CN113529122A - Nickel-organic framework nanosheet array material and preparation method and application thereof - Google Patents
Nickel-organic framework nanosheet 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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- C25B11/055—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
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Abstract
The invention discloses a nickel-organic framework nanosheet array material and a preparation method and application thereof, and the nickel-organic framework nanosheet array material comprises pretreatment of a conductive substrate, preparation of a precursor solution and synthesis of a nanosheet array material.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and particularly relates to a nickel-organic framework nanosheet array material, and a preparation method and application thereof.
Background
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 kinetics of the UOR reaction are relatively slow due to its complex 6 e-transfer pathway. Due to the fact thatThus, high performance electrocatalysts are needed to accelerate the kinetics of urea oxidation reactions to improve the energy conversion efficiency of the above-mentioned urea-related energy storage devices. Although noble metal based catalysts (e.g. Pt, IrO)2And RuO2) Proved to have certain UOR activity, but the large-scale application of the compound is limited due to the defects of high cost, resource scarcity and the like.
In recent years, nickel-based catalysts (including nickel-based oxides, hydroxides, phosphides, nitrides, and composites thereof) have received much attention for low cost and high UOR activity. Studies have shown that the excellent UOR electrocatalytic activity of these nickel-based materials depends to a large extent on the Ni sites that they expose during the reaction, that is, the Ni sites are considered as the active centers of the electrocatalytic UOR. Accordingly, various nickel-rich catalysts having different elemental compositions and microstructures have been reported in succession in an attempt to achieve efficient electrocatalysis of UOR. Recently, researchers have synthesized a material consisting of Ni2+And benzenedicarboxylic acid, and the prepared Ni-MOF has been demonstrated for the first time to have significant electrocatalytic activity on UOR (Chemical communications,2017,53, 10906-.
Metal-organic frameworks (MOFs) are a class of microporous materials composed of metal ions and organic ligands, and have the advantages of adjustable composition, controllable structure, large specific surface area and the like. Among them, due to its fast electron/ion transfer rate and its highly exposed unsaturated metal sites on the surface, ultra-thin two-dimensional MOF nanosheets have shown great potential in electrocatalysis applications, however, up to now, the synthesis of novel ultra-thin two-dimensional Ni-MOF nanosheets is still difficult, and Ni-MOF electrocatalysis materials with efficient UOR activity are still few.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a nickel-organic framework nanosheet 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 purpose, the invention adopts the following technical scheme:
the nickel-organic framework nanosheet array material comprises a reticular substrate and nickel-organic framework nanosheets loaded on the reticular substrate, wherein the nickel-organic framework nanosheets are two-dimensional sheets.
Preferably, the nickel-organic framework nanosheets are synthesized from a divalent nickel salt and 4-dimethylaminopyridine as starting materials.
Preferably, the nickel-organic framework nanosheets have an average thickness of from 3 to 4 nm.
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 foamed nickel, carbon cloth, titanium mesh or stainless steel mesh.
In addition, the invention also claims a preparation method of the nickel-organic framework nanosheet array material, which comprises the following steps:
(1) pretreating the conductive substrate;
(2) preparing a precursor solution: dissolving a divalent nickel salt and 4-dimethylaminopyridine in an organic solvent, and uniformly mixing to obtain a precursor solution;
(3) synthesis of the nanosheet array material: and (3) immersing the conductive substrate treated in the step (1) into the precursor solution prepared in the step (2) for solvothermal reaction, and after the reaction is finished, washing and drying the solid product to obtain the nickel-organic framework nanosheet 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 temperature of the solvothermal reaction is 60-150 ℃, and the reaction time is 4-12 h.
The invention also protects the application of the nickel-organic framework nanosheet array material in the electrocatalytic urea oxidation reaction.
