CN111905819A - Preparation method of two-dimensional NiCoFe-MOF electrocatalyst - Google Patents
Preparation method of two-dimensional NiCoFe-MOF electrocatalyst Download PDFInfo
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- QAYXDWGFSMUTBJ-UHFFFAOYSA-L dipotassium;naphthalene-2,6-dicarboxylate Chemical compound [K+].[K+].C1=C(C([O-])=O)C=CC2=CC(C(=O)[O-])=CC=C21 QAYXDWGFSMUTBJ-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910052759 nickel Inorganic materials 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 150000001868 cobalt Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- UOBYKYZJUGYBDK-UHFFFAOYSA-N 2-naphthoic acid Chemical compound C1=CC=CC2=CC(C(=O)O)=CC=C21 UOBYKYZJUGYBDK-UHFFFAOYSA-N 0.000 claims 1
- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical compound [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- 239000012621 metal-organic framework Substances 0.000 abstract description 30
- 239000002135 nanosheet Substances 0.000 abstract description 7
- 239000013274 2D metal–organic framework Substances 0.000 abstract description 5
- 239000002243 precursor Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- -1 iron ions Chemical class 0.000 abstract description 2
- 239000013110 organic ligand Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 9
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000006260 foam Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
-
- B01J35/33—
-
- B01J35/61—
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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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/847—Nickel
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Abstract
The invention provides a preparation method of a two-dimensional NiCoFe-MOF electrocatalyst, which is characterized in that the two-dimensional NiCoFe double-layer hydroxide reacts with dipotassium 2, 6-naphthalene dicarboxylate to generate the two-dimensional NiCoFe-MOF electrocatalyst. The invention adopts iron ions to hydrolyze, coprecipitate and synthesize NiCoFe-LDH nano-sheets as precursors, and then the precursors and organic ligands perform coordination reaction under mild conditions to obtain the NiCoFe-MOF electrocatalyst with two-dimensional morphology. The 2D MOF nanosheet prepared by the method has a large specific surface area, and the active sites of the 2D MOF nanosheet are directly exposed on the surface, so that the mass transfer resistance is reduced, and further, the mass transfer resistance is shown to be higher than that of commercial IrO2High oxygen evolution activity and stability, and wide application prospect in the field of electrocatalysis.
Description
Technical Field
The invention relates to the technical field of electrocatalysis, in particular to a preparation method of a two-dimensional NiCoFe-MOF electrocatalyst.
Background
As an ideal novel energy source, the hydrogen has high combustion enthalpy, can release more energy during combustion, has no pollution to combustion products, and provides a new way for relieving the fossil energy crisis. At present, the hydrogen preparation method is diversified, wherein the hydrogen preparation by water electrolysis is regarded as one of the most promising hydrogen preparation methods due to the advantages of simple operation, no pollution, high hydrogen preparation purity and the like. The hydrogen production process by water electrolysis relates to the water reduction hydrogen evolution reaction of a cathode and the water oxidation oxygen evolution reaction of an anode. Since water oxidation is difficult in both kinetics and thermodynamics, the anode overpotential is usually much higher than the cathode overpotential, and the anode reaction also becomes a bottleneck limiting the energy conversion efficiency of the whole water decomposition system. At present, the noble metal catalyst with high catalytic activity is difficult to popularize and apply on a large scale due to the scarcity and poor stability of the noble metal catalyst.
In the last few years, Metal Organic Frameworks (MOFs) have attracted considerable attention from researchers and are widely used in the field of energy storage and conversion. Recent research shows that the MOFs material with unique two-dimensional morphology enables active sites to be directly exposed on the surface, reduces mass transfer resistance, and shows more active catalytic activity than MOFs materials with other dimensions. However, many challenges still exist in the synthesis of two-dimensional MOFs materials, such as complex synthesis method, high synthesis condition requirement, low yield, and difficult application to practical production. Therefore, the method has important significance for large-scale synthesis of the 2D MOFs material under the synthesis conditions of simple exploration, mildness and environmental protection.
Disclosure of Invention
The invention aims to provide a preparation method of a two-dimensional NiCoFe-MOF electrocatalyst which is simple in preparation, cheap in raw materials and mild in conditions.
In order to achieve the purpose, the invention provides a preparation method of a two-dimensional NiCoFe-MOF electrocatalyst, which is characterized in that the two-dimensional NiCoFe double-layer hydroxide reacts with 2, 6-naphthalenedicarboxylic acid dipotassium salt to generate the two-dimensional NiCoFe-MOF electrocatalyst.
The method specifically comprises the following steps:
step 1: taking foamed nickel for pretreatment;
step 2: soaking the pretreated foamed nickel in a mixed aqueous solution containing ferric salt and cobalt salt for reaction to obtain a mixed solution of two-dimensional NiCoFe double-layer hydroxide supported by the foamed nickel;
and step 3: adding dipotassium 2, 6-naphthalenedicarboxylate into the mixed solution, and shaking until the dipotassium 2, 6-naphthalenedicarboxylate is completely dissolved;
and 4, after the reaction is completed, drying the mixed solution, taking out the precipitate, cleaning the precipitate, and drying to obtain the two-dimensional NiCoFe-MOF electrocatalyst loaded on the foamed nickel.
