CN113130214B - NF @ molybdenum oxide @ nickel cobalt-LDH composite material and preparation method and application thereof - Google Patents
NF @ molybdenum oxide @ nickel cobalt-LDH composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 91
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910000476 molybdenum oxide Inorganic materials 0.000 title description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 179
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000004070 electrodeposition Methods 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000006260 foam Substances 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 20
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 19
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 19
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 19
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 229910002445 Co(NO3)3·6H2O Inorganic materials 0.000 claims abstract description 16
- 229910017855 NH 4 F Inorganic materials 0.000 claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 77
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 28
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 238000002604 ultrasonography Methods 0.000 claims description 13
- 239000003990 capacitor Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 239000011258 core-shell material Substances 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 238000002484 cyclic voltammetry Methods 0.000 description 24
- 229910021607 Silver chloride Inorganic materials 0.000 description 22
- 239000008367 deionised water Substances 0.000 description 22
- 229910021641 deionized water Inorganic materials 0.000 description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 22
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 22
- -1 polytetrafluoroethylene Polymers 0.000 description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 description 13
- 238000007599 discharging Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 238000010277 constant-current charging Methods 0.000 description 11
- 125000004122 cyclic group Chemical group 0.000 description 11
- 238000000840 electrochemical analysis Methods 0.000 description 11
- 239000008151 electrolyte solution Substances 0.000 description 11
- 229910001220 stainless steel Inorganic materials 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 11
- 239000007772 electrode material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 150000003623 transition metal compounds Chemical class 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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Abstract
The invention relates to NF @ MoO 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise: preparing an ammonium molybdate solution; the NF @ MoO is prepared by taking ammonium molybdate solution as electrodeposition solution and foam nickel as a carrier by adopting a one-step electrodeposition method 3 Precursor, then NF @ MoO 3 Annealing the precursor in air atmosphere to obtain NF @ MoO 3 (ii) a Mixing Ni (NO) 3 ) 2 ·6H 2 O、Co(NO 3 ) 3 ·6H 2 O、NH 4 F. Adding urea into water, stirring, dispersing, transferring the solution into autoclave, soaking in NF @ MoO 3 Hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO 3 The material @ NiCo-LDH. Compared with the prior art, the material prepared by the invention has a unique layered core-shell structure, can provide effective active sites, and not only has MoO 3 The advantages of promoting the diffusion of electrolyte and the transfer of electrons have the advantages of high specific capacitance of NiCo-LDH and good electrochemical performance; the preparation method is environment-friendly, simple and easy to operate, and convenient for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of electrochemistry and nano materials, in particular to NF @ MoO 3 @ NiCo-LDH composite material and preparation thereofA preparation method and application.
Background
Ultracapacitors have attracted considerable interest over the last decades due to their fast charge and discharge rates, high power density (1-2 orders of magnitude higher than batteries), long cycle life (2-3 orders of magnitude longer than batteries), and high reliability. Currently, carbon-based materials, transition metal compounds, conductive polymers and composite-based electrode materials are commonly used as the electrode materials of the super capacitor. The transition metal compound has high specific capacitance and conductivity, so that the method is very suitable for manufacturing high-power and high-energy supercapacitor electrodes.
NiCo-LDH adopted in the prior art has low conductivity, so that the NiCo-LDH has obvious technical bottleneck in the application of supercapacitor materials.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the NF @ MoO 3 The @ NiCo-LDH composite material is prepared by mixing MoO 3 Is compounded with NiCo-LDH to achieve the effect of enhancing the electrochemical performance and further overcome MoO 3 And the NiCo-LDH has the problems of application limitation in the aspect of electrode materials of the supercapacitor and the like.
The purpose of the invention can be realized by the following technical scheme:
the first purpose of the invention is to protect an NF @ MoO 3 The preparation method of the @ NiCo-LDH composite material comprises the following steps:
s1: preparing an ammonium molybdate solution;
s2: the NF @ MoO is prepared by taking the ammonium molybdate solution prepared in the S1 as an electrodeposition solution and foam nickel as a carrier by adopting a one-step electrodeposition method 3 Precursor is washed and dried, and then NF @ MoO is added 3 Annealing the precursor in air atmosphere to obtain NF @ MoO 3 ；
S3: mixing Ni (NO) 3 ) 2 ·6H 2 O、Co(NO 3 ) 3 ·6H 2 O、NH 4 F. Adding urea into water, stirring thoroughly to disperse uniformly, transferring the solution into autoclave, addingNF @ MoO obtained by immersing S2 in an autoclave 3 Carrying out hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO 3 @ NiCo-LDH material.
