CN110538662A - Preparation method of cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution - Google Patents
Preparation method of cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 13
- 239000001257 hydrogen Substances 0.000 title claims abstract description 13
- 239000002135 nanosheet Substances 0.000 title claims abstract description 12
- USWJSZNKYVUTIE-UHFFFAOYSA-N bis(sulfanylidene)rhenium Chemical compound S=[Re]=S USWJSZNKYVUTIE-UHFFFAOYSA-N 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011259 mixed solution Substances 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004744 fabric Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000010411 electrocatalyst Substances 0.000 claims abstract description 8
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 7
- 239000012498 ultrapure water Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims abstract description 4
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims abstract description 4
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000003738 black carbon Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011530 conductive current collector Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 Transition Metal Disulfide Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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- 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- 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
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Abstract
The invention relates to a preparation method of a cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution, which comprises the following steps: adding 2-methylimidazole aqueous solution into cobalt nitrate hexahydrate aqueous solution, and immersing an acid-treated carbon cloth into the mixed solution; after reacting for a period of time, taking a sample, and cleaning the sample with deionized water; and growing in the same solution for a period of time to obtain a ZIF-67 nano array sample named ZIF-67/CC, and finally, cleaning the sample and drying. Dissolving cobalt nitrate hexahydrate in a mixed solution of ultrapure water and ethanol, and putting the prepared ZIF-67/CC into the mixed solution for hydrolysis to obtain a product cobalt hydroxide nano array Co (OH) 2/CC; the product Co-ReS2/CC is obtained. The Co-ReS2/CC prepared by the preparation method is applied to HER electrocatalysts.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and particularly relates to a preparation method of a cobalt hydroxide nano array modified rhenium disulfide nanosheet loaded on carbon cloth.
background
In order to solve the increasing energy demand and environmental pressure in the process of human continuing development, the electrocatalytic hydrogen production technology is well paid attention by researchers due to the advantages of cleanness, low price and sustainability. The existing electrode material for water electrolysis has the defects of high price, small specific surface area, low electrocatalytic activity and the like, so that the potential is too high, the energy consumption is too large, the development of a water electrolysis hydrogen production technology is seriously restricted, and the development of a material which can produce hydrogen efficiently and has low price is urgently needed to solve the problem.
Rhenium disulfide (ReS2) is a two-dimensional (2D) group VII Transition Metal Disulfide (TMD) with a large number of active sites at the edge, and shows the potential of a high-performance catalyst in an energy conversion and storage device like a group VI isotropic TMD material, but rhenium disulfide nanosheets prepared by a common preparation method are difficult to directionally grow and easy to agglomerate, so that the activity of an electrocatalytic hydrogen evolution reaction is greatly reduced. The metal-organic framework (ZIF-67) is often used as an electrocatalyst or a precursor and a template for preparing the electrocatalyst due to excellent physicochemical properties of porosity, various structures, controllable chemical compositions and the like, and metal atoms are introduced in the preparation process, so that the electrocatalytic activity of the material can be greatly improved.
Disclosure of Invention
The invention aims to provide a preparation method of a cobalt-doped rhenium disulfide nanosheet array, the material is formed by growing Co-doped ReS2 on carbon cloth, the preparation process is simple, and the material has good electrochemical performance when used as a HER electrocatalyst. The technical scheme of the invention is as follows:
A preparation method of a cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution comprises the following steps:
(1) Adding an aqueous solution of 2-methylimidazole to an aqueous solution of cobalt nitrate hexahydrate in a molar ratio of Co (NO3) 2.6H 2O: 2-MIM (1: 14-1: 18), and immersing a piece of acid-treated carbon cloth into the mixed solution; after reacting for a period of time, taking a sample, and cleaning the sample with deionized water; and growing in the same solution for a period of time to obtain a ZIF-67 nano array sample named ZIF-67/CC, and finally, cleaning the sample and drying.
(2) Dissolving cobalt nitrate hexahydrate in a mixed solution of ultrapure water and ethanol, and putting the ZIF-67/CC prepared in the step (1) into the mixed solution for hydrolysis to obtain a product, namely a cobalt hydroxide nano array Co (OH) 2/CC.
(3) Dissolving ammonium perrhenate, hydroxylamine hydrochloride and thiourea into deionized water according to the molar ratio of NH4ReO4: HONH3Cl: CH4N2S of 1:3: 4.5-2: 3:4.5, transferring into a high-pressure kettle, placing Co (OH)2/CC prepared in the step (2) into the high-pressure kettle, and preserving the heat for a period of time in an oven at the temperature of 180-220 ℃ to obtain a product Co-ReS 2/CC.
