CN104600327A - Preparation method of carbon-supported nano platinum alloy catalyst - Google Patents
Preparation method of carbon-supported nano platinum alloy catalyst Download PDFInfo
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- CN104600327A CN104600327A CN201410820939.2A CN201410820939A CN104600327A CN 104600327 A CN104600327 A CN 104600327A CN 201410820939 A CN201410820939 A CN 201410820939A CN 104600327 A CN104600327 A CN 104600327A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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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 provides a preparation method of a carbon-supported nano platinum alloy catalyst. The method comprises the following steps: I. dispersing a Pt/C carbon-supported nano platinum catalyst in a 3d transition metal salt solution to prepare Pt/C suspension; II. drying the Pt/C suspension obtained in the step I at a temperature not higher than 80 DEG C to obtain a dried sample; III. grinding the dried sample obtained in the step II, and putting the dried sample in a reducing atmosphere to be reduced and alloyed; IV. dealloying the product obtained in the step III; washing and drying to obtain the carbon-supported nano platinum alloy catalyst. The preparation method has the advantages that the preparation method is simple; the prepared catalyst alloy particles are distributed on a carbon support uniformly and have homogeneous ingredients and high catalytic oxygen reduction property.
Description
Technical field
The present invention relates to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), belong to materials synthesis and technical field of electrochemistry.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) because of its operating temperature low (about 80 DEG C), power density is high, startup is fast, power match speed is fast etc., and advantage is subject to extensive concern.In all eurypalynous fuel cells, H
2/ air PEMFC is the first-selection of light-duty vehicle and building energy supply.
At present, hinder PEMFC principal element of extensive use on automobile be catalyst Pt to support demand too high, thus cause fuel cell car high expensive, compare with vapour/diesel vehicle and lack competitiveness.Wherein solve Pt loading problem, mainly set about, because current negative electrode platinum supports demand accounting be about 90% from reduction negative electrode platinum demand.Reduce negative electrode platinum carrying capacity, inevitable requirement exploitation have high activity, high stability catalyst and improve the utilance of catalyst.
At present, being believed to one of approach being expected to realize the reduction of negative electrode platinum carrying capacity is by Pt and 3d transition metal alloy, and alloying rear catalyst activity can improve more than 2 times.About the preparation method of this alloy catalyst is a lot of, low temperature organic liquid phase reducing process, microemulsion method, vapour deposition process, electrochemical deposition method and dipping-high temperature reduction method etc., by contrast, about the Patents of dipping high temperature reduction method is many, equipment required for the method and raw material commonplace, and process is simple and easy to manipulation, is more hopeful to realize amplification and produces and the production cost reducing alloy catalyst.But the alloy catalyst uniform component sex chromosome mosaicism that dipping-high temperature reduction legal system is standby is at present still more outstanding, and this have impact on the homogeneity of alloy catalyst performance to a great extent.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), overcome existing dipping-high temperature reduction method technology of preparing existing problems; The present invention considers from importances such as dispersing mode, solvent kind and drying modes, a kind of carbon-supported nano alloy catalyst (Pt-alloy/C) synthetic method being simple and easy to realize catalyst homogeneity is provided, adopt made by the method catalyst alloy particle be evenly distributed on carbon, uniform component, and catalytic oxidation-reduction performance is high.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), described preparation method comprises the steps:
Step one, Pt/C carbon-supported nano platinum catalyst to be dispersed in 3d transition metal salt solution, to be prepared into Pt/C suspension;
Step 2, step one gained Pt/C suspension is dry under≤80 DEG C of conditions, obtain drying sample;
Step 3, by step 2 gained drying sample grind, be placed in reducing atmosphere reduction and alloying;
Step 4, product that step 3 obtains is carried out de-alloy treatment; Namely carbon-supported nano platinum alloy catalyst (Pt-alloy/C) is obtained after washing, drying.
Preferably, in step one, the method for described dispersion be standard machinery stir, shear, ultrasonic in one or more.
Preferably, in step one, described 3d transition metal salt solution comprises 3d transition metal salt, non-3d transition metal salt, solvent;
Preferably, described 3d transition metal salt comprises the nitrate of copper, cobalt, nickel, iron, manganese and chromium, sulfate, chlorate, carbonate, acetate, formates or oxalates.
Preferably, described non-3d transition metal salt comprises palladium, rhodium, iridium, osmium, ruthenium, golden chloride, bromide or chlorine complexing hydrochlorate.
