CN112864407B - Ordered Pt-Au/C composite catalyst, preparation method thereof and application thereof in fuel cell - Google Patents
Ordered Pt-Au/C composite catalyst, preparation method thereof and application thereof in fuel cell Download PDFInfo
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
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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
- H01M4/925—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
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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
Abstract
The invention discloses an ordered Pt-Au/C composite catalyst, a preparation method thereof and application thereof in a fuel cell. Mixing a gold source solution and a reducing agent solution for reduction reaction to obtain a nano gold cluster water solution; adding an activated nano carbon carrier material and a platinum source solution into a nano gold cluster aqueous solution, stirring and uniformly mixing, carrying out quick freezing treatment on the obtained mixed solution by adopting liquid nitrogen, and carrying out freeze drying to obtain a fluffy precursor; carrying out thermal reduction and high-temperature ordering treatment on the fluffy precursor to obtain an ordered Pt-Au/C composite catalyst; the composite catalyst has a low platinum content, a high degree of alloying, a high degree of ordering, and a high oxygen reduction catalytic activity and stability for fuel cell catalysts, the catalytic activity being better than commercial 20% pt catalysts.
Description
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) are considered to be one of the most promising energy sources for vehicle and mobile electronic device applications because of their advantages of high energy density, high efficiency and zero emission. Currently, pt-based nanoparticles supported on porous carbon particles are the predominant oxygen reduction (ORR) electrocatalysts currently used in commercial PEMFCs. Due to the scarcity of platinum, it is the subject of research to reduce the amount of Pt in the noble metal catalyst without affecting performance. Noble metals (Ag, au and Pd) having a large storage capacity and low cost have outstanding electrochemical self-stability due to their extremely high chemical inertness, and their use to form Pt-based alloy catalysts can improve the activity and stability of the catalysts. In addition, the ordered alloy catalyst formed by doping Pt with metal can greatly weaken the adsorption of the catalyst surface to the intermediate, thereby improving the catalytic Activity of ORR (Morphology and Activity Tuning of Cu)3Pt/C Ordered Intermetallic Nanoparticles by Selective Electrochemical Dealloying”，Deli Wang，Yingchao，et al.Nano Letters，2015)。
Disclosure of Invention
Aiming at the problems that the fuel cell catalyst in the prior art has high platinum content and is easy to generate Ostwald ripening and the like in a harsh operating environment of the fuel cell, and the service life is influenced. It is a first object of the present invention to provide a Pt-Au/C composite catalyst having a low platinum content, a high degree of alloying, and a high degree of ordering, which has high oxygen reduction catalytic activity and stability, the catalytic activity being superior to commercial 20-percent Pt catalysts.
The second purpose of the invention is to provide a preparation method of the Pt-Au/C composite catalyst with simple operation and low cost.
It is a third object of the present invention to provide the use of an ordered Pt-Au/C composite catalyst having a catalytic activity higher than that of the existing commercial 20% Pt catalyst.
In order to achieve the above technical object, the present invention provides a method for preparing an ordered Pt-Au/C composite catalyst, comprising the steps of:
1) Activating the nano-carbon carrier material by adopting hydrogen peroxide and nitric acid solution to obtain an activated nano-carbon carrier material;
2) Mixing a gold source solution and a reducing agent solution for reduction reaction to obtain a nano gold cluster water solution;
3) Adding an activated nano carbon carrier material and a platinum source solution into a nano gold cluster aqueous solution, stirring and uniformly mixing, carrying out quick freezing treatment on the obtained mixed solution by adopting liquid nitrogen, and carrying out freeze drying to obtain a fluffy precursor;
4) And carrying out thermal reduction and high-temperature ordering treatment on the fluffy precursor to obtain the ordered Pt-Au/C composite catalyst.
As a preferred scheme, the nano carbon carrier material is dispersed to H by ultrasonic2O2/HNO3Soaking the mixture in the mixed solution for 6 to 12 hours; said H2O2/HNO3H in the mixed solution of2O2With HNO3The molar ratio is 1:1-5. The nano-carbon carrier material is activated by adopting a mixed solution of industrial hydrogen peroxide (30%) and industrial concentrated nitric acid, centrifugally washed by adopting deionized water to be neutral after activation is finished, and freeze-dried for later use. By activating the nano carrier material, not only more attachment sites can be provided for the Pt-Au catalytic active material, but also the polar groups generated by oxidation can be utilized to adsorb gold source and platinum source ions, thereby realizing the in-situ generation of the Pt-Au catalytic active material on the carbon material, and being beneficial to improving the load stabilityIt is also good.
