CN108899222B - Preparation method of supercapacitor electrode material - Google Patents

Preparation method of supercapacitor electrode material Download PDF

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CN108899222B
CN108899222B CN201810672662.1A CN201810672662A CN108899222B CN 108899222 B CN108899222 B CN 108899222B CN 201810672662 A CN201810672662 A CN 201810672662A CN 108899222 B CN108899222 B CN 108899222B
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electrode material
copper
nickel
foamed
foam
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CN108899222A (en
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朱挺
刘亚东
刘国强
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Central South University
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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
    • 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
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • 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
    • 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 discloses a preparation method of a super capacitor electrode material, which comprises the following steps: (1) pretreating foamed nickel and foamed copper; (2) and carrying out hydrothermal reaction on the pretreated nickel foam, copper foam and thiourea solution at the temperature of 140-160 ℃, reacting for 5-9h, cooling, cleaning and drying to obtain the supercapacitor electrode material. According to the supercapacitor electrode material produced by the reaction, copper ions are doped in one step, so that the conductivity of the prepared electrode material is enhanced, the specific capacity of the electrode material is improved, and the produced 3D nano flaky structures are staggered and interconnected, so that the supercapacitor electrode material has high mechanical stability, can not easily fall off in the circulation process, keeps the structural stability of the material, enhances the circulation stability, and has good capacity retention rate.

Description

Preparation method of supercapacitor electrode material
Technical Field
The invention belongs to the field of electrode materials, and particularly relates to a preparation method of a super capacitor electrode material with a multistage nanostructure.
Background
Along with the change of energy consumption modes brought by rapid development of science and technology and the requirement of human beings on high-quality living environment, various novel electronic science and technology products and environment-friendly vehicles rapidly enter the daily life of people, and therefore important research is carried out on energy storage elements which can meet the requirements of people on high power energy density, long cycle life and rapid charging and discharging.
The super capacitor is a novel rapid energy storage device which can discharge in a large current, is green and environment-friendly and has excellent performance, and receives great attention from various countries.
The traditional capacitor electrode material is usually prepared by a coating method, and an active material is usually coated on an electrode current collector through an organic adhesive, but the use of the organic adhesive often causes low electrode conductivity and high internal resistance of the prepared material, and active substances fall off in a circulation process to cause poor circulation stability and limit the use of the prepared material.
Recently, methods such as post-vulcanization or step-by-step vulcanization of an electrodeposited electrode current collector substrate are reported to be adopted for preparing electrode materials, but the preparation process is too complicated, the electrode conductivity is not high, and the application of the electrode material is influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background technology, and provide a method for preparing a super capacitor electrode material with a multistage nano structure by directly doping in one step through a codeposition method.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper;
(2) and carrying out hydrothermal reaction on the pretreated nickel foam, copper foam and thiourea solution at the temperature of 140-160 ℃, reacting for 5-9h, cooling, cleaning and drying to obtain the supercapacitor electrode material.
In the preparation method, preferably, in the step (2), the thiourea solution is a mixed solution of thiourea, absolute ethyl alcohol and deionized water; the concentration of the thiourea solution is 1.5-3.5 mg/mL. Deionized water and absolute ethyl alcohol are selected as solvents to dissolve a sulfur source (thiourea), the deionized water mainly dissolves the sulfur source (thiourea), and the absolute ethyl alcohol can also serve as a dispersing agent in the whole reaction system, so that nickel sulfide generated by the reaction is distributed more uniformly. The inventors found that if a sample is produced using a single deionized water as a solvent, nickel sulfide agglomerated nanospheres are formed; if other solvents are adopted or absolute ethyl alcohol is adopted alone, the supercapacitor material with the nano flaky structure is difficult to form.
