CN111640956B - Method for preparing carbon-supported platinum electrocatalyst for fuel cell - Google Patents
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 79
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000446 fuel Substances 0.000 title claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 8
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012876 carrier material Substances 0.000 claims abstract description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- -1 alkali metal formate Chemical class 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000002245 particle Substances 0.000 abstract description 30
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 16
- 238000006722 reduction reaction Methods 0.000 description 13
- 229910000510 noble metal Inorganic materials 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229920005862 polyol Polymers 0.000 description 5
- 150000003077 polyols Chemical class 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000012430 stability testing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 239000004280 Sodium formate Substances 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- UBZYWIKLAYTIOV-UHFFFAOYSA-N [Na].CC=O Chemical compound [Na].CC=O UBZYWIKLAYTIOV-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
Classifications
-
- 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
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
Abstract
The invention provides a method for preparing a carbon-supported platinum electrocatalyst for a fuel cell, which comprises the steps of dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, standing for a certain time, adding a reducing agent compound and a carbon carrier material into the solution, reacting for a certain time, and finally carrying out subsequent treatment of filtering, washing and drying on the reacted system to obtain the carbon-supported platinum electrocatalyst. The preparation method can stably react newly generated platinum nanoparticles, effectively avoid agglomeration of the generated platinum particles, ensure that the loaded metal platinum particles have excellent isotropic performance, small particle size and uniform distribution, and effectively improve the catalytic activity and stability.
Description
Technical Field
The invention relates to a preparation method of a catalyst, in particular to a method for preparing a carbon-supported platinum electrocatalyst for a fuel cell.
Background
At present, the core active material of the fuel cell is still mature as carbon-supported platinum noble metal. The preparation of catalysts by chemical reduction is the most common method used at present. Including dip reduction and polyol reduction. The solid-phase dipping reduction method comprises the steps of dipping a platinum noble metal precursor and a carrier, drying and grinding the platinum noble metal precursor and the carrier, and introducing hydrogen into a tubular furnace for reduction at high temperature (generally more than 200 ℃), wherein the method has high energy consumption and the noble metal is unevenly distributed on the carbon carrier; the liquid phase dipping reduction method is that firstly, a noble metal precursor and a carbon carrier are dipped, and then a strong reducing agent is added for room temperature reduction, although the method is simple, rapid and has no energy consumption, the prepared electro-catalyst has large grain diameter and uneven grain diameter distribution. The most common polyol reduction method is that glycol and other polyols are used as a solvent and a reducing agent at the same time, the noble metal precursor is reduced into the electrocatalyst by heating (120-160 ℃) for 3-8 hours, and the electrocatalyst prepared by the method has small particle size and uniform dispersion because the polyols play a role of a protective agent at the same time, and has the defects of high energy consumption, incapability of recycling and high cost due to the oxidation of the glycol and other polyols in the reaction process. In addition, the platinum particles prepared by these chemical reduction methods have poor stability and still have unsatisfactory catalytic activity because they are anisotropic and have a large particle size and are easily aged and grown during use.
Disclosure of Invention
The invention aims to provide a method for preparing a spherical carbon-supported platinum electrocatalyst with uniform platinum noble metal particle size distribution, small particle size and isotropic performance. The invention is realized by the following scheme.
A method for preparing a carbon-supported platinum electrocatalyst for a fuel cell is implemented according to the following steps in sequence:
dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, keeping the pH value of the solution at 3-8, and standing for 24-72 hours at 10-40 ℃; the platinum precursor compound is selected from one or more of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, potassium chloroplatinate or sodium chloroplatinate, the complexing agent is selected from one or more of formaldehyde, acetaldehyde, citric acid and sodium citrate, and the auxiliary inorganic salt compound is selected from one or more of nitric acid of alkali metal and halide of alkali metal;
(II) adding a reducing agent compound and a carbon carrier material into the solution after standing in the step I, and reacting for 30-180 minutes at 20-50 ℃; the reducing agent compound is selected from one or more of ascorbic acid, formic acid, acetic acid, alkali metal formate, alkali metal acetate, acetaldehyde and alkali metal acetaldehyde compound; the carbon carrier is one or more of carbon black, activated carbon, carbon nanotubes, carbon fibers and graphene;
(III) carrying out subsequent treatment including filtration, washing and drying on the solution obtained after the reaction in the step II, wherein the subsequent treatment can be carried out by adopting the same method in the prior art, and the solution is washed to be neutral and then is dried.