Compared with the prior art, the invention has the following beneficial effects:
(1) the nickel-organic framework nanosheet provided by the invention is a novel MOF material, and has unique morphology, crystal structure and microstructure;
(2) the nickel-organic framework nanosheet prepared by the method has an ultrathin two-dimensional sheet structure, which is beneficial to rapid transfer of electrons/ions, and a large number of unsaturated Ni active sites are directly exposed on the surface of the nanosheet, so that the electrochemical performance of the nanosheet is remarkably improved, and the nanosheet has a wide application prospect in the field of electrocatalysis;
(3) the ultrathin two-dimensional nickel-organic framework nanosheet array can be synthesized on the conductive substrate through one-step solvothermal reaction, the process is simple, and the process is efficient;
(4) according to the preparation method of the nickel-organic framework nanosheet array, the adopted raw materials are inorganic nickel salt and 4-dimethylaminopyridine, and compared with a noble metal-based catalyst applied to industry, the cost is low;
(5) the ultrathin nickel-organic framework nanosheet array provided by the invention 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 framework nanosheet array material provided by the invention can be applied to the technical field of new energy such as direct urea fuel cells and urea-assisted electrolytic hydrogen production.
Drawings
FIG. 1 is a scanning electron micrograph of Ni-DMAP/CC prepared in example 1;
FIG. 2 is a scanning electron micrograph of Ni-DMAP/NF prepared in example 2;
FIG. 3 is an atomic force microscope image of the Ni-DMAP nanosheets prepared in example 2;
FIG. 4 is a transmission electron microscope image of the Ni-DMAP nanosheet prepared in example 2;
FIG. 5 is an X-ray diffraction pattern of the Ni-DMAP nanosheet prepared in example 2;
FIG. 6 is an X-ray photoelectron spectrum of the Ni-DMAP nanosheet prepared in example 2;
FIG. 7 is a graph of the IR spectrum and the Raman spectrum of Ni-DMAP prepared in example 2;
FIG. 8 is a plot of the UOR polarization of the materials prepared in example 2 and comparative example 1;
FIG. 9 is a chart of the UOR stability test results for Ni-DMAP/NF prepared in example 2.
Detailed Description
The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments.
It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.
Example 1
A preparation method of a nickel-organic framework nanosheet array specifically comprises the following steps:
(1) pretreatment of the conductive substrate: cutting the carbon cloth into pieces with the area of 2cm multiplied by 1cm, and carrying out surface hydrophilic treatment on the pieces by adopting oxygen plasma;
(2) preparing a precursor solution: 0.1mol of Ni (NO)3)2·6H2Dissolving O and 0.2mol of 4-dimethylaminopyridine in 200mL of ethanol solvent, and uniformly mixing to obtain a precursor solution;
(3) synthesizing a nanosheet array material: transferring the precursor solution prepared in the step (2) into a reaction kettle liner, vertically immersing the carbon cloth processed in the step (1) into the precursor solution, sealing the reaction kettle, carrying out solvothermal reaction at the reaction temperature of 100 ℃ for 12h, and washing and drying a solid product after the reaction is finished to obtain the nickel-organic framework nanosheet array material (Ni-DMAP/CC) loaded on the carbon cloth substrate.
The scanning electron microscope image of the Ni-DMAP/CC prepared in the example 1 is shown in the attached drawing 1, and the Ni-DMAP can be seen from the drawing to uniformly grow on the surface of the carbon cloth substrate in a thin nanosheet form.
Example 2
A preparation method of a nickel-organic framework nanosheet array specifically comprises the following steps:
(1) pretreatment of the conductive substrate: cutting the foamed nickel into pieces with the area of 2cm multiplied by 1cm, sequentially placing the pieces in ethanol, hydrochloric acid and deionized water for ultrasonic treatment for 10min, and drying for later use;
(2) preparing a precursor solution: 0.1mol of Ni (NO)3)2·6H2Dissolving O and 0.2mol of 4-dimethylaminopyridine in 200mL of ethanol solvent, and uniformly mixing to obtain a precursor solution;
(3) synthesizing a nanosheet array material: and (3) transferring the precursor solution prepared in the step (2) into a reaction kettle liner, vertically immersing the foamed nickel treated in the step (1) into the precursor solution, sealing the reaction kettle, carrying out solvothermal reaction at the reaction temperature of 100 ℃ for 12h, and washing and drying a solid product after the reaction is finished to obtain the nickel-organic framework nanosheet array material (Ni-DMAP/NF) loaded on the foamed nickel substrate.
