CN114956212A - Carbon-coated alpha-Ni (OH) 2 Preparation and application of nanosheet composite material - Google Patents

Carbon-coated alpha-Ni (OH) 2 Preparation and application of nanosheet composite material Download PDF

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CN114956212A
CN114956212A CN202110203590.8A CN202110203590A CN114956212A CN 114956212 A CN114956212 A CN 114956212A CN 202110203590 A CN202110203590 A CN 202110203590A CN 114956212 A CN114956212 A CN 114956212A
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不公告发明人
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Shaanxi Zeming Future Technology Co ltd
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    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C—CHEMISTRY; METALLURGY
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01P2006/40—Electric properties
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention provides a carbon-coated alpha-Ni (OH) 2 A preparation method of a nano-sheet electrode material is characterized in that a nano-sheet is assembled into a three-dimensional micro flower-like ball once. The invention is prepared by a simple and common coprecipitation method in one step. High carbon continuous aldehyde is added as a coating carbon source, and when a complex is formed by nickel coprecipitation, an aldehyde chain participates in forming a macromolecular complex and is positioned at the outermost layer; during heating crystallization, aldehyde chains can be carbonized and coated on the nano sheetsSurface, thereby obtaining carbon-coated alpha-Ni (OH) 2 Nanosheets. Carbon-coated alpha-Ni (OH) prepared by the method 2 The nanosheet has good conductivity and shows excellent electrochemical performance.

