CN111816454A - Foamed nickel loaded NiCo2V2O8Method for assembling flexible supercapacitor - Google Patents
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- 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
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
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- 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
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Abstract
The invention discloses a foam nickel loaded NiCo2V2O8Method for assembling a flexible supercapacitor, the method comprising the steps of 1) preparing NiCo2V2O8A positive electrode material: 2) preparing PVA/KOH gel electrolyte; 3) and assembling the all-solid-state flexible supercapacitor. The preparation method is simple and has low cost. The prepared super capacitor anode material has higher area specific capacityAnd power density, showing good electrochemical performance. And NiCo is constructed on the surface of the foam nickel template for the first time2V2O8The material is innovative; good electrochemical performance and practicability.
Description
Technical Field
The invention belongs to the technical field of synthesis of cathode materials of supercapacitors, and relates to a method for constructing NiCo based on a foamed nickel template2V2O8A method for preparing a layered structure.
Background
With the widespread use of global electronic devices and the increase of energy consumption, research and development of flexible energy storage devices become a research hotspot. Currently, flexible all-solid-state supercapacitors are considered as one of the candidates for energy storage components for portable electronic devices. The research shows that: the super capacitor has the advantages of high power density, long service life, quick charge and discharge and the like; the flexible all-solid-state supercapacitor has the advantages of being light, easy to fold, flexible to attach to any surface and the like, and has application value in the field of intelligent wearable.
The preparation method of the ternary transition metal vanadium-based oxide used for the positive electrode material of the supercapacitor has been reported in documents, but the report of the ternary transition metal vanadium-based oxide used for a flexible supercapacitor system is very little. Hydrothermal method for constructing NiCo on foamed nickel mould2V2O8The nano-sheet array realizes the high specific surface area of the material and improves the specific capacitance; the abundant mesopores uniformly distributed between the interconnected particles further accelerate electron transport and ion diffusion. In addition to this, for quaternary NiCo2V2O8The preparation of the oxide and the flexible electrochemical energy storage performance thereof are hardly reported.
Disclosure of Invention
The invention aims to provide a method for constructing NiCo based on a foam nickel template2V2O8The material is used for a preparation method of the flexible super capacitor. The cathode material is green, environmentally friendly, and has high specific surface area and high conductivity, high power density and area compared to other cathode materials grown in situSpecific capacity. Indicating that the high-power high-safety high.
The purpose of the invention is solved by the following technical scheme:
foamed nickel loaded NiCo2V2O8A method for assembling a flexible supercapacitor, comprising the steps of:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, the nickel foam (1 × 3cm) was immersed in acetone, HCl solution, and then dried in air, as sample a; 0.03-0.07 g of NiCl2·6H2O,0.08~0.12g CoCl2·6H2O and 0.03-0.05 g KVO3Dissolving the mixture in 5-30 ml of ultrapure water, and performing magnetic stirring at normal temperature until a dark red transparent solution is formed, and marking as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material.
2) Preparing PVA/KOH solid electrolyte:
dissolving 2-4 g of polyvinyl alcohol (PVA) in 20-40 mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 2-40 g of potassium hydroxide (KOH) into the dissolved PVA, performing magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to obtain the PVA-KOH gel electrolyte.
3)NiCo2V2O8Positive electrode material, PVA/KOH solid electrolyte and Activated Carbon (AC) assembled all-solid-state supercapacitor
Mixing NiCo2V2O8As a positive electrode material, the mass m (NiCo) of the required negative electrode AC is calculated according to the charge quantity transferred by the positive electrode and the negative electrode2V2O8): m (ac) ═ 1: 3.5-4.5, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
In the step 1), the molar ratio of the nickel chloride hexahydrate, the cobalt chloride hexahydrate and the potassium metavanadate is 1:2: 1.5.
In the step 2), the mass ratio of the polyvinyl alcohol (PVA), the potassium hydroxide (KOH) and the deionized water is 1:1: 10.
In step 3), the positive electrode NiCo2V2O8The mass ratio of the material to the negative electrode AC material was 1: 3.8.
The invention has the following beneficial effects:
the invention relates to a method for constructing NiCo based on a foam nickel template2V2O8A method for preparing a lamellar structure. The preparation method is simple and has low cost. The prepared flexible supercapacitor positive electrode material has high area specific capacity and power density and shows good electrochemical performance. And quaternary NiCo is synthesized on the surface of the foamed nickel for the first time2V2O8The lamellar structure has innovativeness; the material has good electrochemical performance and practicability.