Preferably, described palladium, rhodium, iridium, osmium, ruthenium, gold chlorine complexing hydrochlorate comprise palladium bichloride, palladium bromide, potassium chloropalladate, palladium, rhodium chloride, chlorine rhodium acid ammonium, chlordene rhodium acid potassium, iridous chloride, iridic chloride, chloro-iridic acid, potassium osmate, Osmium Potassium Chloride, ruthenium trichloride, ruthenium hydrochloride ammonium, gold chloride, gold trichloride, sodium terachloraurate or tetra chlorauric acid ammonia.
Preferably, in described 3d transition metal salt solution, solvent is one or more mixed solvents in water, isopropyl alcohol, ethanol, methyl alcohol, ether, acetone, DMF, ethylene glycol, glycerine.
Preferably, described 3d transition metal salt, the metallic atom molar concentration of non-3d transition metal salt in 3d transition metal salt solution are respectively 0.20 ~ 1.0mol/L, 0.01 ~ 0.15mol/L.
Preferably, step one, in described Pt/C carbon-supported nano platinum catalyst and 3d transition metal salt solution, the mass ratio of solvent is 1:(5 ~ 20).
Preferably, in step 2, described drying means is natural drying, heat drying, freeze drying, vacuumize or spraying dry.
Preferably, in step 3, described alloying temperature is 600 ~ 1000 DEG C; Described alloying specifically refers under alloying temperature, and the Platinum Nanoparticles in Pt/C carbon-supported nano platinum catalyst on carbon carrier forms alloy with the metal in the 3d solution be reduced.
Preferably, in step 3, described reducing atmosphere is specially H
2/ N
2mist or H
2/ Ar mist; Wherein, the volume fraction of hydrogen is less than 20%.
Preferably, in step 4, the method for described de-alloy treatment comprises acidleach and takes off alloy or electrochemistry takes off alloy; The mode of washing comprises filter membrane dialysis or filter type; It is dry that drying mode comprises vacuumize, spraying dry, freeze drying or common heating.
Preferably, described acidleach takes off sulfuric acid or the nitric acid that alloy adopts 1M, and condition is 60 ~ 80 DEG C, 12 ~ 48h.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention can significantly improve the composition of nanometer alloy catalyst, distribution and performance uniformity by the solvent composition and solvent burden ratio changing 3d transition metal salt solution;
(2) the present invention can significantly improve the composition of alloy catalyst, distribution and performance uniformity by the dispersing technology of 3d transition metal salt suspensioning liquid improved containing Pt/C;
(3) the present invention can improve reduction reaction (ORR) catalytic activity of alloy catalyst by optimized alloy temperature range and de-alloy condition, and the mass ratio recorded under 0.9V voltage activity is 0.40A/mg
pt, area specific activity is 0.66mA/cm
pt 2.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is Pt-alloy/C TEM photo;
Fig. 2 is the active graph of a relation with cell voltage of the Pt mass ratio that obtains of fuel cell test.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), and described method comprises the steps:
Step 1, adds to 6g Pt/C carbon-supported nano platinum catalyst (platinum content is 30wt%) containing Co (NO under standard machinery stirring condition
3)
26H
2o 16.17g and HAuCl
43H
2the 60ml water of O 0.47g, alcohol mixed solution (volume ratio of water and ethanol is 2:1), follow-up employing is ultrasonic stirs with standard machinery the dispersing mode combined, ultrasonic 30mins, and standard machinery stirs 30mins, repeats twice, obtains suspension;
Step 2, is heated to 80 DEG C by the suspension in step 1 under standard machinery stirring condition, freeze-day with constant temperature 12h;
Step 3, by the drying sample grinding in step 2, is then placed in 10%H
2/ N
2in gaseous mixture, be heated to 800 DEG C, constant temperature 12h;
Step 4, is placed in the 1M HNO of 80 DEG C by the sample obtained in step 3
3de-alloy treatment 48h in solution, washing and filtering is 80 DEG C of vacuumize 8h also.
Effect: as shown in Figure 1, the distribution of alloy nanoparticle on carbon is more even for the TEM photo of embodiment 1 prepared catalyst.As shown in Figure 2, its value is 0.40A/mg to the mass ratio activity recorded under 0.9V voltage
pt.
embodiment 2
The present embodiment is the change case of embodiment 1, and other implementation condition is with embodiment 1, and change part is: the solvent in step 1, changes pure water solvent into by the mixed solvent of water and ethanol.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.31A/mg
pt.
embodiment 3
The present embodiment is the change case of embodiment 1, and other implementation condition is with embodiment 1, and change part is: the acid solution in step 4, by 1M HNO
3solution changes 1M H into
2sO
4solution.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.30A/mg
pt.
embodiment 4
The present embodiment is the change case of embodiment 2, and other implementation condition is with embodiment 2, and change part is only: the drying mode in step 2, changes freeze drying into by heat drying.
