CN109119258A - A kind of preparation method of electrode material - Google Patents
A kind of preparation method of electrode material Download PDFInfo
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- CN109119258A CN109119258A CN201810979691.2A CN201810979691A CN109119258A CN 109119258 A CN109119258 A CN 109119258A CN 201810979691 A CN201810979691 A CN 201810979691A CN 109119258 A CN109119258 A CN 109119258A
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- nickel
- nickel foam
- preparation
- ternary metal
- ethyl alcohol
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000007772 electrode material Substances 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 89
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 46
- 239000006260 foam Substances 0.000 claims abstract description 36
- 229910020630 Co Ni Inorganic materials 0.000 claims abstract description 24
- 229910002440 Co–Ni Inorganic materials 0.000 claims abstract description 24
- 238000003491 array Methods 0.000 claims abstract description 22
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 18
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 18
- 229910052976 metal sulfide Inorganic materials 0.000 claims abstract description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 39
- 235000019441 ethanol Nutrition 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical class O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 5
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- CHSMNMOHKSNOKO-UHFFFAOYSA-L zinc;dichloride;hydrate Chemical compound O.[Cl-].[Cl-].[Zn+2] CHSMNMOHKSNOKO-UHFFFAOYSA-L 0.000 claims description 5
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 150000001455 metallic ions Chemical class 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A kind of preparation method of electrode material, belongs to materials chemistry and electrochemical technology field.The present invention configures the metallic ion mixed liquor of Zn, Co and Ni, and nickel foam is immersed in mixed solution and reacts by the oxide skin(coating) for the nickel surface that defoams, and the nickel foam that surface has Zn-Co-Ni ternary metal oxide nano-chip arrays is prepared；Preparation gained Zn-Co-Ni- nickel foam is reacted with vulcanized sodium, Zn-Co-Ni ternary metal sulfide nanometer sheet is made.The present invention is for traditional single metal sulfide or binary metal sulfide, ternary metal sulfide prepared by the present invention has higher electro-chemical activity, this is because the mutual synergistic effect between three metal ion species results in higher electro-chemical activity.
Description
Technical field
The present invention relates to a kind of preparation methods of electrode material, belong to materials chemistry and electrochemical technology field.
Background technique
Green energy resource is one of the important leverage that human society is capable of sustainable development, and energy storage device is green energy resource
One important component.Supercapacitor is as a kind of novel green energy storage device, in new energy technology, electric car etc.
There is very important broad prospect of application in field.Determine the often electrode material of performance of the supercapacitor.According to energy storage machine
Supercapacitor can be divided into double layer capacitor and Faraday pseudo-capacitance device by the difference of reason.The appearance of double layer capacitor
Relatively early, usually using the carbon material of high specific area and high conductivity as electrode material, and Faraday pseudo-capacitance device is due to existing
Abundant reversible faraday's redox reaction, usually have the specific capacitance higher than double layer capacitor, therefore attracted more
Carry out more research interests.
Summary of the invention
It is an object of the present invention to overcome the above deficiencies, provides a kind of preparation method of electrode material.
According to technical solution provided by the invention, a kind of preparation method of electrode material, steps are as follows: configuration Zn, Co and
Nickel foam is immersed in mixed solution and carries out instead by the metallic ion mixed liquor of Ni, the oxide skin(coating) for the nickel surface that defoams
It answers, the nickel foam that surface has Zn-Co-Ni ternary metal oxide nano-chip arrays is prepared；It will preparation gained Zn-Co-
Ni- nickel foam is reacted with vulcanized sodium, and Zn-Co-Ni ternary metal sulfide nanometer sheet is made.