In the above preparation method, preferably, the volume ratio of the absolute ethyl alcohol to the deionized water in the thiourea solution is 3: 1.
in the preparation method, preferably, the pretreatment process of the foamed nickel and the foamed copper is as follows: the pretreatment process of the foamed nickel and the foamed copper is specifically as follows: respectively putting the foam copper and the foam nickel into 0.5-1mol/L hydrochloric acid for ultrasonic treatment for 5-10min, taking out, cleaning with deionized water for several times, and then putting into acetone for ultrasonic treatment for 5-10 min; performing ultrasonic treatment on the foamed nickel subjected to the ultrasonic treatment by acetone for 3-4 times by using absolute ethyl alcohol, and performing ultrasonic treatment on the foamed copper subjected to the ultrasonic treatment by acetone for 3-4 times by using deionized water; and (5) drying in vacuum to finish pretreatment.
In the preparation method, preferably, the electrode material of the supercapacitor is of a nano-sheet structure.
In the preparation method, preferably, the supercapacitor electrode material is formed by in-situ growth of nickel-copper complex sulfide on a foamed nickel substrate.
In the preparation method, the foam nickel is not only used as a substrate (current collector), but also used as a nickel source; the foam copper is mainly used as a copper source, the conductivity of the copper is excellent, and the performance of the electrode material capacitor can be greatly improved by doping a proper amount of copper ions. The applicant finds that in the preparation process of the composite material, if copper salt is selected as a copper source, copper sulfide can be directly generated in the stirring process of the solution, and a large amount of copper sulfide can deposit on the surface of the foamed nickel, so that the reaction of the foamed nickel and a sulfur source is prevented, and the appearance of a sample is damaged.
According to the invention, a one-step vulcanization method is adopted, the copper-nickel ion exchange is carried out to obtain the composite electrode material with low resistivity and good cycle reversibility by utilizing the difference of solubility product constants of nickel sulfide and copper sulfide and excellent conductivity of copper ions after copper sulfide and nickel sulfide products are generated, the composite electrode material can be directly used as an electrode material of a capacitor, and the experimental process is simple and convenient to operate and high in repeatability.
The invention mechanism of the invention is:
(1) firstly, nickel sulfide is generated on the surface of the foam nickel and copper sulfide is generated on the surface of the foam copper in the reaction process, and copper ions in the copper sulfide replace nickel ions in the nickel sulfide to form a nickel-copper composite sulfide due to different solubility product constants of the nickel sulfide and the copper sulfide, so that the nickel-copper composite sulfide has stronger conductivity and redox activity;
(2) the electrode material of the super capacitor is a multi-stage nano structure formed by the interactive connection of nano-sheets directly growing on a foamed nickel substrate and nano-holes; the nickel-copper complex sulfide generated by the reaction is directly arranged on the foamed nickel substrate, so that the foamed nickel substrate has good mechanical stability and electrical conductivity.
Compared with the prior art, the invention has the advantages that:
(1) the electrode material of the super capacitor has a multi-stage 3D nano sheet structure, so that the specific surface area of the material is increased, more reactive active sites are provided, and the specific capacitance of the material is improved.
(2) According to the supercapacitor electrode material produced by the reaction, copper ions are doped in one step, so that the conductivity of the prepared electrode material is enhanced, the specific capacity of the electrode material is improved, and the produced 3D nano flaky structures are staggered and interconnected, so that the supercapacitor electrode material has high mechanical stability, can not easily fall off in the circulation process, keeps the structural stability of the material, enhances the circulation stability, and has good capacity retention rate.
(3) The product copper sulfide generated by the foam copper can be combined with the electrode material of the super capacitor to form the double-electrode asymmetric capacitor for use.
(4) The preparation method is simple, convenient and feasible, convenient to operate and high in repetition rate, and the active substance copper sulfide/nickel sulfide grows on the foam nickel substrate in situ and can be directly used as an electrode.
Drawings
Fig. 1 is an XRD pattern of the supercapacitor electrode material prepared in example 1 of the present invention.
Fig. 2 is an SEM image of the supercapacitor electrode material prepared in example 1 of the present invention.
FIG. 3 is a cyclic voltammogram of the electrode material of the supercapacitor prepared in example 1 of the present invention.
