CN111146016A - Flaky nickel sulfide/nickel-vanadium double hydroxide/graphene composite material for super capacitor and preparation method thereof - Google Patents
Flaky nickel sulfide/nickel-vanadium double hydroxide/graphene composite material for super capacitor and preparation method thereof Download PDFInfo
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- CN111146016A CN111146016A CN201911219116.3A CN201911219116A CN111146016A CN 111146016 A CN111146016 A CN 111146016A CN 201911219116 A CN201911219116 A CN 201911219116A CN 111146016 A CN111146016 A CN 111146016A
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- 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
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- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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- 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
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- 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
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- 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
A flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for a super capacitor and a preparation method thereof belong to the field of energy storage materials, and aim at providing a sulfide and metal double hydroxide combined composite material with high specific capacitance and good stability and a preparation method thereof2·6H2O、NH4VO3、NH4F and CO (NH)2)2Dissolving in deionized water, stirring, pouring into a reaction kettle, reacting at 180 ℃ for 8 hours to obtain NiV/rGO/NF, putting a precursor nickel vanadium double hydroxide into a sodium sulfide solution, reacting at 120 ℃ to obtain Ni3S2/NiV‑LDH/rGO/NF. The method is simple, easy to control and low in cost, and the prepared electrode material has high specific capacitance, good rate performance and cycling stability, shows high power density and energy density when being manufactured into a device, and can be used as an excellent electrode material of a super capacitor.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a flaky nickel sulfide/nickel-vanadium double hydroxide/graphene composite material for a super capacitor and a preparation method thereof.
Background
With the rapid development of scientific technology, the large-scale use of fossil fuels and serious environmental problems, high-efficiency energy storage devices have been receiving more and more attention from researchers in recent years. Among currently used energy storage devices, a super capacitor has the advantages of a conventional capacitor and a secondary battery, has the advantages of long service life, high charging and discharging speed, high power density, safety, reliability and the like, and is considered to be a promising energy storage device. The performance of supercapacitors depends mainly on the electrode material. The currently studied electrode materials of supercapacitors mainly include: carbon-based material of electric double layer and pseudocapacitance material. Among these electrode materials, Layered Double Hydroxides (LDHs) have received general attention due to excellent redox activity, environmental protection, high surface area, and unique structural properties. Vanadium has the advantages of multiple oxidation states, high energy density, abundant resources, low cost and the like, and is widely applied to mixed metals.
The synergistic effect is one of the main factors for improving the electrochemical performance of the electrode. A new strategy for combining transition metal double hydroxides with sulphides obtained by in situ sulphidation is thus proposed, taking full advantage of the advantages of the components and the synergistic effects between different materials. The introduction of the graphene improves the electrochemical performance of the electrode, and simultaneously avoids the aggregation phenomenon of the double hydroxide in the charging and discharging processes, and by combining the advantages, the prepared composite material is used as the electrode material of the supercapacitor, so that the reasonable utilization of the material performance and the cost can be realized, the composite material has excellent performance which is not possessed by a single material, and the application prospect is very wide.
Disclosure of Invention
The invention aims to provide a composite material combining sulfide and metal double hydroxide with high specific capacitance and good stability and a preparation method thereof.
The invention adopts the following technical scheme:
a flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for a super capacitor has a chemical general formula of Ni3S2the/NiV-LDH/rGO/NF-X represents different vulcanization time, wherein the value of X is more than or equal to 1 and less than or equal to 7.
A preparation method of a flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for a super capacitor comprises the following steps:
firstly, growing reduced graphene oxide on a foamed nickel substrate by a chemical deposition method: adding graphene oxide into deionized water according to a ratio, performing ultrasonic dispersion to obtain a brown dispersion liquid, adding a reducing agent into the dispersion liquid, uniformly stirring to obtain a mixed solution, immersing a foamed nickel substrate cleaned by acetone, hydrochloric acid and absolute ethyl alcohol into the mixed solution, performing hydrothermal bath reduction for 6 hours at 90 ℃, taking out the foamed nickel substrate, washing residues, placing the foamed nickel substrate in a drying oven, and drying for 12 hours at 60 ℃ to obtain the foamed nickel substrate with reduced graphene oxide, wherein the foamed nickel substrate is marked as rGO/NF;
in the second step, nickel chloride (NiCl)2·6H2O), ammonium metavanadate (NH)4VO3) Ammonium fluoride (NH)4F) And urea (CO (NH)2)2) Dissolving in deionized water, stirring at room temperature until a uniform light green precursor solution is formed, pouring the precursor solution into a hydrothermal reaction kettle with the capacity of 100ml, putting rGO/NF into the reaction kettle, keeping the temperature at 180 ℃ for 8 hours, taking out and cleaning to obtain a composite material NiV/rGO/NF;
thirdly, sulfurizing NiV/rGO/NF by hydrothermal method, proportionally mixing Na2S·9H2Dissolving O in deionized water, stirring for dissolving, transferring to a reaction kettle, placing NiV/rGO/NF into the reaction kettle, keeping at 120 deg.C for 1-7h, taking out, cleaning, and drying to obtain Ni with chemical formula3S2/NiV-LDH/rGONF-X composite material.
