CN108987760A - A kind of fuel cell platinum cobalt alloy-catalyst and preparation method with array structure - Google Patents
A kind of fuel cell platinum cobalt alloy-catalyst and preparation method with array structure Download PDFInfo
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- CN108987760A CN108987760A CN201810803539.9A CN201810803539A CN108987760A CN 108987760 A CN108987760 A CN 108987760A CN 201810803539 A CN201810803539 A CN 201810803539A CN 108987760 A CN108987760 A CN 108987760A
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- platinum
- catalyst
- cobalt alloy
- array structure
- fuel cell
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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
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
-
- 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
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention belongs to the technical fields of fuel cell, provide a kind of fuel cell platinum cobalt alloy-catalyst and preparation method with array structure.This method forms Pt/Co organic complex by platinum salt and cobalt salt in organic solvent, under magnetic fields, cobalt is magnetized, and complex groups is driven to be dispersed in around kind of brilliant particle, platinum cobalt alloy array structure is formed by high-temperature heat treatment, platinum cobalt alloy-catalyst is made.It is compared with the traditional method, platinum cobalt alloy-catalyst prepared by the present invention, add magnetic fields outside by the compound rear progress of the strong ferromagnetism and Pt of Co, during heat treatment organic phase is carbonized to form agraphitic carbon clad, effectively inhibit the reunion of nano particle, improve its dispersibility, it is ensured that the stability of catalyst can be widely used for fuel cell field.
Description
Technical field
The invention belongs to the technical fields of fuel cell, provide a kind of fuel cell platinum cobalt alloy with array structure
Catalyst and preparation method.
Background technique
Proton Exchange Membrane Fuel Cells is a kind of fuel cell, is equivalent to " inverse " device of water electrolysis in principle.Its list
Battery is made of anode, cathode and proton exchange membrane, and anode is the place that hydrogen fuel aoxidizes, and cathode is oxidant reduction
The catalyst for accelerating electrode electro Chemical reaction is all contained at place, the two poles of the earth, and medium of the proton exchange membrane as transmitting H+ only allows H+
Pass through, and H2The electronics lost then passes through from conducting wire.A DC power supply, anode, that is, power cathode are equivalent to when work, cathode is
Positive pole.
Proton Exchange Membrane Fuel Cells is low with operating temperature, starting is fast, specific power is high, structure is simple and convenient to operate
Advantage is acknowledged as the preferred energy at electric car, stationary power generation station etc..Proton Exchange Membrane Fuel Cells has the advantages that
Its power generation process is not related to oxyhydrogen combustion, because without being limited by Carnot cycle, energy conversion rate is high；Dirt is not generated when power generation
Dye, power generating modules, high reliablity, assembling and maintenance are all very convenient, also without noise when work.So proton exchange
Membrane cell power supply is a kind of cleaning, efficiently environmentally protective power supply.
The membrane electrode of Proton Exchange Membrane Fuel Cells is its core component, by proton exchange membrane, catalyst, gas diffusion layers
It is combined.Conventional catalyst agent material such as platinum-base material needs to load on the carbon carrier, can not directly load and gas diffusion layers
On.Therefore, carbon carrier is one of critical material of catalyst of fuel batter with proton exchange film, it not only directly affects catalyst
Partial size, dispersion degree and activity, and influence electric conductivity, mass transfer and the electrochemistry specific surface area etc. of Catalytic Layer.The carrier of catalyst
It must conductance with higher and biggish specific surface area.And it is relatively stable under battery operating conditions.Make noble metal height point
It dissipates and its crystallite can be prevented to coalesce again.
It has been taken in terms of Proton Exchange Membrane Fuel Cells technology, especially membrane electrode catalyst and its carrier both at home and abroad at present
Obtained certain effect.Wherein Qin Xiao equality human hair is illustrated the preparation methods of fuel cell alloy catalysts a kind of (Chinese invention is special
Sharp application number 201410637397.5), the invention is using platinum based catalyst as substrate, in the hydroxide of its surface deposition transition metal
Then object is heat-treated under reducing atmosphere, to obtain platinum base-transition metal/charcoal alloy catalyst, obtained alloy is urged
Agent carries out pickling in an acidic solution, removes the transition metal on its surface to get product is arrived；The preparation method that the invention uses
Obtained alloy catalyst shows higher unit mass Pt catalytic activity to hydrogen reduction, and its stability is relative to base
Bottom platinum based catalyst is greatly improved, and is conducive to large-scale production.In addition, bright red et al. has invented a kind of polyaniline-coated carbon
The platinum base of carrier takes off alloy fuel cell catalyst and preparation method thereof (Chinese invention patent application number 201710284291.5),
Platinum cobalt alloy is core, and platinum is shell；60 ~ 80 parts by weight of carrier of polyaniline-coated carbon black；Platinum cobalt metal with coreshell type structure
20 ~ 40 parts by weight；In the core of platinum cobalt alloy, the atomic ratio of platinum and cobalt is 1:0.5 ~ 1:3；The invention polyaniline-coated carbon carrier
Platinum base takes off alloy fuel cell catalyst, and polyaniline is coated on carrier, and acid is effectively reduced in de- alloy process to carbon carrier
Damage, during subsequent catalyst use, polyaniline is able to extend making for de- alloy catalyst than carbon carrier preferential oxidation
Use the service life；The catalytic efficiency of catalyst and the utilization rate of noble metal can be greatly improved, the development of fuel cell will be promoted.