Preferably, the concentration of the gold source solution is 0.05 to 1M. The gold source solution comprises chloroauric acid and/or a chloroaurate salt.
In a preferred embodiment, the concentration of the reducing agent solution is 0.1 to 0.2M. The reducing agent is polypeptide with sulfydryl, the sulfydryl is used for reducing the polypeptide, the reduction process is slow, and the nano-particles with small and uniform sizes can be obtained. A specific choice may be glutathione.
As a preferable mode, the concentration of the platinum source solution is 0.05 to 1M, and the platinum source solution contains chloroplatinic acid and/or chloroplatinic acid salt.
As a preferable scheme, the nanocarbon support material is at least one of carbon black, carbon nanotubes, carbon nanowires, graphene and nano expanded graphite powder.
As a preferred embodiment, the reduction reaction conditions are: reacting for 12-24 h at the constant temperature of 65-75 ℃ under the stirring condition; wherein, the proportion of the gold source solution and the reducing agent solution is measured according to the molar ratio of the gold to the reducing agent of 1:1-1.5. The generation of the nano gold cluster is facilitated under the preferable reduction reaction condition.
As a preferred scheme, adding the activated nano carbon carrier material and the platinum source solution into the nano gold cluster water solution, and stirring for 1-2 hours at the temperature of 65-75 ℃; wherein, the proportion of the platinum source solution and the nano gold cluster water solution is measured according to the molar ratio of gold to platinum of 1. In the preferred mole ratio range of gold and platinum, the Pt-Au alloy catalytic active material with high catalytic activity and good stability can be obtained. Under the preferable stirring condition, the platinum source, the nano-gold cluster and the activated nano-carbon material can be uniformly mixed. The activated nano carbon material has more active sites and the surface contains polar groups, so that the platinum source and the nano gold cluster can be better adsorbed, and the synthesized nano gold cluster (AuNCs) has larger specific surface and can adsorb the Pt source on the surface, thereby being beneficial to the in-situ generation of the Pt-Au alloy.
The invention adopts the method of liquid nitrogen quick freezing and freeze drying to dry the sample, and aims to ensure that the activated nano carbon carrier material, the platinum source and the nano gold cluster are quickly solidified under the condition of high dispersion, thereby strengthening the dispersibility among the raw materials.
As a preferred embodiment, the thermal reduction conditions are: preserving the heat for 1.5 to 2 hours at the temperature of between 200 and 300 ℃ in a reducing atmosphere. The reducing atmosphere is a mixed gas of hydrogen and nitrogen, and H in the mixed gas2And N2The volume ratio of (a) is 1:2-4.
As a preferred scheme, the high-temperature ordering treatment conditions are as follows: preserving the heat for 1.5 to 3 hours at the temperature of between 400 and 800 ℃ in a protective atmosphere. The alloying degree and the ordering of the Pt-Au alloy can be obviously improved through proper high-temperature ordering treatment, so that the catalytic activity of the alloy catalyst is improved. The preferred high temperature ordering temperature is 500-700 ℃, when the temperature is too high, although the crystallization degree is increased, the agglomeration of the nano particles is serious, and when the temperature is too low, the alloying degree is low and the ordering is not obvious.
The invention also provides an ordered Pt-Au/C composite catalyst, which is prepared by the preparation method.
The invention also provides an application of the ordered Pt-Au/C composite catalyst, which is applied as a fuel cell catalyst.
The invention provides a preparation method of an ordered PtAu/C material, which comprises the following specific steps:
1) Preparing a gold source, a platinum source and a reducing agent into aqueous solutions respectively; the concentration of the gold source solution is as follows: 0.05-1M; the concentration of the platinum source solution is 0.05-2M; the concentration of the reducing agent solution is 0.1-0.2M; placing a certain amount of nano carbon carrier in H2O2/HNO3The mixed solution (molar ratio 1:1-5) is soaked for 6-12 h after ultrasonic dispersion, and then is centrifugally washed by deionized water to be neutral, so that the activated nano carbon carrier is obtained.
