CN111617774A - Synthesis and application of quaternary platinum-iron-rhodium-ruthenium nano alloy with hierarchical structure - Google Patents

Synthesis and application of quaternary platinum-iron-rhodium-ruthenium nano alloy with hierarchical structure Download PDF

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CN111617774A
CN111617774A CN202010523420.3A CN202010523420A CN111617774A CN 111617774 A CN111617774 A CN 111617774A CN 202010523420 A CN202010523420 A CN 202010523420A CN 111617774 A CN111617774 A CN 111617774A
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rhodium
iron
platinum
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ruthenium
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CN111617774B (en
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袁强
谢子璇
陈锐
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Guizhou University
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Abstract

The invention discloses synthesis and application of a quaternary platinum-iron-rhodium-ruthenium nano alloy with a hierarchical structure, which is characterized by comprising the following steps of: the quaternary platinum iron rhodium ruthenium nano alloy with the hierarchical structure is novel in appearance and uniform in size, is a hierarchical structure assembled by quaternary platinum iron rhodium ruthenium nano alloy monomers of 42-62 nm, and has mass activity of 4.44A mg at a voltage of-0.07V in an alkaline hydrogen evolution reactionpt ‑1The specific activity was 11.33mA cm‑2Are respectively quotient6.16 times and 11.9 times as much platinum as the commercial carbon. In the stability test, the current density of the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure is kept at 10 mA cm‑2After 20 h, the mass activity dropped only 5% compared to the initial one, while the commercial platinum on carbon dropped 44%.