Further, the preparation process of the ammonium molybdate solution in the S1 comprises the following steps: mixing ammonium molybdate tetrahydrate with water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate and the water to obtain a mixed solution;
the ratio of the molar quantity of the ammonium molybdate tetrahydrate to the adding volume of the water is 1mmol (40-60) mL.
Further, the stirring and ultrasonic dispersion assisted in the step S1 are carried out at room temperature for 5-10min, and a clear mixed solution is obtained after ultrasonic dispersion.
Further, in S2, foamed nickel treated by acetone, ethanol and water in sequence is used as a carrier.
Further, the one-step electrodeposition method described in S2 is carried out at room temperature with a scan rate of 5 to 25mV/S and a scan period of 15 to 35.
Further, the annealing process in the S2 is carried out in a tubular resistance furnace, the atmosphere is air atmosphere, the temperature is 200-400 ℃, and the time is 1.5-2.5h.
Further, ni (NO) described in S3 3 ) 2 ·6H 2 O、Co(NO 3 ) 3 ·6H 2 O、NH 4 F. The molar feeding ratio of the urea is (1-3) to (2-4) to (5-10).
Further, the temperature of the hydrothermal reaction in S3 is 120-180 ℃ and the time is 6-8h.
Further, the drying processes in S2 and S3 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24h.
The second purpose of the invention is to protect NF @ MoO obtained by the preparation method 3 @ NiCo-LDH composite materials.
A third object of the present invention is to protect an NF @ MoO as described above 3 The application of the @ NiCo-LDH composite material in the super capacitor is realized by combining NF @ MoO 3 Grinding the @ NiCo-LDH composite material, uniformly mixing the ground material with carbon black and polytetrafluoroethylene, and then laminating the mixture on a foam nickel sheetAnd finally, obtaining the working electrode of the super capacitor.
Further, in the working electrode, NF @ MoO 3 The mass ratio of the @ NiCo-LDH composite material to the carbon black to the polytetrafluoroethylene is 8 (0.8-1.2) to 0.8-1.2.
Compared with the prior art, the invention has the following technical advantages:
1. NF @ MoO prepared by the invention 3 The @ NiCo-LDH composite material has a unique core-shell layered structure, moO 3 The obvious increase of the medium electroactive sites and the shortening of the ion diffusion length can effectively make up the defect of low conductivity of the NiCo-LDH, and the NiCo-LDH and the medium electroactive sites are compounded to fully utilize the higher specific capacitance of the NiCo-LDH.
2. NF @ MoO prepared by the invention 3 The @ NiCo-LDH composite material is used as a composite material in a supercapacitor, and the cyclic voltammetry curve diagram of the @ NiCo-LDH composite material has obvious redox peak pairs; meanwhile, the charging and discharging curve graph shows that the specific capacitance can at least reach 1500F/g.
3. The preparation method has the advantages of low cost of raw materials, no pollution, no toxicity of solvents generated in the preparation process, and realization of large-scale industrial popularization.
Drawings
FIG. 1 is a cyclic voltammogram at different sweep rates for the product samples obtained in example 1.
Figure 2 is a graph of GCD at different current densities for samples of the product obtained in example 1.
Detailed Description
As part of the concept of the present solution, in this case, transition metal oxides have proven to be pseudocapacitive materials with the potential of impressive high performance supercapacitors. In particular, transition metal oxides, e.g. WO 3 、MnO 2 、Fe 3 O 4 、NiO、RuO 2 And MoO 3 Wherein, moO 3 Considerable attention has been paid to its low cost and environmental friendliness. MoO 3 In a layered crystal structure, the layers are connected to each other by van der waals forces. This structure helps to ensure rapid insertion of ions into the electrode material, thereby achieving high electrochemical performance. Molybdenum elementThe multiple oxidation states of the element enable the molybdenum trioxide to undergo more than one redox reaction during the circulation process, thereby providing a wide electrochemical window.
As part of the concept of the present solution, the present invention relates to MoO 3 Among several candidate materials for recombination, LDH (double metal layer hydroxide) is the most desirable one, especially NiCo-LDH. Layered Double Hydroxides (LDHs), due to their novel layered structure, superior capacitance, high redox activity and environmental friendliness, are sufficiently competitive materials for supercapacitor applications. NiCo-LDH has outstanding capacitive properties due to the synergistic effect of the two elements, cobalt and nickel, which provide different electrochemically active sites through their several oxidation states. However, the inherent low conductivity of LDHs limits their use, and therefore the strategy of the present invention to improve the conductivity of NiCo-LDH supercapacitors is to use highly conductive materials as the framework supporting the active material, thereby shortening the electron transport distance.
