CN111167476B - Carbon-carried RhNi-Ni (OH) 2 Preparation method of composite hydrogen evolution electrocatalyst - Google Patents
Carbon-carried RhNi-Ni (OH) 2 Preparation method of composite hydrogen evolution electrocatalyst Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 6
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229940053662 nickel sulfate Drugs 0.000 claims description 5
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 5
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 5
- TYLYVJBCMQFRCB-UHFFFAOYSA-K trichlororhodium;trihydrate Chemical compound O.O.O.[Cl-].[Cl-].[Cl-].[Rh+3] TYLYVJBCMQFRCB-UHFFFAOYSA-K 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 36
- 239000000243 solution Substances 0.000 abstract description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 15
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000012670 alkaline solution Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000010948 rhodium Substances 0.000 description 9
- 229910000510 noble metal Inorganic materials 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- GPGGPRHLKWIJFR-UHFFFAOYSA-L [Ni](O)O.[Ni].[Rh] Chemical compound [Ni](O)O.[Ni].[Rh] GPGGPRHLKWIJFR-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001075 voltammogram Methods 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
- 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
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/892—Nickel and noble metals
-
- 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
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- 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
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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
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Abstract
The invention relates to a carbon-carried RhNi-Ni (OH) 2 The preparation method of the composite hydrogen evolution electrocatalyst comprises the steps of adding a solution of nickel sulfate and rhodium chloride with a molar ratio of 1:3 to 3:1 into carbon powder dispersion liquid, wherein the mass ratio of metal elements to carbon powder is 3: 7; na is added dropwise 2 CO 3 A solution to adjust the pH to 9.0; then dropwise adding NaBH with the molar weight 40-80 times that of the metal element 4 The solution is fully reduced until no bubble is generated, and then the RhNi-Ni (OH) is obtained after centrifugal separation, washing and freeze drying 2 And C, performing reaction. RhNi-Ni (OH) prepared by the method 2 The composite catalyst shows good hydrogen evolution catalytic activity in alkaline solution. When the current density is 10mA cm ‑2 When the catalyst is used, the hydrogen evolution overpotential is even higher than that of a Pt/C catalyst, so that the catalyst has good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic hydrogen evolution, and relates to a carbon-supported RhNi-Ni (OH) 2 A preparation method of (rhodium nickel-nickel hydroxide) composite hydrogen evolution electrocatalyst.
Background
Hydrogen is considered to be one of the ideal alternatives to fossil fuels as a clean, efficient renewable energy source. The hydrogen evolution reaction is a half-reaction of electrolysis of water and is one of the important ways to prepare hydrogen. However, since the overvoltage of the hydrogen evolution reaction is high and a large amount of electric energy is consumed, it is necessary to develop an electrocatalyst having excellent catalytic performance to lower the energy barrier of the hydrogen evolution reaction. The hydrogen evolution catalyst with outstanding catalytic performance is mainly a noble metal catalyst, and the performance of the platinum-based catalyst is the most excellent at present. The hydrogen production reaction by electrolyzing water is mostly carried out in alkaline solution, and for a bulk catalyst, the catalytic activity of platinum in an alkaline environment is nearly two orders of magnitude lower than that under an acidic condition, andthe catalytic activity of rhodium in alkaline and acidic solutions is only about an order of magnitude different (see Jie Zheng, et al, Universal dependency of hydrogen oxidation and evolution reactivity of platinum-group metals on pH and hydrogen binding energy, Sci. adv.,2016,2: e 1501602). Therefore, by regulating and controlling the components, the morphology and the structure of the rhodium-based catalyst, the hydrogen evolution catalytic performance more outstanding than that of a platinum catalyst in an alkaline solution is expected to be obtained. Currently, researchers have prepared Rh-based hydrogen evolution catalysts with excellent performance in alkaline environment, such as RhNi nano-sponge, Rh nanosheet, Rh nanoflower and the like, by regulating and controlling the morphology and components of the catalysts. However, the proportion of the noble metal element Rh in the Rh-based hydrogen evolution catalyst is still high, which is not favorable for reducing the production cost. Therefore, the development of a method for preparing the Rh-based hydrogen evolution catalyst with lower price has very important practical significance. Studies have found that the hydrogen evolution catalytic performance of noble metals in alkaline solutions can be greatly improved when transition metal hydroxides act in concert with noble metals (see the document Huajie Yin, et al, Ultrathin platinum catalysts grown on single-layered aqueous reaction activity, Nature Communications,2015,6: 6430). In addition, the cost can be reduced by adding non-noble transition metal alloy elements into the noble metal catalyst, and the catalytic activity can be improved by the synergistic action of different elements. Based on The above theory and research foundation, The present invention develops RhCo/C methanol oxidation catalyst by using The method of aging and The like (Yu Chen, et al, The electrochemical performance of carbon ball supported RhCo alloy catalysts for The methanol oxidation reaction in The methanol medium, Journal of Power Source, 2017,371:129-135), developed RhNi-Ni (OH) 2 a/C hydrogen evolution electrocatalyst.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a carbon-supported RhNi-Ni (OH) 2 A preparation method of a composite hydrogen evolution electrocatalyst.