Description

Synthesis and application of quaternary platinum-iron-rhodium-ruthenium nano alloy with hierarchical structure
Technical Field
The invention relates to a high-performance cathode electrocatalyst for hydrogen evolution reaction and a synthesis method thereof, in particular to synthesis and application of a hierarchical quaternary platinum-iron-rhodium-ruthenium nano alloy.
Background
The hydrogen economy system uses hydrogen as an energy carrier and is a renewable clean energy source. Catalysts are key components to accelerate the progress of these reactions, and the synthesis and design of good electrocatalysts is the primary task to achieve this system. Platinum is the best catalyst for hydrogen evolution at present, but the expensive price of platinum prevents the large-scale application of platinum, so that the problem of increasing the catalytic activity of platinum and reducing the dosage of metal platinum is faced in the field. To overcome the above problems, other metals may be added to alloy with platinum to improve the activity and stability of the catalyst. The invention successfully synthesizes the quaternary platinum iron rhodium ruthenium nano alloy with a hierarchical structure assembled by dendritic quaternary platinum iron rhodium ruthenium by using a solvothermal method, enhances the catalytic performance of hydrogen evolution reaction of the catalyst, and simultaneously improves the stability.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure is prepared in an organic solvent, the synthesis method of the catalyst is simple and easy to repeat, the morphology and the size are uniform, and the catalyst has excellent catalytic performance and stability in an alkaline hydrogen evolution reaction.
The technical scheme of the invention is as follows: the quaternary platinum iron rhodium ruthenium nano alloy with the hierarchical structure is novel in appearance and uniform in size and is a hierarchical structure assembled by 42-62 nm nano alloys; wherein the content of rhodium is 9.2-10.2%, and the content of ruthenium is 2.7-3.7%.
The synthesis and application of the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure comprise the following steps: adding a surfactant and four metal salts of platinum salt, iron salt, rhodium salt and ruthenium salt into an organic solvent octylamine, stirring for 10-15 minutes at room temperature, and performing ultrasonic treatment for 10-15 minutes until the metal salts are completely dissolved; (2) adding 10-20 mg of ascorbic acid into the mixed solution obtained in the step (1), and stirring at room temperature; (3) transferring the mixed solution obtained in the step (2) to a high-pressure reaction kettle to react for 6-12 hours, and controlling the temperature at 150-200 ℃; (4) and (4) cooling and washing the product obtained in the step (3), performing centrifugal separation to obtain the quaternary platinum iron rhodium ruthenium nano alloy with the hierarchical structure, and dispersing and storing the sample in ethanol.
The platinum salt in the step (1) is chloroplatinic acid, the ferric salt is ferric acetylacetonate, the rhodium salt is rhodium chloride, and the ruthenium salt is ruthenium chloride.
The dosage of the metal salt is 0.03-0.06 mmol, and the proportion of the platinum salt, the iron salt, the rhodium salt and the ruthenium salt precursor is 25: 8: 3: 7-25: 8: 7: 3
The volume of the octylamine is 6-10 mL.
The quaternary platinum iron rhodium ruthenium nano alloy with the hierarchical structure is used as a cathode electrocatalyst for the application of alkaline hydrogen evolution reaction.
The invention has the beneficial effects that: the invention controls the quaternary platinum iron rhodium ruthenium nano alloy with a synthetic hierarchical structure to be not found in the literature at present. The alloy has the advantages of novel crystal structure, excellent catalytic performance and good stability, and the mass activity of the alloy at the voltage of-0.07V in the alkaline hydrogen evolution reaction is 4.44A mgpt -1The specific activity was 11.33mA cm-26.16 times and 11.9 times, respectively, that of commercial carbon supported platinum. In the stability test, the current density of the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure is kept at 10 mA cm-2After 20 h, the mass activity dropped only 5% compared to the initial one, while the commercial platinum on carbon dropped 44%.
The method can control the product appearance of the quaternary platinum-iron-rhodium-ruthenium nano alloy with a synthetic hierarchical structure. The alloy crystal structure is novel, and is a hierarchical structure assembled by 42-62 nm nano-alloy. The catalyst has excellent catalytic performance and good stability, and has the possibility of replacing the current commercial platinum black or carbon-supported platinum black catalyst.
Drawings
FIG. 1 is a scanning electron microscope observation result diagram of a quaternary platinum-iron-rhodium-ruthenium nano alloy with a hierarchical structure;
FIG. 2 is a diagram of the X-ray diffraction results of a quaternary platinum-iron-rhodium-ruthenium nano alloy with a hierarchical structure;
FIG. 3 is a high-angle annular dark-field scanning transmission electron microscope observation result graph and a line scanning graph of a quaternary platinum-iron-rhodium-ruthenium nano alloy monomer with a hierarchical structure;
FIG. 4 is a graph comparing the catalytic performance of a hierarchical quaternary Pt-Fe-Rh-Ru nano-alloy with a commercial Pt-on-carbon alkaline hydrogen evolution reaction;
FIG. 5 is a graph comparing the catalytic performance of alkaline hydrogen evolution reactions at-0.07V and-0.1V for a hierarchical quaternary platinum-iron-rhodium-ruthenium nanoalloy and a commercial platinum on carbon, respectively;
FIG. 6 is a graph of the catalytic stability (chronopotentiometry) of a hierarchical quaternary Pt-Fe-Rh-Ru nano-alloy with commercial Pt on carbon.
Detailed Description
Example 1:
the synthesis and application of the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure comprise the following steps:
(1) 36.4mg of hexadecyl trimethyl ammonium bromide (CTAB) is used as a surfactant, four metal salts of chloroplatinic acid, iron acetylacetonate, rhodium chloride and ruthenium chloride are added into an organic solvent octylamine together, the metal dosage is 0.043mmol, and the metal precursors of platinum salt, iron salt, rhodium salt and ruthenium salt have the ratio of 25: 8: 5: 5, stirring the added volume of the octylamine at 6.2 mL at room temperature for 10 minutes, and carrying out ultrasonic treatment for 10 minutes until the metal salt is completely dissolved;
(2) adding ascorbic acid into the mixed solution obtained in the step (1), wherein the dosage of the ascorbic acid is 18 mg, and stirring the mixture for 10 minutes at room temperature;
(3) transferring the mixed solution obtained in the step (2) to a high-pressure reaction kettle for reacting for 8 hours, and controlling the temperature at 190 ℃;
(4) and (4) cooling and washing the product obtained in the step (3), performing centrifugal separation to obtain the quaternary platinum iron rhodium ruthenium nano alloy with the hierarchical structure, and dispersing and storing the sample in ethanol.
Example 2:
(1) 36.4mg of hexadecyl trimethyl ammonium bromide (CTAB) is used as a surfactant, four metal salts of chloroplatinic acid, iron acetylacetonate, rhodium chloride and ruthenium chloride are added into an organic solvent octylamine together, the metal dosage is 0.043mmol, and the metal precursors of platinum salt, iron salt, rhodium salt and ruthenium salt have the ratio of 25: 8: 7: 3, stirring the added volume of the octylamine at 6.2 mL at room temperature for 10 minutes, and carrying out ultrasonic treatment for 10 minutes until the metal salt is completely dissolved;
(2) adding ascorbic acid into the mixed solution obtained in the step (1), wherein the dosage of the ascorbic acid is 18 mg, and stirring the mixture for 10 minutes at room temperature;
(3) transferring the mixed solution obtained in the step (2) to a high-pressure reaction kettle for reacting for 8 hours, and controlling the temperature at 190 ℃;
(4) and (4) cooling the product obtained in the step (3), washing, performing centrifugal separation to obtain the quaternary platinum-iron-rhodium-ruthenium nano alloy, and dispersing and storing the sample in ethanol.
Example 3:
(1) 36.4mg of hexadecyl trimethyl ammonium bromide (CTAB) is used as a surfactant, four metal salts of chloroplatinic acid, iron acetylacetonate, rhodium chloride and ruthenium chloride are added into an organic solvent octylamine together, the metal dosage is 0.043mmol, and the metal precursors of platinum salt, iron salt, rhodium salt and ruthenium salt have the ratio of 25: 8: 3: 7, stirring the added volume of the octylamine at 6.2 mL at room temperature for 10 minutes, and carrying out ultrasonic treatment for 10 minutes until the metal salt is completely dissolved;
(2) adding ascorbic acid into the mixed solution obtained in the step (1), wherein the dosage of the ascorbic acid is 18 mg, and stirring the mixture for 10 minutes at room temperature;
(3) transferring the mixed solution obtained in the step (2) to a high-pressure reaction kettle for reacting for 8 hours, and controlling the temperature at 190 ℃;
(4) and (4) cooling the product obtained in the step (3), washing, performing centrifugal separation to obtain the quaternary platinum-iron-rhodium-ruthenium nano alloy, and dispersing and storing the sample in ethanol.