In the first step, the mass-to-volume ratio of the graphene oxide to the water is 1mg:3mL, the reducing agent is ascorbic acid, and the mass ratio of the graphene oxide to the reducing agent is 1: 3.
In the second step, the ratio of the nickel chloride to the deionized water is 0.9mmol to 70mL, the ratio of the ammonium metavanadate to the deionized water is 0.3mmol to 70mL, the ratio of the ammonium fluoride to the deionized water is 4mmol to 70mL, and the ratio of the urea to the deionized water is 5mmol to 70 mL.
In the third step, Na is described2S·9H2The ratio of O to deionized water was 1 mmol:70 mL.
The invention has the following beneficial effects:
graphene has an ultrahigh theoretical surface area as a novel carbon material, is applied to novel composite materials and construction of high-performance electrochemical new energy devices, combines the characteristics of cobalt molybdenum sulfide and graphene, and can be used as an electrode material of a supercapacitor, so that reasonable utilization of material performance and cost can be realized, excellent performance which is not possessed by a single material is realized, and the application prospect is very wide.
The vulcanization time in the invention has obvious influence on the specific capacitance of the super capacitor. When the sulfuration reaction is carried out for 3 hours, the prepared nickel sulfide/nickel vanadium double hydroxide has larger specific capacitance (3004 Fg) when being used as the electrode material of the super capacitor-1) And excellent cycle stability (the capacity retention rate is 92.2 percent after 5000 charge-discharge cycles), the nickel sulfide/nickel vanadium double hydroxide prepared by taking reduced graphene oxide supported by foamed nickel as a current collector is taken as a positive electrode material, and a super capacitor device assembled by taking activated carbon as a negative electrode material has the volume of 59.4 Wh kg-1The energy density of the super capacitor can be used as a positive electrode material of the super capacitor.
Drawings
FIG. 1 shows the NiV/rGO/NF and Ni obtained in examples 2 to 63S2XRD curves of/NiV-LDH/rGO/NF vulcanized at different times;
wherein: a is NiV/rGO/NF;
b is Ni3S2/NiV-LDH/rGO/NF-1；
c is Ni3S2/NiV-LDH/rGO/NF-3；
d is Ni3S2/NiV-LDH/rGO/NF-5；
e is Ni3S2/NiV-LDH/rGO/NF-7。
FIG. 2 is a scanning electron micrograph of nickel sulfide/nickel vanadium double hydroxide from example 4 taken at different magnifications.
FIG. 3 is a plot of the voltammetric cycling profile of the electrode material prepared in example 4 in a 2mol/L KOH solution.
FIG. 4 is a constant current charge and discharge curve diagram of the electrode material prepared in example 4 in 2mol/L KOH solution.
Fig. 5 is a graph of energy density versus power density for the supercapacitor device prepared in example 7.
Detailed Description
Detecting, analyzing and characterizing the microstructure and the electrochemical performance of the prepared composite material:
microstructural analysis was performed with a scanning electron microscope, model MIRA 3;
electrochemical performance testing was performed with CHI660E electrochemical workstation.