As it can be seen that the catalyst of Proton Exchange Membrane Fuel Cells in the prior art needs to load on the carbon carrier, Wu Fazhi
It connects on load and gas diffusion layers, and there are nano particles the disadvantages of reuniting in recombination process seriously, influencing catalytic activity.
Summary of the invention
In response to this, it is proposed that a kind of fuel cell platinum cobalt alloy-catalyst and preparation side with array structure
Method significantly improves the dispersibility of catalyst, avoids agglomeration, it is ensured that the stability of catalyst improves fuel cell
Chemical property.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure, by platinum salt and cobalt salt organic molten
Pt/Co organic complex is formed in agent, under magnetic fields, cobalt is magnetized, and complex groups is driven to be dispersed in kind of a brilliant particle week
It encloses, platinum cobalt alloy array structure is formed by high-temperature heat treatment, platinum cobalt alloy-catalyst is made, specific step is as follows for preparation:
(1) it will be placed in organic solvent by kind of a base material for brilliant processing, platinum salt and cobalt salt be then added, stirs evenly, then
Complexing agent is added, platinum salt and cobalt salt is made to form Pt/Co organic complex in organic solvent；
(2) certain time is slowly stirred under magnetic fields, cobalt is magnetized and complex groups is driven to be dispersed in base material
Around the brilliant particle of kind；
(3) base material is taken out, is placed in Muffle furnace, be then passed through hydrogen under protection of argon gas and carry out pre-burning and sintering, lead to
It crosses high-temperature heat treatment and forms platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer；
(4) it dries, the platinum cobalt alloy-catalyst for being carried on the array structure of substrate material surface is made.
Preferably, the parts by weight of step (1) each raw material are 12 ~ 15 parts by weight of base material, organic solvent 69 ~ 78
Parts by weight, 4 ~ 6 parts by weight of platinum salt, 5 ~ 8 parts by weight of cobalt salt, 1 ~ 2 parts by weight of complexing agent.
Preferably, step (1) organic solvent is trichloro ethylene, ethylene glycol ether, triethanolamine, acetonitrile, ether
One of.
Preferably, step (1) platinum salt is at least one of platinum nitrate, chloroplatinic acid, platinum tetrachloride.
Preferably, step (1) cobalt salt is cobalt chloride, cobaltous bromide, cobalt carbonate, cobaltous sulfate, at least one in cobalt nitrate
Kind.
Preferably, step (1) complexing agent is tartaric acid, heptose hydrochlorate, sodium gluconate, sodium alginate, three second of ammonia
At least one of sour sodium, sodium ethylene diamine tetracetate.
Preferably, the intensity in step (2) described magnetic field is 0.2 ~ 0.3T, and mixing speed is 80 ~ 100r/min, time 30
~40min。
Preferably, the temperature of step (3) described pre-burning is 200 ~ 300 DEG C, and the time is 20 ~ 30min.
Preferably, the temperature of step (3) described sintering is 500 ~ 600 DEG C, and the time is 90 ~ 120min.
The present invention also provides the fuel cell platinum cobalt conjunctions with array structure that a kind of above-mentioned preparation method is prepared
Au catalyst.
The preparation method of the catalyst is to form Pt/Co organic complex in organic solvent by platinum salt and cobalt salt, by
In under magnetic fields, cobalt is easily magnetized, and drives complex groups to be dispersed in around kind of brilliant particle, passes through high-temperature heat treatment shape
At platinum cobalt alloy array structure, platinum cobalt alloy-catalyst is made.It is compared with the traditional method, platinum cobalt alloy catalysis prepared by the present invention
Agent, by the strong ferromagnetism of Co and Pt it is compound after carry out outside plus magnetic fields, organic phase is carbonized shape during heat treatment
At agraphitic carbon clad, the reunion of nano particle is effectively inhibited, improves its dispersibility, it is ensured that the stabilization of catalyst
Property, it can be widely used for fuel cell field.