2) Mixing the gold source solution and the reducing agent solution according to the molar ratio of the Au to the reducing agent of 1:1-1.5, and then stirring at constant speed in a constant-temperature water bath at 65-75 ℃ for reaction for 12-24 h to obtain the Au NCs aqueous solution.
3) Sequentially adding an activated nano carbon carrier material and a Pt source solution into an Au NCs aqueous solution, wherein the adding amount of the Pt source is measured according to the molar ratio of Au to Pt of 1.5-1, uniformly stirring in a water bath at 65-75 ℃ for 1-2 hours, then carrying out quick freezing treatment on the mixed solution by using liquid nitrogen, and then carrying out freeze drying to obtain fluffy precursor powder;
4) And finally, carrying out high-temperature heat treatment on the fluffy precursor powder, wherein the high-temperature heat treatment process comprises the following steps: firstly, N is2And H2The mixed gas is insulated for 1.5 to 2 hours at the temperature of between 200 and 300 ℃ and then is added with N at the temperature of between 400 and 800 DEG C2And carrying out ordering treatment in the atmosphere to obtain the highly ordered PtAu/C catalyst.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
the ordered Pt-Au/C composite catalyst provided by the invention has the active component of a platinum-gold alloy, and the mass ratio of platinum is 1/3-1/2, so that the cost of the catalyst is greatly reduced.
The ordered Pt-Au/C composite catalyst provided by the invention has higher alloying degree, has a highly ordered crystal structure, shows high oxygen reduction catalytic activity and stability, and has catalytic activity superior to that of a commercial 20% Pt catalyst.
The preparation method of the ordered Pt-Au/C composite catalyst provided by the invention is simple to operate, low in cost and beneficial to large-scale production.
Drawings
FIG. 1 is a TEM image of PtAu/C catalysts prepared in examples 1 to 3.
FIG. 2 is an XRD pattern of PtAu/C catalysts prepared in examples 1 to 3.
FIG. 3 is a cyclic voltammogram of the PtAu/C catalysts prepared in examples 1 to 4.
Fig. 4 is a CV diagram of the PtAu/C catalyst prepared in example 3 before and after 5000 voltage cycles.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
In the following examples, the specific preparation method of the activated nanocarbon support material is as follows: ultrasonic dispersing nano carbon carrier material into H2O2/HNO3The mixed solution of (30%) industrial hydrogen peroxide and industrial concentrated nitric acid, wherein, H2O2With HNO31:3), soaking for 8h, then centrifugally washing with deionized water to neutrality, and freeze-drying for later use.
Example 1 (comparative example)
First, 1.5mL of GSH solution (0.1M) was added rapidly to 10mL of HAuCl at room temperature with stirring4To the solution (0.01M), stir until colorless. Subsequently, the mixed solution was stirred in an oil bath at a constant temperature of 70 ℃ for 24 hours to finally prepare an aqueous Au NCs solution. Then 50mg of activated and ultrasonically dispersed carbon black (CB, XC-72) and 1mL of H are sequentially added2PtCl6The solution (0.1M) was added to the prepared Au NCs solution with stirring. GSH to PtCl on Au NCs surface6 4+Adsorbed on the surface of Au NCs. Then adding liquid nitrogen into the slurry, quickly freezing, and freeze-drying to obtain a powdery precursor material. Finally, the precursor material is filled into a quartz boat and is subjected to H treatment at 200 DEG C2/N2(1:3) the platinum ions were reduced by incubation for 2 hours in a mixed atmosphere. From a-b in fig. 1, the prepared alloy nano particles are small in particle size, low in alloying degree and almost free of ordered structures.
Example 2
First, 1.5mL of GSH solution (0.1M) was added rapidly to 10mL of HAuCl at room temperature with stirring4In solution (0.01M), stir until colorless. And then, placing the mixed solution in an oil bath kettle, and stirring at the constant temperature of 70 ℃ for 24 hours to finally prepare the Au NCs aqueous solution. Then 50mg of activated and ultrasonically dispersed carbon black (CB, XC-72) and 1mLH are sequentially added2PtCl6The solution (0.1M) was added to the prepared Au NCs solution with stirring. GSH to PtCl on Au NCs surface6 4+Adsorbed on the surface of Au NCs. Then adding liquid nitrogen into the slurry for quick freezing, and freezing and drying to obtain the powdery catalyst. Finally, the powdered catalyst is loaded into a quartz boat, H2/N2Keeping the temperature for 2 hours under the mixed atmosphere to reduce the platinum ionsN at 400 ℃ before2And carrying out ordering heat treatment for 120min under the atmosphere. Comparing the TEM of example 2 (fig. 1C-d) with that of example 1 (fig. 1 a-b) through fig. 1, it is found that the PtAu alloy nanoparticles in the PtAu/C catalyst prepared in example 2 are increased, but the degree of alloying is increased, and the ordered structure is obvious. In addition, the catalytic performance of the PtAu/C catalyst prepared in example 2 was found to be superior to that of example 1 in the CV curve comparison of fig. 3.