Claims (6)

1. The quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure is characterized in that: the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure is novel in appearance and uniform in size, and is a hierarchical structure assembled by 42-62 nm nano alloys; wherein the content of rhodium is 9.2-10.2%, and the content of ruthenium is 2.7-3.7%.
2. The method of claim 1, wherein the hierarchical structure of the quaternary platinum-iron-rhodium-ruthenium nano-alloy comprises: the method comprises the following steps: (1) adding a surfactant and four metal salts of platinum salt, iron salt, rhodium salt and ruthenium salt into an organic solvent octylamine, stirring for 10-15 minutes at room temperature, and performing ultrasonic treatment for 10-15 minutes until the metal salts are completely dissolved; (2) adding 10-20 mg of ascorbic acid into the mixed solution obtained in the step (1), and stirring for 10 minutes at room temperature; (3) transferring the mixed solution obtained in the step (2) to a high-pressure reaction kettle to react for 6-12 hours, and controlling the temperature at 150-200 ℃; (4) and (4) cooling the product obtained in the step (3), washing, and performing centrifugal separation to obtain the quaternary platinum-iron-rhodium-ruthenium nano alloy with the hierarchical structure.
3. The method for synthesizing hierarchical quaternary platinum-iron-rhodium-ruthenium nano-alloy according to claim 2, wherein the hierarchical structure comprises: the platinum salt in the step (1) is chloroplatinic acid, the ferric salt is ferric acetylacetonate, the rhodium salt is rhodium chloride, and the ruthenium salt is ruthenium chloride.
4. The method for synthesizing hierarchical quaternary platinum-iron-rhodium-ruthenium nano-alloy according to claim 2, wherein the hierarchical structure comprises: the dosage of the metal salt is 0.03-0.06 mmol, and the proportion of the platinum salt, the iron salt, the rhodium salt and the ruthenium salt precursor is 25: 8: 3: 7-25: 8: 7: 3.
5. the method for synthesizing hierarchical quaternary platinum-iron-rhodium-ruthenium nano-alloy according to claim 2, wherein the hierarchical structure comprises: the volume of the octylamine added in the step (1) is 6-10 mL.
6. The use of a layered quaternary platinum-iron-rhodium-ruthenium nano-alloy as claimed in any of claims 1 to 5 as a cathodic electrocatalyst for alkaline hydrogen evolution reactions.
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CN113394418B (en) * 2021-06-12 2022-04-22 贵州大学 High-performance oxygen reduction catalyst for actual methanol fuel cell

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