CN110767915A - Silver-manganese bimetallic composite catalyst for oxygen reduction reaction in alkaline medium and synthesis method thereof - Google Patents
Silver-manganese bimetallic composite catalyst for oxygen reduction reaction in alkaline medium and synthesis method thereof Download PDFInfo
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- CN110767915A CN110767915A CN201911118661.3A CN201911118661A CN110767915A CN 110767915 A CN110767915 A CN 110767915A CN 201911118661 A CN201911118661 A CN 201911118661A CN 110767915 A CN110767915 A CN 110767915A
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- H01M4/00—Electrodes
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- H01M4/90—Selection of catalytic material
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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
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
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- 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 a silver-manganese bimetallic composite catalyst for oxygen reduction reaction in an alkaline medium and a synthesis method thereof. The invention prepares colloid silver-manganese composite metal particles with manganese element atom content of 2-25% by a chemical reduction method. Then the metal nano particles are loaded on activated carbon to prepare a corresponding carbon-loaded nano silver-manganese composite metal catalyst, and the performance of the carbon-loaded nano silver-manganese composite metal catalyst as an oxygen reduction electrocatalyst is further researched, so that the catalyst shows good catalytic performance in an alkaline electrolyte.
Description
Technical Field
The invention belongs to the technical field of preparation of oxygen reduction electrocatalysts, and particularly relates to a bimetallic nano catalyst for oxygen reduction reaction in an alkaline medium and a preparation method thereof.
Background
Fuel cell technology is a very promising energy conversion technology, which directly converts chemical energy into electrical energy, and thus has high energy conversion efficiency and environmental friendliness. Over the past few decades, research and development of fuel cells has made a series of important advances. Proton exchange membrane fuel cells are the main subject of research on this technology, but due to the corrosion problem caused by the acidity of the electrolyte, the catalyst of the proton exchange membrane fuel cells depends heavily on the noble metal Pt, which results in increased cell cost and hinders further commercialization of this technology. Hydrogen-oxygen exchange membrane fuel cells employing alkaline electrolytes have received increasing attention in recent years because cheaper catalysts and bipolar plates can be used, which will be far less costly than proton exchange membrane fuel cells.
In a hydrogen-oxygen exchange membrane fuel cell, an Ag-based oxygen reduction catalyst is considered as the most promising cathode catalyst for replacing Pt, the price of Ag is only 1/50 of Pt, and the Ag has better electrochemical stability under alkaline conditions. The Ag-based catalyst is the cathode catalyst which does not contain platinum group metal and has the best performance in the hydrogen-oxygen exchange membrane fuel cell application at present, but has certain difference with the catalytic performance of Pt. The rotating disc test shows that the specific surface area activity of Ag is only about one tenth of that of Pt, and the half-wave potential of the oxygen reduction reaction is about 150mV lower than that of Pt. Further development of highly efficient Ag-based catalysts to completely replace Pt still requires a great deal of research work.
Disclosure of Invention
The invention aims to provide a novel composite catalyst for oxygen reduction reaction in an alkaline medium and a preparation method thereof, and solves the problems of low oxygen reduction electrocatalytic activity and low electrochemical stability of the existing silver-based nano catalyst.
The invention provides a composite catalyst for an oxygen reduction reaction in an alkaline medium, which comprises silver-manganese bimetal composite particles.
According to the invention, transition metal Mn is added into Ag nano particles to prepare the silver-manganese composite metal nano catalyst, so that a novel oxygen reduction nano catalyst is obtained. Compared with the traditional silver-based oxygen reduction catalyst, the novel composite catalyst provided by the invention has the advantages that the electrocatalytic performance and the electrochemical stability of the oxygen reduction reaction are obviously improved.
In some embodiments, the atomic ratio of the silver element in the silver-manganese bimetal composite particle ranges from 75% to 98%, and the atomic ratio of the manganese element in the silver-manganese bimetal composite particle ranges from 2% to 25%.
In some embodiments, the silver manganese bimetal composite particles have an average particle size ranging from 2 to 50 nm.
In some embodiments, the silver manganese bimetal composite particles have an average particle size ranging from 5 to 20 nm.
By controlling the element composition and the particle size range of the silver-manganese bimetal composite particles, the performance of the composite catalyst can be optimized, and the composite catalyst is suitable for different application scenes. Within the above preferred mass ratio range and particle size range, the composite catalyst of the present invention shows superior electrocatalytic performance as well as electrochemical stability.
In some embodiments, the composite catalyst includes a support material and silver-manganese bimetallic composite particles distributed on the surface of the support material.
In some embodiments, the support material comprises a one-, two-, or three-dimensional structure of a carbon material or a metal oxide material.