Example 3
First, 1.5mL of GSH solution (0.1M) was added rapidly to 10mL of HAuCl at room temperature with stirring4To the solution (0.01M), stir until colorless. Subsequently, the mixed solution was stirred in an oil bath pan at a constant temperature of 70 ℃ for 24 hours to finally prepare an aqueous solution of Au NCs. Then sequentially mixing activated and ultrasonically dispersed 50mg of carbon black (CB, XC-72) and 1mLH2PtCl6The solution (0.1M) was added to the prepared Au NCs solution with stirring. GSH to PtCl on Au NCs surface6 4+Adsorbed on the surface of Au NCs. Then adding liquid nitrogen into the slurry for quick freezing, and freezing and drying to obtain the powdery catalyst. Finally, the powdered catalyst is loaded into a quartz boat, H2/N2The platinum ions are reduced by keeping the temperature for two hours under the mixed atmosphere and then N is added at 600 DEG C2And carrying out ordering heat treatment for 120min under the atmosphere. From FIGS. 1 c-d, it can be seen that the grain size of the alloy nanoparticles produced is increased compared to example 1, but the degree of alloying is significantly increased. Comparing the TEM of example 3 (fig. e-f) with that of example 2 (fig. C-d) with fig. 1, the PtAu alloy nanoparticles in the PtAu/C catalyst prepared in example 3 were found to be larger, but the degree of alloying was increased, and the degree of ordering was increased (fig. 1f internal diagram), indicating that the degree of ordering of the PtAu/C catalyst subjected to heat treatment at 600 ℃ was the greatest. In addition, from the XRD pattern of fig. 2, it can be found that the diffraction peak of PtAu alloy of PtAu/C heat-treated at 600 ℃ becomes sharper (the particle size becomes larger), and the diffraction peak intensity is stronger, because the extent to which PtAu, which is originally disordered, is alloyed by interaction at high temperature, increases. In the comparison of the CV curves of FIG. 3, it was found that the PtAu/C catalyst prepared in example 3 has better catalytic performance than those prepared in examples 1 and 2. From the CV curve in FIG. 4, it can be seen that the PtAu/C catalyst prepared in example 3 was stabilized at 5000 accelerationsAfter the qualitative voltage cycling, the catalytic activity was hardly decreased, indicating that the increased degree of ordering was effective in preventing ostwald ripening.
Example 4 (comparative example)
First, 1.3mL of GSH solution (0.1M) was added rapidly to 10mL of HAuCl at room temperature with stirring4To the solution (0.01M), stir until colorless. Subsequently, the mixed solution was stirred in an oil bath at a constant temperature of 70 ℃ for 24 hours to finally prepare an aqueous Au NCs solution. Then sequentially mixing activated and ultrasonically dispersed 50mg of carbon black (CB, XC-72) and 0.5mLH2PtCl6The solution (0.1M) was added to the prepared Au NCs solution with stirring. GSH to PtCl on Au NCs surface6 4+Adsorbed on the surface of Au NCs. Then adding liquid nitrogen into the slurry for quick freezing, and freezing and drying to obtain the powdery catalyst. Finally, the powdered catalyst is loaded into a quartz boat, H2/N2The platinum ions are reduced by keeping the temperature for two hours under the mixed atmosphere and then N is added at 600 DEG C2And carrying out ordering heat treatment for 120min under the atmosphere. The catalytic performance of the PtAu/C catalyst prepared in example 4 was found to be inferior to that of example 3 by comparison of the CV curves of fig. 2.
