CN113522318A - Difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution and preparation method thereof - Google Patents
Difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution and preparation method thereof Download PDFInfo
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- CN113522318A CN113522318A CN202110696341.7A CN202110696341A CN113522318A CN 113522318 A CN113522318 A CN 113522318A CN 202110696341 A CN202110696341 A CN 202110696341A CN 113522318 A CN113522318 A CN 113522318A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000001301 oxygen Substances 0.000 title claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000001257 hydrogen Substances 0.000 title claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 21
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 12
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 4
- 125000000101 thioether group Chemical group 0.000 claims abstract description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 13
- 239000010937 tungsten Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 239000011268 mixed slurry Substances 0.000 claims description 6
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- OMAWWKIPXLIPDE-UHFFFAOYSA-N (ethyldiselanyl)ethane Chemical compound CC[Se][Se]CC OMAWWKIPXLIPDE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000010411 electrocatalyst Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/049—Sulfides with chromium, molybdenum, tungsten or polonium with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution, which consists of W, Co and S in a sulfide form, is coated in graphene and then loaded on carbon paper, and has a general formula of WxCoySz@ CP where x/y is greater than 0 and less than or equal to 10 and z is greater than 0 and less than or equal to 10. In addition, a preparation method of the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution is also disclosed. W integrated by the inventionxCoySzThe @ CP catalytic material is used as an electrocatalyst in OER and HER, shows the required difunctional electrocatalytic activity, and has the remarkable characteristics of low cost, high efficiency, durability, sufficient source, high stability and environmental friendlinessThe method can be widely applied to various oxygen evolution and hydrogen evolution electrolytic catalysis, and provides a new idea for designing a new electrode material with high catalytic activity, thereby having great value for large-scale industrial popularization and use.
Description
Technical Field
The invention relates to the technical field of catalytic materials, in particular to a bimetallic catalyst and a preparation method thereof.
Background
Increasing environmental concerns and the consumption of non-renewable fossil fuels have stimulated interest in sustainable energy development and energy storage conversion technology research. In these green energy systems, having high rates of oxygen reduction (ORR), Oxygen Evolution (OER) and Hydrogen Evolution (HER) at lower overpotentials is critical for energy utilization and output. Currently, the bottleneck in electrolytic water technology and rechargeable metal-air batteries is the lack of electrocatalysts of high efficiency and durability.
Zinc-air batteries have high theoretical energy density, are environmentally friendly, and have high safety, but their operating voltage is hindered due to the inefficient oxygen evolution and oxygen reduction catalytic properties of electrocatalysts. Hydrogen evolution is a crucial half-reaction in water splitting processes, also requiring efficient electrocatalysts. Platinum-based, ruthenium-based and iridium-based materials are highly efficient electrolytic water catalysts, but their high scarcity, high cost and inadequate long-term stability limit their large-scale commercial application.
Therefore, there is an urgent need to develop a low-cost, efficient, durable, abundant and stable electrolytic water dual-or tri-functional electrocatalyst to promote the reaction and thus improve the energy conversion efficiency. At present, although a lot of reports are made on transition metal bimetallic catalysts, reports on bifunctional tungsten-cobalt bimetallic electrolytic water catalysts for hydrogen evolution and oxygen evolution are not found yet.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution so as to obtain a tungsten single-metal electrolytic water catalytic material with high catalytic activity and stable performance. The invention also aims to provide a preparation method of the double-function tungsten-cobalt double-metal electrolytic water catalyst for hydrogen and oxygen evolution.
The purpose of the invention is realized by the following technical scheme:
the invention provides a bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution, which consists of W, Co and S in sulfide form, is coated in graphene and then loaded on carbon paper, and has a general formula of WxCoySz@ CP where x/y is greater than 0 and less than or equal to 10 and z is greater than 0 and less than or equal to 10.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution, which is provided by the invention, comprises the following steps:
(1) adding cobalt tungstate into a mixed solution consisting of hydrogen peroxide and hydrochloric acid according to the proportion of 1-20 mmol to 5-15 ml to 10-20 ml, and uniformly stirring to obtain mixed slurry containing tungsten and cobalt;
(2) soaking the carbon paper in ultrapure water and ethanol in sequence, ultrasonically cleaning for 3-8 min, and drying to obtain treated carbon paper;
(3) placing the treated carbon paper in mixed slurry containing tungsten and cobalt for dipping, and calcining at the temperature of 300-600 ℃ for 10-40 min to obtain carbon paper loaded with tungsten and cobalt oxide seed crystals;
(4) placing the carbon paper loaded with the tungsten and cobalt oxide seed crystals into a tube furnace, and introducing CS under the protection of argon or nitrogen2And (3) treating the solution at the temperature of 600-1000 ℃ for 0.5-3 h, and cooling to room temperature to obtain the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution.
