalyst adds 0.5mL ethanol and 50 μ L mass concentrations are 5%（PFSA）Solution, ultrasonic disperse about 10min, with micro-
Amount injector takes 15 μ L to be coated onto through the uniform suspension of ultrasonic disperse on bright and clean glass-carbon electrode, can be surveyed after being dried at room temperature for
Examination, electric performance test result is as shown in Figure 2.
Fuel-cell catalyst produced by the present invention has a good hydrogen reduction electro catalytic activity, integrated embodiment 1 and right
Ratio 1-4 can be seen that the sulphur, nitrogen, manganese codoped carbon material of preparation are double-deck ghost spherical structure（Fig. 1）；Electric performance test knot
Really（Fig. 2）In, curve a is the electrical property figure of catalyst prepared by embodiment 1, and b, c, d, e correspond to comparative example 3, comparative example respectively
4th, the electrical property of comparative example 1 and the catalyst prepared by comparative example 2, compared with comparative example 1-4, catalyst prepared by embodiment 1
Carrying current and half wave potential are maximum, illustrate hydrogen reduction electro catalytic activity highest；We think, this special material group
Into and appearance structure for the transmission of electrolyte provide passage, and then improve the specific surface area of catalyst, be effectively increased elctro-catalyst
Catalytic activity, show catalyst electro catalytic activity excellent performance produced by the present invention, be it is a kind of have broad prospect of application
Fuel-cell catalyst.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of preparation method of fuel cell oxygen reduction electrocatalyst, it is characterised in that concretely comprise the following steps：By 2- amino -1,
The mercaptan of 3,5- triazines -4,6- two and quality do to be well mixed through ultrasonic disperse with deionized water for 37% formalin be made into it is molten
Liquid, adds manganese chloride and is uniformly mixed and obtain suspension, and obtained suspension is transferred in autoclave and sealed,
6 h are reacted in 160 DEG C, reaction naturally cools to room temperature after terminating, obtained product is washed with deionized until filtrate becomes
To be colourless, put into vacuum drying chamber and dried in 80 DEG C to constant weight, then in N23h is calcined in 800 DEG C obtain double-deck sky under atmosphere
Shell spherical structure sulphur, nitrogen, manganese codoped carbon material are fuel cell oxygen reduction electrocatalyst.
2. the preparation method of fuel cell oxygen reduction electrocatalyst according to claim 1, it is characterised in that：The 2- ammonia
The mass ratio that feeds intake of the mercaptan of base -1,3,5- triazines -4,6- two, the formalin that mass concentration is 37% and manganese chloride is 1:6:10.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108470916A (en) * | 2018-02-07 | 2018-08-31 | 深圳大学 | It is a kind of using three-dimensional porous carbon material as the fuel cell oxygen reduction catalyst of raw material and preparation method |
| CN109346735A (en) * | 2018-09-28 | 2019-02-15 | 东华大学 | Nano carbon balls oxygen reduction catalyst and its preparation and application derived from porous polymer |
| CN109473684A (en) * | 2018-09-29 | 2019-03-15 | 中国科学院山西煤炭化学研究所 | The elctro-catalyst and preparation method of a kind of sulphur-nitrogen-carbon-based oxygen reduction of transition metal codope and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108470916A (en) * | 2018-02-07 | 2018-08-31 | 深圳大学 | It is a kind of using three-dimensional porous carbon material as the fuel cell oxygen reduction catalyst of raw material and preparation method |
| CN108470916B (en) * | 2018-02-07 | 2020-09-01 | 深圳大学 | Fuel cell oxygen reduction catalyst taking three-dimensional porous carbon material as raw material and preparation method thereof |
| CN109346735A (en) * | 2018-09-28 | 2019-02-15 | 东华大学 | Nano carbon balls oxygen reduction catalyst and its preparation and application derived from porous polymer |
| CN109473684A (en) * | 2018-09-29 | 2019-03-15 | 中国科学院山西煤炭化学研究所 | The elctro-catalyst and preparation method of a kind of sulphur-nitrogen-carbon-based oxygen reduction of transition metal codope and application |
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