CN110581284A - Electrocatalysis function V2O3Preparation method and application of @ Co - Google Patents
Electrocatalysis function V2O3Preparation method and application of @ Co Download PDFInfo
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- CN110581284A CN110581284A CN201910941264.XA CN201910941264A CN110581284A CN 110581284 A CN110581284 A CN 110581284A CN 201910941264 A CN201910941264 A CN 201910941264A CN 110581284 A CN110581284 A CN 110581284A
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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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
- H01M4/9041—Metals or alloys
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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
Electrocatalysis function V2O3a preparation method and application of @ Co. Firstly, dry-mixing urea, ammonium metavanadate and cobalt nitrate hexahydrate, adding ethanol, grinding and drying to obtain a mixture; grinding the mixture, sieving, loading into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively; introducing inert gas into the tubular atmosphere furnace to exhaust the air in the tube, controlling the air pressure in the tube to be-1-0 MPa, heating to 600-; after the heat preservation is finished, opening the gas valve, introducing inert gas by 700-900 sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas to obtain a target product V2O3@ Co. Prepared V2O3the application of @ Co in enhancing the activity of hydrogen and oxygen production. Electrocatalytic function V prepared by the invention2O3The @ Co has good hydrogen and oxygen production performance, and can be widely applied to excellent electrocatalysts for water electrolysis in industry. The catalyst may be electrolysisWater provides a clean, sustainable energy source.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to an electrocatalytic function V2O3A preparation method of @ Co and an electrocatalyst applied to enhance hydrogen-producing and oxygen-producing activity.
Background
The problems faced by fossil energy are becoming more and more serious, and in order to follow the development of modern energy technology, the research on electrode materials for hydrogen-producing and oxygen-producing reactions with good performance is required. To date, platinum-based nanomaterials have become the primary and best electrocatalysts for promoting hydrogen production and oxygen production. However, the scarcity and high price of platinum has hindered its practical application in fuel cell devices.
Recently, a common transition metal cobalt and its oxide show good hydrogen and oxygen production functions. However, insufficient electron conductivity of cobalt oxide has hindered its further development as an oxygen-producing electrocatalyst. One strategy to increase the hydrogen and oxygen production activity of cobalt-based electrocatalysts is to combine the electrocatalyst with other highly conductive materials and have demonstrated that the hydrogen and oxygen production performance of cobalt-based electrocatalysts can be effectively improved when combined with highly conductive materials. However, cobalt-based electrocatalysts are generally randomly distributed on the conductive agent without close adhesion and coupling, resulting in high contact resistance and reduced hydrogen and oxygen production activity. In some severe cases, loss or agglomeration of catalyst can shorten the lifetime. Therefore, it is very important to design and manufacture a novel structure composed of a cobalt-based electrocatalyst having high activity to reduce contact resistance, loss and aggregation, thereby improving the performance of hydrogen generation and oxygen generation.
Disclosure of Invention
the invention aims to provide an electrocatalysis function V which has simple preparation process, easily controlled conditions, low production cost and easy industrial production2O3A preparation method of @ Co.
another object of the present invention is to provideelectrocatalysis function V2O3The application of @ Co in enhancing the activity of hydrogen production and oxygen production has good performance of hydrogen production and oxygen production, and simultaneously has good stability and good cycle performance.
In order to achieve the above purpose, the preparation method of the invention comprises the following steps:
1) firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2O ═ 4-6: (1-3): (1-3) dry-mixing in a mass ratio, adding ethanol, grinding and drying to obtain a mixture;
2) grinding the mixture, sieving with a 40-60 mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas into the tubular atmosphere furnace to exhaust the air in the tube, controlling the air pressure in the tube to be-1-0 MPa, heating to 600-;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas by 700-900 sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas to obtain a target product V2O3@Co。
The grinding time in the step 1) is 10-20 min.
the step 1) drying is drying in an oven at 50 ℃ for 10 hours.
The grinding time in the step 2) is 20-30 min.
And 3) introducing inert gas into the tubular atmosphere furnace to perform air extraction and air supplement for 3 times.
The inert gas is argon.
v prepared by the above preparation method2O3The application of @ Co in enhancing the activity of hydrogen and oxygen production.
The invention has simple preparation process, easily controlled conditions, low production cost and easy industrial production, and the prepared V is2O3the @ Co nano material has uniform chemical composition and high purity and crystallinity. The prepared electro-catalyst has the characteristics of small overpotential, long service life, small Tafel slope and the likehas great potential in water cracking and related application.
The invention proves that the crystallization, surface chemical state and porosity of vanadium trioxide are regulated by compounding the vanadium trioxide as a structure inducer. The obtained material shows good catalytic activity to hydrogen-producing and oxygen-producing reactions in an alkaline medium. This excellent electrocatalytic performance is mainly due to the high pyridine and graphite co-doping of cobalt, which helps to increase electron conductivity, and helps to expose the nanoporous structure of many catalytically active sites.
Electrocatalytic function V prepared by the invention2O3The @ Co has good hydrogen and oxygen production performance, and can be widely applied to excellent electrocatalysts for water electrolysis in industry. The catalyst can provide a clean and sustainable energy source for water electrolysis, and can remove the barrier that high-cost platinum-based materials are widely applied to the industry.
Drawings
FIG. 1 shows a nano electrocatalytic function V prepared in example 6 of the present invention2O3the XRD pattern of @ Co.