The invention is described in detail below with reference to the figures and the specific embodiments.
Example 1:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and secondly, taking the ammonium molybdate solution obtained in the first step as an electrodeposition solution, placing the solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, taking a platinum wire as a counter electrode, taking Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning rate is 20mV/s, and the scanning period is 30. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly to disperse uniformly, transferring the solution into 50mL polytetrafluoroethylene inner lining stainless steel autoclave, and obtaining 1cm x 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (note MNC-1).
The Chenhua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method, and adopts a three-electrode system to perform electrochemical test: the method comprises the following steps of taking a nickel foam sheet of MNC-1 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1466.7F/g under the condition of 2mol/L KOH solution and the current density of 0.5A/g.
FIG. 1 shows NF @ MoO obtained in this example 3 CV diagram of the @ NiCo-LDH composite material at different sweep rates, wherein the sweep rates are 5, 10, 15, 20, 30, 40 and 50mV/s respectively. As can be seen from the figure, at a voltage range of 0-0.5V, there are a pair of symmetrical redox peaks, and as the sweep rate increases, the oxidation peak and the reduction peak move to the right and left, respectively. The above-mentioned phenomena indicate that the prepared NF @ MoO 3 The @ NiCo-LDH composite material has good reversibility and stability.
FIG. 2 is the NF @ MoO produced 3 The GCD curve at current densities of 0.5, 1, 2A/g for the @ NiCo-LDH composite.
Example 2:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate with 40mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (note MNC-2).
The Chenhua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method, and adopts a three-electrode system to perform electrochemical test: the preparation method comprises the following steps of taking a foam nickel sheet of MNC-2 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1421.13F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 3:
this exampleMiddle NF @ MoO 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 60mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electro-deposition is finished, washing the foamed nickel for three times by deionized water, putting the foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then placed into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (note MNC-3).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a nickel foam sheet of MNC-3 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1386.27F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 4:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and secondly, taking the ammonium molybdate solution obtained in the first step as an electrodeposition solution, placing the solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, taking a platinum wire as a counter electrode, taking Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning rate is 10mV/s, and the scanning period is 30. Taking out the foamed nickel after the electro-deposition is finished, washing the foamed nickel for three times by deionized water, putting the foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-4).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a nickel foam sheet of MNC-4 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1268.53F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 5:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate with 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 20 scanning cycles. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-5).
The Chenhua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method, and adopts a three-electrode system to perform electrochemical test: the preparation method comprises the following steps of taking a foam nickel sheet of MNC-5 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1249.54F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 6:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a scanning speed of 10mV/s for 20 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-6).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a MNC-6 foam nickel sheet as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1140.68F/g under the condition of 2mol/L KOH solution and the current density of 0.5A/g.
Example 7:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and secondly, taking the ammonium molybdate solution obtained in the first step as an electrodeposition solution, placing the solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, taking a platinum wire as a counter electrode, taking Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning rate is 20mV/s, and the scanning period is 30. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then placed into a resistance furnace to be calcined for 2 hours at the temperature of 200 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water, heating at 120 deg.C for 8 hr, cooling to room temperature, and mixing with the above mixtureWashing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-7).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a MNC-7 foam nickel sheet as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1289.16F/g under the condition of 2mol/L KOH solution and the current density of 1A/g.
Example 8:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 2mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly and dispersing uniformly, mixingTransferring the solution into a 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm x 1cm NF @ MoO in the second step 3 Soaking in water at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite material. The foam nickel loaded with the composite material is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-8).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a MNC-8 foam nickel sheet as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1312.1F/g in 2mol/L KOH solution and at a current density of 2A/g.
