CN110323081B - Method for preparing nickel hydroxide/basic cobaltous carbonate composite material on current collector - Google Patents
Method for preparing nickel hydroxide/basic cobaltous carbonate composite material on current collector 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
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of preparation of inorganic materials, and particularly relates to a method for directly preparing nickel hydroxide/basic cobaltous carbonate Ni (OH) on a current collector2/Co2(CO3)(OH)2The method for compounding the electrode material can be directly used as an electrode of a super capacitor, and has good specific capacity and excellent cycling stability. According to the invention, firstly, a nickel hydroxide nanoparticle layer is precipitated and grown on the inner surface and the outer surface of the current collector, so that the firmness of the active material and the surface of the current collector is improved, a seed crystal material is provided for a composite material grown on the nickel hydroxide nanoparticle layer by hydrothermal method in the second step, and the stability of the composite material on the surface of a current collector skeleton structure is ensured; then in the second hydrothermal reaction synthesis process, by strictly controlling the proportion between Ni ions and Co ions, the finally synthesized composite material is uniformly distributed on the surface of nickel hydroxide nano particles of the framework inside and outside the current collector sheet, and presents a spherical structure, and the spheres are tightly connected with each other, so that the specific capacity of the capacitor can be effectively improved.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic materials, and particularly relates to a method for directly preparing nickel hydroxide/basic cobaltous carbonate (Ni (OH)) on a current collector2/Co2(CO3)(OH)2) The method for compounding the electrode material can be directly used as an electrode of a super capacitor, and has good specific capacity and excellent cycling stability.
Background
The super capacitor is a promising electrochemical energy storage device, has a fast charge and discharge speed, but has a low specific capacity. The specific capacity of a supercapacitor is largely determined by the electrochemical properties of the electrode material. In order to realize wide practical application of the supercapacitor, it is crucial to prepare an electrode material having excellent electrochemical properties. The nickel and cobalt oxide or hydroxide electrode material has high specific capacity, and the morphology, size, specific surface area, surface property and the like of the electrode material are important factors influencing the electrochemical properties of the electrode material. Generally, the electrode material with a multilevel structure with a large specific surface area is beneficial to the contact between the electrolyte and the active surface of the electrolyte, so that the redox reaction is generated, and high specific capacity can be obtained.
The manufacturing process of the electrode of the super capacitor also has great influence on the specific capacity of the super capacitor, and at present, two methods exist: coating methods and direct growth methods.
The coating method is that firstly, nickel and cobalt oxide or hydroxide active materials are prepared, then the active materials, conductive agents (such as carbon black) and binding agents are fully mixed, and the mixture is coated on a current collector (such as a foamed nickel sheet, a stainless steel net, a carbon cloth and the like). For example, patent 201210359037.4 discloses a nickel-cobalt double metal hydroxide hollow microsphere powder prepared by using a silica template, and the electrode is prepared by coating the hollow microsphere powder with the nickel-cobalt double metal hydroxide. However, the material coated on the current collector is easily agglomerated, it is difficult to achieve sufficient coating on the inner and outer surfaces of the current collector, which is not favorable for contact with the electrolyte, and the agglomerated active material is easily released from the current collector, resulting in degradation of capacity and cycle performance.
The direct growth method is to directly grow nickel, cobalt oxide or hydroxide active materials on a current collector without a conductive agent and a binder, so that the specific capacity of the capacitor can be improved. Compared with a coating method, the active material directly grown on the current collector has good dispersibility, is dispersed on the surface and each position inside the current collector, has large effective use area, can be fully contacted with electrolyte to generate electrochemical oxidation-reduction reaction, and thus can obtain high specific capacity.
However, the traditional hydrothermal direct growth method easily leads the active material to grow and accumulate too much on the surface of the current collector, has poor porosity, is not beneficial to the further permeation of the electrolyte in the active material, and influences the capacity of the capacitor. Meanwhile, the active material may fall off from the surface of the current collector during long-term charge and discharge, so that the firmness of the active material and the surface of the current collector needs to be further improved.