The invention has the following beneficial effects:
(1) the invention successfully prepares the double-function tungsten-cobalt double-metal electrolytic water catalyst for hydrogen evolution and oxygen evolution by adopting the methods of impregnation, hydrothermal treatment and calcination for the first time, and provides a feasible method for preparing a high-performance catalytic material. Integrated WxCoySzThe @ CP nanowire catalyst acts as an electrocatalyst in OER and HER, showing the desired bifunctional electrocatalytic activity. Therefore, the catalyst has wide prospect in zinc-air batteries and water decomposition catalysis.
(2) Compared with other methods adopted at present, the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst has the remarkable characteristics of low cost, high efficiency, durability, sufficient source, high stability and environmental friendliness, provides a new thought for designing a new electrode material with high catalytic activity, and has great value for large-scale industrial popularization and use.
The present invention will be described in further detail with reference to examples.
Detailed Description
The embodiment of the difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution comprises W, Co and S in sulfide form, and is coated in graphene and then loaded on carbon paper, and the general formula of the catalyst is WxCoySz@ CP where x/y is greater than 0 and less than or equal to 10 and z is greater than 0 and less than or equal to 10. The formulation parameters for each example are shown in table 1.
TABLE 1 examples W of the inventionxCoySzFormula parameters of @ CP catalyst
| Examples | x | y | z |
| Example one | 2 | 1 | 2 |
| Example two | 1 | 1 | 2 |
| EXAMPLE III | 3 | 1 | 2 |
| Example four | 1 | 3 | 2 |
The preparation method of the difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution in the embodiment of the invention comprises the following steps:
(1) adding 1-20 mmol of cobalt tungstate, 5-15 ml of hydrogen peroxide and 10-20 ml of hydrochloric acid into a mixed solution consisting of hydrogen peroxide and hydrochloric acid, and stirring and mixing for 15min to obtain uniform mixed slurry containing tungsten and cobalt; the dosage of the ingredients of each example is shown in table 2;
TABLE 2 dosage of ingredients for each example of the invention
(2) Cutting the carbon paper into a rectangle with the size of 3cm multiplied by 6cm, sequentially soaking the carbon paper in ultrapure water and ethanol for 10min respectively, cleaning the carbon paper by an ultrasonic cleaner for 3-8 min, taking out the carbon paper, and drying the carbon paper in a vacuum oven at the temperature of 60 ℃ for 0.5h to obtain the treated carbon paper; the process parameters for each example are shown in table 3;
table 3 processing parameters of carbon paper of various embodiments of the present invention
(3) Soaking the treated carbon paper in mixed slurry containing tungsten and cobalt for 15min, and calcining the carbon paper in a tubular furnace at the temperature of 300-600 ℃ for 10-40 min to obtain carbon paper loaded with tungsten and cobalt oxide seed crystals; the process parameters for each example are shown in table 4;
TABLE 4 Process parameters in step (3) of the examples of the present invention
(4) Placing the carbon paper loaded with the tungsten and cobalt oxide seed crystals into a tube furnace, and introducing CS under the protection of argon or nitrogen2And (3) treating the solution at the temperature of 600-1000 ℃ for 0.5-3 h, and cooling to room temperature to obtain the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution. The process parameters for each example are shown in table 5.
TABLE 5 examples of the invention access CS2Processing parameters of
The electrochemical properties of the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution prepared in each example of the invention are shown in table 6.
TABLE 6 electrochemical Properties of catalysts prepared according to the examples of the invention
Claims (2)
1. A dual-function tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution is characterized in that: consists of W, Co and S in sulfide form, is wrapped in graphene and then loaded on carbon paper, and has a general formula of WxCoySz@ CP where x/y is greater than 0 and less than or equal to 10 and z is greater than 0 and less than or equal to 10.
2. The preparation method of the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution in claim 1 is characterized by comprising the following steps:
(1) adding cobalt tungstate into a mixed solution consisting of hydrogen peroxide and hydrochloric acid according to the proportion of 1-20 mmol to 5-15 ml to 10-20 ml, and uniformly stirring to obtain mixed slurry containing tungsten and cobalt;
(2) soaking the carbon paper in ultrapure water and ethanol in sequence, ultrasonically cleaning for 3-8 min, and drying to obtain treated carbon paper;
(3) placing the treated carbon paper in mixed slurry containing tungsten and cobalt for dipping, and calcining at the temperature of 300-600 ℃ for 10-40 min to obtain carbon paper loaded with tungsten and cobalt oxide seed crystals;
(4) placing the carbon paper loaded with the tungsten and cobalt oxide seed crystals into a tube furnace, and introducing CS under the protection of argon or nitrogen2And (3) treating the solution at the temperature of 600-1000 ℃ for 0.5-3 h, and cooling to room temperature to obtain the bifunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution.
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