Fig. 4 is a graph showing the result of the charge and discharge performance test of the supercapacitor electrode material prepared in example 1 of the present invention.
Fig. 5 is a graph showing the results of the cycle stability test of the supercapacitor electrode material prepared in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper: cutting foamed nickel into 1cm x 3cm, cutting foamed copper into 1cm x 1cm, respectively putting the foamed copper and the foamed nickel into 1mol/L hydrochloric acid for ultrasonic treatment for 5min, taking out, cleaning with deionized water for several times, putting into acetone for ultrasonic treatment for 5min, finally, respectively performing ultrasonic treatment on the foamed nickel and the foamed copper with absolute ethyl alcohol and deionized water for 3-4 times, and drying in a vacuum drying oven at 50 ℃;
(2) weighing 60mg of thiourea, adding the thiourea into 20mL of mixed solution of absolute ethyl alcohol and deionized water in a ratio of 3:1, and uniformly stirring to obtain thiourea solution;
(3) transferring the pretreated foam nickel, foam copper and thiourea solution to a polytetrafluoroethylene stainless steel reaction kettle, and carrying out hydrothermal reaction for 6 hours at 150 ℃; and after the reaction is finished, naturally cooling the reaction solution to room temperature, taking out a sample, repeatedly washing the sample by using deionized water and absolute ethyl alcohol for multiple times, and drying the sample in a 50 ℃ oven for 12 hours to obtain the supercapacitor electrode material (the nickel-copper composite sulfide/foamed nickel electrode material with the multilevel structure).
FIG. 1 is an X-ray diffraction (XRD) spectrum of the electrode material for the supercapacitor prepared in this example, from which it can be seen that sharp diffraction peaks are from metallic nickel, and relatively weak diffraction peaks are compared with standard PDF card, corresponding to Ni respectively3S2And CuS2The diffraction peak of (1).
Fig. 2 is a Scanning Electron Microscope (SEM) spectrum of the supercapacitor electrode material prepared in this example. As can be seen from the figure, the electrode material is formed by the interactive connection and assembly of nano sheets and nano-scale micropores, wherein the nano sheets are directly grown on a foam nickel substrate, the thickness of the nano sheets is dozens of nanometers, and the nano sheets and the nano-scale micropores form a 3D nano flaky structure.
Fig. 3 is a cyclic voltammogram of the electrode material of the supercapacitor prepared in this example. As can be seen from the figure, under the voltage window of 0V-0.6V, different sweep rates all have oxidation reduction peaks, and as the sweep rate is increased, the closed area is increased, and the specific capacitance is improved.
Fig. 4 shows the result of the charge and discharge performance test of the supercapacitor electrode material prepared in this example. As can be seen from the figure, the electrode material of the super capacitor with the multilevel structure is 1A g-1，2A g-1，3A g-1，5A g-1，10A g-11657F g for specific capacitance-1，1384F g-1，1165F g-1，823F g-1，608F g-1。
Fig. 5 shows the result of the cycling stability test of the electrode material of the supercapacitor prepared in this example. As can be seen, at a current density of 10A g-1Under the condition of (1), the capacity of 10000 cycles of charge-discharge cycle can still be kept at 540F g-1。
Example 2:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper: cutting foamed nickel into 1cm x 3cm, cutting foamed copper into 1cm x 1cm, respectively putting the foamed copper and the foamed nickel into 1mol/L hydrochloric acid for ultrasonic treatment for 5min, taking out, cleaning with deionized water for several times, putting into acetone for ultrasonic treatment for 5min, finally, respectively performing ultrasonic treatment on the foamed nickel and the foamed copper with absolute ethyl alcohol and deionized water for 3-4 times, and drying in a vacuum drying box at 50 ℃;
(2) weighing 45mg of thiourea, adding the thiourea into 20mL of mixed solution of absolute ethyl alcohol and deionized water in a ratio of 3:1, and uniformly stirring to obtain thiourea solution;
(3) and transferring the pretreated nickel foam, copper foam and thiourea solution to a polytetrafluoroethylene stainless steel reaction kettle, carrying out hydrothermal reaction for 6 hours at 150 ℃, naturally cooling the reaction solution to room temperature after the reaction is finished, taking out a sample, repeatedly washing the sample with deionized water and absolute ethyl alcohol for multiple times, and drying the sample in a 50 ℃ oven for 12 hours to obtain the nickel-copper composite sulfide/foamed nickel electrode material with the multilevel structure.