The present invention provides a kind of fuel cell platinum cobalt alloy-catalyst and preparation method with array structure, and it is existing
Technology is compared, and the feature and excellent effect protruded is:
1. platinum cobalt alloy-catalyst prepared by the present invention, can be widely used for fuel cell field.
2. preparation method of the invention, by the strong ferromagnetism and Pt of Co it is compound after, under the action of an external magnetic field uniformly point
Cloth effectively inhibits the reunion of nano particle, improves its dispersibility by kind of a base material surface layer for brilliant processing.
3. organic phase is carbonized to form agraphitic carbon clad by preparation method of the invention during heat treatment, can protect
The stability of Pt/Co composite catalyzing material is demonstrate,proved, and then ensures catalytic activity.
Detailed description of the invention:
Fig. 1 is the Local map using the catalyst array distribution produced by the present invention of SEM scanning electron microscopic observation.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
It will be placed in 74kg trichloro ethylene by kind of a 13kg base material for brilliant processing, 5kg platinum nitrate and 7kg chlorination be then added
Cobalt stirs evenly, and adds 1kg tartaric acid, forms Pt/Co organic complex；Intensity be 0.2T magnetic fields under with
The revolving speed of 92r/min stirs 36min, and base material is taken out, is placed in Muffle furnace, be then passed through under protection of argon gas hydrogen into
Row pre-burning and sintering, the temperature of pre-burning are 260 DEG C, time 24min, and the temperature of sintering is 540 DEG C, time 105min, shape
At platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get substrate material surface is carried on
Array structure platinum cobalt alloy-catalyst.
Test method:
Catalyst distribution feature: using SEM scanning electron microscopic observation catalyst produced by the present invention, and observation Pt/Co catalyst is carrying
Distribution characteristics on body；Array distribution is uniform.As shown in Figure 1.
Embodiment 2
To be placed in 78kg ethylene glycol ether by kind of a 12kg base material for brilliant processing, be then added 4kg chloroplatinic acid with
5kg cobalt chloride, stirs evenly, and adds 1kg heptose hydrochlorate, forms Pt/Co organic complex；Make in the magnetic field that intensity is 0.2T
40min is stirred with the revolving speed of 80r/min under, base material is taken out, is placed in Muffle furnace, is then passed through under protection of argon gas
Hydrogen carries out pre-burning and sintering, and the temperature of pre-burning is 200 DEG C, time 30min, and the temperature of sintering is 500 DEG C, and the time is
120min forms platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get base is carried on
The platinum cobalt alloy-catalyst of the array structure on bottom material surface.
Embodiment 3
It will be placed in 69kg triethanolamine by kind of a 15kg base material for brilliant processing, 6kg platinum tetrachloride and 8kg be then added
Cobaltous bromide stirs evenly, and adds 2kg sodium gluconate, forms Pt/Co organic complex；Make in the magnetic field that intensity is 0.3T
30min is stirred with the revolving speed of 100r/min under, base material is taken out, is placed in Muffle furnace, is then led under protection of argon gas
Enter hydrogen and carry out pre-burning and sintering, the temperature of pre-burning is 300 DEG C, time 20min, and the temperature of sintering is 600 DEG C, and the time is
90min forms platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get substrate is carried on
The platinum cobalt alloy-catalyst of the array structure of material surface.
Embodiment 4
It will be placed in 76kg acetonitrile by kind of a 13kg base material for brilliant processing, 4kg platinum nitrate and 6kg cobalt carbonate be then added,
It stirs evenly, adds 1kg sodium alginate, form Pt/Co organic complex；Intensity be 0.2T magnetic fields under with
The revolving speed of 85r/min stirs 38min, and base material is taken out, is placed in Muffle furnace, be then passed through under protection of argon gas hydrogen into
Row pre-burning and sintering, the temperature of pre-burning are 220 DEG C, time 28min, and the temperature of sintering is 510 DEG C, time 110min, shape
At platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get substrate material surface is carried on
Array structure platinum cobalt alloy-catalyst.
Embodiment 5
It will be placed in 69 ~ 78kg ether by kind of a 14kg base material for brilliant processing, 6kg platinum nitrate and 7kg sulfuric acid be then added
Cobalt stirs evenly, and adds 2kg sodium ammonium triacetate, forms Pt/Co organic complex；In the case where intensity is the magnetic fields of 0.3T
32min is stirred with the revolving speed of 95r/min, base material is taken out, is placed in Muffle furnace, is then passed through hydrogen under protection of argon gas
Pre-burning and sintering are carried out, the temperature of pre-burning is 280 DEG C, time 23min, and the temperature of sintering is 570 DEG C, time 95min, shape
At platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get substrate material surface is carried on
Array structure platinum cobalt alloy-catalyst.
