CN108899222A - A kind of preparation method of electrode material for super capacitor - Google Patents
A kind of preparation method of electrode material for super capacitor Download PDFInfo
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- CN108899222A CN108899222A CN201810672662.1A CN201810672662A CN108899222A CN 108899222 A CN108899222 A CN 108899222A CN 201810672662 A CN201810672662 A CN 201810672662A CN 108899222 A CN108899222 A CN 108899222A
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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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- 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 kind of preparation methods of electrode material for super capacitor, include the following steps：(1) nickel foam and foam copper are pre-processed；(2) pretreated nickel foam, foam copper and thiourea solution are subjected at 140-160 DEG C hydro-thermal reaction, react 5-9h, cooling, cleaning is dried to get the electrode material for super capacitor is arrived.The present invention reacts the electrode material for super capacitor generated, one step of copper ion mixes so that preparing the enhancing of electrode material electric conductivity, its specific capacity is improved, and the 3D flaky nanometer structure generated staggeredly interconnects, with stronger mechanical stability, can electrode material is not easily to fall off in cyclic process, keep the structural stability of material, cyclical stability enhancing, has good capacity retention ratio.
Description
Technical field
The invention belongs to electrode material field more particularly to a kind of electrode of super capacitor materials with multi-level nano-structure
The preparation method of material.
Background technique
The transformation for rapidly developing bring energy-consuming mode with science and technology and the mankind are for high-quality life environment
It is required that various novel electronics technology products and daily life is quickly entered for the environmental-friendly vehicles,
Therefore for can satisfy the energy storage member that people's power energy density used in everyday is high, has extended cycle life, can be quickly charged and discharged
Part has carried out the research of emphasis.
Supercapacitor be grow up at present it is a kind of can instantaneous high-current discharge, it is environmentally protective, have excellent performance
Novel fast energy storage device receives the huge concern of various countries.
Traditional capacitor electrode material generallys use rubbing method to be prepared, and active material is usually passed through organic gel
Glutinous agent is coated on electrode current collecting body, but the use of Organic adhesive often result in prepare material electrode conductivity is low, internal resistance
Height, and in cyclic process active material fall off cause its cyclical stability difference and limit its use.
It is also had been reported that recently using electrodeposited electrode collector substrate after cure or is carried out using the methods of substep vulcanization
Electrode material is prepared, but preparation process is excessively cumbersome, and electrode conductivity is not high, influences its application.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Kind has the preparation method of the electrode material for super capacitor of multi-level nano-structure by the direct doping in one step preparation of co-electrodeposition method.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam and foam copper are pre-processed；
(2) pretreated nickel foam, foam copper and thiourea solution are subjected to hydro-thermal reaction in the case where being 140-160 DEG C, instead
5-9h is answered, cooling, cleaning is dried to get the electrode material for super capacitor is arrived.
Above-mentioned preparation method, it is preferred that in the step (2), thiourea solution refers to thiocarbamide and dehydrated alcohol, deionization
The mixed solution of water；The concentration of the thiourea solution is 1.5-3.5mg/mL.Select deionized water and dehydrated alcohol as solvent
It dissolves sulphur source (thiocarbamide), deionized water mainly dissolves sulphur source (thiocarbamide), dehydrated alcohol can also fill in entire reaction system
Work as dispersing agent, so that the distribution that the nickel sulfide of reaction generation is more uniform.Inventors have found that making according to single deionized water
Sample, which is generated, for solvent forms the nanosphere that nickel sulfide is reunited；It is formed according to other solvents or individually using dehydrated alcohol is difficult
The super capacitor material of flaky nanometer structure.
Above-mentioned preparation method, it is preferred that the volume ratio of dehydrated alcohol and deionized water is 3 in the thiourea solution：1.
Above-mentioned preparation method, it is preferred that nickel foam and foam copper progress preprocessing process are specially：Nickel foam and foam
Copper carries out preprocessing process：Foam copper and nickel foam are respectively put into ultrasound 5-10min in 0.5-1mol/L hydrochloric acid, taken
After out for several times using deionized water cleaning, then it is put in ultrasound 5-10min in acetone；It will be used by the nickel foam of acetone ultrasonic treatment
Dehydrated alcohol ultrasound 3-4 times, the foam copper by acetone ultrasonic treatment is with deionized water ultrasound 3-4 times；Vacuum drying is completed pre-
Processing.
Above-mentioned preparation method, it is preferred that the electrode material for super capacitor is flaky nanometer structure.
Above-mentioned preparation method, it is preferred that the electrode material for super capacitor is raw in situ by ambrose alloy complex sulfide
It is longer than and is formed in foam nickel base.
Nickel foam serves not only as substrate (collector) in preparation method of the invention, while being also nickel source；And foam copper master
If the excellent electric conductivity of copper is suitable copper ion doped greatly to improve the electrode material capacitor performance as copper source.