Using the electrochemical Performance test method of example 1, the material of this example, when used as an electrode of a supercapacitor, was tested at 1A g-1Has a specific capacitance of 895F g-1(ii) a At 10A g-1The capacity can maintain 89% of the initial capacity after 10000 cycles of circulation under the current density.
Example 3:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper: cutting foamed nickel into 1cm x 3cm, cutting foamed copper into 1cm x 1cm, respectively adding foamed copper and foamed nickel into 1mol L-1Performing ultrasonic treatment in hydrochloric acid for 5min, taking out, cleaning with deionized water for several times, performing ultrasonic treatment in acetone for 5min, and finally performing ultrasonic treatment on the foamed nickel and the foamed copper for 3-4 times respectively with absolute ethyl alcohol and deionized water, and drying in a vacuum drying oven at 50 ℃;
(2) weighing 75mg of thiourea, adding the thiourea into 20mL of mixed solution of absolute ethyl alcohol and deionized water in a ratio of 3:1, and uniformly stirring to obtain thiourea solution;
(3) and transferring the pretreated nickel foam, copper foam and thiourea solution to a polytetrafluoroethylene stainless steel reaction kettle, carrying out hydrothermal reaction for 6 hours at 150 ℃, naturally cooling the reaction solution to room temperature after the reaction is finished, taking out a sample, repeatedly washing the sample with deionized water and absolute ethyl alcohol for multiple times, and drying the sample in a 50 ℃ oven for 12 hours to obtain the nickel-copper composite sulfide/foamed nickel electrode material with the multilevel structure.
When the copper sulfide/nickel foam material with a multilevel structure of the present example is used as an electrode of a supercapacitor by the electrochemical performance test method in example 1, the electrochemical performance test method is 1A g-1Has a specific capacitance of 1421F g-1(ii) a At 10Ag-1The capacity can maintain 90% of the initial capacity after 10000 cycles of circulation under the current density of (1).
Example 4:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper: cutting foamed nickel into 1cm x 3cm, cutting foamed copper into 1cm x 1cm, respectively putting the foamed copper and the foamed nickel into 1mol/L hydrochloric acid for ultrasonic treatment for 5min, taking out, cleaning with deionized water for several times, putting into acetone for ultrasonic treatment for 5min, finally, respectively performing ultrasonic treatment on the foamed nickel and the foamed copper with absolute ethyl alcohol and deionized water for 3-4 times, and drying in a vacuum drying oven at 50 ℃;
(2) weighing 60mg of thiourea, adding the thiourea into 20mL of mixed solution of absolute ethyl alcohol and deionized water in a ratio of 3:1, and uniformly stirring to form thiourea solution;
(3) and transferring the pretreated nickel foam, copper foam and thiourea solution to a polytetrafluoroethylene stainless steel reaction kettle, carrying out hydrothermal reaction for 9h at 150 ℃, naturally cooling the reaction solution to room temperature after the reaction is finished, taking out a sample, repeatedly washing the sample with deionized water and absolute ethyl alcohol for multiple times, and drying the sample in a 50 ℃ oven for 12h to obtain the nickel-copper composite sulfide/foamed nickel electrode material with the multilevel structure.
Using the electrochemical Performance test method of example 1, the material of this example, when used as an electrode of a supercapacitor, was tested at 1A g-1Has a specific capacitance of 1316F g-1(ii) a At 10A g-1The capacity can maintain 85% of the initial capacity after 10000 cycles of circulation under the current density of (1).
