CN113529122B - Nickel-organic framework nano-sheet array material and preparation method and application thereof - Google Patents
Nickel-organic framework nano-sheet array material and preparation method and application thereof Download PDFInfo
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- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
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- 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
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- Y02E60/30—Hydrogen technology
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Abstract
The application discloses a nickel-organic framework nano-sheet array material, a preparation method and application thereof, wherein the nickel-organic framework nano-sheet array material comprises pretreatment of a conductive substrate, preparation of a precursor solution and synthesis of the nano-sheet array material.
Description
Technical Field
The application belongs to the technical field of electrocatalysis, and particularly relates to a nickel-organic framework nanosheet array material, a preparation method and application thereof.
Background
The urea oxidation reaction (Urea Oxidation Reaction, UOR) is the core reaction of new energy technologies such as direct urea fuel cells, urea-assisted rechargeable zinc-air cells, and urea-assisted electrolytic hydrogen production. However, the UOR reaction kinetics are relatively slow due to its complex 6 e-transfer pathway. Therefore, there is a need for high performance electrocatalysts to accelerate the urea oxidation reaction kinetics to increase the energy conversion efficiency of the above described urea-related energy storage devices. Although noble metal-based catalysts (e.g. Pt, irO 2 And RuO (Ruo) 2 ) Has been shown to have some UOR activity but has limited their large-scale use due to the high cost and scarcity of resources.
In recent years, low cost and high UOR activity nickel-based catalysts (including nickel-based oxides, hydroxides, phosphides, nitrides and composites thereof, etc.) have received widespread attention. Studies have shown that the excellent UOR electrocatalytic activity of these nickel-based materials depends to a large extent on their presence in the reactionThe Ni sites exposed in the process, that is, ni sites are considered to be active sites of the electrocatalytic UOR. Accordingly, various nickel-rich catalysts having different elemental compositions and microstructures have been reported successively in order to achieve efficient electrocatalysis for UOR. Recently, researchers have synthesized a material consisting of Ni 2+ And a nickel-organic framework (Ni-MOF) material composed of benzene dicarboxylic acid, and it was demonstrated for the first time that the prepared Ni-MOF had significant electrocatalytic activity towards UOR (Chemical communications,2017,53,10906-10909).
Metal-organic frameworks (MOFs) are a class of microporous materials composed of metal ions and organic ligands, with the advantages of adjustable composition, controllable structure, large specific surface area, etc. Among them, ultra-thin two-dimensional MOF nanoplatelets show great potential in electrocatalytic applications due to their rapid electron/ion transfer rate and highly exposed unsaturated metal sites on their surface, however, to date, the synthesis of novel ultra-thin two-dimensional Ni-MOF nanoplatelets has been difficult and Ni-MOF electrocatalytic materials with high-efficiency UOR activity have remained few.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide a nickel-organic framework nano-sheet array material, a preparation method and application thereof, and solves the technical problems of low electrocatalytic activity and poor stability of the existing nickel-based material UOR.
In order to achieve the above purpose, the present application adopts the following technical scheme:
the nickel-organic frame nano sheet array material comprises a reticular substrate and nickel-organic frame nano sheets loaded on the reticular substrate, wherein the nickel-organic frame nano sheets are two-dimensional sheet-shaped.
Preferably, the nickel-organic framework nano-sheet is synthesized by taking divalent nickel salt and 4-dimethylaminopyridine as raw materials.
Preferably, the average thickness of the nickel-organic framework nanoplatelets is 3-4nm.
Preferably, the divalent nickel salt is any one of nickel chloride, nickel nitrate, nickel acetate or nickel sulfate.
Preferably, the mesh substrate is any one of foam nickel, carbon cloth, titanium mesh or stainless steel mesh.
In addition, the application also claims a preparation method of the nickel-organic framework nano-sheet array material, which comprises the following steps:
(1) Pretreatment of a conductive substrate;
(2) Preparing a precursor solution: dissolving divalent nickel salt and 4-dimethylaminopyridine in an organic solvent, and uniformly mixing to obtain a precursor solution;
(3) Synthesis of nanoplatelet array materials: immersing the conductive substrate treated in the step (1) into the precursor solution prepared in the step (2) for solvothermal reaction, washing and drying a solid product after the reaction is finished, and thus obtaining the nickel-organic framework nano-sheet array material.
Preferably, in the step (2), the molar ratio of the divalent nickel salt to the 4-dimethylaminopyridine is 0.5-2:1.