Technical scheme
Carbon-supported RhNi-Ni (OH) 2 The preparation method of the composite hydrogen evolution electrocatalyst is characterized by comprising the following steps:
step 1: heat-treating the carbon powder in argon atmosphere at 500 deg.C for 3 hr;
step 2: ultrasonically dispersing carbon powder for 1 hour at room temperature by using deionized water;
and 3, step 3: dissolving nickel sulfate and rhodium chloride in a molar ratio of 1:3 to 3:1 in deionized water to form a solution;
and 4, step 4: adding the solution into carbon powder dispersion liquid to ensure that the mass ratio of the metal elements to the carbon powder is 3:7, and fully stirring and mixing;
and 5: then Na is added dropwise 2 CO 3 A solution to adjust the pH to 9.0;
step 6: heating and stirring the mixture in water bath at the temperature of between 60 and 70 ℃ for 5 to 7 hours;
and 7: then dropwise adding NaBH with the molar weight 40-80 times that of the metal element 4 The solution is fully reduced until no bubbles are generated, and then is centrifugally separated, washed and freeze-dried to obtain RhNi-Ni (OH) 2 /C。
And XC-72R carbon powder is adopted as the carbon powder.
The nickel sulfate adopts nickel sulfate hexahydrate.
The rhodium chloride adopts rhodium chloride trihydrate.
Advantageous effects
The invention provides a carbon-carried RhNi-Ni (OH) 2 The preparation method of the composite hydrogen evolution electrocatalyst comprises the steps of adding a solution of nickel sulfate and rhodium chloride with a molar ratio of 1:3 to 3:1 into carbon powder dispersion liquid, wherein the mass ratio of metal elements to carbon powder is 3: 7; na was added dropwise 2 CO 3 A solution to adjust the pH to 9.0; then dropwise adding NaBH with the molar weight 40-80 times that of the metal element 4 The solution is fully reduced until no bubble is generated, and then the RhNi-Ni (OH) is obtained after centrifugal separation, washing and freeze drying 2 and/C. RhNi-Ni (OH) prepared by the method 2 The composite catalyst shows good hydrogen evolution catalytic activity in alkaline solution. When the current density is 10mA cm -2 When the catalyst is used, the hydrogen evolution overpotential is even higher than that of a Pt/C catalyst, and thus the catalyst has good performanceAnd (4) industrial application prospect.
The invention has the following beneficial effects:
(1) the carbon carrier is subjected to heat treatment in an inert gas environment, so that pollutants on the surface of the carbon black can be decomposed, and the content of oxygen-containing functional groups on the surface is increased, so that the dispersity of the catalyst particles on the surface is effectively improved. Compared with other preparation methods, the method does not need high-temperature acid washing on the carbon carrier, thereby avoiding the volatilization of corrosive gas and the generation of toxic gas, and shortening the preparation time and difficulty.
(2) The invention relates to a method for preparing transition metal hydroxide Ni (OH) 2 The catalyst is combined with metal alloy RhNi to form a composite catalyst, compared with a commercial Rh/C, Pt/C catalyst, the dosage of noble metal in the preparation process is greatly reduced, and the production cost is obviously reduced.
(3) The carbon ball prepared by the invention loads RhNi-Ni (OH) 2 The composite catalyst exhibits better hydrogen evolution activity in alkaline solution than commercial Pt/C catalysts, e.g., when the current density is 10mA cm -2 When the catalyst is used, the hydrogen evolution overpotential is higher than that of a Pt/C catalyst, so that the catalytic efficiency of the catalyst is higher than that of the Pt/C catalyst.
