CN115710723A - Preparation method of stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production - Google Patents
Preparation method of stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production Download PDFInfo
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- CN115710723A CN115710723A CN202211563479.0A CN202211563479A CN115710723A CN 115710723 A CN115710723 A CN 115710723A CN 202211563479 A CN202211563479 A CN 202211563479A CN 115710723 A CN115710723 A CN 115710723A
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production, which comprises the following steps: oxygen evolution reaction polar net electrocatalyst and hydrogen evolution reaction polar net electrocatalyst. The preparation method of the invention uses the stainless steel mesh with low cost as the catalytic substrate for water cracking, so that the production cost can be greatly reduced; the surface of the stainless steel mesh is doped with heteroatoms such as nitrogen, phosphorus and sulfur, and metal oxides such as nickel, molybdenum and cobalt grow on the surface of the stainless steel mesh, all the modifications enable atoms to be combined in a chemical bonding mode, the surface stability and the adhesion of a surface layer are superior to those of the traditional high-temperature plasma spraying technology, and the unique surface appearance has excellent electrocatalysis performance. The oxygen evolution reaction performance of the stainless steel electrode net electrocatalyst is superior to that of commercial iridium oxide, and the hydrogen evolution reaction performance is equivalent to that of platinum; compared with the traditional nickel mesh electrocatalyst, the catalyst has lower overpotential, so the electrolysis voltage is lower, and the energy consumption of the system is reduced.
Description
Technical Field
The invention relates to the field of electrolytic hydrogen production, in particular to a preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production.
Background
The current density of the alkaline electrolyzed water is limited due to the limitation of the performance of the traditional nickel mesh electro-catalyst at present in the process of electrolyzing the alkaline electrolyzed water in the hydrogen production; meanwhile, the price of the nickel net electrocatalyst is increased due to the increase of the price of the nickel, and the input cost is increased.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the stainless steel electrode net electrocatalyst for electrolytic hydrogen production is provided, and the stainless steel electrode net electrocatalyst prepared by the preparation method has the advantages of low production cost, excellent hydrogen evolution and oxygen evolution reaction performance and lower overpotential.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production is characterized by comprising the following steps: the stainless steel electrode mesh electrocatalyst comprises: an oxygen evolution reaction polar net electrocatalyst and a hydrogen evolution reaction polar net electrocatalyst;
the preparation method of the oxygen evolution reaction polar net electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, then heating the etching liquid to 100-200 ℃, and then preserving heat to enable the stainless steel mesh to be etched and reacted in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is finished, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatoms;
(3) Placing the stainless steel net in an ammonia gas atmosphere, heating to 300-500 ℃, preserving heat for 2-5 hours, and then cooling the stainless steel net to room temperature to obtain the nitrogen-doped oxygen evolution reaction polar net electrocatalyst;
the preparation method of the hydrogen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, then preserving heat, enabling the stainless steel mesh to perform etching reaction in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is completed, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatom;
(3) Heating the stainless steel mesh to 300-500 ℃ in the atmosphere of ammonia gas and phosphine or ammonia gas and hydrogen sulfide, preserving the heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus or sulfur atoms;
(4) Mixing sodium molybdate hydrate, ammonium fluoride and urea, adding the mixture into deionized water to obtain a mixed solution, and then stirring and ultrasonically mixing the mixed solution fully and uniformly;
(5) Putting the stainless steel mesh and the mixed solution in the fourth step into a reaction container, heating to 150-250 ℃, preserving heat for 12-24 hours, and taking out the stainless steel mesh and cooling to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus or sulfur atoms and growing iron-molybdenum;
(6) The stainless steel mesh is cleaned by pure water, then is heated to 300-500 ℃ in the atmosphere of hydrogen and is kept warm for 1-3 hours, and then is taken out and cooled to room temperature, so that the hydrogen evolution reaction polar mesh electrocatalyst doped with nitrogen-phosphorus or sulfur atoms and grown with iron-molybdenum oxide can be obtained.
Further, the preparation method of the stainless steel electrode mesh electrocatalyst for hydrogen production by electrolysis comprises the following steps: the mass ratio of the sodium molybdate hydrate to the ammonium fluoride to the urea is 1:1:3.
further, the preparation method of the stainless steel electrode mesh electrocatalyst for hydrogen production by electrolysis comprises the following steps: the mass ratio of the acid substances to the lithium chloride in the etching liquid is (3-5): 1.
further, the preparation method of the stainless steel electrode mesh electrocatalyst for hydrogen production by electrolysis comprises the following steps: the mass ratio of ammonia gas to phosphine is as follows: (3-6): 1, the mass ratio of ammonia gas to hydrogen sulfide is as follows: (3-6): 1.
further, the preparation method of the stainless steel electrode mesh electrocatalyst for hydrogen production by electrolysis comprises the following steps: the concentration of the acid substances is 10-20%.
