CN110853937A - Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor - Google Patents

Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor Download PDF

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CN110853937A
CN110853937A CN201911200616.2A CN201911200616A CN110853937A CN 110853937 A CN110853937 A CN 110853937A CN 201911200616 A CN201911200616 A CN 201911200616A CN 110853937 A CN110853937 A CN 110853937A
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nickel
cobalt
reaction
carbon composite
selenide
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李中春
蔡雄英
贾海琳
田美姣
严明杰
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Jiangsu University of Technology
Jiangsu Institute of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a preparation method of a nickel-cobalt bimetallic selenide/carbon compound for a supercapacitor, belonging to the field of preparation of energy storage materials, and the preparation method mainly comprises the following steps: firstly, preparing a nickel-cobalt bimetal-organic framework compound by using soluble nickel salt, soluble cobalt salt and 2-methylimidazole as main raw materials through a solvothermal method; and then under the protection of inert gas, selenizing and carbonizing the nickel-cobalt bimetal-organic framework compound to obtain the nickel-cobalt bimetal selenide/carbon compound. The preparation method disclosed by the invention has the characteristics of simple process, easiness in operation and low requirement on equipment, is suitable for industrial production, organically combines the nickel-cobalt bimetallic selenide nano-particles with nano-carbon, is favorable for increasing active sites and improving the conductivity and stability of materials, and has wide application prospects in the fields of supercapacitors, lithium ion batteries, electrocatalysis and the like.

Description

Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor
Technical Field
The invention relates to the field of energy storage material preparation, in particular to a preparation method of a nickel-cobalt bimetallic selenide/carbon composite for a supercapacitor.
Background
In the field of supercapacitors, nickel-cobalt-based metal oxides and metal sulfides exhibit better supercapacitor performance due to their unique crystal structures, and have attracted widespread attention from technologists in the field of material science. Selenium element in the same main group with oxygen and sulfur is less applied in the field of super capacitors, but nickel-cobalt-based selenides gradually begin to attract attention in the field of semiconductors and other fields and show more prominent advantages.
CoSe2、NiSe、NiSe2And selenides such as NiSe-CoSe and the like are used as electrode materials of the super capacitor and show better electrochemical performance. Guo et al directly utilizes hydrothermal reaction on foamed nickel through anion displacement reaction to synthesize Ni precursor microspheres, and then performs selenylation reaction after drying to prepare the mesh lamellar electrode active material with a three-dimensional nanostructure. At 0.5A/g, the specific capacitance was 492F/g. After the circulation is carried out for 2000 circles under the condition of 0.5A/g, the capacity reaches 97 percent of the original capacity, and good circulation stability is shown. Gong et al synthesized Ni on the surface of foamed nickel by hydrothermal reaction0.8Se electrode material. Ni0.8Se has higher specific capacitance, and Ni is added under the condition of 1A/g0.8The specific capacity of the Se electrode material can reach 115F/g at most. After 1000 cycles, the cycle capacity is still 91.7% of the original cycle capacity. Yu et al grown CoSe on carbon cloth by hydrothermal reaction2A flexible composite structural material of nanoclusters. Firstly, the cobalt precursor is prepared by reaction on carbon cloth, and then the cobalt precursor is calcined in the air to generate Co3O4Finally selenizing by Se powder. This CoSe2The carbon cloth composite type super-capacitor electrode material shows excellent electrochemical performance at 1 mA/cm2Under the conditions ofThe specific capacitance of the capacitor reaches 1.77F/cm2
Transition metal compounds containing two or more transition metals exhibit better electrochemical properties due to the combined contribution of each transition metal. Chen et al prepared NiSe-CoSe nanoparticles of different Ni/Co ratios by hydrothermal reaction. By changing the Ni/Co atomic ratio, the specific capacitance of the prepared NiSe-CoSe nano-particles can reach 584F/g at the current density of 1A/g, and the capacity of the prepared NiSe-CoSe nano-particles can still be kept at about 77.3 percent at the current density of 20A/g. An, etc. using foamed nickel as substrate by hydrothermal method to synthesize NiCo-MOF, then using Na2SeO3Reacting with NiCo-MOF to prepare nano rod-shaped Ni0.9Co1.92Se4A material. The material shows excellent performance in electrochemical test, and the current density is 2 mA/cm2When the specific capacitance is high, the specific capacitance is 785.7F/g. After 5000 cycles of charge and discharge, the cycle efficiency remained at 88.4%. However, due to the weak rate capability, the unsatisfactory energy density and durability of selenide, the electrochemical performance of these electrode materials is still not satisfactory, and a new electrode material is still needed to be developed to further improve the electrochemical performance of the supercapacitor.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a preparation method of a nickel-cobalt bimetallic selenide/carbon composite for a supercapacitor. The nickel-cobalt double-metal selenide/carbon compound prepared by the method has high specific capacity; and the preparation process is simple, the conditions are mild, the preparation cost is low, and the method is suitable for industrial production.