The invention also provides a synthetic method of the composite catalyst, which comprises the following steps: forming a precursor solution comprising a silver source and a manganese source; heating the precursor solution to a preset temperature, and maintaining the preset reaction time to form a reaction solution in which the composite catalyst is dispersed; separating and purifying the reaction solution to obtain the composite catalyst nano-particles.
In some embodiments, the synthesis methods are all formed in an oxygen-scavenging environment.
In some embodiments, the predetermined temperature range is 180 ℃ to 240 ℃ and the predetermined reaction time is 0.5 to 4 hours.
In some embodiments, the separated and purified composite catalyst particles are supported on a support material.
The synthetic method is simple to operate, can obtain the high-performance catalyst suitable for the oxygen reduction reaction in the alkaline medium, has uniform particle size distribution, and obviously improves the electrocatalytic performance and the electrochemical stability.
Drawings
Fig. 1 is an XRD pattern of silver manganese composite metal nanoparticles obtained in example 1 of the present invention;
FIG. 2 is a TEM image of silver manganese composite metal nanoparticles of the present invention obtained from example 1;
FIG. 3 is a TEM image of the silver manganese composite metal nanoparticles of the present invention obtained from example 2;
FIG. 4 is a TEM image of the silver-manganese metal nanoparticles on carbon obtained in example 1;
FIG. 5 is a polarization curve of oxygen reduction test of the catalysts obtained in examples 1 to 4 and comparative example 1;
FIG. 6 is an oxygen reduction accelerated aging test curve for the silver manganese on carbon composite catalyst of example 1;
FIG. 7 is an oxygen reduction accelerated aging test curve for the silver nanoparticle catalyst of comparative example 1;
FIG. 8 is a TEM image of the catalyst obtained in comparative example 1 after 5K cycles of accelerated aging test.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It is to be noted that, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a composite catalyst for oxygen reduction reaction in an alkaline medium, which comprises silver-manganese bimetal composite particles.
In some embodiments, the atomic ratio of silver in the silver-manganese bimetallic composite particle ranges from 75% to 98%, and the atomic ratio of manganese ranges from 2 at% to 25 at%. In some embodiments, the silver-manganese bimetallic composite particles have an average particle size in the range of 2 to 50nm, preferably in the range of 5 to 20 nm. The grain size range of the silver-manganese bimetal composite particles is controlled by different synthesis conditions, and the grain size distribution of the silver-manganese bimetal composite particles synthesized under the same synthesis conditions or in the same batch is uniform, as shown in figure 2 or figure 3. In some embodiments, the silver-manganese bimetallic composite particles synthesized under the same synthesis conditions or in the same batch have a proportion of particles within 10% of the average particle size of 70% or more, preferably 80% or more. By controlling the element composition and the particle size range of the silver-manganese bimetal composite particles, the performance of the composite catalyst can be optimized, and the composite catalyst is suitable for different application scenes. Within the above preferred mass ratio range and particle size range, the composite catalyst of the present invention shows superior electrocatalytic performance as well as electrochemical stability. In some embodiments, the silver-manganese bimetallic composite particle is at least partially silver-manganese alloy.
In some embodiments, the composite catalyst includes a support material and silver-manganese bimetallic composite particles distributed on the surface of the support material. The support material comprises a one-, two-or three-dimensional structure of a carbon material or a metal oxide material. In some embodiments, the support material is Vulcan XC-72, BP2000, acetylene black, carbon nanotubes, graphite, graphitized carbon, graphene, Al2O3And manganese oxide, or a mixture of two or more thereof.
The invention also provides a synthetic method of the composite catalyst, which comprises the following steps: forming a precursor solution comprising a silver source and a manganese source; heating the precursor solution to 180-240 ℃, and maintaining for 0.5-4 hours to form a reaction solution dispersed with the composite catalyst; separating and purifying the reaction solution to obtain the composite catalyst nano-particles. And further loading the composite catalyst particles obtained by separation and purification on a carrier material to obtain the composite catalyst material applied to the alkaline fuel cell. The inert atmosphere is one or more of nitrogen, argon and helium.
In some embodiments, a silver source and a manganese source are dissolved into a solvent to form a precursor solution. The solvent comprises an organic phase and an aqueous phase. Preferably, the solvent is an amine organic phase. More preferably, the solvent includes an amino group and an amine-based organic reagent having not less than 8 carbon atoms. In some embodiments, the organic phase solvent comprises a saturated or unsaturated amine reagent such as oleylamine, dodecylamine, tetradecylamine, and the like.
In some embodiments, the silver source includes, but is not limited to, one or more of silver nitrate, silver acetate, silver acetylacetonate, and silver trifluoroacetate. In some embodiments, the manganese source includes, but is not limited to, one or more of manganese nitrate, manganese carbonyl, potassium permanganate.