The preparation method of the electrode material, the specific steps are as follows:
(1) preparation of ternary metal oxide nano-chip arrays:
A, nickel foam is taken, handles 10min in the ultra sonic bath of the 40KHz of 5M aqueous hydrochloric acid solution, the surface oxidation for the nickel that defoams
Nitride layer, and respectively rinsed three times with ethyl alcohol and water；
B, at room temperature, by six chloride hydrate zinc of 1mmol, 1mmol Nickel dichloride hexahydrate, 2 mmol cobalt chloride hexahydrates and
5mmol hexa is dissolved in the aqueous solution of 70mL ethyl alcohol, and stirring 30min forms clear solution；
C, step b acquired solution is transferred in the reaction kettle that volume is 100mL, is then immersed in pretreated obtained by step a
Clean nickel foam；Reaction kettle is heated in an oven and in 100-150 DEG C of holding 8h；
D, after reaction kettle natural cooling, nickel foam is taken out, is rinsed with water three times, then in 70 DEG C of air drying 12h, that is, prepares
The nickel foam that surface has Zn-Co-Ni ternary metal oxide nano-chip arrays is obtained；
(2) vulcanize: step (1) preparation gained surface being taken to have the foam of Zn-Co-Ni ternary metal oxide nano-chip arrays
Nickel is put it into stainless steel cauldron, and 70mL is then added and contains the aqueous solution of 0.6-1.2g vulcanized sodium, by reaction kettle plus
Heat is to 100-120 DEG C and maintains 10h；After cooling, with water and ethyl alcohol cleaning sample, and at 60-80 DEG C vacuum degree be less than-
0.07MPa dries 12h, and Zn-Co-Ni ternary metal sulfide nanometer sheet is made.
In step (1) b, the aqueous solution of ethyl alcohol, water: the volume ratio of ethyl alcohol is 1:1.
Beneficial effects of the present invention: the present invention relative to traditional single metal sulfide or binary metal sulfide and
It says, ternary metal sulfide prepared by the present invention has higher electro-chemical activity, this is because between three metal ion species
It is mutual synergistic effect result in higher electro-chemical activity.
Detailed description of the invention
Fig. 1 is the SEM figure of Zn-Co-Ni ternary metal sulfide nanometer sheet prepared by the embodiment of the present invention 1.
It (A) is the SEM figure of the foam nickel base of blank, (B-D) is Zn-Co-Ni tri- prepared by the embodiment of the present invention 1
The SEM of first nano metal sulfide chip arrays schemes.
Fig. 2 is the electrochemistry of Zn-Co-Ni ternary metal sulfide nano-chip arrays prepared by the embodiment of the present invention 1
Test result.
It (A) is cyclic voltammetry curve, (B) constant current charge/discharge curve.
Specific embodiment
Embodiment 1
(1) Zn-Co-Ni ternary metal oxide nano-chip arrays are prepared in foam nickel surface
The oxide layer that nickel foam is handled to 10min foam-expelling nickel in the ultra sonic bath of 5M aqueous hydrochloric acid solution first, is used in combination
Second alcohol and water rinses for several times.Then, at room temperature, by six chloride hydrate zinc of 1mmol, 1mmol Nickel dichloride hexahydrate, 2 mmol
Cobalt chloride hexahydrate and 5mmol hexa are dissolved in the mixed of 70 mL water and ethyl alcohol (the volume ratio 1:1 of water and ethyl alcohol)
It closes in solution, stirring 30min forms clear solution.Transferring the solution into volume is 100mL with polytetrafluoroethyllining lining
In stainless steel cauldron, it is then immersed in one piece of pretreated clean nickel foam.Then reaction kettle is heated simultaneously in an oven
In 105 DEG C of holding 8h.After reaction kettle natural cooling, nickel foam is taken out, is rinsed with water for several times, then in 70 DEG C of air dryings
Zn-Co-Ni ternary metal oxide nano-chip arrays have been prepared in foam nickel surface in 12h.
(2) Zn-Co-Ni ternary metal sulfide nano-chip arrays are prepared in foam nickel surface
The stainless steel that the Zn-Co-Ni ternary metal oxide nano-chip arrays prepared in step 1 are put into Teflon liner is anti-
It answers in kettle, the aqueous solution that 70mL contains 0.6g vulcanized sodium is then added, reaction kettle is heated to 100 DEG C and maintains 10h.It is cooling
Afterwards, with water and ethyl alcohol cleaning sample, and 12h is dried in vacuo at 60 DEG C.