Drawings
FIG. 1 shows a carbon-supported RhNi-Ni (OH) prepared in example 1 of the present invention 2 TEM topography of hydrogen evolution catalysts;
FIG. 2 is the carbon-supported RhNi-Ni (OH) prepared in example 1 2 XRD pattern of electrocatalyst;
FIG. 3 is a carbon loaded RhNi-Ni (OH) with different rhodium to nickel ratios 2 Linear sweep voltammogram of electrocatalyst and noble metal Pt/C in basic solution.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
Heat-treating XC-72R carbon powder in argon atmosphere at 500 ℃ for 3 hours, dispersing the heat-treated carbon powder in deionized water by using ultrasonic waves, preparing 2mL of nickel sulfate hexahydrate and rhodium chloride trihydrate solution with the molar ratio of 1:1, adding the solution into the carbon powder dispersion liquid, and fully adding the solutionStirring and mixing uniformly, then dropwise adding 0.5mol/L sodium carbonate solution to adjust the pH value to 9.0, heating and stirring in water bath at 60 ℃ for 7 hours, and adding 4mL of NaBH containing 70 times of metal salt in molar quantity at room temperature 4 Dripping the solution into the dispersion, fully stirring until the reaction is complete and no bubbles are generated, centrifugally separating the dispersion, fully washing with deionized water, and freeze-drying for 12 hours to obtain RhNi-Ni (OH) 2 A catalyst.
Example 2
Heat-treating XC-72R carbon powder for 3 hours in an argon atmosphere at 500 ℃, dispersing the heat-treated carbon powder in deionized water by using ultrasonic waves, preparing 2mL of nickel sulfate hexahydrate and rhodium chloride trihydrate solution with the molar ratio of 3:1, adding the solution into the carbon powder dispersion liquid, fully stirring and uniformly mixing, then dropwise adding 0.5mol/L sodium carbonate solution to adjust the pH value to 9.0, heating and stirring in a water bath at 65 ℃ for 6 hours, and adding 4mL of NaBH containing 60 times of metal salt in molar weight at room temperature 4 Dripping the solution into the dispersion, fully stirring until the reaction is complete and no bubbles are generated, centrifugally separating the dispersion, fully washing with deionized water, and freeze-drying for 12 hours to obtain RhNi-Ni (OH) 2 A catalyst.
Example 3
Heat-treating XC-72R carbon powder for 3 hours in an argon atmosphere at 500 ℃, dispersing the heat-treated carbon powder in deionized water by using ultrasonic waves, preparing 2mL of nickel sulfate hexahydrate and rhodium chloride trihydrate solution with the molar ratio of 1:3, adding the solution into the carbon powder dispersion liquid, fully stirring and uniformly mixing, then dropwise adding 0.5mol/L sodium carbonate solution to adjust the pH value to 9.0, heating and stirring in a water bath at 70 ℃ for 5 hours, and adding 4mL of NaBH containing 80 times of metal salt in molar weight at room temperature 4 Dripping the solution into the dispersion, fully stirring until the reaction is complete and no bubbles are generated, centrifugally separating the dispersion, fully washing with deionized water, and freeze-drying for 12 hours to obtain RhNi-Ni (OH) 2 A catalyst.
Claims (4)
1. Carbon-carried RhNi-Ni (OH) 2 The preparation method of the composite hydrogen evolution electrocatalyst is characterized by comprising the following steps:
step 1: heat-treating the carbon powder in argon atmosphere at 500 deg.C for 3 hr;
step 2: ultrasonically dispersing carbon powder for 1 hour at room temperature by using deionized water;
and step 3: dissolving nickel sulfate and rhodium chloride in a molar ratio of 1:3 to 3:1 in deionized water to form a solution;
and 4, step 4: adding the solution into the carbon powder dispersion liquid to ensure that the mass ratio of the metal elements to the carbon powder is 3:7, and fully stirring and mixing;
and 5: then Na is added dropwise 2 CO 3 A solution to adjust the pH to 9.0;
step 6: heating and stirring the mixture in water bath at the temperature of between 60 and 70 ℃ for 5 to 7 hours;
and 7: then dropwise adding NaBH with the molar weight 40-80 times that of the metal element 4 The solution is fully reduced until no bubbles are generated, and then is centrifugally separated, washed and freeze-dried to obtain RhNi-Ni (OH) 2 /C。
2. The carbon-supported RhNi-ni (oh) of claim 1 2 The preparation method of the composite hydrogen evolution electrocatalyst is characterized by comprising the following steps: and XC-72R carbon powder is adopted as the carbon powder.
3. The carbon-supported RhNi-Ni (OH) of claim 1 2 The preparation method of the composite hydrogen evolution electrocatalyst is characterized by comprising the following steps: the nickel sulfate is nickel sulfate hexahydrate.
4. The carbon-supported RhNi-Ni (OH) of claim 1 2 The preparation method of the composite hydrogen evolution electrocatalyst is characterized by comprising the following steps: the rhodium chloride adopts rhodium chloride trihydrate.
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