CN113130214A - 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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- 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
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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
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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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Abstract
The invention relates to NF @ MoO3The @ NiCo-LDH composite material and the preparation method and the application thereof comprise: preparing an ammonium molybdate solution; preparing NF @ MoO by one-step electrodeposition with ammonium molybdate solution as electrodeposition solution and foam nickel as carrier3Precursor, followed by NF @ MoO3Annealing the precursor in the air atmosphere to obtain NF @ MoO3(ii) a Mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2O、NH4F. Adding urea into water, stirring and dispersing uniformly, transferring the solution into a high-pressure kettle, and immersing into NF @ MoO3Hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO3@ NiCo-LDH material. Compared with the prior art, the material prepared by the invention has a unique layered core-shell structureCan provide effective active sites, not only has MoO3The 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 @ MoO3A @ NiCo-LDH composite material, a preparation method and application thereof.
Background
Supercapacitors have attracted considerable interest over the last few 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 of the prior art and provide NF @ MoO3The @ NiCo-LDH composite material is prepared by mixing MoO3Is compounded with NiCo-LDH to achieve the effect of enhancing the electrochemical performanceAnd further overcome MoO3And 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 NF @ MoO3The preparation method of the @ NiCo-LDH composite material comprises the following steps:
s1: preparing an ammonium molybdate solution;
s2: preparing NF @ MoO by using ammonium molybdate solution prepared in S1 as electrodeposition solution and foamed nickel as a carrier through one-step electrodeposition3Precursor, washing and drying, and then, NF @ MoO3Annealing the precursor in the air atmosphere to obtain NF @ MoO3；
S3: mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2O、NH4F. Adding urea into water, stirring thoroughly, dispersing, transferring the solution into autoclave, and immersing NF @ MoO obtained in S2 in the autoclave3Carrying out hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO3@ NiCo-LDH material.
Further, the preparation process of the ammonium molybdate solution in the 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.
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, nickel foam treated with acetone, ethanol, and water in this order was used as a carrier.
Further, the one-step electrodeposition method described in S2 was carried out at room temperature, with the electrodeposition being carried out at a scan rate of 5 to 25mV/S and with a scan period of 15 to 35.
Further, the annealing process in S2 is performed in a tubular resistance furnace, the atmosphere is air atmosphere, the temperature is 200-400 ℃, and the time is 1.5-2.5 h.
Further, Ni (NO) in S33)2·6H2O、Co(NO3)3·6H2O、NH4F. 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 6-8 h.
Further, the drying processes in S2 and S3 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
The second purpose of the invention is to protect the NF @ MoO obtained by the preparation method3@ NiCo-LDH composite materials.
The third purpose of the invention is to protect the NF @ MoO3The application of the @ NiCo-LDH composite material in the super capacitor is realized by mixing NF @ MoO3Grinding the @ NiCo-LDH composite material, uniformly mixing the ground material with carbon black and polytetrafluoroethylene, and then pressing the mixture on a foam nickel sheet to obtain the working electrode of the supercapacitor.
Further, in the working electrode, NF @ MoO3The 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 invention3The @ NiCo-LDH composite material has a unique core-shell layered structure, MoO3The 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 invention3The @ 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 for impressive high performance supercapacitors. In particular, transition metal oxides, e.g. WO3、MnO2、Fe3O4、NiO、RuO2And MoO3Wherein, MoO3Considerable attention has been paid to its low cost and environmental friendliness. MoO3In 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. The multiple oxidation states of the molybdenum element enable the molybdenum trioxide to generate more than one oxidation-reduction reaction in the circulation process, thereby providing a wide electrochemical window.
As part of the concept of the present solution, the method is related to MoO3Among 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 specific embodiments.
Example 1:
NF @ MoO in this example3The @ 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (note MNC-1).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for 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 in 2mol/L KOH solution and at a current density of 0.5A/g.
FIG. 1 is a representation of NF @ MoO prepared in this example3CV diagram of @ NiCo-LDH composite material under different sweep rates, wherein the sweep rates are respectively 5, 10, 15, 20, 30, 40 and 50 mV/s. 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 phenomena indicate that the prepared NF @ MoO3The @ NiCo-LDH composite material has good reversibility and stability.
FIG. 2 is a graph of the NF @ MoO produced3The GCD curve at current densities of 0.5, 1, 2A/g for the @ NiCo-LDH composite.