Resulting Zn-Co-Ni ternary metal sulfide nano-chip arrays with field emission scanning electron microscope (FESEM,
Hitachi S4800) (SEM) characterized, and photo is shown in Fig. 1.Electrochemical Characterization result is shown in Fig. 2.
Embodiment 2
The preparation method of the electrode material, the specific steps are as follows:
(1) preparation of ternary metal oxide nano-chip arrays:
A, nickel foam is taken, handles 10min in the ultra sonic bath of the 40KHz of 5M aqueous hydrochloric acid solution, the surface oxidation for the nickel that defoams
Nitride layer, and three times with the rinsing of second alcohol and water；
B, at room temperature, by six chloride hydrate zinc of 1mmol, 1mmol Nickel dichloride hexahydrate, 2 mmol cobalt chloride hexahydrates and
5mmol hexa is dissolved in the aqueous solution of 70mL ethyl alcohol, and stirring 30min forms clear solution；
C, step b acquired solution is transferred in the reaction kettle that volume is 100mL, is then immersed in pretreated obtained by step a
Clean nickel foam；Reaction kettle is heated in an oven and in 100 DEG C of holding 8h；
D, after reaction kettle natural cooling, nickel foam is taken out, is rinsed with water three times, then in 70 DEG C of air drying 12h, that is, is steeping
Zn-Co-Ni ternary metal oxide nano-chip arrays have been prepared in foam nickel surface；
(2) vulcanize: taking nickel foam of step (1) preparation gained containing Zn-Co-Ni ternary metal oxide nano-chip arrays, it will
It is put into stainless steel cauldron, and the aqueous solution that 70mL contains 0.6g vulcanized sodium is then added, autoclave is heated to 100 DEG C
And maintain 10h；After cooling, with water and ethyl alcohol cleaning sample, and at 60 DEG C, vacuum degree is less than the dry 12h of -0.07MPa.
In step (1) b, the volume ratio of water and ethyl alcohol is 1:1.
Embodiment 3
The preparation method of the electrode material, the specific steps are as follows:
(1) preparation of ternary metal oxide nano-chip arrays:
A, nickel foam is taken, handles 10min in the ultra sonic bath of the 40KHz of 5M aqueous hydrochloric acid solution, the surface oxidation for the nickel that defoams
Nitride layer, and three times with the rinsing of second alcohol and water；
B, at room temperature, by six chloride hydrate zinc of 1mmol, 1mmol Nickel dichloride hexahydrate, 2 mmol cobalt chloride hexahydrates and
5mmol hexa is dissolved in the aqueous solution of 70mL ethyl alcohol, and stirring 30min forms clear solution；
C, step b acquired solution is transferred in the reaction kettle that volume is 100mL, is then immersed in pretreated obtained by step a
Clean nickel foam；Reaction kettle is heated in an oven and in 150 DEG C of holding 8h；
D, after reaction kettle natural cooling, nickel foam is taken out, is rinsed with water three times, then in 70 DEG C of air drying 12h, that is, is steeping
Zn-Co-Ni ternary metal oxide nano-chip arrays have been prepared in foam nickel surface；
(2) vulcanize: taking nickel foam of step (1) preparation gained containing Zn-Co-Ni ternary metal oxide nano-chip arrays, it will
It is put into stainless steel cauldron, and the aqueous solution that 70mL contains 1.2g vulcanized sodium is then added, reaction kettle is heated to 120 DEG C
And maintain 10h；After cooling, with water and ethyl alcohol cleaning sample, and at 80 DEG C, vacuum degree is less than the dry 12h of -0.07MPa.
In step (1) b, the volume ratio of water and ethyl alcohol is 1:1.
Claims (3)
1. a kind of preparation method of electrode material, it is characterized in that steps are as follows: the metal ion mixing of configuration Zn, Co and Ni are molten
Liquid, the oxide skin(coating) for the nickel surface that defoams, nickel foam is immersed in mixed solution and is reacted, and surface is prepared and has
The nickel foam of Zn-Co-Ni ternary metal oxide nano-chip arrays；Gained Zn-Co-Ni- nickel foam will be prepared and vulcanized sodium is anti-
It answers, Zn-Co-Ni ternary metal sulfide nanometer sheet is made.