Preferably, in the step (2), the organic solvent is any one of methanol, ethanol, ethylene glycol or N, N-dimethylformamide.
Preferably, in the step (3), the solvothermal reaction temperature is 60-150 ℃ and the reaction time is 4-12h.
The application also protects the application of the nickel-organic framework nano-sheet array material in the electrocatalytic urea oxidation reaction.
Compared with the prior art, the application has the following beneficial effects:
(1) The nickel-organic framework nano sheet provided by the application is a novel MOF material and has unique morphology, crystal structure and microstructure;
(2) The nickel-organic framework nano-sheet prepared by the application has an ultrathin two-dimensional sheet structure, which is not only beneficial to the rapid transfer of electrons/ions, but also has a large number of unsaturated Ni active sites directly exposed on the surface of the nano-sheet, thereby endowing the nano-sheet with remarkably improved electrochemical performance and having wide application prospect in the field of electrocatalysis;
(3) The ultrathin two-dimensional nickel-organic framework nano-sheet array can be synthesized on the conductive substrate through one-step solvothermal reaction, and the method has the advantages of simple process and high flow;
(4) The preparation method of the nickel-organic frame nano-sheet array provided by the application adopts inorganic nickel salt and 4-dimethylaminopyridine as raw materials, and has low cost compared with a noble metal-based catalyst applied industrially;
(5) The ultrathin nickel-organic framework nano sheet array provided by the application can be directly used as a self-supporting electrode for electrocatalytic urea oxidation reaction, and has excellent UOR electrocatalytic performance and excellent stability;
(6) The ultrathin nickel-organic frame nano-sheet array material provided by the application can be applied to the technical fields of new energy such as direct urea fuel cells and urea-assisted hydrogen production by electrolysis.
Drawings
FIG. 1 is a scanning electron microscope image of Ni-DMAP/CC prepared in example 1;
FIG. 2 is a scanning electron microscope image of Ni-DMAP/NF prepared in example 2;
FIG. 3 is an atomic force microscope image of Ni-DMAP nanoplatelets prepared in example 2;
FIG. 4 is a transmission electron microscope image of the Ni-DMAP nanoplatelets prepared in example 2;
FIG. 5 is an X-ray diffraction pattern of the Ni-DMAP nanoplatelets prepared in example 2;
FIG. 6 is an X-ray photoelectron spectrum of the Ni-DMAP nanoplatelets prepared in example 2;
FIG. 7 is an infrared spectrum and a Raman spectrum of Ni-DMAP prepared in example 2;
FIG. 8 is a graph of the UOR polarization of the materials prepared in example 2 and comparative example 1;
FIG. 9 is a graph showing the results of UOR stability test of Ni-DMAP/NF prepared in example 2.
Detailed Description
The present application will be described in further detail with reference to the following preferred examples, but the present application is not limited to the following examples.
Unless otherwise specified, the chemical reagents involved in the present application are all commercially available.
Example 1
The preparation method of the nickel-organic frame nano-sheet array specifically comprises the following steps:
(1) Pretreatment of a conductive substrate: cutting carbon cloth into pieces with the area of 2cm multiplied by 1cm, and carrying out surface hydrophilization treatment on the pieces by adopting oxygen ions;
(2) Preparing a precursor solution: 0.1mol of Ni (NO 3 ) 2 ·6H 2 O and 0.2mol of 4-dimethylaminopyridine are dissolved in 200mL of ethanol solvent, and the precursor solution is obtained after uniform mixing;
(3) Synthesizing a nano-sheet array material: transferring the precursor solution prepared in the step (2) into a liner of a reaction kettle, vertically immersing the carbon cloth processed in the step (1) into the precursor solution, sealing the reaction kettle, performing solvothermal reaction at a reaction temperature of 100 ℃ for 12 hours, washing and drying a solid product after the reaction is finished, and obtaining the nickel-organic framework nano sheet array material (Ni-DMAP/CC) loaded on the carbon cloth substrate.
The scanning electron microscope image of the Ni-DMAP/CC prepared in example 1 is shown in FIG. 1, and it can be seen from the image that Ni-DMAP is uniformly grown on the surface of the carbon cloth substrate in the form of thin nano-sheets.