Applicant passes through the study found that in the preparation process of composite material, if selecting mantoquita for copper source, the meeting in solution whipping process
Copper sulfide is directly generated, copper sulfide can largely deposit foam nickel surface, and nickel foam is hindered to react with sulphur source and destroy sample topography.
The method that the present invention uses step vulcanization, it is excellent using the difference and copper ion of nickel sulfide and copper sulfide solubility product constant
Different electric conductivity, generate copper sulfide, vulcanization nickel product after cupro-nickel ion-exchange one-stage be prepared with low-resistivity, circulation can
The inverse good combination electrode material of property, can carry out directly as the electrode material of capacitor using experimentation is easy to operate and can
Repetitive rate is high.
Invention mechanism of the invention is：
(1) a step co-electrodeposition method is used, first in nickel foam Surface Creation nickel sulfide, foam copper surface first in reaction process
Copper sulfide is generated, since nickel sulfide and copper sulfide solubility product constant are different, copper ion in copper sulfide can be made to replace in nickel sulfide
Nickel ion forms ambrose alloy complex sulfide, so that it is with stronger electric conductivity and redox active；
(2) electrode material for super capacitor in the present invention is the nanoscale by being grown directly upon in foam nickel base
Multi-level nano-structure made of the hole of nanometer sheet and nanoscale interactive connection；It is direct to react the ambrose alloy complex sulfide generated
In foam nickel base, so that it is with good mechanical stability and electric conductivity.
Compared with the prior art, the advantages of the present invention are as follows：
(1) electrode material for super capacitor of the invention has multistage 3D flaky nanometer structure, so that material specific surface area
Increase and more reactivity sites are provided, so that the specific capacitance of material improves.
(2) electrode material for super capacitor that present invention reaction generates, one step of copper ion mix so that preparing electrode material
Electric conductivity enhancing, the 3D flaky nanometer structure that specific capacity is improved, and generates staggeredly interconnect, and have stronger mechanical steady
It is qualitative, can electrode material is not easily to fall off in cyclic process, keep the structural stability of material, cyclical stability enhancing, tool
There is good capacity retention ratio.
(3) the product copper sulfide that foam copper generates in the present invention can be formed with electrode material for super capacitor of the invention
Bipolar electrode asymmetric capacitor uses.
(4) preparation method of the present invention is simple and feasible, high convenient for operation, repetitive rate, and active material copper sulfide/nickel sulfide is former
Position is grown on foam nickel base, can be directly used as electrode use.
Detailed description of the invention
Fig. 1 is the XRD diagram of electrode material for super capacitor prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM figure of electrode material for super capacitor prepared by the embodiment of the present invention 1.
Fig. 3 is the cyclic voltammetry curve figure of electrode material for super capacitor prepared by the embodiment of the present invention 1.
Fig. 4 is the charge-discharge performance test result figure of electrode material for super capacitor prepared by the embodiment of the present invention 1.
Fig. 5 is the result figure of electrode material for super capacitor cyclical stability test prepared by the embodiment of the present invention 1.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam, foam copper pretreatment：Nickel foam is cut into 1cm*3cm, foam copper is cut into 1cm*1cm, foam copper and
Nickel foam is respectively put into ultrasound 5min in the hydrochloric acid of 1mol/L, after taking-up for several times using deionized water cleaning, then is put in acetone
Ultrasonic 5min, finally, nickel foam and foam copper are used into dehydrated alcohol and deionized water ultrasound 3-4 times respectively, it is true at 50 DEG C
It is dried in empty drying box；
(2) dehydrated alcohol of 20mL is added in the thiocarbamide for weighing 60mg and deionized water ratio is 3:In 1 mixed solution, stir
It mixes uniformly, obtains thiourea solution；
(3) pretreated nickel foam, foam copper and thiourea solution are transferred in polytetrafluoroethylene (PTFE) stainless steel cauldron,
Hydro-thermal reaction 6 hours at 150 DEG C；After reaction, so that reaction solution cooled to room temperature, take out sample, using go from
Sub- water and the multiple repeated flushing of dehydrated alcohol, 50 DEG C of oven drying 12h, obtain electrode material for super capacitor (multilevel structure
Ambrose alloy complex sulfide/foamed nickel electrode material).
Fig. 1 is X-ray diffraction (XRD) map of electrode material for super capacitor manufactured in the present embodiment, can be with from figure
Sharp diffraction maximum is found out from metallic nickel, and relatively weak diffraction maximum respectively corresponds Ni compared with standard PDF card pair3S2With
CuS2Diffraction maximum.
Fig. 2 is scanning electron microscope (SEM) map of electrode material for super capacitor manufactured in the present embodiment.From figure
As can be seen that the electrode material is by the nanometer sheet and nanoscale that are grown directly upon in foam nickel base with a thickness of tens nanometers
Micropore interactive connection assembles, and forms 3D flaky nanometer structure.