The technical scheme of the invention is as follows: a preparation method of a nickel-cobalt bimetallic selenide/carbon composite for a super capacitor comprises the following steps:
(1) dissolving soluble nickel salt and soluble cobalt salt in a polyol solvent to obtain a reaction solution A;
(2) dissolving 2-methylimidazole in a polyalcohol solvent to obtain a reaction solution B;
(3) dropwise adding the reaction liquid A into the reaction liquid B, and uniformly mixing by ultrasonic waves to obtain a mixed liquid C;
(4) transferring the mixed solution C into a reaction kettle with a polytetrafluoroethylene lining for solvothermal reaction, cooling the reaction kettle to room temperature after the reaction is finished, and carrying out post-treatment on the reaction mixture to obtain a nickel-cobalt bimetal-organic framework compound;
(5) mixing the nickel-cobalt bimetallic-organic framework compound obtained in the step 4 with selenium powder, and grinding;
(6) selenizing and carbonizing the powder obtained in the step 5 at high temperature under the protection of argon or nitrogen to obtain NiCoxSeya/C complex.
Further, in the step 1, the soluble nickel salt is one of nickel nitrate, nickel chloride or nickel acetate; the soluble cobalt salt is one of cobalt nitrate, cobalt chloride or cobalt acetate.
Further, the polyol in steps 1 and 2 is one of ethylene glycol, glycerol or triethylene glycol.
Further, the temperature of the solvent thermal reaction in the step 4 is 120-180 ℃, and the reaction time is 6-12 hours.
Further, the post-treatment process in the step 4 is to carry out centrifugal separation on the product after the reaction, wash and separate the product by using distilled water and ethanol in sequence, and then dry the precipitate at 60-90 ℃ in vacuum.
Further, the temperature for performing high-temperature selenization and carbonization in the step 6 is 400-600 ℃.
The invention has the beneficial effects that:
1. the nickel-cobalt double-metal selenide/carbon composite prepared by the method has higher specific capacitance and can be applied to a super capacitor with high energy density;
2. the nickel-cobalt double-metal selenide nano-particles and the nano-carbon are organically combined together, so that the active sites can be increased, the conductivity and the stability of the material can be improved, and the electrochemical energy storage performance of the composite material can be further improved;
3. the preparation process disclosed by the invention is simple, mild in condition, simple and convenient to operate, free of complex equipment and low in cost, and is suitable for industrial production.
Drawings
Fig. 1 is an XRD pattern of the dual metal selenide/carbon composite prepared in example 1;
fig. 2 is an SEM photograph of the dual metal selenide/carbon composite prepared in example 1;
fig. 3 is a CV diagram of the double metal selenide/carbon composite prepared in example 1;
fig. 4 is a graph of specific capacitance of the dual metal selenide/carbon composite prepared in example 1 at different scan rates;
fig. 5 is a GCD curve of the bimetallic selenide/carbon composite prepared in example 1;
fig. 6 is a graph showing the specific capacitance of the dual metal selenide/carbon composite prepared in example 1 at different current densities.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
Example 1.