Disclosure of Invention
Aiming at the problems or the defects, the invention provides a method for preparing a nickel hydroxide/basic cobaltous carbonate composite electrode material on a current collector, which is directly used as a high-capacity supercapacitor electrode, in order to solve the problems of capacity and firmness in the preparation of a capacitor electrode by the conventional hydrothermal direct growth method.
The preparation method comprises the following specific steps:
step 1, ultrasonically washing a current collector (a foam nickel sheet, a stainless steel net, a carbon cloth and the like) by sequentially adopting 1-5 mol/L hydrochloric acid solution, ethanol and deionized water to obtain a current collector sheet A with a pure surface.
Step 2, adding Ni (NO)3)2.6H2O and CO (NH)2)2Respectively adding the mixture into deionized water, and stirring for 3-10 minutes to obtain reaction solutions. Ni (NO) in reaction solution3)2.6H2O concentration of 0.05-0.10 mol/L, CO (NH)2)2The concentration is 0.10-0.30 mol/L. Ni (NO)3)2.6H2O and CO (NH)2)2Is 1: 1-1: 6.
and 3, transferring the reaction solution prepared in the step 2 into a hydrothermal kettle, then putting the cleaned current collector piece A into the hydrothermal kettle, sealing the hydrothermal kettle, and carrying out hydrothermal reaction at the temperature of 80-120 ℃ for 10-15 hours (h).
And 4, respectively cleaning the current collector sheet prepared in the step 3 by using deionized water and absolute ethyl alcohol, and drying at 60-110 ℃ for 2-5h to obtain a current collector sheet B with a nickel hydroxide nanoparticle layer attached to the surface.
Step 5, adding Co (NO)3)2.6H2O、Ni(NO3)2.6H2O, Urea (CO (NH)2)2) And Cetyl Trimethyl Ammonium Bromide (CTAB) are sequentially added into water, stirred and dissolved sufficiently to obtain a reaction solution. Co (NO) in the reaction solution3)2.6H2O concentration of 0.01 to 0.03mol/L, Ni (NO)3)2.6H2O concentration of 0.01 to 0.03mol/L, CO (NH)2)2The concentration is 0.10-0.30 mol/L, and the CTAB concentration is 0.005-0.01 mol/L. Added Co (NO)3)2.6H2O and Ni (NO)3)2.6H2The molar ratio of O is 1: 0.5-1: 2. total molar amount of nickel and cobalt and CO (NH)2)2The ratio of (1): 3-1: 10. the total molar amount of nickel and cobalt and the ratio of CTAB was 1: 0.1-1: 0.5.
and 6, transferring the reaction solution prepared in the step 5 into a hydrothermal kettle, then putting the current collector sheet B with the surface attached with the nickel hydroxide nanoparticle layer prepared in the step 4, sealing, and carrying out hydrothermal reaction for 8-12 h at 100-140 ℃.
Step 7, cleaning the current collector sheet obtained in the step 6 by using deionized water and absolute ethyl alcohol respectively, and then drying the current collector sheet in vacuum at 50-100 ℃ for 6-12 h to obtain the current collector sheet with the surface attached with Ni (OH)2/Co2(CO3)(OH)2A current collector sheet of composite material.
The invention adopts a two-step hydrothermal method to directly grow an active material on the surface of a current collector to be used as a super capacitor electrode. And growing a nano-particle layer on the surface of the current collector. Firstly, carrying out hydrothermal reaction on nickel nitrate and urea, and precipitating and growing a nickel hydroxide nanoparticle layer on the inner surface and the outer surface of a current collector, wherein the particle diameter is 3-4 microns; the nanoparticle layer is tightly bonded to the inner and outer skeleton surfaces of the current collector, so that the firmness of the active material and the surface of the current collector is improved, the current collector is not easy to fall off, and the current collector is Ni (OH) hydrothermally grown on the nanoparticle layer in the second step2/Co2(CO3)(OH)2The composite material provides seed material while ensuring Ni (OH)2/Co2(CO3)(OH)2The stability of the composite structure material on the surface of the current collector skeleton structure is not easy to fall off.