Example 2
The preparation method of the nickel-organic frame nano-sheet array specifically comprises the following steps:
(1) Pretreatment of a conductive substrate: cutting foam nickel into pieces with the area of 2cm multiplied by 1cm, sequentially placing the pieces in ethanol, hydrochloric acid and deionized water, respectively carrying out ultrasonic treatment for 10min, and drying for later use;
(2) Preparing a precursor solution: 0.1mol of Ni (NO 3 ) 2 ·6H 2 O and 0.2mol of 4-dimethylaminopyridine are dissolved in 200mL of ethanol solvent, and the precursor solution is obtained after uniform mixing;
(3) Synthesizing a nano-sheet array material: transferring the precursor solution prepared in the step (2) into a liner of a reaction kettle, vertically immersing the foam nickel processed in the step (1) into the precursor solution, sealing the reaction kettle, performing solvothermal reaction at a reaction temperature of 100 ℃ for 12 hours, washing and drying a solid product after the reaction is finished, and obtaining the nickel-organic frame nano-sheet array material (Ni-DMAP/NF) loaded on the foam nickel substrate.
The loading amount of the Ni-DMAP nanoplatelets on the substrate in this example was calculated according to formula (1) by the differential method:
load = (Ni-DMAP/NF nanoplatelet array mass-foam nickel substrate mass)/foam nickel maximum area (1);
through calculation, in the material disclosed by the application, the load capacity of the ultrathin Ni-DMAP nano sheet on the foam nickel substrate is about 1.2mg cm -2 。
The scanning electron microscope image of the Ni-DMAP/NF prepared in the embodiment 2 is shown in the attached figure 2, and the appearance of the Ni-DMAP is shown as an ultrathin nano sheet, the nano sheet is uniformly fixed on the surface of a foam nickel substrate, and the whole nano sheet is in a nano sheet array structure.
The atomic force microscope image and thickness distribution of the Ni-DMAP nanoplatelets prepared in example 2 are shown in fig. 3, from which it can be seen that Ni-DMAP exhibits an ultra-thin two-dimensional nanoplatelet morphology with an average thickness of only 3-4nm, exposing a large number of Ni active sites and providing a channel for rapid charge transfer.
The transmission electron microscope image of the Ni-DMAP nano-sheet prepared in the example 2 is shown in the attached figure 4, and it can be seen from the image that the Ni-DMAP presents a large-area ultrathin nano-sheet morphology.
The X-ray diffraction pattern of the Ni-DMAP nanoplatelets prepared in example 2 is shown in fig. 5, and it can be seen from the figure that the obtained Ni-DMAP nanoplatelets show good crystallinity, and the diffraction characteristic peak positions are completely consistent with the simulation result, which indicates that the novel nickel-metal organic framework nanoplatelet material is successfully synthesized.
The X-ray photoelectron spectrum of the Ni-DMAP nanoplatelets prepared in example 2 is shown in fig. 6, and it can be seen from the graph that the material includes C, N, ni and O elements, and the atomic content ratio of the elements is 28.7:3.3:22.1:45.9.
The infrared spectrum and Raman spectrum of the Ni-DMAP prepared in example 2 are shown in FIG. 7, from which it can be seen that Ni-DMAPBoth the IR spectrum and the Raman spectrum of (C) prove that the molecular structure of the (C) has-CH 3 The presence of functional groups such as C-H, C =c and c=n, indicates that Ni-DMAP as a whole exhibits a chemical structure highly similar to that of its ligand (4-dimethylaminopyridine).
Comparative example 1
The preparation method of the metal-based catalytic material specifically comprises the following steps:
(1) Pretreatment of a conductive substrate: cutting foam nickel into pieces with the area of 2cm multiplied by 1cm, sequentially placing the pieces in ethanol, hydrochloric acid and deionized water, respectively carrying out ultrasonic treatment for 10min, and drying for later use;
(2) Preparing a dispersion liquid: 2.4mg of commercial RuO 2 (99.95 wt.%) the catalyst was uniformly dispersed in 200mL of an absolute ethanol solution to obtain a dispersion;
(3) Synthesizing a catalytic material: dripping the dispersion prepared in the step (2) on the foam nickel substrate treated in the step (1) to prepare RuO 2 Nickel foam (RuO) 2 /NF，RuO 2 The loading was 1.2mg cm -2 ) Catalytic material.