Description

Carbon-coated alpha-Ni (OH) 2 Preparation and application of nanosheet composite material
Technical Field
The invention relates to the field of nano material preparation, in particular to a preparation method of a nano material as a super capacitor electrode.
Background
The super capacitor has the advantages of high power energy density, namely short charging and discharging time, and has the defect of low energy density. To overcome this drawback, nanoelectrode materials with high specific capacitance can be prepared. Among many metal oxides, nickel hydroxide has a theoretical specific capacity of up to 3082F/g, and is a potential electrode material. Nickel hydroxide classified as hydrotalcite-like alpha-Ni (OH) 2 And brucite-like beta-Ni (OH) 2 Two kinds of structures, phasebeta-Ni (OH) 2 ，α-Ni(OH) 2 The wide interlayer structure is beneficial to ion diffusion, so that the capacitor has higher specific capacitance. As an electrode material, alpha-Ni (OH) 2 Have the disadvantages of poor conductivity and unstable structure.
The carbon material has high conductivity and good mechanical properties. Thus alpha-Ni (OH) 2 The specific capacitance of the composite carbon material can be further improved. The literature reports that the prior compounding methods include: (1) alpha-Ni (OH) 2 Growth on carbon nanotubes (Journal of Alloys and Compounds 743 (2018) 1-10.); (2) alpha-Ni (OH) 2 Nanoparticle composite graphene and nickel foam (Electrochimica Acta 368 (2021) 137589); (3) alpha-Ni (OH) 2 Grown on carbon spheres to form core-shell structures (Synthetic Metals 270 (2020) 116580). They all exhibit advantages over alpha-Ni (OH) alone 2 Specific capacitance of the nanosheet. However, the cost of the carbon nano tube and the graphene is higher, and the carbon sphere @ alpha-Ni (OH) is constructed 2 The core-shell structure is complicated in process, and the pairs prevent industrial ton-level mass production of alpha-Ni (OH) 2 Production and market application of the composite carbon material.
Disclosure of Invention
The invention aims to make up for the defects of the prior art and provide simple and easily-obtained carbon-coated alpha-Ni (OH) 2 A preparation method of a nano-sheet electrode material.
The raw materials of the method are easy to obtain, the preparation process is a simple one-step coprecipitation method, and the method is suitable for large-scale production. In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the method comprises the following steps: adding 0.1-3g of nickel source, 1-6ml of high-carbon chain aldehyde and 0.1-8g of precipitator into 5-60ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two: reacting the dispersion liquid for 2-12h in an air environment with the temperature of 120-160 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at 60 ℃ to obtain carbon-coated alpha-Ni (OH) 2 A nanosheet material;
the nickel source comprises: any one of nickel acetate and nickel carbonate.
The high carbon chain includes: any one of glutaraldehyde, citral, and heptaldehyde.
The precipitating agent comprises: trimethylamine, KOH, and LiOH.
The invention has the following remarkable effects:
(1) the invention provides a simple and easily-released production method of carbon-coated alpha-Ni (OH) 2 The preparation method of the nanosheet material is that the nanosheet material is prepared by a simple one-step coprecipitation method. The preparation method is simple and easy to operate, does not need special equipment, has low cost, is suitable for large-scale preparation, and can meet the requirements of practical application;
(2) compared with carbon nano tubes, graphene and the like, the carbon source required by the method is cheap and easily available, aldehyde chemical industry such as glutaraldehyde and the like is large in quantity and low in price, and the carbon-coated alpha-Ni (OH) prepared by the method 2 The nano-sheet material has good electrochemical performance as a super-electrode material.
Drawings
FIG. 1 shows carbon-coated α -Ni (OH) prepared in examples 1 and 2 2 X-ray powder diffraction spectrum of the nano-sheet.
FIG. 2 shows carbon-coated α -Ni (OH) prepared in examples 4 and 4 2 Scanning electron microscopy of the nanoplatelets.
FIG. 3 shows carbon-coated α -Ni (OH) prepared in examples 1 and 4 2 Transmission electron microscopy of the nanoplatelets.
FIG. 4 shows carbon-coated α -Ni (OH) prepared in example 4 2 And the nanosheet is used as a charging performance graph of the electrode material of the supercapacitor.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Referring to the drawings, the present invention is a carbon-coated alpha-Ni (OH) 2 The preparation method of the nanosheet electrode material is characterized by comprising the following steps:
step one, mixing raw materials
Adding 0.1-3g of nickel source, 1-6ml of high-carbon chain aldehyde and 0.1-8g of precipitator into 5-60ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two, preparation by coprecipitation method
Reacting the dispersion liquid for 2-12h in an air environment with the temperature of 120-160 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at 60 ℃ to obtain carbon-coated alpha-Ni (OH) 2 A nanosheet material;
the nickel source comprises: any one of nickel acetate and nickel carbonate.
The high carbon chain includes: any one of glutaraldehyde, citral, and heptaldehyde.
The precipitating agent comprises: trimethylamine, KOH, and LiOH.
Example 1 preparation of carbon coated alpha-Ni (OH) by the method 2 Nano-sheet
The method comprises the following steps: adding 0.1g of nickel acetate, 1ml of glutaraldehyde and 0.1g of trimethylamine into 5ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two: reacting the dispersion liquid for 12h in an air environment with the temperature of 120 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at the temperature of 60 ℃ to obtain carbon-coated alpha-Ni (OH) 2 A nanosheet material;
example 2 preparation of carbon coated alpha-Ni (OH) by the method 2 Nano-sheet
The method comprises the following steps: adding 0.8g of nickel carbonate, 2ml of glutaraldehyde and 0.5g of KOH into 20ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two: reacting the dispersion liquid for 10h in an air environment with the temperature of 130 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at the temperature of 60 ℃ to obtain carbon-coated alpha-Ni (OH) 2 A nanosheet material;
example 3 preparation of carbon coated alpha-Ni (OH) by the method 2 Nano-sheet
The method comprises the following steps: adding 1.5g of nickel acetate, 4ml of citral and 5g of LiOH into 40ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two: reacting the dispersion liquid for 5h in an air environment with the temperature of 140 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and thenDrying at 60 ℃ for 5h to obtain carbon-coated cobalt-doped alpha-Ni (OH) 2 A nanosheet material;
example 4 preparation of carbon coated alpha-Ni (OH) Using this method 2 Nano-sheet
The method comprises the following steps: adding 3g of nickel carbonate, 6ml of heptaldehyde and 8g of KOH into 60ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid;
step two: reacting the dispersion liquid for 2h in an air environment with the temperature of 160 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at the temperature of 60 ℃ to obtain carbon-coated cobalt-doped alpha-Ni (OH) 2 A nanosheet material;
example 5 three-electrode superperformance test
Carbon coated alpha-Ni (OH) using Chenghua 660E electrochemical workstation 2 And loading the nanosheet onto foamed nickel for performance testing of the supercapacitor. Carbon-coated alpha-Ni (OH) with platinum wire as counter electrode and silver/silver chloride as reference electrode 2 The nano-sheet is a working electrode, and 4 mol of KOH aqueous solution per liter is electrolyte solution. In the voltage range of 0-0.4V, the charge-discharge test is carried out at the sweep rate of 1A/g, and the charge-discharge curve can be obtained.
Referring to the drawings, FIG. 1 is a carbon-coated α -Ni (OH) prepared in examples 1 and 2 2 X-ray powder diffraction spectrum of the nano-sheet. Wherein the abscissa is an angle; the ordinate is the relative intensity. alpha-Ni (OH) is shown to be obtained 2 The material has characteristic diffraction peak (001), (110) and (300) crystal planes at diffraction angles of 11.6 degrees, 33.6 degrees and 59.6 degrees.
FIG. 2 shows carbon-coated α -Ni (OH) prepared in examples 3 and 4 2 Scanning electron microscopy of the nanoplatelets. The figure shows that the carbon-coated alpha-Ni (OH) is obtained 2 Nanosheets, and the nanoflowers are assembled into nanoflowers.
FIG. 3 shows carbon-coated α -Ni (OH) prepared in examples 1 and 4 2 Transmission electron microscopy of nanoplatelets. The figure shows that the carbon layer is tightly coated on the lattice stripe alpha-Ni (OH) 2 About 3 nm thick.
FIG. 4 shows carbon-coated α -Ni (OH) prepared in example 4 2 Made of nano-sheetIs a charging curve diagram of the electrode material of the super capacitor. It can be seen that the specific capacitances at current densities of 1, 5 and 10A/g were 2307, 2162 and 2100F/g in the voltage range of 0-0.4V.
The present invention is not limited to the above-mentioned embodiments, and those skilled in the art can make various equivalent modifications, equivalent substitutions, additions, deletions, and rearrangements to constitute more new embodiments according to the working principle of the present invention and the above-mentioned embodiments.