FIG. 2 shows a nano-electrocatalytic function V prepared in example 6 of the present invention2O3SEM image of @ Co.
FIG. 3 shows a nano-electrocatalytic function V prepared in example 6 of the present invention2O3The hydrogen production performance diagram of @ Co.
FIG. 4 shows a nano electro-catalytic function V prepared in example 6 of the present invention2O3@ Co oxygen evolution performance diagram.
The specific implementation mode is as follows:
Example 1:
1) Firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2o is 4: 1: 1, dry mixing in a mass ratio, adding ethanol, grinding for 10min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) Grinding the mixture for 20min, sieving with a 40-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 600 ℃ at the heating rate of 10 ℃/min and preserving heat for 120 min;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas argon by 700sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
Example 2:
1) Firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2o is 5: 2: 2, dry mixing in a mass ratio, adding ethanol, grinding for 15min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) Grinding the mixture for 25min, sieving with a 50-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 700 ℃ at the heating rate of 10 ℃/min and preserving heat for 160 min;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas argon by 800sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
Example 3:
1) firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2o ═ 6: 3: 3, dry mixing in a mass ratio, adding ethanol, grinding for 13min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) Grinding the mixture for 22min, sieving with a 45-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 800 ℃ at the heating rate of 10 ℃/min and preserving heat for 140 min;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas argon by 700sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
Example 4:
1) Firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2O is 4: 1: 1, dry mixing in a mass ratio, adding ethanol, grinding for 18min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) Grinding the mixture for 28min, sieving with a 60-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 600 ℃ at the heating rate of 10 ℃/min and preserving the heat for 180 min;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas argon by 900sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
Example 5:
1) firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2O is 5: 2: 2, dry mixing in a mass ratio, adding ethanol, grinding for 20min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) Grinding the mixture for 30min, sieving with a 55-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 700 ℃ at the heating rate of 10 ℃/min and preserving heat for 150 min;
4) after the heat preservation is finished, opening the gas valve, introducing inert gas argon by 800sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
Example 6:
1) Firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2O ═ 6: 3: 3, dry mixing in a mass ratio, adding ethanol, grinding for 20min, and drying in a 50 ℃ oven for 10 hours to obtain a mixture;
2) grinding the mixture for 30min, sieving with a 60-mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas argon into the tubular atmosphere furnace, performing air extraction for 3 times, supplementing air and exhausting air in the furnace, controlling the air pressure in the furnace to be-1-0 MPa, heating to 800 ℃ at the heating rate of 10 ℃/min and preserving heat for 180 min;
4) after the heat preservation is finished, opening the gas valve, introducing inert gas argon by 900sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas argon to obtain a target product V2O3@Co。
It can be seen from fig. 1 that the diffraction peak of the sample prepared in this example is well matched with the standard card, and the intensity is high, which shows that V obtained in this example2O3@ Co is very crystalline.
it can be seen from fig. 2 that the sample prepared in this example has a small particle shape and good sample dispersibility.
FIG. 3 shows the nano-V prepared in this example2O3The hydrogen production performance diagram of @ Co shows that the current density is 10mA/cm under the test condition of pH 142when the scanning speed is 3mV/s, the overpotential of the sample is 280mV, which shows that the sample has good hydrogen production performance.
FIG. 4 shows the nano-V prepared in this example2O3Graph of oxygen evolution Performance of @ Co, showing the current density of 10mA/cm under the test condition of pH 142when the scanning speed is 3mV/s, the overpotential of the sample is 270mV, which shows that the sample has excellent oxygen generation performance.
Claims (7)
1. Electrocatalysis function V2O3The preparation method of @ Co is characterized by comprising the following steps of:
1) Firstly, urea, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the formula of CO (NH)2)2：NH4VO3：Co(NO3)2·6H2O ═ 4-6: (1-3): (1-3) dry-mixing in a mass ratio, adding ethanol, grinding and drying to obtain a mixture;
2) Grinding the mixture, sieving with a 40-60 mesh sieve, placing into a porcelain boat, placing the porcelain boat in a tubular atmosphere furnace, and placing two furnace plugs at two ends of the tube respectively at an interval of 5 cm;
3) Introducing inert gas into the tubular atmosphere furnace to exhaust the air in the tube, controlling the air pressure in the tube to be-1-0 MPa, heating to 600-;
4) After the heat preservation is finished, opening the gas valve, introducing inert gas by 700-900 sccm gas flow, discharging gas generated in the heat preservation process, and then cooling to room temperature under the inert gas to obtain a target product V2O3@Co。
2. Electrocatalytic function V according to claim 12O3The preparation method of @ Co is characterized by comprising the following steps: the grinding time in the step 1) is 10-20 min.
3. Electrocatalytic function V according to claim 12O3the preparation method of @ Co is characterized by comprising the following steps: the step 1) drying is drying in an oven at 50 ℃ for 10 hours.
4. Electrocatalytic function V according to claim 12O3the preparation method of @ Co is characterized by comprising the following steps: said step (c) is2) the grinding time is 20-30 min.
5. Electrocatalytic function V according to claim 12O3The preparation method of @ Co is characterized by comprising the following steps: and 3) introducing inert gas into the tubular atmosphere furnace to perform air extraction and air supplement for 3 times.
6. Electrocatalytic function V according to claim 12O3The preparation method of @ Co is characterized by comprising the following steps: the inert gas is argon.
7. v prepared by the preparation method of claim 12O3The application of @ Co in enhancing the activity of hydrogen and oxygen production.
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