In some embodiments, the silver manganese composite catalyst is synthesized by the following steps:
A) dissolving silver nitrate as silver source and manganese nitrate as manganese source in a certain amount of oleylamine2Under protection, heating to 180-240 ℃, and keeping for 1-6 hours to obtain the silver-manganese composite metal nanoparticles with the average particle size of 2-50 nm.
B) The prepared metal nanoparticles are mixed with a certain amount (volume ratio 1: 1) dispersing isopropanol and ethanol, repeating centrifugal separation for 2 times, and dispersing in cyclohexane;
C) and (2) dropwise adding the metal nanoparticles dispersed in the cyclohexane into the cyclohexane in which a certain amount of activated carbon powder is dissolved, stirring to load the metal nanoparticles on the activated carbon, then carrying out suction filtration and washing by using absolute ethyl alcohol, and drying to obtain the corresponding carbon-supported metal catalyst.
Qualitative analysis was performed on the prepared product using Shimadu XRD-6000 type powder X-ray diffractometer, qualitative analysis was performed on the prepared product using Thermo-Fisher ICPS-6300 type inductively coupled plasma emission spectrometer, sample morphology analysis was performed using JEM-2100 type transmission electron microscope, and rotating disk test was performed on the corresponding electrocatalyst using CHI760E electrochemical workstation.
The following is further illustrated with reference to specific examples.
Example 1
A preparation method of a silver-manganese composite catalyst comprises the following steps:
1. taking 110mg AgNO3And 20. mu.l of a 50 wt% manganese nitrate solution was dissolved in 10ml of oleylamine, and then the solution was charged into a 50ml three-necked flask, and N was introduced at room temperature2And keeping for 30min, and removing oxygen dissolved in the oleylamine. Then heated to 220 ℃ for 1 hour.
2. 30ml (volume ratio 1: 1) of isopropanol and ethanol are added into the oleylamine after the reaction is finished, and centrifugal separation is carried out at 10000rpm for 3 min. The supernatant was decanted and the pellet redispersed in 30ml (1: 1 by volume) of isopropanol and ethanol and the centrifugation process repeated once. The precipitate obtained is redispersed in 30ml of cyclohexane.
3. 150mg of activated carbon powder (Vulcan XC-72) was added to 150ml of cyclohexane and dispersed ultrasonically for 30 min. And (3) dropwise adding the silver-manganese metal nanoparticles prepared in the step (2) into cyclohexane in which activated carbon powder is dispersed, and stirring for 5 hours to load the metal nanoparticles on the activated carbon. And then, carrying out suction filtration and washing by using absolute ethyl alcohol, and standing and drying in a drying oven at 60 ℃ to obtain the carbon-supported silver-manganese composite metal nanoparticle catalyst marked as Ag-Mn-1.
And (3) taking 2mg of the carbon-supported silver-manganese composite metal nanoparticle catalyst prepared in the step (3), adding 10 mu l of 5 wt% Nafion solution into a mixed solvent of 790 mu l of absolute ethyl alcohol and 200 mu l of deionized water, and performing ultrasonic dispersion for 2 hours. And obtaining the uniformly dispersed carbon-supported silver-manganese catalyst ink.
20 μ l of the ink was applied in portions (5 μ l each, 4 times) to a glassy carbon electrode, and then the oxygen reduction activity was measured by rotating a disk electrode. The electrolyte was 0.1M oxygen saturated KOH solution and the rotating disk was rotated at 1600 rpm.
Through the characterization, from the XRD pattern of the carbon-supported silver-manganese composite metal nanoparticle catalyst in fig. 1, it can be known that the silver-manganese catalyst mainly exhibits a face-centered cubic structure of Ag. Characteristic diffraction peaks of silver appear at θ of 38.1 °, 44.3 °, 64.4 °, 77.5 °, and 81.5 °, which are (111), (200), (220), (311), and (222) crystal planes of Ag, respectively, demonstrating that the metal is manganese-doped silver. From the ICP-ACE results, the atomic ratios of silver and manganese were 84 at% and 16 at%, respectively. From the TEM images of the silver-manganese nanoparticles in fig. 2 and the carbon-supported silver-manganese catalyst in fig. 3, it can be seen that the silver-manganese nanoparticles are uniformly distributed and have a uniform particle size of about 13 nm.
Example 2
A preparation method of a silver-manganese composite catalyst comprises the following steps:
1. 134mg of silver acetylacetonate and 20. mu.l of a 50 wt% manganese nitrate solution were dissolved in 10ml of oleylamine, and the solution was charged into a 50ml three-necked flask, and N was introduced thereinto at room temperature2And keeping for 30min, and removing oxygen dissolved in the oleylamine. Then heated to 220 ℃ for 1 hour.