The Co-ReS2/CC prepared by the preparation method is applied to HER electrocatalysts.
Compared with the prior art, the invention has the advantages that:
(1) The invention utilizes the ZIF-67 hydrolysate Co (OH)2 nano array as a template to grow the directionally vertical ReS2 nano sheet, exposes a large amount of active sites and improves the electro-catalytic hydrogen evolution performance.
(2) The invention utilizes ZIF-67 as a Co source to be doped into ReS2, and improves the hydrogen evolution reaction activity of ReS2 under alkaline conditions.
(3) The product grows on the surface of the carbon cloth in situ, the prepared self-supporting structure can be directly used as an electrode to carry out electrocatalytic hydrogen evolution reaction, and a high-price binder is not required to be added to coat the surface of the glassy carbon electrode, so that the preparation process is simple, the cost is reduced, more active sites are exposed, and the electrocatalytic activity is improved.
Drawings
FIG. 1 is an SEM photograph of Co-ReS2/CC obtained in example 1 of the present invention. The figure clearly shows that the Co-ReS2/CC presents lamellar morphology, and the ReS2 nanosheet grows on the surface of the carbon cloth in an oriented and vertical mode.
FIG. 2 is an XRD photograph of Co-ReS2/CC obtained in example 1 of the present invention. It is evident from this figure that the re 2 phase remains after Co doping.
FIG. 3 is a graph of the HER performance of Co-ReS2/CC obtained in example 1 of the present invention. The excellent catalytic performance of the electrocatalyst is evident from this figure.
Nothing in this specification is said to apply to the prior art.
Specific examples of the production method of the present invention are given below. These examples are only intended to illustrate the preparation process of the present invention in detail and do not limit the scope of protection of the claims of the present application.
Detailed Description
Example 1
0.291g of 2-methylimidazole is respectively weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution A, 1.3136g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution B, and the solution A is quickly added into the solution B to be stirred for 30min to obtain mixed solution C. A piece of nitric acid treated carbon cloth (WOS109 type, 1 x 1.5 x 0.036cm3) was immersed in the C solution. After 4h of reaction, samples were taken, washed repeatedly with deionized water, and then grown in the same solution for another 4 h. Finally, the sample was washed with deionized water, dried overnight under vacuum at 60 ℃ and a layer of purple sample (ZIF-67/CC) was loaded onto a black carbon cloth.
0.5g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of mixed solution of ultrapure water and ethanol with the volume ratio of 1:9, the prepared ZIF-67/CC is put into the mixed solution, the mixed solution is stirred for 30min at room temperature, a sample is taken out, the mixed solution is repeatedly washed by deionized water, and the sample is dried in vacuum at 60 ℃ overnight, so that a purple sample becomes light blue (Co (OH) 2/CC).
0.161g of ammonium perrhenate, 0.205g of thiourea and 0.125g of hydroxylamine hydrochloride are weighed and dissolved in 20ml of deionized water, stirred for 30min and then transferred to a 50ml hydrothermal kettle, and then the prepared sample is put in. And (3) placing the hydrothermal kettle in a blast oven, and keeping the temperature at 200 ℃ for 21 h. After the reaction, the mixture is washed by absolute ethyl alcohol and deionized water for three times respectively, and then dried in a constant temperature oven at 60 ℃ overnight, and a light blue sample turns into black.
Example 2
0.407g of 2-methylimidazole is respectively weighed, dissolved in 40ml of water and stirred for 10min to obtain solution A, 1.3136g of cobalt nitrate hexahydrate is weighed, dissolved in 40ml of water and stirred for 10min to obtain solution B, and the solution A is quickly added into the solution B and stirred for 30min to obtain mixed solution C. A piece of nitric acid treated carbon cloth (WOS109 type, 1 x 1.5 x 0.036cm3) was immersed in the C solution. After 4h of reaction, samples were taken, washed repeatedly with deionized water, and then grown in the same solution for another 4 h. Finally, the sample was washed with deionized water, dried overnight under vacuum at 60 ℃ and a layer of purple sample (ZIF-67/CC) was loaded onto a black carbon cloth.
0.5g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of mixed solution of ultrapure water and ethanol with the volume ratio of 1:9, the prepared ZIF-67/CC is put into the mixed solution, the mixed solution is stirred for 30min at room temperature, a sample is taken out, the mixed solution is repeatedly washed by deionized water, and the sample is dried in vacuum at 60 ℃ overnight, so that a purple sample becomes light blue (Co (OH) 2/CC).