Fig. 3 is the cyclic voltammetry curve of electrode material for super capacitor manufactured in the present embodiment.It can be seen from the figure that
Under the voltage window of 0V-0.6V, there are redox peaks in different speed of sweeping, and with the increase for sweeping speed, closed area
Increase, specific capacitance is improved.
Fig. 4 is the result that the charge-discharge performance of electrode material for super capacitor manufactured in the present embodiment is tested.It can be with from figure
Find out, the electrode material for super capacitor of multilevel structure is in 1A g-1, 2A g-1, 3A g-1, 5A g-1, 10A g-1Current density
Under, specific capacitance is respectively 1657F g-1, 1384F g-1, 1165F g-1, 823F g-1, 608F g-1。
Fig. 5 is the result of electrode material for super capacitor cyclical stability manufactured in the present embodiment test.It can from figure
It out, is 10A g in current density-1Under conditions of, charge and discharge cycles 10000 are enclosed its capacity and are still able to maintain in 540F g-1。
Embodiment 2：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam, foam copper pretreatment：Nickel foam is cut into 1cm*3cm, after foam copper is cut into 1cm*1cm, by foam
Copper and nickel foam are respectively put into ultrasound 5min in the hydrochloric acid of 1mol/L, after taking-up for several times using deionized water cleaning, then are put in third
Ultrasound 5min in ketone, finally, nickel foam and foam copper are used dehydrated alcohol and deionized water ultrasound 3-4 times respectively, at 50 DEG C
Vacuum oven in dry；
(2) dehydrated alcohol of 20mL is added in the thiocarbamide for weighing 45mg and deionized water ratio is 3:In 1 mixed solution, stir
It mixes uniformly, obtains thiourea solution；
(3) pretreated nickel foam, foam copper and thiourea solution are transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron,
Hydro-thermal reaction 6 hours at 150 DEG C, after reaction, so that reaction solution cooled to room temperature, takes out sample, use deionization
Water and the multiple repeated flushing of dehydrated alcohol, 50 DEG C of oven drying 12h obtain ambrose alloy complex sulfide/nickel foam of multilevel structure
Electrode material.
Using the electrochemical property test method in embodiment 1, the material of the present embodiment is used as the electrode of supercapacitor
When, in 1A g-1Current density under, specific capacitance be 895F g-1；In 10A g-1Current density under circulation 10000 circle, capacity
It can maintain the 89% of its preliminary examination capacity.
Embodiment 3：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam, foam copper pretreatment：Nickel foam is cut into 1cm*3cm, after foam copper is cut into 1cm*1cm, foam copper
1molL is respectively put into nickel foam-1Hydrochloric acid in ultrasound 5min, take out using deionized water cleaning for several times, then be put in acetone
Ultrasonic 5min, finally, nickel foam and foam copper are used into dehydrated alcohol and deionized water ultrasound 3-4 times respectively, it is true at 50 DEG C
It is dried in empty drying box；
(2) dehydrated alcohol of 20mL is added in the thiocarbamide for weighing 75mg and deionized water ratio is 3:In 1 mixed solution, stir
It mixes uniformly, obtains thiourea solution；
(3) pretreated nickel foam, foam copper and thiourea solution are transferred in polytetrafluoroethylene (PTFE) stainless steel cauldron,
Sample so that reaction solution cooled to room temperature, is taken out after reaction in hydro-thermal reaction 6 hours at 150 DEG C, using go from
Sub- water and the multiple repeated flushing of dehydrated alcohol, 50 DEG C of oven drying 12h obtain ambrose alloy complex sulfide/foam of multilevel structure
Nickel electrode material.
Using the electrochemical property test method in embodiment 1, copper sulfide/nickel sulfide of the multilevel structure of the present embodiment/
When foam nickel material is used as the electrode of supercapacitor, in 1A g-1Current density under, specific capacitance be 1421F g-1；In 10A
g-1Current density under 10000 circle of circulation, capacity can maintain the 90% of its preliminary examination capacity.
Embodiment 4：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam, foam copper pretreatment：Nickel foam is cut into 1cm*3cm, after foam copper is cut into 1cm*1cm, by foam
Copper and nickel foam are respectively put into ultrasound 5min in the hydrochloric acid of 1mol/L, take out using deionized water cleaning for several times, then be put in acetone
Middle ultrasound 5min, finally, nickel foam and foam copper are used dehydrated alcohol and deionized water ultrasound 3-4 times respectively, at 50 DEG C
It is dried in vacuum oven；
(2) dehydrated alcohol of 20mL is added in the thiocarbamide for weighing 60mg and deionized water ratio is 3:In 1 mixed solution, stir
It mixes uniformly, forms thiourea solution；
(3) pretreated nickel foam, foam copper and thiourea solution are transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron,
The hydro-thermal reaction 9h at 150 DEG C, after reaction, so that reaction solution cooled to room temperature, takes out sample, use deionized water
And the multiple repeated flushing of dehydrated alcohol, 50 DEG C of oven drying 12h, obtain ambrose alloy complex sulfide/nickel foam electricity of multilevel structure
Pole material.