Example 5
First, 1.5mL of GSH solution (0.1M) was added rapidly to 10mL of HAuCl at room temperature with stirring4To the solution (0.01M), stir until colorless. Subsequently, the mixed solution was stirred in an oil bath pan at a constant temperature of 70 ℃ for 24 hours to finally prepare an aqueous solution of Au NCs. Then sequentially mixing activated and ultrasonically dispersed 50mg of carbon black (CB, XC-72) and 1mLH2PtCl6The solution (0.1M) was added to the prepared Au NCs solution with stirring. GSH to PtCl on Au NCs surface6 4+Adsorbed on the surface of Au NCs. Then adding liquid nitrogen into the slurry for quick freezing, and freezing and drying to obtain the powdery catalyst. Finally, the powdered catalyst is loaded into a quartz boat, H2/N2The temperature is kept for two hours under the mixed atmosphere to reduce platinum ions and then N is added at 800 DEG C2And carrying out ordering heat treatment for 120min under the atmosphere. The electrochemical performance of the nano-particles is analyzed to find that the performance of the nano-particles is not good at 600 ℃, which is mainly because the ordering degree is improved after the heat treatment at 800 ℃, but the agglomeration among the nano-particles is realizedAnd more serious, the performance is relatively reduced.
Claims (8)
1. A preparation method of an ordered Pt-Au/C composite catalyst is characterized by comprising the following steps: the method comprises the following steps:
1) Activating the nano-carbon carrier material by adopting hydrogen peroxide and nitric acid solution to obtain an activated nano-carbon carrier material;
2) Mixing a gold source solution and a reducing agent solution for reduction reaction to obtain a nano gold cluster water solution;
3) Adding an activated nano carbon carrier material and a platinum source solution into a nano gold cluster aqueous solution, stirring and uniformly mixing, carrying out quick freezing treatment on the obtained mixed solution by adopting liquid nitrogen, and carrying out freeze drying to obtain a fluffy precursor; the platinum source solution comprises chloroplatinic acid and/or chloroplatinic acid salt;
4) Carrying out thermal reduction and high-temperature ordering treatment on the fluffy precursor to obtain an ordered Pt-Au/C composite catalyst; the high-temperature ordering treatment conditions are as follows: preserving the heat for 1.5 to 3 hours at the temperature of between 500 and 700 ℃ in a protective atmosphere.
2. The method for preparing an ordered Pt-Au/C composite catalyst according to claim 1, wherein: ultrasonic dispersion of nano carbon carrier material to H2O2/HNO3Soaking the mixture in the mixed solution for 6 to 12 hours; said H2O2/HNO3H in the mixed solution of2O2With HNO3The molar ratio is 1:1-5.
3. The method for preparing an ordered Pt-Au/C composite catalyst according to claim 1, wherein:
the concentration of the gold source solution is 0.05-1M; the gold source solution comprises chloroauric acid and/or chloroaurate;
the concentration of the reducing agent solution is 0.1-0.2M, and the reducing agent is polypeptide with sulfydryl;
the concentration of the platinum source solution is 0.05-1M;
the nano carbon carrier material is at least one of carbon black, carbon nano tubes, carbon nano wires, graphene and nano expanded graphite powder.
4. The method for preparing an ordered Pt-Au/C composite catalyst according to claim 1, wherein: the reduction reaction conditions are as follows: reacting for 12-24 h at the constant temperature of 65-75 ℃ under the stirring condition; wherein, the proportion of the gold source solution and the reducing agent solution is measured according to the molar ratio of the gold to the reducing agent of 1:1-1.5.
5. The method for preparing an ordered Pt-Au/C composite catalyst according to claim 1, wherein: adding the activated nano carbon carrier material and a platinum source solution into a nano gold cluster water solution, and stirring for 1-2 h at the temperature of 65-75 ℃; wherein, the proportion of the platinum source solution and the nano gold cluster water solution is measured according to the molar ratio of gold to platinum of 1.
6. The method for preparing an ordered Pt-Au/C composite catalyst according to claim 1, wherein: the conditions of the thermal reduction are as follows: preserving the heat for 1.5 to 2 hours at the temperature of between 200 and 300 ℃ in a reducing atmosphere.
7. An ordered Pt-Au/C composite catalyst characterized by: obtained by the process of any one of claims 1 to 6.
8. The use of an ordered Pt-Au/C composite catalyst according to claim 7 wherein: as a fuel cell catalyst.
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