Example 5:
a preparation method of a supercapacitor electrode material comprises the following steps:
(1) pretreating foamed nickel and foamed copper: cutting foamed nickel into 1cm x 3cm, cutting foamed copper into 1cm x 1cm, respectively putting the foamed copper and the foamed nickel into 1mol/L hydrochloric acid for ultrasonic treatment for 5min, taking out, cleaning with deionized water for several times, putting into acetone for ultrasonic treatment for 5min, finally, respectively performing ultrasonic treatment on the foamed nickel and the foamed copper with absolute ethyl alcohol and deionized water for 3-4 times, and drying in a vacuum drying oven at 50 ℃;
(2) weighing 60mg of thiourea, adding the thiourea into 20mL of mixed solution of absolute ethyl alcohol and deionized water in a ratio of 3:1, and uniformly stirring to form thiourea solution;
(3) and transferring the pretreated nickel foam, copper foam and thiourea solution to a polytetrafluoroethylene stainless steel reaction kettle, carrying out hydrothermal reaction for 6h at 140 ℃, naturally cooling the reaction solution to room temperature after the reaction is finished, taking out a sample, repeatedly washing the sample with deionized water and absolute ethyl alcohol for multiple times, and drying the sample in a 50 ℃ oven for 12h to obtain the nickel-copper composite sulfide/foamed nickel electrode material with the multilevel structure.
Using the electrochemical Performance test method of example 1, the material of this example, when used as an electrode of a supercapacitor, was tested at 1A g-1Has a specific capacitance of 1251F g at a current density of-1(ii) a At 10A g-1The capacity can maintain 80% of the initial capacity after 10000 cycles of circulation under the current density of (1).

Claims (4)

1. A preparation method of a supercapacitor electrode material is characterized by comprising the following steps:
(1) pretreating foamed nickel and foamed copper;
(2) carrying out hydrothermal reaction on the pretreated nickel foam, copper foam and thiourea solution at the temperature of 140-160 ℃, reacting for 5-9h, cooling, cleaning and drying to obtain the supercapacitor electrode material, wherein the prepared supercapacitor electrode material is in a nano sheet structure; wherein, the thiourea solution is a mixed solution of thiourea, absolute ethyl alcohol and deionized water; the concentration of the thiourea solution is 1.5-3.5 mg/mL.
2. The method of claim 1, wherein the volume ratio of absolute ethanol to deionized water in the thiourea solution is 3: 1.
3. the preparation method according to claim 1, wherein the pretreatment process of the nickel foam and the copper foam is specifically as follows: respectively putting the foam copper and the foam nickel into 0.5-1mol/L hydrochloric acid for ultrasonic treatment for 5-10min, taking out, cleaning with deionized water for several times, and then putting into acetone for ultrasonic treatment for 5-10 min; performing ultrasonic treatment on the foamed nickel subjected to the ultrasonic treatment by acetone for 3-4 times by using absolute ethyl alcohol, and performing ultrasonic treatment on the foamed copper subjected to the ultrasonic treatment by acetone for 3-4 times by using deionized water; and (5) drying in vacuum to finish pretreatment.
4. The method of any one of claims 1-3, wherein the supercapacitor electrode material is formed from in situ growth of nickel copper sulfide complex on a foamed nickel substrate.
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CN110461137B (en) * 2019-07-31 2020-09-22 西北工业大学 Three-dimensional foam type composite wave-absorbing material and preparation method thereof
CN110504109A (en) * 2019-08-30 2019-11-26 广东工业大学 A kind of electrode material based on fiber line and preparation method thereof and wearable supercapacitor
CN110752096B (en) * 2019-10-25 2021-11-23 青岛科技大学 Multi-dimensional structure Ni3S2/Co3S4Preparation of (A) and application in a supercapacitor
CN110867326B (en) * 2019-11-19 2023-12-19 上海季丰电子股份有限公司 Copper sulfide-foam nickel three-dimensional composite material and preparation method thereof
CN113299491B (en) * 2021-05-31 2022-06-21 中南大学 Photo-thermal enhanced supercapacitor electrode material and preparation method thereof

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