Preparation of a bimetallic selenide/carbon composite for a supercapacitor:
(1) mixing Co (NO)3)2·6H2O (1.5 mmol) and Ni (NO)3)2·6H2Dissolving O (1.5 mmol) in 15.0 mL of glycol to obtain a reaction solution A;
(2) dissolving 10 mmol of 2-methylimidazole in 15.0 mL of glycol to obtain a reaction solution B;
(3) dropwise adding the reaction liquid A into the reaction liquid B, and uniformly mixing by ultrasonic waves to obtain a mixed liquid C;
(4) transferring the mixed solution C into a 50 mL stainless steel autoclave with a polytetrafluoroethylene lining, reacting for 12 hours at the temperature of 150 ℃, cooling to room temperature, centrifugally collecting a product, washing with distilled water and ethanol for several times, and drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain NiCo-MOF;
(5) weighing 200 mg of NiCo-MOF and 200 mg of selenium powder, uniformly mixing in a mortar and grinding;
(6) and flatly spreading the sample in a corundum crucible, placing the crucible in a tubular furnace, and calcining at 500 ℃ under the protection of argon to obtain the nickel-cobalt double-metal selenide/carbon composite. XRD and SEM photographs of the samples are shown in fig. 1 and 2. As can be seen from fig. 1, the diffraction peak intensity of the sample is large, and the half-peak width is small, which indicates that the prepared nickel-cobalt double-metal selenide/carbon composite sample has high crystallinity. As can be seen in FIG. 2, NiCoxSeyThe nano particles are uniformly distributed on the nano carbon generated by pyrolysis, which is not only beneficial to the wetting of electrolyte, the increase of electroactive sites and the improvement of the specific capacity of the electrode; meanwhile, NiCo in the charging and discharging process can be reducedxSeyAnd (4) agglomeration of the nano particles. In addition, the existence of the nano carbon can also improve the conductivity of the electrode material, thereby further improving the rate capacity and the cycling stability of the electrode.
Example 2
The difference from example 1 is that the calcination temperature in step 6 was 600 ℃. The other process conditions were the same as in example 1.
Example 3
The difference from example 1 is that the calcination temperature in step 6 was 400 ℃. The other process conditions were the same as in example 1.
Example 4
The difference from example 1 is that CoCl is added in step 12·6H2O (1.5 mmol) and NiCl2·6H2Dissolving O (1.5 mmol) in 15.0 mL of glycol to obtain a reaction solution A; the calcination temperature in step 6 was 500 ℃.
The other process conditions were the same as in example 1.
Example 5
The difference from example 1 is that Co (NO) is added in step 13)2·6H2O (1.5 mmol) and Ni (NO)3)2·6H2Dissolving O (1.5 mmol) in 15.0 mL of triethylene glycol to obtain a reaction solution A;
dissolving 10 mmol of 2-methylimidazole in 15.0 mL of triethylene glycol in the step 2 to obtain a reaction solution B;
the other process conditions were the same as in example 1.
Electrochemical performance test
The nickel cobalt bimetallic selenide/carbon composite prepared in example 1 was fabricated into an electrode. A nickel-cobalt double-metal selenide/carbon composite electrode is used as a working electrode, a Pt sheet electrode is used as a counter electrode, and an Hg/HgO electrode is used as a reference electrode to form a three-electrode system for electrochemical performance test.
Fig. 3 is a CV curve of a nickel-cobalt dual-metal selenide/carbon composite at different scan rates. As can be seen from fig. 3, the CV curve exhibits non-rectangular characteristics with distinct redox peaks, indicating that the material relies primarily on redox reactions to store energy. Fig. 4 is a graph of the change of the specific capacitance of the nickel-cobalt double-metal selenide/carbon composite electrode with the scanning rate. When the scanning speed is 5mV/s, the mass specific capacitance of the nickel-cobalt double metal selenide/carbon composite electrode is 852.5F/g. When the scan rate was increased to 40 mV/s, the mass specific capacitance of the nickel cobalt duplex selenide/carbon composite was 476.8F/g. Fig. 5 is a charge-discharge curve of the nickel-cobalt double-metal selenide/carbon composite electrode under different current densities. The charge-discharge curve is nonlinear, which shows that the material has battery-like characteristics. Fig. 6 is the specific capacitance of the nickel-cobalt double-metal selenide/carbon composite electrode calculated according to the charging and discharging curve under different current densities. When the current density is 1A/g, the mass specific capacitance is 1073.1F/g; the current density is improved by 20 times, the mass specific capacitance is 727.8F/g, and the capacity retention rate is 67.8%, which shows that the nickel-cobalt double-metal selenide/carbon composite electrode has larger specific capacity and excellent rate performance. Therefore, the nickel-cobalt double-metal selenide/carbon composite is an excellent electrode material of the super capacitor.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.