Secondly, putting the current collector sheet with the nickel hydroxide nano particle layer on the surface into a mixed solution of nickel nitrate, cobalt nitrate, urea and a surfactant Cetyl Trimethyl Ammonium Bromide (CTAB), performing a second hydrothermal reaction, and further growing Ni (OH) on the nickel hydroxide nano particle layer on the current collector2/Co2(CO3)(OH)2A composite material. By strictly controlling the ratio of Ni ions to Co ions in the synthesis process, finally synthesized Ni (OH)2/Co2(CO3)(OH)2The composite material is uniformly distributed on the surface of the framework inside and outside the current collector sheet, the current collector sheet presents a spherical structure, the size is uniform, the spheres are tightly connected, the surface of the current collector sheet is provided with dense nano-scale thorn-shaped objects, the length of the thorn-shaped objects is 0.5-1 micrometer, and the total diameter of the internal particles and the external thorn-shaped objects of the composite material is 4-6 micrometers. The active material composed of the thorn-shaped substance has loose inside and large effective use area, is beneficial to the full permeation of electrolyte, and thus can effectively improve the specific capacity of the capacitor.
The load prepared by the method of the invention is Ni (OH)2/Co2(CO3)(OH)2The direct application of the current collector sheet of the composite material to the positive electrode of the supercapacitor has the following three advantages: firstly, the nickel hydroxide nano layer is tightly combined with the surfaces of the inner and outer frameworks of the current collector, so that the whole material is not easy to fall off in the energy storage process, and the service life is prolonged; secondly, the thorn-shaped structure greatly increases the contact area with the electrolyte, is beneficial to the electrochemical oxidation-reduction reaction of the surface of the thorn-shaped structure, and experiments prove that the thorn-shaped structure can obtain high specific capacity and excellent stability; and thirdly, the current collector sheet loaded with the composite material can be directly used for a super capacitor electrode, so that the process of coating an active material on a current collector is avoided, and meanwhile, the use of a binder and a conductive agent is avoided. The method has the advantages of low cost, simple production process, strong controllability and easy industrial large-scale production.
Drawings
FIG. 1: example 1 prepared supporting Ni (OH)2/Co2(CO3)(OH)2Scanning electron microscope images of the foam nickel sheet of the composite material;
FIG. 2: example 1 preparation of Ni (OH)2/Co2(CO3)(OH)2Scanning electron micrographs of the composite.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
1.16g of nickel nitrate hexahydrate and 0.96g of urea are added into 80mL of deionized water, and are stirred to be completely dissolved, so that mixed solutions with the concentrations of 0.05mol/L of nickel nitrate hexahydrate and 0.20mol/L of urea are obtained. And (3) ultrasonically washing the foamed nickel sheet (3 x 5cm) by sequentially adopting 1-5 mol/L hydrochloric acid solution, ethanol and deionized water to obtain a clean foamed nickel sheet.
And transferring the obtained mixed solution and the foamed nickel sheet into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 12 hours at 100 ℃ to obtain the foamed nickel sheet with light green precipitates.
And (3) washing the light green foam nickel sheet subjected to the hydrothermal reaction with deionized water and ethanol for three times respectively, and then drying the light green foam nickel sheet in vacuum at the temperature of 60 ℃ for 12 hours. 0.29g of cobalt nitrate hexahydrate, 0.29g of nickel nitrate hexahydrate, 0.72g of urea and 0.15g of cetyltrimethylammonium bromide (CTAB) were added to 80mL of deionized water to obtain mixed solutions having concentrations of 0.0125mol/L of cobalt nitrate hexahydrate, 0.0125mol/L of nickel nitrate hexahydrate, 0.15mol/L of urea and 0.005mol/L of LCTAB, respectively.
And transferring the mixed solution and the light green foamed nickel sheet into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 120 ℃ for 10 hours to obtain the foamed nickel sheet attached with brown precipitate.
And (3) washing the brown foam nickel sheet subjected to the hydrothermal reaction with deionized water and ethanol for three times respectively, and then drying the brown foam nickel sheet at the temperature of 60 ℃ in vacuum for 12 hours. Obtaining Ni (OH) directly grown on the foam nickel2/Co2(CO3)(OH)2A composite material.