Drawings
NiCo is known from FIG. 12V2O8Successfully loaded on the surface of the foamed nickel.
FIG. 2 shows NiCo on the surface of the foamed nickel2V2O8The structure is sheet-shaped, and the nano-sheets are distributed with uniform mesopores.
FIG. 3 shows NiCo2V2O8PVA/KOH, AC, and their Ragon curves.
Detailed Description
Referring to FIG. 1, NiCo2V2O8And calcined NiCo2V2O8Diffraction peaks at 29.8 °,35.4 ° and 63.5 ° with orthorhombic Co3V2O8Phase (JCPDS 74-1487) or orthorhombic Ni3V2O8The phase (JCPDS 74-1484) is similar. From this, NiCo is known2V2O8Successfully loaded on NiCo2S4A surface.
Referring to FIG. 2, NiCo2V2O8The nano sheets are uniformly covered on the surface of the foamed nickel and are mutually stacked to form a nano flower, and the interior of the nano sheets are mutually connected to enable the nano sheet array which is orderly arranged to present the characteristics of a highly open and porous structure.
Referring to FIG. 3, (a) represents the Ragon curve for an all-solid ASC device at 16.89Wh kg-1The power density of the energy density of the power generator can reach 400.03W kg-1And at a high power density of 4000.8W kg-1The energy density can be maintained at 5.438Wh kg-1And (b) and (c) are physical photographs of all-solid-state ASC devices, and it was found that the devices could be bent 180 °, indicating their better flexibility.
Example 1:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, the nickel foam (1 × 3cm) was immersed in acetone, HCl solution, and then dried in air, as sample a; 0.0507g of NiCl2·6H2O,0.1019g CoCl2·6H2O and 0.044g KVO3Dissolving the mixture in 15mL of ultrapure water, and magnetically stirring the mixture at normal temperature until a dark red transparent solution is formed and is marked as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material.
2) Preparing PVA/KOH solid electrolyte:
dissolving 3g of polyvinyl alcohol (PVA) in 30mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 3g of potassium hydroxide (KOH) into the dissolved PVA for magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to be used as PVA-KOH gel electrolyte.
3)NiCo2V2O8Positive electrode material, PVA/KOH solid electrolyte and Activated Carbon (AC) assembled all-solid-state supercapacitor
Mixing NiCo2V2O8As a positive electrode material, the mass m (NiCo) of the required negative electrode AC is calculated according to the charge quantity transferred by the positive electrode and the negative electrode2V2O8): m (ac) ═ 1:3.8, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
Example 2:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, the nickel foam (1 × 3cm) was immersed in acetone, HCl solution, and then dried in air, as sample a; 0.114g of NiCl2·6H2O,0.2038g CoCl2·6H2O and 0.088g KVO3Dissolving the mixture in 15mL of ultrapure water, and magnetically stirring the mixture at normal temperature until a dark red transparent solution is formed and is marked as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material.
2) Preparing PVA/KOH solid electrolyte:
dissolving 3g of polyvinyl alcohol (PVA) in 30mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 3g of potassium hydroxide (KOH) into the dissolved PVA for magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to be used as PVA-KOH gel electrolyte.
3)NiCo2V2O8Positive electrode material, PVA/KOH solid electrolyte and Activated Carbon (AC) assembled all-solid-state supercapacitor
Mixing NiCo2V2O8As a positive electrode material, the mass m (NiCo) of the required negative electrode AC is calculated according to the charge quantity transferred by the positive electrode and the negative electrode2V2O8): m (ac) ═ 1:3.8, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
Example 3:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, the nickel foam (1 × 3cm) was immersed in acetone, HCl solution, and then dried in air, as sample a; 0.0507g of NiCl2·6H2O,0.1019g CoCl2·6H2O and 0.044g KVO3Dissolving the mixture in 15mL of ultrapure water, and magnetically stirring the mixture at normal temperature until a dark red transparent solution is formed and is marked as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material.
2) Preparing PVA/KOH solid electrolyte:
dissolving 4g of polyvinyl alcohol (PVA) in 30mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 3g of potassium hydroxide (KOH) into the dissolved PVA for magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to be used as PVA-KOH gel electrolyte.