Embodiment 6
It will be placed in 73kg trichloro ethylene by kind of a 14kg base material for brilliant processing, 5kg chloroplatinic acid and 6kg nitric acid be then added
Cobalt stirs evenly, and adds 2kg sodium ethylene diamine tetracetate, forms Pt/Co organic complex；In the magnetic that intensity is 0.2 ~ 0.3T
35min is stirred with the revolving speed of 90r/min under field action, base material is taken out, is placed in Muffle furnace, then under protection of argon gas
It is passed through hydrogen and carries out pre-burning and sintering, the temperature of pre-burning is 250 DEG C, time 25min, and the temperature of sintering is 550 DEG C, and the time is
100min forms platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer.Drying is to get base is carried on
The platinum cobalt alloy-catalyst of the array structure on bottom material surface.
Claims (10)
1. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure, which is characterized in that pass through platinum salt
Form Pt/Co organic complex in organic solvent with cobalt salt, under magnetic fields, cobalt is magnetized, and drives complex groups point
It is dispersed in around kind of brilliant particle, platinum cobalt alloy array structure is formed by high-temperature heat treatment, platinum cobalt alloy-catalyst is made, preparation
Specific step is as follows:
(1) it will be placed in organic solvent by kind of a base material for brilliant processing, platinum salt and cobalt salt be then added, stirs evenly, then
Complexing agent is added, platinum salt and cobalt salt is made to form Pt/Co organic complex in organic solvent；
(2) certain time is slowly stirred under magnetic fields, cobalt is magnetized and complex groups is driven to be dispersed in base material
Around the brilliant particle of kind；
(3) base material is taken out, is placed in Muffle furnace, be then passed through hydrogen under protection of argon gas and carry out pre-burning and sintering, lead to
It crosses high-temperature heat treatment and forms platinum cobalt alloy array structure, while complex groups are carbonized to form carbon coating layer；
(4) it dries, the platinum cobalt alloy-catalyst for being carried on the array structure of substrate material surface is made.
2. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: the parts by weight of step (1) each raw material are, 12 ~ 15 parts by weight of base material, 69 ~ 78 parts by weight of organic solvent,
4 ~ 6 parts by weight of platinum salt, 5 ~ 8 parts by weight of cobalt salt, 1 ~ 2 parts by weight of complexing agent.
3. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: step (1) organic solvent is one of trichloro ethylene, ethylene glycol ether, triethanolamine, acetonitrile.
4. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: step (1) platinum salt is at least one of platinum nitrate, chloroplatinic acid, platinum tetrachloride.
5. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: step (1) cobalt salt is at least one of cobalt chloride, cobaltous bromide, cobalt carbonate, cobaltous sulfate, cobalt nitrate.
6. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: step (1) complexing agent is tartaric acid, heptose hydrochlorate, sodium gluconate, sodium alginate, sodium ammonium triacetate, second
At least one of sodium ethylene diamine tetracetate.
7. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: the intensity in step (2) described magnetic field be 0.2 ~ 0.3T, mixing speed be 80 ~ 100r/min, the time be 30 ~
40min。
8. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: the temperature of step (3) described pre-burning is 200 ~ 300 DEG C, and the time is 20 ~ 30min.
9. a kind of preparation method of the fuel cell platinum cobalt alloy-catalyst with array structure according to claim 1,
Be characterized in that: the temperature of step (3) described sintering is 500 ~ 600 DEG C, and the time is 90 ~ 120min.
10. the platinum cobalt alloy-catalyst that any one of claim 1 ~ 9 preparation method is prepared.
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| CN201810803539.9A CN108987760A (en) | 2018-07-20 | 2018-07-20 | A kind of fuel cell platinum cobalt alloy-catalyst and preparation method with array structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830376A (en) * | 2019-01-18 | 2019-05-31 | 上海大学 | The method that additional electromagnetic field auxiliary prepares metal oxide and biomass carbon combination electrode material |
| CN112993271A (en) * | 2021-02-19 | 2021-06-18 | 江苏擎动新能源科技有限公司 | Catalyst and preparation method thereof |
-
2018
- 2018-07-20 CN CN201810803539.9A patent/CN108987760A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830376A (en) * | 2019-01-18 | 2019-05-31 | 上海大学 | The method that additional electromagnetic field auxiliary prepares metal oxide and biomass carbon combination electrode material |
| CN112993271A (en) * | 2021-02-19 | 2021-06-18 | 江苏擎动新能源科技有限公司 | Catalyst and preparation method thereof |
| CN112993271B (en) * | 2021-02-19 | 2022-05-06 | 江苏擎动新能源科技有限公司 | Catalyst and preparation method thereof |
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Application publication date: 20181211 |