Claims (6)

1. A preparation method of a nickel-cobalt bimetallic selenide/carbon composite for a super capacitor is characterized by comprising the following steps:
(1) dissolving soluble nickel salt and soluble cobalt salt in a polyol solvent to obtain a reaction solution A;
(2) dissolving 2-methylimidazole in a polyalcohol solvent to obtain a reaction solution B;
(3) dropwise adding the reaction liquid A into the reaction liquid B, and uniformly mixing by ultrasonic waves to obtain a mixed liquid C;
(4) transferring the mixed solution C into a reaction kettle with a polytetrafluoroethylene lining for solvothermal reaction, cooling the reaction kettle to room temperature after the reaction is finished, and carrying out post-treatment on the reaction mixture to obtain a nickel-cobalt bimetal-organic framework compound;
(5) mixing the nickel-cobalt bimetallic-organic framework compound obtained in the step 4 with selenium powder, and grinding;
(6) selenizing and carbonizing the powder obtained in the step 5 at high temperature under the protection of argon or nitrogen to obtain NiCoxSeya/C complex.
2. The method of claim 1, wherein the soluble nickel salt in step 1 is one of nickel nitrate, nickel chloride or nickel acetate; the soluble cobalt salt is one of cobalt nitrate, cobalt chloride or cobalt acetate.
3. The method of claim 1, wherein the polyol used in steps 1 and 2 is one of ethylene glycol, glycerol or triethylene glycol.
4. The method for preparing the nickel-cobalt bimetallic selenide/carbon composite for the supercapacitor according to claim 1, wherein the solvothermal reaction is carried out in the step 4 at a temperature of 120-180 ℃ for 6-12 h.
5. The method for preparing the nickel-cobalt double-metal selenide/carbon composite for the supercapacitor according to claim 1, wherein the post-treatment process in the step 4 is to centrifugally separate a product after reaction, wash and separate the product by distilled water and ethanol in sequence, and dry the precipitate at 60-90 ℃ in vacuum.
6. The method for preparing the nickel-cobalt double-metal selenide/carbon composite for the supercapacitor according to claim 1, wherein the temperature for the high-temperature selenization and carbonization treatment in the step 6 is 400-600 ℃.
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CN111554896A (en) * 2020-04-27 2020-08-18 上海工程技术大学 Cobalt nickel selenide nitrogen doped amorphous carbon nano composite negative electrode material and preparation and application thereof
CN111924809A (en) * 2020-07-28 2020-11-13 中国科学技术大学 Iron-nickel bimetallic selenide nano material, preparation method thereof and lithium ion battery
CN111939945A (en) * 2020-08-20 2020-11-17 安阳师范学院 CoSe2NiSe2Preparation of-CC composite material and application of electrolytic water hydrogen evolution performance thereof
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CN112837943A (en) * 2021-04-22 2021-05-25 中国科学院过程工程研究所 Ultrathin two-dimensional nanosheet layer NiCo-MOF material, and preparation method and application thereof
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CN111554896A (en) * 2020-04-27 2020-08-18 上海工程技术大学 Cobalt nickel selenide nitrogen doped amorphous carbon nano composite negative electrode material and preparation and application thereof
CN111924809A (en) * 2020-07-28 2020-11-13 中国科学技术大学 Iron-nickel bimetallic selenide nano material, preparation method thereof and lithium ion battery
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CN115246630B (en) * 2021-10-18 2023-12-22 齐齐哈尔大学 Preparation method of defect type hollow nickel cobalt selenide nanocube
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