Example 9:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then placed into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、3mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly to disperse uniformly, transferring the solution into 50mL polytetrafluoroethylene inner lining stainless steel autoclave, and obtaining 1cm x 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (note MNC-9).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a foam nickel sheet of MNC-9 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1407.61F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 10:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate with 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and put into a resistance furnace in an air atmosphere, 30 DEGCalcining at 0 deg.C for 2 hr, and heating at 2 deg.C/min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 8mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm x 1cm NF @ MoO in the second step 3 Soaking in water, hydrothermal at 120 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite material. The foam nickel loaded with the composite material is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (Note MNC-10).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a foam nickel sheet of MNC-10 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1253.38F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 11:
NF @ MoO in this example 3 The @ NiCo-LDH composite material and the preparation method and the application thereof comprise the following steps:
step one, mixing 1mmol of ammonium molybdate tetrahydrate with 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate to obtain a mixed solution;
and step two, taking the ammonium molybdate solution obtained in the step one as an electrodeposition solution, placing the electrodeposition solution in an electrodeposition device, taking foamed nickel of 8mm multiplied by 1cm which is sequentially treated by acetone, ethanol and water as a working electrode, a platinum wire as a counter electrode, ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, and carrying out scanning at a rate of 20mV/s for 30 scanning periods. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, and putting the foamed nickel into vacuumDrying in an oven at 60 deg.C for 12h to obtain NF @ MoO 3 And (3) precursor. Take out NF @ MoO 3 The precursor is treated and then put into a resistance furnace to be calcined for 2 hours at the temperature of 300 ℃ in the air atmosphere, and the heating rate is 2 ℃ min -1 Finally obtaining NF @ MoO 3 ；
Thirdly, 1mmol of Ni (NO) 3 ) 2 ·6H 2 O、2mmol Co(NO 3 ) 3 ·6H 2 O、2mmol NH 4 F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing uniformly, transferring the solution into 50mL stainless steel autoclave with polytetrafluoroethylene lining, and obtaining 1cm × 1cm NF @ MoO in the second step 3 Soaking in water at 160 deg.C for 8 hr, cooling to room temperature, washing with deionized water for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain NF @ MoO 3 @ NiCo-LDH composite material. The composite material-loaded foam nickel is used as a working electrode, namely MoO 3 The @ NiCo-LDH working electrode (note MNC-11).
The Chenghua CHI760e electrochemical workstation adopts a cyclic voltammetry and constant current charging and discharging method and adopts a three-electrode system for electrochemical test: the preparation method comprises the following steps of taking a foam nickel sheet of MNC-11 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 1247.1F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. NF @ MoO for super capacitor 3 The preparation method of the @ NiCo-LDH composite material is characterized by comprising the following steps of:
s1: preparing an ammonium molybdate solution;
s2: the preparation method comprises the steps of taking the ammonium molybdate solution prepared in S1 as electrodeposition liquid, taking foam nickel as a carrier, and preparing NF @ MoO by adopting a one-step electrodeposition method 3 Precursor, washing and drying, then NF @ MoO 3 Annealing the precursor in air atmosphere to obtain NF @ MoO 3 ；
S3: mixing Ni (NO) 3 ) 2 ·6H 2 O、Co (NO 3 ) 3 ·6H 2 O、NH 4 F. Adding urea into water, stirring thoroughly to disperse uniformly, transferring the solution into autoclave, and soaking in NF @ MoO obtained from S2 3 Carrying out hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO 3 @ NiCo-LDH material;
s2, the one-step electrodeposition method is carried out at room temperature, the scanning rate for electrodeposition is 5-25mV/S, and the scanning period is 15-35;
s2, the annealing process is carried out in a tubular resistance furnace, the atmosphere is air atmosphere, the temperature is 200-400 ℃, and the time is 1.5-2.5 h;
the temperature of the hydrothermal reaction in the S3 is 120-180 ℃, and the time is 6-8h.
2. NF @ MoO for super capacitor according to claim 1 3 The preparation method of the @ NiCo-LDH composite material is characterized in that the preparation process of the ammonium molybdate solution in S1 is as follows: mixing ammonium molybdate tetrahydrate with water, stirring and uniformly dispersing by ultrasound to completely dissolve the ammonium molybdate tetrahydrate and the water to obtain a mixed solution;
the ratio of the molar weight of the ammonium molybdate tetrahydrate to the added volume of the water is 1mmol (40-60) mL.
3. NF @ MoO for super capacitor according to claim 1 3 A preparation method of the @ NiCo-LDH composite material is characterized in that Ni (NO) in S3 3 ) 2 ·6H 2 O、Co (NO 3 ) 3 ·6H 2 O、NH 4 F. The molar feeding ratio of the urea is (1-3) to (2-4) to (5-10).
4. NF @ MoO for super capacitor according to claim 1 3 The preparation method of the @ NiCo-LDH composite material is characterized in that the drying processes in S2 and S3 are both vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24h.
5. NF @ MoO for supercapacitor obtained by the preparation method according to any one of claims 1 to 4 3 @ NiCo-LDH composite materials.
6. NF @ MoO as claimed in claim 5 3 The application of the @ NiCo-LDH composite material in the super capacitor is characterized in that NF @ MoO is adopted 3 The @ NiCo-LDH composite material is used as a working electrode of a supercapacitor.
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