In the step I, the molar ratio of platinum of the platinum precursor compound to the complexing agent is 1 (1-20), and the reaction is more complete.
In the step I, the molar ratio of platinum of the platinum precursor compound to the auxiliary inorganic salt compound is 1 (5-30), so that granular agglomeration can be effectively prevented in the subsequent reduction reaction.
And in the second step, adding the reducing agent compound according to the molar ratio of the reducing agent compound to platinum of the platinum precursor compound of (10-50) to 1, so that the reaction is more complete.
In the step II, when the molar concentration of the reducing agent compound is 0.01-0.05 mol/L, the reaction of reducing platinum is more moderate, and the particles are not agglomerated.
And in the second step, adding a carbon carrier material according to the mass ratio of the platinum to the carbon of the platinum precursor compound of 20-70%.
Compared with the existing method for preparing the carbon-supported platinum electrocatalyst for the fuel cell, the method has the following advantages:
1. in the preparation method, because the auxiliary inorganic salt compound is added in the step I, the newly generated platinum nano particles can be stably reacted, the agglomeration of the generated noble metal platinum particles is effectively avoided, and the utilization rate of platinum can be improved.
2. The preparation method adopts a two-step method, namely the reducing agent is added after the solution in the step I is kept still for a certain time, so that the carbon-supported platinum electrocatalyst-supported metal platinum particles with excellent isotropy and uniform particle size distribution can be prepared, the average particle size is 1.0-2.5 nm, the platinum particles prepared by the existing one-step method are in a fork shape, the average particle size is about 3.0-7.0 nm, and the platinum particles are anisotropic.
3. The catalytic activity of the carbon-loaded platinum electrocatalyst prepared by the method is greater than 0.2A/mg Pt @0.9V RHE, and the catalytic activity performance of the carbon-loaded platinum electrocatalyst is improved by more than 60% compared with that of the existing catalyst.
4. The preparation method has the advantages of mild conditions, easy batch preparation, easily controlled process and lower energy consumption.
Drawings
FIG. 1 Transmission Electron microscopy of carbon-Supported platinum electrocatalyst for example 1
FIG. 2 Transmission Electron microscopy of carbon-Supported platinum electrocatalyst for comparative example 1
FIG. 3 particle size distribution diagram of carbon-supported platinum electrocatalyst according to example 1
Detailed Description
Example 1
A method for preparing a carbon-supported platinum electrocatalyst for a fuel cell is implemented according to the following steps in sequence:
dissolving 0.1mmol of chloroplatinic acid, 1mmol of sodium citrate and 0.5mmol of sodium nitrate in water to form a solution, adjusting the pH value of the solution to be 3-5 by using sodium hydroxide, and standing the solution at 10 ℃ for 72 hours;
(II) adding 100ml of ascorbic acid with a concentration of 0.01mol/L and 80 mg of activated carbon to the solution after the standing in the step I, and reacting at 20 ℃ for 180 minutes.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
In the carbon-supported platinum electrocatalyst prepared through the above steps, the existing commercialized carbon-supported platinum electrocatalyst with the same platinum loading capacity (for example, the platinum-carbon catalyst of JM company in england) is used as comparative example 1, and transmission electron microscopes under the same conditions are respectively shown in fig. 1 and 2, fig. 1 is the carbon-supported platinum electrocatalyst of the embodiment 1, and fig. 2 is the carbon-supported platinum electrocatalyst of the comparative example 1, and it is apparent from comparing the two figures that the metal platinum particles supported by the carbon-supported platinum electrocatalyst of the embodiment 1 are not agglomerated, while the metal platinum supported by the carbon-supported platinum electrocatalyst of the comparative example 1 is in a significant branch shape, which indicates that a certain amount of agglomeration exists. In contrast, the platinum particles supported by the carbon-supported platinum electrocatalyst in example 1 are spherical, and the isotropy is substantially good for the utilization efficiency of the noble metal platinum when used as a catalyst.