0.161g of ammonium perrhenate, 0.205g of thiourea and 0.125g of hydroxylamine hydrochloride are weighed and dissolved in 20ml of deionized water, stirred for 30min and then transferred to a 50ml hydrothermal kettle, and then the prepared sample is put in. And (3) placing the hydrothermal kettle in a blast oven, and keeping the temperature at 200 ℃ for 21 h. After the reaction, the mixture is washed by absolute ethyl alcohol and deionized water for three times respectively, and then dried in a constant temperature oven at 60 ℃ overnight, and a light blue sample turns into black.
Example 3
0.52g of 2-methylimidazole is respectively weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution A, 1.3g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution B, and the solution A is quickly added into the solution B to be stirred for 30min to obtain mixed solution C. A piece of nitric acid treated carbon cloth (WOS109 type, 1 x 1.5 x 0.036cm3) was immersed in the C solution. After 4h of reaction, samples were taken, washed repeatedly with deionized water, and then grown in the same solution for another 4 h. Finally, the sample was washed with deionized water, dried overnight under vacuum at 60 ℃ and a layer of purple sample (ZIF-67/CC) was loaded onto a black carbon cloth.
0.5g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of mixed solution of ultrapure water and ethanol with the volume ratio of 1:9, the prepared ZIF-67/CC is put into the mixed solution, the mixed solution is stirred for 30min at room temperature, a sample is taken out, the mixed solution is repeatedly washed by deionized water, and the sample is dried in vacuum at 60 ℃ overnight, so that a purple sample becomes light blue (Co (OH) 2/CC).
0.161g of ammonium perrhenate, 0.205g of thiourea and 0.125g of hydroxylamine hydrochloride are weighed and dissolved in 20ml of deionized water, stirred for 30min and then transferred to a 50ml hydrothermal kettle, and then the prepared sample is put in. And (3) placing the hydrothermal kettle in a blast oven, and keeping the temperature at 200 ℃ for 21 h. After the reaction, the mixture is washed by absolute ethyl alcohol and deionized water for three times respectively, and then dried in a constant temperature oven at 60 ℃ overnight, and a light blue sample turns into black.
example 4
0.291g of 2-methylimidazole is respectively weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution A, 1.3136g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of water to be stirred for 10min to obtain solution B, and the solution A is quickly added into the solution B to be stirred for 30min to obtain mixed solution C. A piece of nitric acid treated carbon cloth (WOS109 type, 1 x 1.5 x 0.036cm3) was immersed in the C solution. After 4h of reaction, samples were taken, washed repeatedly with deionized water, and then grown in the same solution for another 4 h. Finally, the sample was washed with deionized water, dried overnight under vacuum at 60 ℃ and a layer of purple sample (ZIF-67/CC) was loaded onto a black carbon cloth.
0.5g of cobalt nitrate hexahydrate is weighed and dissolved in 40ml of mixed solution of ultrapure water and ethanol with the volume ratio of 1:9, the prepared ZIF-67/CC is put into the mixed solution, the mixed solution is stirred for 30min at room temperature, a sample is taken out, the mixed solution is repeatedly washed by deionized water, and the sample is dried in vacuum at 60 ℃ overnight, so that a purple sample becomes light blue (Co (OH) 2/CC).
0.322g of ammonium perrhenate, 0.205g of thiourea and 0.125g of hydroxylamine hydrochloride are weighed and dissolved in 20ml of deionized water, stirred for 30min and then transferred to a 50ml hydrothermal kettle, and then the prepared sample is put in. And (3) placing the hydrothermal kettle in a blast oven, and keeping the temperature at 200 ℃ for 21 h. After the reaction, the mixture is washed by absolute ethyl alcohol and deionized water for three times respectively, and then dried in a constant temperature oven at 60 ℃ overnight, and a light blue sample turns into black.
The invention uses ZIF-67 as a template to grow the rhenium disulfide nanosheet to prepare the high-efficiency hydrogen evolution reaction electrocatalyst. Carbon Cloth (CC) is used as a conductive current collector, a ZIF-67 nanorod array vertically grows on the surface of the conductive current collector, then is hydrolyzed, a hydrolysis product is used as a template, and a cobalt-doped rhenium disulfide nanosheet array (Co-ReS2/CC) is prepared through a hydrothermal reaction. Electrochemical tests prove that Co-ReS2/CC has excellent HER activity, and the HER overpotential is 120mV when the current density is 10mAcm & lt-2 & gt in a 1M KOH electrolyte.