Example 2:
NF @ MoO in this example3The @ 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 40mL 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol urea into 50mL water, stirring thoroughly, dispersing, transferring the solution into 50mL polytetrafluoroethylene liningIn a stainless steel autoclave, 1cm multiplied by 1cm NF @ MoO obtained in the second step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-2).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a nickel foam 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:
NF @ MoO in this example3The @ 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 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (note MNC-3).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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 example3The @ 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 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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 increased2℃·min-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-4).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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 example3The @ 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 20. 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 at the temperature of 60 ℃ 12h to obtain NF @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-5).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: the 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 example3The @ 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;
secondly, taking the ammonium molybdate solution obtained in the first step as an electrodeposition solution, putting 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, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, and an electrodeposition solution maintaining chamberThe temperature, the scanning rate is 10mV/s, and the scanning period is 20. 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-6).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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, 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 1140.68F/g in 2mol/L KOH solution and at a current density of 0.5A/g.
Example 7:
NF @ MoO in this example3The @ 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;
secondly, taking the ammonium molybdate solution obtained in the first step as an electrodeposition solution, and placing the electrodeposition solution in electrodepositionIn the device, 8mm × 1cm × 1cm foamed nickel treated by acetone, ethanol and water in sequence is used as a working electrode, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, the electrodeposition solution is maintained at room temperature, the scanning speed 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The precursor is treated and then put 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-7).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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, 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 1289.16F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 8:
NF @ MoO in this example3The @ 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 2mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-8).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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, 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 1312.1F/g in 2mol/L KOH solution and at a current density of 2A/g.
Example 9:
NF @ MoO in this example3@ NiCo-LDH composite materialThe 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、3mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-9).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a nickel foam 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 example3The @ 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. 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 step3Immersing in the solution, heating at 120 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-10).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, 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 example3The @ 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 @ MoO3And (3) precursor. Taking out NF @ MoO3The 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-1Finally obtaining NF @ MoO3；
Thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2O、2mmol NH4F. Adding 5mmol 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 step3Immersing in the solution, heating at 160 deg.C for 8h, cooling to room temperature, washing with deionized water for 3 times, and vacuum drying at 60 deg.C for 12h to obtain NF @ MoO3@ NiCo-LDH composite materials. The composite material-loaded foam nickel is used as a working electrode, namely MoO3The @ NiCo-LDH working electrode (Note MNC-11).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: the method comprises the following steps of taking a nickel foam 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 (10)
1. NF @ MoO3The preparation method of the @ NiCo-LDH composite material is characterized by comprising the following steps of:
s1: preparing an ammonium molybdate solution;
s2: preparing NF @ MoO by using ammonium molybdate solution prepared in S1 as electrodeposition solution and foamed nickel as a carrier through one-step electrodeposition3Precursor, washing and drying, and then, NF @ MoO3Annealing the precursor in the air atmosphere to obtain NF @ MoO3；
S3: mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2O、NH4F. Adding urea into water, stirring thoroughly, dispersing, transferring the solution into autoclave, and immersing NF @ MoO obtained in S2 in the autoclave3Carrying out hydrothermal reaction, cooling, washing and drying to obtain NF @ MoO3@ NiCo-LDH material.
2. The NF @ MoO of claim 13The preparation method of the @ NiCo-LDH composite material is characterized in that S1The preparation process of the medium ammonium molybdate solution 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 weight of the ammonium molybdate tetrahydrate to the added volume of the water is 1mmol (40-60) mL.
3. The NF @ MoO of claim 13The preparation method of the @ NiCo-LDH composite material is characterized in that the one-step electrodeposition method in S2 is carried out at room temperature, the scanning rate for electrodeposition is 5-25mV/S, and the scanning period is 15-35.
4. The NF @ MoO of claim 13The preparation method of the @ NiCo-LDH composite material is characterized in that the annealing process in S2 is carried out in a tubular resistance furnace, the atmosphere is air atmosphere, the temperature is 200-400 ℃, and the time is 1.5-2.5 h.
5. The NF @ MoO of claim 13A method for preparing a @ NiCo-LDH composite material, characterized in that Ni (NO) is described in S33)2·6H2O、Co(NO3)3·6H2O、NH4F. The molar feeding ratio of the urea is (1-3) to (2-4) to (5-10).
6. The NF @ MoO of claim 13The preparation method of the @ NiCo-LDH composite material is characterized in that the temperature of the hydrothermal reaction in S3 is 120-180 ℃, and the time is 6-8 h.
7. The NF @ MoO of claim 13The preparation method of the @ NiCo-LDH composite material is characterized in that the drying processes in S2 and S3 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 hours.
8. NF @ MoO obtained by the production method according to any one of claims 1 to 73@ NiCo-LDH composite materials.
9. The NF @ MoO of claim 83The application of the @ NiCo-LDH composite material in the super capacitor is characterized in that NF @ MoO is used3Grinding the @ NiCo-LDH composite material, uniformly mixing the ground material with carbon black and polytetrafluoroethylene, and then pressing the mixture on a foam nickel sheet to obtain the working electrode of the supercapacitor.
10. The NF @ MoO of claim 93The application of the @ NiCo-LDH composite material in the supercapacitor is characterized in that NF @ MoO in the working electrode3The 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.
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