The finally prepared foam nickel sheet is used as a super capacitor electrode and is tested and found to be at 2mA/cm2The capacity of the capacitor reaches 1.79F/cm at the current density of2. After 1 ten thousand cycles, the specific capacity of the material still keeps 95.1 percent.
FIG. 1 shows Ni (OH) -loaded nanoparticles prepared in this example2/Co2(CO3)(OH)2Scanning electron microscope images of the foam nickel sheet of the composite material; FIG. 2 shows Ni (OH) prepared in this example2/Co2(CO3)(OH)2Scanning electron micrographs of the composite.
Therefore, the invention strictly controls the proportion of Ni ions and Co ions in the synthesis process to finally synthesize Ni (OH)2/Co2(CO3)(OH)2The composite material is uniformly distributed on the surface of nickel hydroxide nano particles of the framework inside and outside the current collector sheet, and presents a spherical structure with uniform size, the spheres are tightly connected, and the surface of the composite material is provided with dense nano-scale thorn-shaped objects. The active material composed of the thorn-shaped substance has loose inside and large effective use area, is beneficial to the full permeation of electrolyte, and thus can effectively improve the specific capacity of the capacitor.
Example 2
3.32g of nickel nitrate hexahydrate and 1.92g of urea are added into 80mL of deionized water, and are stirred to be completely dissolved, so that mixed solutions with the concentrations of 0.10mol/L of nickel nitrate hexahydrate and 0.40mol/L of urea are obtained. And (3) ultrasonically washing the foamed nickel sheet (3 x 5cm) by sequentially adopting 1-5 mol/L hydrochloric acid solution, ethanol and deionized water to obtain a clean foamed nickel sheet.
And transferring the obtained mixed solution and the foamed nickel sheet into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 12 hours at 100 ℃ to obtain the foamed nickel sheet with light green precipitates. And (3) washing the light green foam nickel sheet subjected to the hydrothermal reaction with deionized water and ethanol for three times respectively, and then drying the light green foam nickel sheet in vacuum at the temperature of 60 ℃ for 12 hours. 0.58g of cobalt nitrate hexahydrate, 0.58g of nickel nitrate hexahydrate, 1.74g of urea and 0.30g of cetyltrimethylammonium bromide (CTAB) were added to 80mL of deionized water to obtain mixed solutions having concentrations of 0.025mol/L of cobalt nitrate hexahydrate, 0.025mol/L of nickel nitrate hexahydrate, 0.30mol/L of urea and 0.01mol/L of LCTAB, respectively.
And transferring the mixed solution and the light green foamed nickel sheet into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 120 ℃ for 10 hours to obtain the foamed nickel sheet attached with brown precipitate. And (3) washing the brown foam nickel sheet subjected to the hydrothermal reaction with deionized water and ethanol for three times respectively, and then drying the brown foam nickel sheet at the temperature of 60 ℃ in vacuum for 12 hours. Obtaining Ni (OH) directly grown on the foam nickel2/Co2(CO3)(OH)2A composite material.
The foamed nickel sheet is used as an electrode test of a super capacitor and found to be at 2mA/cm2The capacity of the capacitor reaches 1.68F/cm at the current density of2. After 1 ten thousand cycles, the specific capacity of the material still keeps 94.2 percent.