The particle size distribution of the platinum particles supported on the carbon-supported platinum electrocatalyst according to the present example is shown in fig. 3, from which it can be seen that the average particle size is 2.0nm and the particle size distribution is uniform.
Electrochemical tests show that the catalyst prepared in the example has an electrochemical active area of 110m2·g-1(ii) a At 0.5mol · L-1H2SO4In solution at 50mV s-1The scan speed of (2) was scanned for 2000 revolutions, and then the electrochemically active area decay of the catalyst was calculated. It was found that the catalyst, after stability testing, had 90% electrochemically active area remaining, whereas the catalyst of comparative example 1 had 25% electrochemically active area remaining under the same testing conditions. The catalyst prepared in example 1 had an oxygen reduction mass activity of 0.22 A.g at 0.9V (vs. standard hydrogen electrode)-1Is more commercially catalyzedThe mass activity of the agent is 83 percent.
Example 2
A method for preparing a carbon-supported platinum electrocatalyst is implemented according to the following steps in sequence:
dissolving 0.1mmol of potassium chloroplatinite, 2mmol of acetaldehyde and 3mmol of potassium chloride in water to form a solution, adjusting and maintaining the pH value of the solution to be 4-8 by using potassium hydroxide, and standing for 50 hours at 30 ℃;
(II) adding 100ml of sodium formate with the concentration of 0.05mol/L and 28 mg of carbon fiber into the solution after standing in the step I, and reacting for 30 minutes at 50 ℃.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
The carbon-supported platinum electrocatalyst prepared by the steps is basically free of agglomeration after being observed by a transmission electron microscope, and the average particle size of the metal platinum particles supported by the carbon-supported platinum electrocatalyst is 2.4nm and the particle size distribution is uniform through a particle size test.
Electrochemical tests found that the catalyst prepared in this example had an electrochemically active area of 85m2·g-1(ii) a At 0.5mol · L-1H2SO4In solution at 50mV s-1The scan speed of (2) was scanned for 2000 revolutions, and then the electrochemically active area decay of the catalyst was calculated. It was found that the catalyst prepared in this example 2 had an oxygen reduction mass activity of 0.24A g at 0.9V (relative to a standard hydrogen electrode) at 88% electrochemically active area remaining after stability testing of the catalyst-1。
Example 3
A method for preparing a carbon-supported platinum electrocatalyst is implemented according to the following steps in sequence:
dissolving 0.1mmol of sodium chloroplatinate, 0.1mmol of sodium citrate and 1.5mmol of sodium nitrate in water to form a solution, adjusting and maintaining the pH value of the solution to be 3-7 by using sodium hydroxide, and standing for 24 hours at 40 ℃;
(II) adding 60ml of acetaldehyde sodium with the concentration of 0.05mol/L and 25 mg of carbon nano tubes into the solution after standing in the step I, and reacting for 120 minutes at the temperature of 30 ℃.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
The carbon-supported platinum electrocatalyst prepared by the steps is basically free of agglomeration through transmission electron microscope observation, and the average particle size of the metal platinum particles supported by the carbon-supported platinum electrocatalyst is 2.2nm through particle size distribution test, and the particle size distribution is uniform.