Example 1
Nickel chloride (NiCl) in a molar amount of 0.9mmol2·6H2O) and 0.3mmol of ammonium metavanadate (NH)4VO3) 4mmol of ammonium fluoride (NH)4F) And 5mmol of urea (CO (NH)2)2) Dissolved in 70mL of deionized water and stirred at room temperature until a homogeneous greenish precursor solution is formed. Putting the precursor solution and the cleaned NF into a reaction kettle, keeping the reaction kettle at 180 ℃ for 8 hours, and taking out the reaction kettle to obtain a material NiV-LDH/NF; the prepared NiV-LDH/NF is used as the anode material of the super capacitor to carry out electrochemical performance test in a three-electrode system (electrolyte is 2mol/L KOH), and the specific capacitance is 979F g-1。
Example 2
Ultrasonically decomposing 10mg of graphene oxide into 30mL of distilled waterAfter a uniform brown solution is formed, adding 30mg of ascorbic acid, carrying out ultrasonic stirring uniformly, placing foamed nickel cleaned by acetone, hydrochloric acid and absolute ethyl alcohol into the dispersion liquid, depositing for 6 hours at the temperature of 90 ℃ in a water bath kettle, washing the surface of a sample by deionized water, and drying for 12 hours at the temperature of 70 ℃ to obtain rGO/NF. Nickel chloride (NiCl) in a molar amount of 0.9mmol2·6H2O) and 0.3mmol of ammonium metavanadate (NH)4VO3) 4mmol of ammonium fluoride (NH)4F) And 5mmol of urea (CO (NH)2)2) Dissolved in 70mL of deionized water and stirred at room temperature until a homogeneous greenish precursor solution is formed. Putting the precursor solution and the rGO/NF into a reaction kettle, keeping the reaction kettle at 180 ℃ for 8 hours, taking out and cleaning to obtain a composite material NiV/rGO/NF; the prepared NiV/rGO/NF composite material is used as a positive electrode material of a super capacitor to carry out electrochemical performance test in a three-electrode system (electrolyte is 2mol/L KOH), and the specific capacitance is 1818F g-1。
Example 3
Adding 1mmoL Na2S·9H2O is dissolved in 70mL of deionized water, stirred and dissolved, then transferred to a reaction kettle, and NiV/rGO/NF prepared in example 2 is placed in the reaction kettle, kept at 120 ℃ for 1 hour, the surface of the sample is washed by the deionized water, and the sample is dried overnight at 60 ℃. The prepared composite is named as Ni3S2The NiV-LDH/rGO/NF-1 is used as a positive electrode material of a super capacitor to carry out electrochemical performance test in a three-electrode system (2 mol/L KOH electrolyte), and the specific capacitance is 2534F g-1。
Example 4
Adding 1mmoL Na2S·9H2O is dissolved in 70mL of deionized water, stirred and dissolved, then transferred to a reaction kettle, and NiV/rGO/NF prepared in example 1 is placed in the reaction kettle, kept at 120 ℃ for 3 hours, the surface of the sample is washed by the deionized water, and dried at 60 ℃ for one night. The prepared composite is named as Ni3S2NiV-LDH/rGO/NF-3 as the anode material of a super capacitor in a three-electrode system (electrolyte is 2mol/L KOH)The specific capacitance of the test piece is 3004F g-1。
Example 5
Adding 1mmoL Na2S·9H2O is dissolved in 70mL of deionized water, stirred and dissolved, then transferred to a reaction kettle, and NiV/rGO/NF prepared in example 1 is placed in the reaction kettle, kept at 120 ℃ for 5 hours, the surface of the sample is washed by the deionized water, and dried at 60 ℃ for one night. The prepared composite is named as Ni3S2The NiV-LDH/rGO/NF-5 is used as a positive electrode material of a super capacitor to carry out electrochemical performance test in a three-electrode system (2 mol/L KOH electrolyte), and the specific capacitance of the material is 2445F g-1。
Example 6
Adding 1mmoL Na2S·9H2O was dissolved in 70mL of deionized water, stirred and dissolved, and transferred to a reaction vessel, and NiV/rGO/NF obtained in example 1 was placed therein, and kept at 120 ℃ for 7 hours, and the surface of the sample was washed with deionized water and dried overnight at 60 ℃. The prepared composite is named as Ni3S2The NiV-LDH/rGO/NF-7 is used as a positive electrode material of a super capacitor to carry out electrochemical performance test in a three-electrode system (2 mol/L KOH electrolyte), and the specific capacitance is 2261F g-1。
Example 7
Mixing acetylene black, active carbon and polyvinylidene fluoride according to the mass ratio of 8:1:1, uniformly grinding, coating on foamed nickel, drying at 60 ℃ for 12h to serve as a negative electrode material, and taking Ni as a negative electrode material3S2the/NiV-LDH/rGO/NF-3 is used as an anode material to be assembled into an asymmetric super capacitor device, and electrochemical performance test is carried out on the asymmetric super capacitor device; the power density of the prepared asymmetric device of the super capacitor is 852.3W kg-1It was shown to be as high as 59.4 Wh kg-1The energy density of (1).