Claims (1)
1. The method for preparing the nickel hydroxide/basic cobaltous carbonate composite electrode material on the current collector comprises the following specific steps:
step 1, ultrasonically washing a current collector by sequentially adopting 1-5 mol/L hydrochloric acid solution, ethanol and deionized water to obtain a current collector sheet A with a pure surface;
step 2, adding Ni (NO)3)2.6H2O and CO (NH)2)2Respectively adding the mixture into deionized water and stirring for 3-10 minutes to obtain reaction solution; ni (NO) in reaction solution3)2.6H2O concentration of 0.05-0.10 mol/L, CO (NH)2)2The concentration is 0.10-0.30 mol/L; ni (NO)3)2.6H2O and CO (NH)2)2Is 1: 1-1: 6;
step 3, transferring the reaction solution prepared in the step 2 into a hydrothermal kettle, then putting the cleaned current collector piece A into the hydrothermal kettle, sealing the hydrothermal kettle, and carrying out hydrothermal reaction at 80-120 ℃ for 10-15 hours;
step 4, respectively cleaning the current collector sheet prepared in the step 3 by using deionized water and absolute ethyl alcohol, and drying at 60-110 ℃ for 2-5h to obtain a current collector sheet B with a nickel hydroxide nanoparticle layer attached to the surface;
step 5, adding Co (NO)3)2.6H2O、Ni(NO3)2.6H2O, Urea CO (NH)2)2And Cetyl Trimethyl Ammonium Bromide (CTAB) are sequentially added into water and are fully stirred and dissolved to obtain a reaction solution; co (NO) in the reaction solution3)2.6H2O concentration of 0.01 to 0.03mol/L, Ni (NO)3)2.6H2O concentration of 0.01-0.03 mol/L, CO (NH)2)2The concentration is 0.10-0.30 mol/L, and the CTAB concentration of cetyl trimethyl ammonium bromide0.005-0.01 mol/L; added Co (NO)3)2.6H2O and Ni (NO)3)2.6H2The molar ratio of O is 1: 0.5-1: 2, total molar amount of nickel and cobalt and CO (NH)2)2The ratio of (1): 3-1: 10, the total molar amount of nickel and cobalt and the ratio CTAB being 1: 0.1-1: 0.5;
step 6, transferring the reaction solution prepared in the step 5 into a hydrothermal kettle, then placing the current collector sheet B with the surface attached with the nickel hydroxide nanoparticle layer prepared in the step 4, sealing, and carrying out hydrothermal reaction for 8-12 h at 100-140 ℃;
step 7, cleaning the current collector sheet obtained in the step 6 by using deionized water and absolute ethyl alcohol respectively, and then drying the current collector sheet in vacuum at 50-100 ℃ for 6-12 h to obtain the current collector sheet with the surface attached with Ni (OH)2/Co2(CO3)(OH)2A current collector sheet of composite material;
the current collector is foamed nickel, stainless steel mesh or carbon cloth;
the current collector sheet B with the nickel hydroxide nanoparticle layer attached to the surface, obtained in the step 4, is tightly combined on the surfaces of the inner and outer frameworks of the current collector, so that the firmness of the active material and the surface of the current collector is improved, and the current collector sheet B is not easy to fall off; and Ni (OH) hydrothermally grown thereon for the second step2/Co2(CO3)(OH)2The composite provides a seed material while retaining Ni (OH)2/Co2(CO3)(OH)2The stability of the composite structure material on the surface of a current collector skeleton structure is not easy to fall off, and the diameter of the nickel hydroxide nano-particles is 3-4 microns;
finally obtained Ni (OH)2/Co2(CO3)(OH)2The composite material is uniformly distributed on the surface of the framework inside and outside the current collector sheet, the current collector sheet presents a spherical structure, the size is uniform, the spheres are tightly connected, the surface of the current collector sheet is provided with dense nano-scale thorn-shaped objects, the length of the thorn-shaped objects is 0.5-1 micron, the total diameter of the inner particles and the outer thorn-shaped objects of the composite material is 4-6 microns, and the composite material can be directly used as an electrode of a super capacitor.
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| CN110335760B (en) * | 2019-04-30 | 2021-02-02 | 安徽大学 | Preparation method of nickel-doped banded nano basic cobalt carbonate electrode material |
| CN111370782B (en) * | 2020-03-20 | 2023-09-19 | 湖南源达新材料有限公司 | Polymer electrolyte for zinc-nickel battery, zinc-nickel battery and preparation method of polymer electrolyte |
| CN111627720B (en) * | 2020-06-19 | 2021-10-01 | 太原理工大学 | Ni-doped composite electrode material and preparation method thereof |
| CN114180645A (en) * | 2020-09-15 | 2022-03-15 | 香港城市大学深圳研究院 | Multi-metal hydroxide and preparation method and application thereof |
| CN112133570A (en) * | 2020-09-17 | 2020-12-25 | 吉林化工学院 | Co9S8Preparation method of/Ni-Co-Mo oxyhydroxide hollow core-shell electrode material |
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