3)NiCo2V2O8Positive electrode material, PVA/KOH solid electrolyte and Activated Carbon (AC) assembled all-solid-state supercapacitor
Mixing NiCo2V2O8As a positive electrode material, the mass m (NiCo) of the required negative electrode AC is calculated according to the charge quantity transferred by the positive electrode and the negative electrode2V2O8): m (ac) ═ 1:3.8, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
Example 4:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, the nickel foam (1 × 3cm) was immersed in acetone, HCl solution, and then dried in air, as sample a; 0.0507g of NiCl2·6H2O,0.1019g CoCl2·6H2O and 0.044g KVO3Dissolving the mixture in 15mL of ultrapure water, and magnetically stirring the mixture at normal temperature until a dark red transparent solution is formed and is marked as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material.
2) Preparing PVA/KOH solid electrolyte:
dissolving 3g of polyvinyl alcohol (PVA) in 30mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 3g of potassium hydroxide (KOH) into the dissolved PVA for magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to be used as PVA-KOH gel electrolyte.
3)NiCo2V2O8Positive electrode material, PVA/KOH solid electrolyte and Activated Carbon (AC) assembled all-solid-state supercapacitor
Mixing NiCo2V2O8As a positive electrode material, the mass m (NiCo) of the required negative electrode AC is calculated according to the charge quantity transferred by the positive electrode and the negative electrode2V2O8): m (ac) ═ 1: 4, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
Claims (4)
1. Foamed nickel loaded NiCo2V2O8A method for assembling a flexible supercapacitor, comprising the steps of:
1) preparation of NiCo2V2O8A positive electrode material:
before synthesis, sequentially immersing foamed nickel of 1 multiplied by 3cm into acetone and HCl solution, and then drying in the air, and marking as a sample A; 0.03-0.07 g of NiCl2·6H2O,0.08~0.12g CoCl2·6H2O and 0.03-0.05 g KVO3Dissolving the mixture in 5-30 ml of ultrapure water, and performing magnetic stirring at normal temperature until a dark red transparent solution is formed, and marking as a solution B; simultaneously transferring the sample A and the solution B into a 10-50 ml high-pressure autoclave with a polytetrafluoroethylene lining, keeping the high-pressure autoclave at the temperature of 120-160 ℃ for 9-15 hours, naturally cooling the high-pressure autoclave to room temperature, and obtaining the NiCo loaded with foamed nickel2V2O8Ultrasonically washing the sample C for 3 times by using ultrapure water and ethanol, and drying the washed sample C; collecting the prepared foam nickel sample, drying the foam nickel sample at 50-70 ℃ in vacuum overnight, recording the dried foam nickel sample as a sample D, and preparing NiCo with a sheet structure2V2O8A material;
2) preparing PVA/KOH solid electrolyte:
dissolving 2-4 g of polyvinyl alcohol (PVA) in 20-40 mL of deionized water, heating in a water bath until the PVA is completely dissolved, adding 2-40 g of potassium hydroxide (KOH) into the dissolved PVA for magnetic stirring until a transparent mixed solution is formed, and cooling to a gel state at room temperature to obtain PVA-KOH gel electrolyte;
3)NiCo2V2O8the positive electrode material, PVA/KOH solid electrolyte and active carbon AC are assembled into the all-solid-state supercapacitor, and NiCo is added into the all-solid-state supercapacitor2V2O8As the anode material, the mass m (NiCo) of the required cathode active carbon AC is calculated according to the charge quantity transferred by the anode and the cathode2V2O8): m (ac) ═ 1: 3.5-4.5, mixing AC, PVDF and acetylene black in a ratio of 8: 1: mixing at a ratio of 1, adding NMP solution, grinding to uniformity, coating on a foamed nickel current collector, drying, and mixing with NiCo2V2O8The positive electrode material and the PVA/KOH gel electrolyte are assembled into the all-solid-state supercapacitor.
2. The method of claim 1, wherein: in the step 1), the molar ratio of the nickel chloride hexahydrate, the cobalt chloride hexahydrate and the potassium metavanadate is 1:2: 1.5.
3. The method of claim 1, wherein: in the step 2), the mass ratio of the polyvinyl alcohol PVA to the potassium hydroxide KOH to the deionized water is 1:1: 10.
4. The method of claim 1, wherein: in step 3), the positive electrode NiCo2V2O8The mass ratio of the material to the negative active carbon AC material is 1: 3.8.
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CN113921290A (en) * | 2021-04-30 | 2022-01-11 | 惠州市钰芯电子材料有限公司 | Based on NiCo2O4Asymmetric all-solid-state supercapacitor with/Ni-P composite electrode and preparation method thereof |
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