The loading of Ni-DMAP nanoplatelets on the substrate in this example was calculated by the differential method according to formula (1):
the loading capacity is (Ni-DMAP/NF nanosheet array mass-foam nickel substrate mass)/foam nickel maximum area (1);
by calculation, the loading amount of the ultrathin Ni-DMAP nanosheet on the foamed nickel substrate in the material 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 drawing 2, and it can be seen from the drawing that the Ni-DMAP is in the shape of an ultrathin nanosheet, the nanosheet is uniformly immobilized on the surface of the foam nickel substrate, and the whole structure is in a nanosheet array structure.
An atomic force microscope image and thickness distribution of the Ni-DMAP nanosheet prepared in the embodiment 2 are shown in the attached drawing 3, and it can be seen from the drawing that Ni-DMAP shows an ultrathin two-dimensional nanosheet shape, the average thickness of the nanosheet is only 3-4nm, a large number of Ni active sites can be exposed, and a channel for rapid charge transfer is provided.
The transmission electron microscope image of the Ni-DMAP nanosheet prepared in the embodiment 2 is shown in the attached drawing 4, and it can be seen that the Ni-DMAP shows a large-area ultrathin nanosheet shape.
The X-ray diffraction spectrum of the Ni-DMAP nanosheet prepared in example 2 is shown in fig. 5, and it can be seen from the figure that the obtained Ni-DMAP nanosheet shows good crystallinity, and the diffraction characteristic peak position thereof is completely consistent with the simulation result, which indicates that the novel nickel-metal organic framework nanosheet material is successfully synthesized.
An X-ray photoelectron spectrum of the Ni-DMAP nanosheet prepared in the example 2 is shown in the attached figure 6, and as can be seen from the figure, the material comprises C, N, Ni and O elements, and the atomic content ratio of the elements is 28.7:3.3:22.1: 45.9.
The IR spectrum and Raman spectrum of Ni-DMAP prepared in example 2 are shown in FIG. 7, and it can be seen that the molecular structure of Ni-DMAP is confirmed to have-CH3The presence of functional groups such as C-H, C ═ C and C ═ N suggests that Ni-DMAP as a whole exhibits a chemical structure highly similar to its ligand (4-dimethylaminopyridine).
Comparative example 1
A preparation method of a metal-based catalytic material specifically comprises the following steps:
(1) pretreatment of the conductive substrate: cutting the foamed nickel into pieces with the area of 2cm multiplied by 1cm, sequentially placing the pieces in ethanol, hydrochloric acid and deionized water for ultrasonic treatment for 10min, and drying for later use;
(2) preparing a dispersion liquid: 2.4mg of commercial RuO2(99.95 wt.%) catalyst was uniformly dispersed in 200mL of absolute ethanol solution to give a dispersion;
(3) synthesizing a catalytic material: dripping the dispersion liquid prepared in the step (2) on the foamed nickel substrate treated in the step (1) to prepare RuO2Foamed nickel (RuO)2/NF，RuO2The loading capacity is 1.2mg cm-2) A catalytic material.