The invention has the advantages that: the preparation method uses the stainless steel mesh with low cost as the catalytic substrate for water cracking, the stainless steel mesh is cheaper than the nickel mesh, is doped with nonmetal and has less consumption of metal elements for growth, and the production cost can be greatly reduced; the surface of the stainless steel mesh is doped with heteroatoms such as nitrogen, phosphorus and sulfur, and metal oxides such as nickel, molybdenum and cobalt grow on the surface of the stainless steel mesh, all the modifications enable atoms to be combined in a chemical bonding mode, the surface stability and the adhesion of a surface layer are superior to those of the traditional high-temperature plasma spraying technology, and the unique surface appearance has excellent electrocatalysis performance. The oxygen evolution reaction performance of the prepared stainless steel electrode net electrocatalyst is superior to that of commercial iridium oxide, and the hydrogen evolution reaction performance of the prepared stainless steel electrode net electrocatalyst is equivalent to that of platinum; compared with the traditional nickel mesh electrocatalyst, the catalyst has lower overpotential, so the electrolysis voltage is lower, and the energy consumption of the system is reduced.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production comprises the following steps: an oxygen evolution reaction polar net electrocatalyst and a hydrogen evolution reaction polar net electrocatalyst;
the preparation method of the oxygen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, and then preserving heat, so that the stainless steel mesh is etched and reacted in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, and the mass ratio of the acid substances to the lithium chloride in the etching liquid is (3-5): 1, the concentration of acid substances is 10-20%, after the etching reaction is finished, cooling the stainless steel mesh to room temperature, cleaning the stainless steel mesh by using deionized water, and drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatoms;
(3) Placing the stainless steel mesh in an ammonia gas atmosphere, heating to 300-500 ℃, preserving heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature to obtain the nitrogen-doped oxygen evolution reaction polar net electrocatalyst;
the preparation method of the hydrogen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, then preserving heat, enabling the stainless steel mesh to perform etching reaction in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is completed, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatom;
(3) Heating the stainless steel mesh to 300-500 ℃ in the atmosphere of ammonia and phosphine, preserving heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus atoms, wherein the mass ratio of the ammonia to the phosphine is as follows: (3-6): 1;
(4) Mixing sodium molybdate hydrate, ammonium fluoride and urea, adding the mixture into deionized water to obtain a mixed solution, stirring and ultrasonically mixing the mixed solution to be uniformly mixed, wherein the mass ratio of the sodium molybdate hydrate to the ammonium fluoride to the urea is 1:1:3;
(5) Putting the stainless steel mesh and the mixed solution in the fourth step into a reaction container, heating to 150-250 ℃, preserving heat for 12-24 hours, and taking out the stainless steel mesh and cooling to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus atoms and grown with iron-molybdenum;
(6) The stainless steel mesh is cleaned by pure water, then the stainless steel mesh is placed in a hydrogen atmosphere and heated to 300-500 ℃, and then is kept warm for 1-3 hours, and then the stainless steel mesh is taken out and cooled to room temperature, so that the hydrogen evolution reaction polar mesh electrocatalyst doped with nitrogen-phosphorus atoms and grown with iron-molybdenum oxide can be obtained.
Example 2
A preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production comprises the following steps: an oxygen evolution reaction polar net electrocatalyst and a hydrogen evolution reaction polar net electrocatalyst;
the preparation method of the oxygen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, and then preserving heat, so that the stainless steel mesh is etched and reacted in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, and the mass ratio of the acid substances to the lithium chloride in the etching liquid is (3-5): 1, the concentration of acid substances is 10-20%, after the etching reaction is finished, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh by using deionized water, and drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatoms;
(3) Placing the stainless steel mesh in an ammonia gas atmosphere, heating to 300-500 ℃, preserving heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature to obtain the nitrogen-doped oxygen evolution reaction polar net electrocatalyst;
the preparation method of the hydrogen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, then preserving heat, enabling the stainless steel mesh to perform etching reaction in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is completed, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatom;
(3) Heating the stainless steel mesh to 300-500 ℃ in the atmosphere of ammonia and hydrogen sulfide, preserving heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-sulfur atoms, wherein the mass ratio of the ammonia to the hydrogen sulfide is as follows: (3-6): 1;
(4) Mixing sodium molybdate hydrate, ammonium fluoride and urea, adding the mixture into deionized water to obtain a mixed solution, stirring and ultrasonically mixing the mixed solution to be uniformly mixed, wherein the mass ratio of the sodium molybdate hydrate to the ammonium fluoride to the urea is 1:1:3;
(5) Placing the stainless steel mesh and the mixed solution in the fourth step into a reaction container, heating to 150-250 ℃, preserving heat for 12-24 hours, and then taking out the stainless steel mesh and cooling to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-sulfur atoms and grown with iron-molybdenum;
(6) The stainless steel mesh is cleaned by pure water, then is heated to 300-500 ℃ in the atmosphere of hydrogen and is kept warm for 1-3 hours, and then is taken out and cooled to room temperature, so that the hydrogen evolution reaction polar mesh electrocatalyst doped with nitrogen-sulfur atoms and grown with iron-molybdenum oxide can be obtained.