Preferably, in step 1, the pretreatment comprises ultrasonic washing of the nickel foam in 3M hydrochloric acid, ethanol and deionized water for 15min in sequence, and drying for later use.
Preferably, in the step 2, the foamed nickel is immersed in the mixed aqueous solution containing the iron salt and the cobalt salt for reaction for 1-2 hours.
Preferably, in step 2, the iron salt and the cobalt salt are nitrate or chlorate; the molar concentration of the metal salt in the mixed aqueous solution containing the ferric salt and the cobalt salt is 5-30mmol L-1。
Preferably, in step 3, the dipotassium 2, 6-naphthalenedicarboxylate is added into the mixed solution, the mixed solution is shaken until the dipotassium 2, 6-naphthalenedicarboxylate is completely dissolved, and then the mixed solution is transferred into an oven to react for 16-24 hours at 60-90 ℃.
Preferably, in step 3, the mole number of the dipotassium 2, 6-naphthalenedicarboxylate added is 1-2 times that of the metal salt in the solution.
Preferably, in step 4, the precipitate is washed with ethanol and deionized water.
Preferably, the two-dimensional NiCoFe-MOF electrocatalyst is used directly in water oxidation applications.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts iron ions to hydrolyze, coprecipitate and synthesize NiCoFe-LDH nano-sheets as precursors, and then the precursors and organic ligands perform coordination reaction under mild conditions to obtain the NiCoFe-MOF electrocatalyst with two-dimensional morphology.
(2) The 2D MOF nanosheet prepared by the method has a large specific surface area, and the active sites of the 2D MOF nanosheet are directly exposed on the surface, so that the mass transfer resistance is reduced, and further, the mass transfer resistance is shown to be higher than that of commercial IrO2High oxygen evolution activity and stability, and wide application prospect in the field of electrocatalysis.
Drawings
FIG. 1 is a scanning electron micrograph of two-dimensional (2D) NiCoFe-LDH/NF prepared in example 1.
FIG. 2 is a scanning electron micrograph of the two-dimensional (2D) NiCoFe-MOF/NF prepared in example 1, which shows that the nanosheets grow further.
FIG. 3 shows two-dimensional (2D) NiCoFe-MOF/NF and commercial IrO prepared in example 12Polarization profile of water oxidation.
FIG. 4 is a scanning electron micrograph of two-dimensional (2D) NiCoFe-MOF/NF prepared in example 2.
FIG. 5 is a scanning electron micrograph of two-dimensional (2D) NiCoFe-MOF/NF prepared in example 3.
FIG. 6 is a scanning electron micrograph of two-dimensional (2D) NiFe-MOF/NF prepared in example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further described below.
Example 1:
preparation method of two-dimensional NiCoFe-MOF electrocatalyst and water oxidation application thereof
(2)NiCoFe-LDH+Ni2++Co2++Fe3++ Ligand → NiCoFe-MOF coordination reaction
Foamed nickel (2 cm)2) Ultrasonic washing with dilute hydrochloric acid, ethanol and deionized water for 15min, and oven drying. Dissolving 22mg of ferric nitrate and 12mg of cobalt nitrate in 3mL of deionized water, uniformly stirring, then adding the pretreated nickel foam, and standing at room temperature for 1h to obtain 2D NiCoFe-LDH/NF, wherein the morphology of the 2D NiCoFe-LDH/NF is shown in figure 1. Adding 30mg of 2, 6-naphthalenedicarboxylic acid dipotassium salt into the mixed solution, shaking to completely dissolve the mixture, and transferring the mixture into an oven to react for 20 hours at the temperature of 60 ℃; and cleaning the reacted foamed nickel by using ethanol and deionized water, and drying to obtain 2D NiCoFe-MOF/NF, wherein the morphology of the obtained catalyst is shown in figure 2. The obtained material can be directly used as working electrode in electrochemical engineeringThe electrocatalytic water oxidation performance of the catalyst is tested by a station. From the LSV chart of FIG. 3, it can be seen that the catalyst is at 100mA cm-2Only 271mV of over-potential is needed under the current density of (1), compared with commercial IrO2The catalyst has higher activity.
Example 2:
preparation method of two-dimensional NiCoFe-MOF electrocatalyst
Foamed nickel (2 cm)2) Ultrasonic washing with dilute hydrochloric acid, ethanol and deionized water for 15min, and oven drying. Dissolving 11mg of ferric nitrate and 24mg of cobalt nitrate in 3mL of deionized water, uniformly stirring, then adding the pretreated nickel foam, and standing at room temperature for 1h to obtain 2D NiCoFe-LDH/NF. Adding 30mg of 2, 6-naphthalenedicarboxylic acid dipotassium salt into the mixed solution, shaking to completely dissolve the mixture, and transferring the mixture into an oven to react for 20 hours at the temperature of 60 ℃; and cleaning the reacted foamed nickel by using ethanol and deionized water, and drying to obtain 2D NiCoFe-MOF/NF, wherein the morphology of the obtained catalyst is shown in figure 4.