Using the electrochemical property test method in embodiment 1, the material of the present embodiment is used as the electrode of supercapacitor
When, in 1A g-1Current density under, specific capacitance be 1316F g-1；In 10A g-1Current density under circulation 10000 circle, capacity
It can maintain the 85% of its preliminary examination capacity.
Embodiment 5：
A kind of preparation method of electrode material for super capacitor, includes the following steps：
(1) nickel foam, foam copper pretreatment：Nickel foam is cut into 1cm*3cm, after foam copper is cut into 1cm*1cm, by foam
Copper and nickel foam are respectively put into ultrasound 5min in the hydrochloric acid of 1mol/L, take out using deionized water cleaning for several times, then be put in acetone
Middle ultrasound 5min, finally, nickel foam and foam copper are used dehydrated alcohol and deionized water ultrasound 3-4 times respectively, at 50 DEG C
It is dried in vacuum oven；
(2) dehydrated alcohol of 20mL is added in the thiocarbamide for weighing 60mg and deionized water ratio is 3:In 1 mixed solution, stir
It mixes uniformly, forms thiourea solution；
(3) pretreated nickel foam, foam copper and thiourea solution are transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron,
The hydro-thermal reaction 6h at 140 DEG C, after reaction, so that reaction solution cooled to room temperature, takes out sample, use deionized water
And the multiple repeated flushing of dehydrated alcohol, 50 DEG C of oven drying 12h, obtain ambrose alloy complex sulfide/nickel foam electricity of multilevel structure
Pole material.
Using the electrochemical property test method in embodiment 1, the material of the present embodiment is used as the electrode of supercapacitor
When, in 1A g-1Current density under, specific capacitance be 1251F g-1；In 10A g-1Current density under circulation 10000 circle, capacity
It can maintain the 80% of its preliminary examination capacity.
Claims (6)
1. a kind of preparation method of electrode material for super capacitor, which is characterized in that include the following steps：
(1) nickel foam and foam copper are pre-processed；
(2) pretreated nickel foam, foam copper and thiourea solution are subjected at 140-160 DEG C hydro-thermal reaction, react 5-9h,
Cooling, cleaning is dried to get the electrode material for super capacitor is arrived.
2. preparation method as described in claim 1, which is characterized in that in the step (2), thiourea solution refers to thiocarbamide and nothing
The mixed solution of water-ethanol, deionized water；The concentration of the thiourea solution is 1.5-3.5mg/mL.
3. preparation method as claimed in claim 2, which is characterized in that dehydrated alcohol and deionized water in the thiourea solution
Volume ratio is 3：1.
4. preparation method as described in claim 1, which is characterized in that nickel foam and foam copper progress preprocessing process are specific
For：Foam copper and nickel foam are respectively put into ultrasound 5-10min in 0.5-1mol/L hydrochloric acid, cleaned after taking-up using deionized water
For several times, then it is put in ultrasound 5-10min in acetone；By the nickel foam by acetone ultrasonic treatment with dehydrated alcohol ultrasound 3-4 times, warp
The foam copper of acetone ultrasonic treatment is crossed with deionized water ultrasound 3-4 times；Vacuum drying completes pretreatment.
5. preparation method according to any one of claims 1-4, which is characterized in that the electrode material for super capacitor is to receive
Rice laminated structure.
6. preparation method according to any one of claims 1-4, which is characterized in that the electrode material for super capacitor be by
Ambrose alloy complex sulfide growth in situ in foam nickel base in forming.
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| CN110461137A (en) * | 2019-07-31 | 2019-11-15 | 西北工业大学 | A kind of three-dimensional foam type composite wave-suction 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 |
| CN110752096A (en) * | 2019-10-25 | 2020-02-04 | 青岛科技大学 | Multidimensional structure metal sulfide Ni3S2/Co3S4Preparation of (A) and its use in supercapacitors |
| CN110867326A (en) * | 2019-11-19 | 2020-03-06 | 上海季丰电子股份有限公司 | Copper sulfide-foamed nickel three-dimensional composite material and preparation method thereof |
| CN113299491A (en) * | 2021-05-31 | 2021-08-24 | 中南大学 | Photo-thermal enhanced supercapacitor electrode material and preparation method thereof |
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| 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 |
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| CN113299491A (en) * | 2021-05-31 | 2021-08-24 | 中南大学 | Photo-thermal enhanced supercapacitor electrode 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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