The materials prepared in example 2 and comparative example 1 were subjected to a UOR electrocatalytic performance test, comprising the following specific steps: the materials prepared in the example 2 and the comparative example 1 are respectively used as working electrodes, carbon rods are used as counter electrodes, Hg/HgO electrodes are used as reference electrodes, a linear voltammetry scanning test is carried out under a standard three-electrode system to evaluate the UOR electrocatalytic activity of the materials, and the tested electrolyte is a mixed solution of 1.0M potassium hydroxide and 0.5M ureaScan rate of 5mV s-1。
The UOR polarization curves of the materials prepared in example 2 and comparative example 1 are shown in FIG. 8, from which it can be seen that the UOR starting potential of the samples prepared in example 2 of the present invention is only 1.30V (vs. RHE) reaching 10, 50 and 100mA cm-2The current density of the catalyst is only 1.34V (vs. RHE), 1.40V (vs. RHE) and the UOR electrocatalytic activity of the catalyst is obviously better than that of a commercial noble metal-based catalyst (RuO) under the same conditions2/NF)。
The potentials required for the materials prepared in example 2 and comparative example 1 at different UOR current densities are shown in the table below:
as can be seen from the table, the material prepared in example 2 of the present invention is comparable to a commercial noble metal-based catalyst (RuO) under the same electrochemical test conditions2/NF) has a lower UOR onset potential; at the same implementation potential, compared to commercial RuO2The material prepared in example 2 of the present invention has a higher UOR current density.
The material prepared in example 2 was subjected to electrocatalytic stability testing, the specific experimental steps were 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 a 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 a nickel-organic framework nanosheet 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 plot of Ni-DMAP/NF prepared in example 2 is shown in FIG. 9, from which it can be seen that the catalyst is close to 100mA cm-2After continuous catalysis for 10 hours under high current density, the retention rate of the UOR current density still exceeds 90 percent, and the better UOR electrocatalytic stability is shown.
Finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.
Claims (10)
1. The nickel-organic framework nanosheet array material is characterized by comprising a reticular substrate and nickel-organic framework nanosheets loaded on the reticular substrate, wherein the nickel-organic framework nanosheets are two-dimensional sheets.
2. A nickel-organic framework nanosheet array material of claim 1, wherein the nickel-organic framework nanosheets are synthesized from a divalent nickel salt and 4-dimethylaminopyridine as starting materials.
3. A nickel-organic framework nanosheet array material as set forth in claim 1, wherein the nickel-organic framework nanosheets have an average thickness of from 3 to 4 nm.
4. A nickel-organic framework nanosheet array material as claimed in claim 1 wherein the divalent nickel salt is any one of nickel chloride, nickel nitrate, nickel acetate or nickel sulphate.
5. A nickel-organic framework nanosheet array material as set forth in claim 1, wherein the mesh substrate is any one of foamed nickel, carbon cloth, titanium mesh, or stainless steel mesh.
6. A method of preparing a nickel-organic framework nanosheet array material of any one of claims 1 to 5, comprising the steps of:
(1) pretreating the conductive substrate;
(2) preparing a precursor solution: dissolving a divalent nickel salt and 4-dimethylaminopyridine in an organic solvent, and uniformly mixing to obtain a precursor solution;
(3) synthesis of the nanosheet array material: and (3) immersing the conductive substrate treated in the step (1) into the precursor solution prepared in the step (2) for solvothermal reaction, and after the reaction is finished, washing and drying the solid product to obtain the nickel-organic framework nanosheet array material.
7. A method of preparing a nickel-organic framework nanosheet array material of claim 6, wherein in step (2), the molar ratio of divalent nickel salt to 4-dimethylaminopyridine is from 0.5 to 2: 1.
8. The method for preparing a nickel-organic framework nanosheet array material of claim 6, wherein in step (2), the organic solvent is any one of methanol, ethanol, ethylene glycol or N, N-dimethylformamide.
9. The method for preparing a nickel-organic framework nanosheet array material of claim 6, wherein in step (3), the solvothermal reaction is at a temperature of 60-150 ℃ for a reaction time of 4-12 h.
10. Use of a nickel-organic framework nanosheet array material of any one of claims 1 to 5 in an electrocatalytic urea oxidation reaction.
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| CN114367313A (en) * | 2022-01-18 | 2022-04-19 | 安徽大学 | Preparation method and application of catalytic material based on Ni-MOF |
| CN114920333A (en) * | 2022-05-31 | 2022-08-19 | 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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