Claims (2)
1. A preparation method of a cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution comprises the following steps:
(1) Adding an aqueous solution of 2-methylimidazole to an aqueous solution of cobalt nitrate hexahydrate in a molar ratio of Co (NO3) 2.6H 2O: 2-MIM (1: 14-1: 18), and immersing a piece of acid-treated carbon cloth into the mixed solution; after reacting for a period of time, taking a sample, and cleaning the sample with deionized water; and growing in the same solution for a period of time to obtain a ZIF-67 nano array sample named ZIF-67/CC, and finally, cleaning the sample and drying.
(2) Dissolving cobalt nitrate hexahydrate in a mixed solution of ultrapure water and ethanol, and putting the ZIF-67/CC prepared in the step (1) into the mixed solution for hydrolysis to obtain a product, namely a cobalt hydroxide nano array Co (OH) 2/CC.
(3) Dissolving ammonium perrhenate, hydroxylamine hydrochloride and thiourea into deionized water according to the molar ratio of NH4ReO4: HONH3Cl: CH4N2S of 1:3: 4.5-2: 3:4.5, transferring into a high-pressure kettle, placing Co (OH)2/CC prepared in the step (2) into the high-pressure kettle, and preserving the heat for a period of time in an oven at the temperature of 180-220 ℃ to obtain a product Co-ReS 2/CC.
2. The production method according to claim 1,
The Co-ReS2/CC prepared by the preparation method of claim 1 is applied to HER electrocatalyst.
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CN111403180A (en) * | 2020-02-26 | 2020-07-10 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Nickel hydroxide/cobalt disulfide composite material and preparation method and application thereof |
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CN111740092A (en) * | 2020-07-24 | 2020-10-02 | 广州大学 | Heterostructure material and preparation method and application thereof |
CN112023944A (en) * | 2020-07-27 | 2020-12-04 | 天津大学 | Preparation method for in-situ synthesis of rhenium and rhenium disulfide heterostructure composite material |
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CN113279005A (en) * | 2021-04-19 | 2021-08-20 | 江苏大学 | Cobalt doped MoS2/NiS2Preparation method of porous heterostructure material and application of material in electrocatalytic hydrogen evolution |
CN115448376A (en) * | 2022-09-05 | 2022-12-09 | 中国科学院深圳先进技术研究院 | Preparation method of cobalt-based nanosheet, cobalt-based nanosheet and application |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106277064A (en) * | 2016-07-22 | 2017-01-04 | 电子科技大学 | A kind of method preparing rhenium disulfide nanometer sheet |
CN107640791A (en) * | 2017-10-26 | 2018-01-30 | 陕西科技大学 | A kind of micron-stage sheet-like beta cobaltous hydroxide and its environment-friendly preparation method thereof |
WO2018098451A1 (en) * | 2016-11-28 | 2018-05-31 | North Carolina State University | Catalysts for hydrogen evolution reaction including transition metal chalcogenide films and methods of forming the same |
CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
-
2019
- 2019-07-01 CN CN201910586815.5A patent/CN110538662A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106277064A (en) * | 2016-07-22 | 2017-01-04 | 电子科技大学 | A kind of method preparing rhenium disulfide nanometer sheet |
WO2018098451A1 (en) * | 2016-11-28 | 2018-05-31 | North Carolina State University | Catalysts for hydrogen evolution reaction including transition metal chalcogenide films and methods of forming the same |
CN107640791A (en) * | 2017-10-26 | 2018-01-30 | 陕西科技大学 | A kind of micron-stage sheet-like beta cobaltous hydroxide and its environment-friendly preparation method thereof |
CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
Non-Patent Citations (2)
Title |
---|
JING PAN ET AL.: ""Transition metal doping activated basal-plane catalytic activity of two-dimensional 1T"-ReS2 for hydrogen evolution reaction: a first-principles calculation study"", 《NANOSCALE》 * |
罗浩: ""ZIF-67衍生双金属氢氧化物复合材料的制备与电容性能研究"", 《中国优秀硕士博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 * |
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CN112023944A (en) * | 2020-07-27 | 2020-12-04 | 天津大学 | Preparation method for in-situ synthesis of rhenium and rhenium disulfide heterostructure composite material |
CN112058268A (en) * | 2020-09-07 | 2020-12-11 | 北京理工大学 | Preparation method of zeolite imidazolyl metal organic framework nanosheet for oxygen reduction reaction |
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CN115448376A (en) * | 2022-09-05 | 2022-12-09 | 中国科学院深圳先进技术研究院 | Preparation method of cobalt-based nanosheet, cobalt-based nanosheet and application |
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