The other synthesis and testing procedures were the same as in example 1.
The prepared carbon-supported metal catalyst is marked as Ag-Mn-2. The Ag-Mn-2 nano-particles are characterized by being uniformly distributed and having the particle size of about 9nm as shown in figure 3. From the ICP-ACE results, the atomic ratios of silver and manganese were 89 at% and 11 at%, respectively.
Example 3
A preparation method of a silver-manganese composite catalyst comprises the following steps:
1. 110mg of silver nitrate and 20mg of manganese nitrate tetrahydrate were dissolved in 10ml of oleylamine, and the solution was charged into a 50ml three-necked flask, and N was introduced thereinto at room temperature2And keeping for 30min, and removing oxygen dissolved in the oleylamine. Then heated to 220 ℃ for 1 hour.
The other synthesis and testing procedures were the same as in example 1. The prepared carbon-supported metal catalyst is marked as Ag-Mn-3. The characteristics show that the atomic proportions of the silver and the manganese are 81at percent and 19at percent respectively.
Example 4
A preparation method of a silver-manganese composite catalyst comprises the following steps:
1. taking 110mg AgNO3And 5. mu.l of a 50 wt% manganese nitrate solution was dissolved in 10ml of oleylamine, and then the solution was charged into a 50ml three-necked flask, and N was introduced at room temperature2And keeping for 30min, and removing oxygen dissolved in the oleylamine. Then heated to 220 ℃ for 1 hour.
The other synthesis and testing procedures were the same as in example 1. The prepared carbon-supported metal catalyst is marked as Ag-Mn-3. The characteristics show that the atomic proportions of the silver and the manganese are respectively 96at percent and 4at percent.
Comparative example 1
A preparation method of a silver nanoparticle catalyst comprises the following steps:
1. taking 110mg AgNO3Dissolved in 10ml of oleylamine, after which the solution was charged into a 50ml three-necked flask and N was passed through the flask at room temperature2And keeping for 30min, and removing oxygen dissolved in the oleylamine. Then heated to 220 ℃ for 1 hour.
The other steps are the same as in example 1.
As can be seen from fig. 5, the oxygen reduction electrocatalytic activity of the carbon-supported silver-manganese catalysts of examples 1 and 2 is greatly improved compared with the activity of the carbon-supported nano-silver catalyst.
As can be seen from a comparison of fig. 6 and 7, the catalytic stability of the carbon supported copper silver manganese catalyst of example 1 was significantly improved compared to the silver catalyst of comparative example 1. In the accelerated aging test, after 5000 CV cycles, the half-wave potential and the limiting current of the silver particle catalyst in the comparative example 1 are obviously reduced, while the catalytic activity of the silver particle catalyst in the example 1 is still higher. As can be seen from fig. 8, the silver particles are significantly agglomerated by the accelerated aging test.
Both example 3 and example 4 can obtain the composite catalyst of the present invention, and as shown in fig. 5, both the catalytic activity and the catalytic stability are improved compared to those of comparative example 1.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The composite catalyst for oxygen reduction reaction in alkaline medium is characterized by comprising silver-manganese bimetal composite particles.
2. The composite catalyst according to claim 1, wherein the atomic ratio of silver element in the silver-manganese bimetal composite particle is 75-98%, and the atomic ratio of manganese element is 2-25%.
3. The composite catalyst according to claim 1, wherein the average particle size of the silver-manganese bimetal composite particles is in the range of 2 to 50 nm.
4. The composite catalyst according to claims 1 to 3, wherein the composite catalyst comprises a support material and silver-manganese bimetallic composite particles distributed on the surface of the support material.
5. The composite catalyst according to claim 4, wherein the support material comprises a one-, two-or three-dimensional structure of a carbon material or a metal oxide material.
6. A synthetic method of a composite catalyst for oxygen reduction reaction in an alkaline medium is characterized by comprising the following steps:
forming a precursor solution comprising a silver source and a manganese source;
heating the precursor solution to a preset temperature, and maintaining the preset reaction time to form a reaction solution in which the composite catalyst is dispersed;
separating and purifying the reaction solution to obtain the composite catalyst nano-particles.
7. The composite catalyst of claim 5, wherein the synthesis methods are all formed in an oxygen-scavenging environment.
8. The composite catalyst according to claim 5, wherein the predetermined temperature range is 180 ℃ to 240 ℃ and the predetermined reaction time is 0.5 to 4 hours.
9. The composite catalyst according to claims 5 to 7, wherein the composite catalyst particles obtained by separation and purification are supported on a support material.
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| CN112242530A (en) * | 2020-09-30 | 2021-01-19 | 复旦大学 | Preparation method of high-stability low-load carbon-coated platinum catalyst |
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Application publication date: 20200207 |