Claims (4)

1. Carbon coated alpha-Ni (OH) 2 A method of making a nanoplate, comprising: step one, mixing raw materials: adding 0.1-3g of nickel source, 1-6ml of high-carbon chain aldehyde and 0.1-8g of precipitator into 5-60ml of water, and stirring the mixture for 0.5h to obtain a dispersion liquid; step two, preparation by a coprecipitation method: reacting the dispersion liquid for 2-12h in an air environment with the temperature of 120-160 ℃, naturally cooling to room temperature after the reaction is finished, then washing for 3 times by using water and ethanol respectively, and then drying for 5h at 60 ℃ to obtain carbon-coated alpha-Ni (OH) 2 A nanosheet material.
2. The carbon-coated α -Ni (OH) of claim 1 2 A method for producing a nanosheet, comprising: the nickel source comprises: any one of nickel acetate and nickel carbonate.
3. The carbon-coated α -Ni (OH) of claim 1 2 The preparation method of the nano-sheet is characterized by comprising the following steps: the high carbon chain aldehydes include: any one of glutaraldehyde, citral, and heptaldehyde.
4. The carbon-coated α -Ni (OH) of claim 1 2 The preparation method of the nano-sheet is characterized by comprising the following steps: the precipitating agent comprises: trimethylamine, KOH, and LiOH.
CN202110203590.8A 2021-02-24 2021-02-24 Carbon-coated alpha-Ni (OH) 2 Preparation and application of nanosheet composite material Pending CN114956212A (en)

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