Claims (5)
1. A preparation method of a stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production is characterized by comprising the following steps: the stainless steel electrode mesh electrocatalyst comprises: an oxygen evolution reaction electrode grid electrocatalyst and a hydrogen evolution reaction electrode grid electrocatalyst;
the preparation method of the oxygen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, then preserving heat, enabling the stainless steel mesh to perform etching reaction in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is completed, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatom;
(3) Placing the stainless steel net in an ammonia gas atmosphere, heating to 300-500 ℃, preserving heat for 2-5 hours, and then cooling the stainless steel net to room temperature to obtain the nitrogen-doped oxygen evolution reaction polar net electrocatalyst;
the preparation method of the hydrogen evolution reaction electrode grid electrocatalyst comprises the following steps:
(1) Cleaning the stainless steel mesh with deionized water, performing surface coarse impurity removal, and then ultrasonically cleaning the stainless steel mesh in ethanol or acetone for at least three times;
(2) Placing the cleaned stainless steel mesh in an oven for drying, then placing the stainless steel mesh in etching liquid, heating the etching liquid to 100-200 ℃, then preserving heat, enabling the stainless steel mesh to perform etching reaction in the etching liquid for 1-3 hours, wherein the etching liquid is formed by mixing acid substances and lithium chloride, the acid substances are one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and phosphoric acid, after the etching reaction is completed, cooling the stainless steel mesh to room temperature, then cleaning the stainless steel mesh with deionized water, and then drying the stainless steel mesh, wherein the stainless steel mesh can be used as a precursor for doping heteroatom;
(3) Heating the stainless steel mesh to 300-500 ℃ in the atmosphere of ammonia gas and phosphine or ammonia gas and hydrogen sulfide, preserving the heat for 2-5 hours, and then cooling the stainless steel mesh to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus or sulfur atoms;
(4) Mixing sodium molybdate hydrate, ammonium fluoride and urea, adding the mixture into deionized water to obtain a mixed solution, and then stirring and ultrasonically mixing the mixed solution fully and uniformly;
(5) Putting the stainless steel mesh and the mixed solution in the fourth step into a reaction container, heating to 150-250 ℃, preserving heat for 12-24 hours, and taking out the stainless steel mesh and cooling to room temperature, thereby obtaining the stainless steel mesh doped with nitrogen-phosphorus or sulfur atoms and growing iron-molybdenum;
(6) The stainless steel mesh is cleaned by pure water, then is heated to 300-500 ℃ in the atmosphere of hydrogen and is kept warm for 1-3 hours, and then is taken out and cooled to room temperature, so that the hydrogen evolution reaction polar mesh electrocatalyst doped with nitrogen-phosphorus or sulfur atoms and grown with iron-molybdenum oxide can be obtained.
2. The method for preparing the stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production according to claim 1, wherein the method comprises the following steps: the mass ratio of the sodium molybdate hydrate to the ammonium fluoride to the urea is 1:1:3.
3. the method for preparing the stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production according to claim 1 or 2, characterized in that: the mass ratio of the acid substances to the lithium chloride in the etching liquid is (3-5): 1.
4. the method for preparing the stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production according to claim 1 or 2, characterized in that: the mass ratio of ammonia gas to phosphine is as follows: (3-6): 1, the mass ratio of ammonia gas to hydrogen sulfide is as follows: (3-6): 1.
5. the method for preparing the stainless steel electrode mesh electrocatalyst for electrolytic hydrogen production according to claim 1 or 2, characterized in that: the concentration of the acid substances is 10-20%.
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- 2022-12-07 CN CN202211563479.0A patent/CN115710723A/en active Pending
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| CN108754532A (en) * | 2018-05-29 | 2018-11-06 | 武汉工程大学 | A kind of iron of molybdenum doping/nickel layer shape array@nickel foam based combined electrode materials and the preparation method and application thereof |
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| CN113457689A (en) * | 2021-06-23 | 2021-10-01 | 浙江工业大学 | Three-dimensional structure iron-doped cobalt-molybdenum oxide composite material and preparation method and application thereof |
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