Electrochemical tests found that the catalyst prepared in this example had an electrochemically active area of 88m2·g-1(ii) a At 0.5mol · L-1H2SO4In solution at 50mV s-1The scan speed of (2) was scanned for 2000 revolutions, and then the electrochemically active area decay of the catalyst was calculated. It was found that the catalyst prepared in example 3 had an oxygen reduction mass activity of 0.21A g at 0.9V (relative to a standard hydrogen electrode) at 87% of the electrochemically active area remaining after stability testing of the catalyst-1。
Claims (6)
1. A method for preparing a carbon-supported platinum electrocatalyst for a fuel cell, characterized by: the method is implemented according to the following steps in sequence,
dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, keeping the pH value of the solution at 3-8, and standing for 24-72 hours at 10-40 ℃; the platinum precursor compound is selected from one or more of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, potassium chloroplatinate or sodium chloroplatinate, the complexing agent is selected from one or more of formaldehyde, acetaldehyde, citric acid and sodium citrate, and the auxiliary inorganic salt compound is selected from one or more of nitric acid of alkali metal and halide of alkali metal;
(II) adding a reducing agent compound and a carbon carrier material into the solution after standing in the step I, and reacting for 30-180 minutes at 20-50 ℃; the reducing agent compound is selected from one or more of ascorbic acid, formic acid, acetic acid, alkali metal formate, alkali metal acetate, acetaldehyde and alkali metal acetaldehyde compound; the carbon carrier is one or more of carbon black, activated carbon, carbon nanotubes, carbon fibers and graphene;
(III) carrying out subsequent treatment comprising filtration, washing and drying on the solution obtained after the reaction in the step II.
2. The method for preparing a carbon-supported platinum electrocatalyst for a fuel cell according to claim 1, wherein: in the step I, the molar ratio of platinum of the platinum precursor compound to the complexing agent is 1 (1-20).
3. The method for producing a carbon-supported platinum electrocatalyst for a fuel cell according to claim 1 or 2, characterized in that: in the step I, the molar ratio of platinum of the platinum precursor compound to the auxiliary inorganic salt compound is 1 (5-30).
4. The method for producing a carbon-supported platinum electrocatalyst for a fuel cell according to claim 1 or 2, characterized in that: and in the second step, adding a reducing agent compound according to the molar ratio of the reducing agent compound to platinum of the platinum precursor compound of (10-50) to 1.
5. The method for producing a carbon-supported platinum electrocatalyst for a fuel cell according to claim 4, wherein: and in the step II, adding a reducing agent compound with the molar concentration of 0.01-0.05 mol/L.
6. The method for producing a carbon-supported platinum electrocatalyst for a fuel cell according to claim 1 or 2, characterized in that: and in the second step, adding a carbon carrier material according to the use amount of the platinum precursor compound with the mass ratio of platinum to carbon of 20-70%.
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| CN114243038A (en) * | 2021-12-07 | 2022-03-25 | 中国科学院山西煤炭化学研究所 | High-voltage corrosion-resistant platinum-carbon catalyst and preparation method thereof |
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|---|---|---|---|---|
| CN108963273A (en) * | 2018-06-27 | 2018-12-07 | 华南理工大学 | A kind of branch shape platinum elctro-catalyst and the preparation method and application thereof |
| CN109014237A (en) * | 2018-07-12 | 2018-12-18 | 西安交通大学 | A kind of platinum-non-noble metal alloy nano wire and its aqueous synthesis method and application |
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2020
- 2020-06-11 CN CN202010527333.5A patent/CN111640956B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108963273A (en) * | 2018-06-27 | 2018-12-07 | 华南理工大学 | A kind of branch shape platinum elctro-catalyst and the preparation method and application thereof |
| CN109014237A (en) * | 2018-07-12 | 2018-12-18 | 西安交通大学 | A kind of platinum-non-noble metal alloy nano wire and its aqueous synthesis method and application |
Non-Patent Citations (1)
| Title |
|---|
| Stable and active Pt colloid preparation by modified citrate reduction and a mechanism analysis of inorganic additives;Yuexia Li等;《Journal of Colloid and Interface Science》;20200320;第572卷;第74-82页 * |
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