Preparing an asymmetric super capacitor device:
acetylene black, activated carbon and polyvinylidene fluoride are mixed according to the mass ratio of 8:1:1, the mixture is uniformly ground and then coated on foamed nickel, the mixture is dried at 80 ℃ and then used as a negative electrode material, a nickel sulfide/nickel vanadium double hydroxide is used as a positive electrode material, a cellulose film is used as a diaphragm, a KOH alkaline solution is used as an electrolyte to assemble a liquid asymmetric supercapacitor device, and electrochemical performance test is carried out on the liquid asymmetric supercapacitor device.
And (4) conclusion: the specific capacitance of the prepared single nickel-vanadium double hydroxide is 979F g-1(ii) a In addition, the current collector has a great influence on the electrochemical performance of the electrode material, and when the reduced graphene oxide supported by the foamed nickel is used as the current collector, the specific capacitance of the prepared electrode material is greatly improved to 1818 Fg-1(ii) a The specific capacitance of the nickel sulfide/nickel vanadium double hydroxide formed after partial vulcanization of the hydroxide as the anode material of the super capacitor is up to 3004F g-1The energy density of the prepared super capacitor device is as high as 59.4 Wh kg-1。
Claims (5)
1. A flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for a super capacitor is characterized in that: has a chemical formula of Ni3S2the/NiV-LDH/rGO/NF-X represents different vulcanization time, wherein the value of X is more than or equal to 1 and less than or equal to 7.
2. A method for preparing the flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for the supercapacitor according to claim 1, which is characterized in that: the method comprises the following steps:
firstly, growing reduced graphene oxide on a foamed nickel substrate by a chemical deposition method: adding graphene oxide into deionized water according to a ratio, performing ultrasonic dispersion to obtain a brown dispersion liquid, adding a reducing agent into the dispersion liquid, uniformly stirring to obtain a mixed solution, immersing a foamed nickel substrate cleaned by acetone, hydrochloric acid and absolute ethyl alcohol into the mixed solution, performing hydrothermal bath reduction for 6 hours at 90 ℃, taking out the foamed nickel substrate, washing residues, placing the foamed nickel substrate in a drying oven, and drying for 12 hours at 60 ℃ to obtain the foamed nickel substrate with reduced graphene oxide, wherein the foamed nickel substrate is marked as rGO/NF;
secondly, dissolving nickel chloride, ammonium metavanadate, ammonium fluoride and urea in deionized water, stirring at room temperature until a uniform light green precursor solution is formed, pouring the precursor solution into a hydrothermal reaction kettle with the capacity of 100ml, putting rGO/NF into the reaction kettle, keeping the temperature at 180 ℃ for 8 hours, taking out and cleaning to obtain a composite material NiV/rGO/NF;
thirdly, sulfurizing NiV/rGO/NF by hydrothermal method, proportionally mixing Na2S·9H2Dissolving O in deionized water, stirring for dissolving, transferring to a reaction kettle, placing NiV/rGO/NF into the reaction kettle, keeping at 120 deg.C for 1-7h, taking out, cleaning, and drying to obtain Ni with chemical formula3S2The composite material of/NiV-LDH/rGO/NF-X.
3. The preparation method of the flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for the supercapacitor according to claim 2, characterized by comprising the following steps: in the first step, the mass-to-volume ratio of the graphene oxide to the water is 1mg:3mL, the reducing agent is ascorbic acid, and the mass ratio of the graphene oxide to the reducing agent is 1: 3.
4. The preparation method of the flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for the supercapacitor according to claim 2, characterized by comprising the following steps: in the second step, the ratio of the nickel chloride to the deionized water is 0.9mmol to 70mL, the ratio of the ammonium metavanadate to the deionized water is 0.3mmol to 70mL, the ratio of the ammonium fluoride to the deionized water is 4mmol to 70mL, and the ratio of the urea to the deionized water is 5mmol to 70 mL.
5. The preparation method of the flaky nickel sulfide/nickel vanadium double hydroxide/graphene composite material for the supercapacitor according to claim 2, characterized by comprising the following steps: in the third step, Na is described2S·9H2The ratio of O to deionized water was 1 mmol:70 mL.
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| CN115274310B (en) * | 2022-08-10 | 2023-06-02 | 桂林电子科技大学 | Polyhedral cobalt sulfide loaded NiGa-LDH electrode material and preparation method and application thereof |
| CN116377504A (en) * | 2023-06-01 | 2023-07-04 | 中石油深圳新能源研究院有限公司 | Hydrogen and oxygen evolution catalyst, preparation method thereof, electrolysis device and electrode thereof |
| CN116377504B (en) * | 2023-06-01 | 2023-09-01 | 中石油深圳新能源研究院有限公司 | Hydrogen and oxygen evolution catalyst, preparation method thereof, electrolysis device and electrode thereof |
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