Effect: the mass ratio activity recorded under 0.9V voltage is 0.34A/mg
pt.
embodiment 5
The present embodiment is the change case of embodiment 1, and other implementation condition is with embodiment 1, and change part is: the alloying temperature in step 3 changes 900 DEG C into by 800 DEG C.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.34A/mg
pt.
embodiment 6
The present embodiment is the change case of embodiment 1, and other implementation condition is with embodiment 1, and change part is: the alloying temperature in step 3 changes 700 DEG C into by 800 DEG C.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.30A/mg
pt.
embodiment 7
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1, Co (NO
3)
26H
2the concentration of O is 0.20mol/L, HAuCl
43H
2the concentration of O is 0.15mol/L.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.43A/mg
pt.
embodiment 8
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1,3d transition metal salt is copper chloride, and non-3d transition metal salt is iridic chloride.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.41A/mg
pt.
embodiment 9
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1, the mass ratio of Pt/C carbon-supported nano platinum catalyst and solvent is 1:5.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.44A/mg
pt.
embodiment 10
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1, the mass ratio of Pt/C carbon-supported nano platinum catalyst and solvent is 1:20.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.40A/mg
pt.
embodiment 11
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1, in step 3, alloying temperature is 600 DEG C.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.34A/mg
pt.
embodiment 12
The present embodiment is the change case of embodiment 1, and other conditions are identical with embodiment 1, and change part is: in step 1, in step 3, alloying temperature is 1000 DEG C.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by the present embodiment records under 0.9V voltage is 0.38A/mg
pt 2.
comparative example 1
This comparative example is the comparative example of embodiment 1, and other condition is with embodiment 1, and difference is: the solvent volume in step 1 becomes 300ml from 60ml, and the quality of Pt/C carbon-supported nano platinum catalyst is 30g, now Co (NO
3)
26H
2o concentration is less than 0.2mol/L, HAuCl
43H
2the concentration of O is less than 0.01mol/L.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by this comparative example records under 0.9V voltage is 0.28A/mg
pt.
comparative example 2
This comparative example is the comparative example of embodiment 1, and other condition is with embodiment 1, and difference is: the alloying temperature in step 3 changes 1200 DEG C into by 800 DEG C.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by this comparative example records under 0.9V voltage is 0.20A/mg
pt.
comparative example 3
This comparative example is the comparative example of embodiment 1, and other condition is with embodiment 1, and difference is: the time of the de-alloy treatment in step 4 becomes 6h from 48h.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by this comparative example records under 0.9V voltage is 0.31A/mg
pt.
comparative example 4
This comparative example is the comparative example of embodiment 1, and other condition is with embodiment 1, and difference is: the constant temperature time in step 4 becomes 55h from 48h.
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by this comparative example records under 0.9V voltage is 0.26A/mg
pt.
comparative example 5
This comparative example is the comparative example of embodiment 1, and other condition is with embodiment 1, and difference is: the constant temperature time in step 4 becomes 10h from 48h.。
Effect: the mass ratio activity that carbon-supported nano platinum alloy catalyst prepared by this comparative example records under 0.9V voltage is 0.30A/mg
pt.
comparative example 6
This comparative example is the comparative example of comparative example 1, and difference is, the Pt/C carbon-supported nano platinum catalyst of this comparative example without the process of step one to four, direct-detection performance: the mass ratio activity recorded under 0.9V voltage is 0.13A/mg
pt.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (9)
1. a preparation method for carbon-supported nano platinum alloy catalyst, is characterized in that, described preparation method comprises the steps:
Step one, Pt/C carbon-supported nano platinum catalyst to be dispersed in 3d transition metal salt solution, to be prepared into Pt/C suspension;
Step 2, step one gained Pt/C suspension is dry under≤80 DEG C of conditions, obtain drying sample;
Step 3, by step 2 gained drying sample grind, be placed in reducing atmosphere reduction and alloying;
Step 4, product that step 3 obtains is carried out de-alloy treatment; Carbon-supported nano platinum alloy catalyst is obtained after washing, drying.
2. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step one, the method for described dispersion be mechanical agitation, shearing, ultrasonic in one or more.
3. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step one, described 3d transition metal salt solution comprises 3d transition metal salt, non-3d transition metal salt, solvent;
Described 3d transition metal salt comprises the nitrate of copper, cobalt, nickel, iron, manganese and chromium, sulfate, chlorate, carbonate, acetate, formates or oxalates;
Described non-3d transition metal salt comprises palladium, rhodium, iridium, osmium, ruthenium, golden chloride, bromide or chlorine complexing hydrochlorate;
Described solvent is one or more mixed solvents in water, isopropyl alcohol, ethanol, methyl alcohol, ether, acetone, DMF, ethylene glycol, glycerine.
4. the preparation method of the carbon-supported nano platinum alloy catalyst according to claim 1 or 3, is characterized in that, in step one, in described Pt/C carbon-supported nano platinum catalyst and 3d transition metal salt solution, the mass ratio of solvent is 1:(5 ~ 20).
5. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step 2, the method for described drying comprises natural drying, heat drying, freeze drying, vacuumize or spraying dry.
6. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step 3, the temperature of described alloying is 600 ~ 1000 DEG C.
7. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step 3, described reducing atmosphere is specially H
2/ N
2mist or H
2/ Ar mist; Wherein, the volume fraction of hydrogen is less than 20%.
8. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, is characterized in that, in step 4, the method for described de-alloy treatment comprises acidleach and takes off alloy or electrochemistry takes off alloy; The mode of washing comprises filter membrane dialysis or filter type; It is dry that drying mode comprises vacuumize, spraying dry, freeze drying or common heating.
9. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 8, is characterized in that, described acidleach takes off sulfuric acid or the nitric acid that alloy adopts 1M, and condition is 60 ~ 80 DEG C, 12 ~ 48h.
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Cited By (9)
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CN106960962A (en) * | 2017-04-26 | 2017-07-18 | 北京化工大学 | A kind of platinum base of polyaniline-coated carbon carrier takes off alloy fuel cell catalyst and preparation method thereof |
CN107088415A (en) * | 2017-04-10 | 2017-08-25 | 南京大学 | A kind of preparation method of platinum alloy nanometer powder catalyst |
CN108786791A (en) * | 2018-06-10 | 2018-11-13 | 江苏经贸职业技术学院 | A method of synthesis pt atom cluster is heat-treated based on complexing |
CN109390592A (en) * | 2017-08-04 | 2019-02-26 | 上海汽车集团股份有限公司 | A kind of membrane electrode and preparation method thereof |
CN111092235A (en) * | 2019-12-27 | 2020-05-01 | 苏州擎动动力科技有限公司 | Platinum-cobalt alloy catalyst and preparation method thereof |
CN111725525A (en) * | 2020-06-18 | 2020-09-29 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
CN114628699A (en) * | 2022-04-01 | 2022-06-14 | 南京大学 | Preparation method of noble metal alloy/carbon material supported catalyst |
CN114784305A (en) * | 2022-02-16 | 2022-07-22 | 同济大学 | Multi-component platinum alloy carbon-supported catalyst doped with non-metallic elements and preparation method thereof |
WO2023109510A1 (en) * | 2021-12-17 | 2023-06-22 | 华南理工大学 | Fuel cell carbon-supported platinum-based anti-reverse electrode catalyst that has undergone surface modification using small amount of highly dispersed iridium, preparation method therefor, and use thereof |
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CN107088415B (en) * | 2017-04-10 | 2020-05-08 | 南京大学 | Preparation method of platinum alloy nano powder catalyst |
CN106960962A (en) * | 2017-04-26 | 2017-07-18 | 北京化工大学 | A kind of platinum base of polyaniline-coated carbon carrier takes off alloy fuel cell catalyst and preparation method thereof |
CN109390592B (en) * | 2017-08-04 | 2021-12-31 | 上海汽车集团股份有限公司 | Membrane electrode and preparation method thereof |
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CN111725525A (en) * | 2020-06-18 | 2020-09-29 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
CN111725525B (en) * | 2020-06-18 | 2022-03-15 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
WO2023109510A1 (en) * | 2021-12-17 | 2023-06-22 | 华南理工大学 | Fuel cell carbon-supported platinum-based anti-reverse electrode catalyst that has undergone surface modification using small amount of highly dispersed iridium, preparation method therefor, and use thereof |
CN114784305A (en) * | 2022-02-16 | 2022-07-22 | 同济大学 | Multi-component platinum alloy carbon-supported catalyst doped with non-metallic elements and preparation method thereof |
CN114628699A (en) * | 2022-04-01 | 2022-06-14 | 南京大学 | Preparation method of noble metal alloy/carbon material supported catalyst |
CN114628699B (en) * | 2022-04-01 | 2024-05-28 | 南京大学 | Preparation method of noble metal alloy/carbon material supported catalyst |
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