Example 3:
preparation method of two-dimensional NiCoFe-MOF electrocatalyst
Foamed nickel (2 cm)2) Ultrasonic washing with dilute hydrochloric acid, ethanol, and deionized water for 15min, and oven drying. Dissolving 22mg of ferric nitrate and 12mg of cobalt nitrate in 3mL of deionized water, uniformly stirring, then adding the pretreated foamed nickel, and standing at room temperature for 1h to obtain 2D NiCoFe-LDH/NF. Adding 30mg of 2, 6-naphthalenedicarboxylic acid dipotassium salt into the mixed solution, shaking to completely dissolve the mixture, and transferring the mixture into an oven to react for 16 hours at the temperature of 60 ℃; and cleaning the reacted foamed nickel by using ethanol and deionized water, and drying to obtain 2D NiCoFe-MOF/NF, wherein the morphology of the obtained catalyst is shown in figure 5.
Example 4:
preparation method of two-dimensional NiFe-MOF electrocatalyst
Foamed nickel (2 cm)2) Ultrasonic washing with dilute hydrochloric acid, ethanol and deionized water for 15min, and oven drying. Dissolving 35mg of ferric nitrate in 3mL of deionized water, uniformly stirring, then adding the pretreated nickel foam, and standing at room temperature for 1h to obtain 2D NiFe-LDH/NF. Adding 30mg of dipotassium 2, 6-naphthalenedicarboxylate into the mixed solution, shaking to completely dissolve, and transferring to a containerReacting for 20 hours in an oven at 60 ℃; and cleaning the reacted foam nickel by using ethanol and deionized water, and drying to obtain 2DNiFe-MOF/NF, wherein the morphology of the obtained catalyst is shown in figure 6.
The above description is only a preferred embodiment of the present invention, and does not limit the present invention in any way. It will be understood by those skilled in the art that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of a two-dimensional NiCoFe-MOF electrocatalyst is characterized in that the two-dimensional NiCoFe double-layer hydroxide reacts with dipotassium 2, 6-naphthalene dicarboxylate to generate the two-dimensional NiCoFe-MOF electrocatalyst.
2. The method for preparing a two-dimensional NiCoFe-MOF electrocatalyst according to claim 1, characterized in that it comprises the following steps:
step 1: taking foamed nickel for pretreatment;
step 2: soaking the pretreated foamed nickel in a mixed aqueous solution containing ferric salt and cobalt salt for reaction to obtain a mixed solution of two-dimensional NiCoFe double-layer hydroxide supported by the foamed nickel;
and step 3: adding dipotassium 2, 6-naphthalenedicarboxylate into the mixed solution, and shaking until the dipotassium 2, 6-naphthalenedicarboxylate is completely dissolved;
and 4, after the reaction is completed, drying the mixed solution, taking out the precipitate, cleaning the precipitate, and drying to obtain the two-dimensional NiCoFe-MOF electrocatalyst loaded on the foamed nickel.
3. The preparation method of the two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, characterized in that in step 1, the pretreatment comprises ultrasonic washing of the foamed nickel in 3M hydrochloric acid, ethanol and deionized water for 15min in sequence, and drying for standby.
4. The method for preparing two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, characterized in that in step 2, the foamed nickel is immersed in the mixed aqueous solution containing iron salt and cobalt salt for reaction for 1-2 h.
5. A method of preparing a two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, wherein in step 2, the iron and cobalt salts are nitrates or chlorates; the molar concentration of the metal salt in the mixed aqueous solution containing the ferric salt and the cobalt salt is 5-30mmol L-1。
6. The preparation method of the two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, wherein in step 3, the dipotassium 2, 6-naphthalenedicarboxylate is added into the mixed solution, the mixture is shaken until the dipotassium 2, 6-naphthalenedicarboxylate is completely dissolved, and then the mixture is transferred into an oven to react for 16-24 hours at 60-90 ℃.
7. The method of claim 2, wherein in step 3, the amount of dipotassium 2, 6-naphthalate added is 1-2 times the amount of metal salt in solution.
8. A method of making a two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, characterized in that in step 4, the precipitate is washed with ethanol and de-ionized water.
9. A method of making a two-dimensional NiCoFe-MOF electrocatalyst according to claim 2, wherein the two-dimensional NiCoFe-MOF electrocatalyst is directly used in water oxidation applications.
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Cited By (2)
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CN117144412A (en) * | 2023-08-28 | 2023-12-01 | 西湖大学 | Catalyst and preparation method and application thereof |
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