The materials prepared in example 2 and comparative example 1 were subjected to UOR electrocatalytic performance testing, as follows: the materials prepared in example 2 and comparative example 1 are respectively used as working electrodes, a carbon rod is used as a counter electrode, hg/HgO electrode is used as a reference electrode, and a linear voltammetry scanning test is carried out under a standard three-electrode system to evaluate the UOR electrocatalytic activity of the materials, wherein the tested electrolyte is 1.0M potassium hydroxide+0.5M urea mixed solution, and the scanning rate is 5mV s -1 。
The UOR polarization graphs of the materials prepared in example 2 and comparative example 1 are shown in FIG. 8, from which it can be seen that the sample prepared in example 2 of the present application has a UOR onset potential of only 1.30V (vs. RHE) to 10, 50 and 100mA cm -2 The potentials at current densities of (2) are also only 1.34, 1.40 and 1.45V (vs. RHE), respectively, the UOR electrocatalytic activity is significantly better than that of the commercial noble metal-based catalysts (RuO) under the same conditions 2 /NF)。
The required potentials for the materials prepared in example 2 and comparative example 1 at different UOR current densities are shown in the following table:
as can be seen from the table, the material prepared in example 2 of the present application was compared to commercial noble metal-based catalyst (RuO 2 /NF) has a lower UOR initiation potential; at the same implementation potential, compared with commercial RuO 2 The material prepared in example 2 of the present application has a higher UOR current density.
The material prepared in example 2 was subjected to electrocatalytic stability testing, the specific experimental procedure being as follows: the material prepared in example 2 (Ni-DMAP/NF) was used as a working electrode, a carbon rod was used as a counter electrode, and Hg/HgO electrode was used as a reference electrode, and a current-time response test was performed under a standard three-electrode system to evaluate the UOR electrocatalytic stability of the nickel-organic framework nanoplatelet array, with a constant test voltage of 1.45V (vs. RHE), and the electrolyte tested was a 1.0M potassium hydroxide+0.5M urea mixed solution.
The UOR current-time response curve of Ni-DMAP/NF produced in example 2 is shown in FIG. 9, from which it can be seen that the catalyst was in the vicinity of 100mA cm -2 After continuous catalysis for 10 hours at the high current density of (2), the retention rate of the UOR current density is still more than 90%, and the UOR electrocatalytic stability is better.
Finally, it should be noted that: the above examples are not intended to limit the present application in any way. Modifications and improvements will readily occur to those skilled in the art upon the basis of the present application. Accordingly, any modification or improvement made without departing from the spirit of the application is within the scope of the application as claimed.
Claims (8)
1. The nickel-organic frame nano sheet array material is characterized by comprising a reticular substrate and nickel-organic frame nano sheets loaded on the reticular substrate, wherein the nickel-organic frame nano sheets are two-dimensional sheets;
the preparation method of the nickel-organic framework nano-sheet array material comprises the following steps:
(1) Pretreatment of a conductive substrate;
(2) Preparing a precursor solution: dissolving divalent nickel salt and 4-dimethylaminopyridine in an organic solvent, and uniformly mixing to obtain a precursor solution;
(3) Synthesis of nanoplatelet array materials: immersing the conductive substrate treated in the step (1) into the precursor solution prepared in the step (2) for solvothermal reaction, washing and drying a solid product after the reaction is finished, and thus obtaining the nickel-organic framework nano-sheet array material.
2. The nickel-organic framework nanoplatelet array material of claim 1, wherein the nickel-organic framework nanoplatelets have an average thickness of 3-4nm.
3. The nickel-organic framework nanoplatelet array material of claim 1, wherein the divalent nickel salt is any one of nickel chloride, nickel nitrate, nickel acetate, or nickel sulfate.
4. The nickel-organic framework nanoplatelet array material of claim 1, wherein the mesh substrate is any one of a foam nickel, carbon cloth, titanium mesh, or stainless steel mesh.
5. The nickel-organic framework nanoplatelet array material of claim 1, wherein in step (2), the molar ratio of divalent nickel salt to 4-dimethylaminopyridine is 0.5-2:1.
6. The nickel-organic framework nanoplatelet array material of claim 1, wherein in step (2), the organic solvent is any one of methanol, ethanol, ethylene glycol, or N, N-dimethylformamide.
7. The nickel-organic framework nanoplatelet array material of claim 1, wherein in step (3), the solvothermal reaction temperature is 60-150 ℃ and the reaction time is 4-12h.
8. Use of the nickel-organic framework nanoplatelet array material of any of claims 1-5 in an electrocatalytic urea oxidation reaction.
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| CN114920333B (en) * | 2022-05-31 | 2023-05-19 | 重庆大学溧阳智慧城市研究院 | Treatment method of high-concentration ammonia nitrogen wastewater |
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