2. the preparation method of electrode material according to claim 1, it is characterized in that specific step is as follows:
(1) preparation of ternary metal oxide nano-chip arrays:
A, nickel foam is taken, handles 10min in the ultra sonic bath of the 40KHz of 5M aqueous hydrochloric acid solution, the surface oxidation for the nickel that defoams
Nitride layer, and respectively rinsed three times with ethyl alcohol and water；
B, at room temperature, by six chloride hydrate zinc of 1mmol, 1mmol Nickel dichloride hexahydrate, 2 mmol cobalt chloride hexahydrates and
5mmol hexa is dissolved in the aqueous solution of 70mL ethyl alcohol, and stirring 30min forms clear solution；
C, step b acquired solution is transferred in the reaction kettle that volume is 100mL, is then immersed in pretreated obtained by step a
Clean nickel foam；Reaction kettle is heated in an oven and in 100-150 DEG C of holding 8h；
D, after reaction kettle natural cooling, nickel foam is taken out, is rinsed with water three times, then in 70 DEG C of air drying 12h, that is, prepares
The nickel foam that surface has Zn-Co-Ni ternary metal oxide nano-chip arrays is obtained；
(2) vulcanize: step (1) preparation gained surface being taken to have the foam of Zn-Co-Ni ternary metal oxide nano-chip arrays
Nickel is put it into stainless steel cauldron, and 70mL is then added and contains the aqueous solution of 0.6-1.2g vulcanized sodium, by reaction kettle plus
Heat is to 100-120 DEG C and maintains 10h；After cooling, with water and ethyl alcohol cleaning sample, and at 60-80 DEG C vacuum degree be less than-
0.07MPa dries 12h, and Zn-Co-Ni ternary metal sulfide nanometer sheet is made.
3. the preparation method of electrode material according to claim 2, it is characterized in that: in step (1) b, the aqueous solution of ethyl alcohol,
Water: the volume ratio of ethyl alcohol is 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810979691.2A CN109119258A (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810979691.2A CN109119258A (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of electrode material |
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| Publication Number | Publication Date |
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| CN109119258A true CN109119258A (en) | 2019-01-01 |
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| CN201810979691.2A Pending CN109119258A (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of electrode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110415993A (en) * | 2019-07-16 | 2019-11-05 | 上海应用技术大学 | A kind of preparation method and applications of Mn-Co-S/Co-MOF nano material |
| CN114094115A (en) * | 2021-10-13 | 2022-02-25 | 中国长江三峡集团有限公司 | Columnar copper array current collector and preparation method and application thereof |
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| US20090123851A1 (en) * | 2007-11-14 | 2009-05-14 | Sony Corporation | Positive-electrode active material for lithium-ion secondary battery, positive electrode, manufacturing method thereof, and lithium-ion secondary battery |
| CN106920698A (en) * | 2017-03-24 | 2017-07-04 | 东华大学 | A kind of ultracapacitor NixCo3‑xS4/NiCo2O4Composite and preparation method thereof |
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2018
- 2018-08-27 CN CN201810979691.2A patent/CN109119258A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090123851A1 (en) * | 2007-11-14 | 2009-05-14 | Sony Corporation | Positive-electrode active material for lithium-ion secondary battery, positive electrode, manufacturing method thereof, and lithium-ion secondary battery |
| CN106920698A (en) * | 2017-03-24 | 2017-07-04 | 东华大学 | A kind of ultracapacitor NixCo3‑xS4/NiCo2O4Composite and preparation method thereof |
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| V. VIGNESH ETC.: "Spherical-Like Ball-by-Ball Architecture of Ni-Co-Zn-S Electrodes for Electrochemical Energy Storage Application in Supercapacitors", 《ECS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110415993A (en) * | 2019-07-16 | 2019-11-05 | 上海应用技术大学 | A kind of preparation method and applications of Mn-Co-S/Co-MOF nano material |
| CN110415993B (en) * | 2019-07-16 | 2021-09-28 | 上海应用技术大学 | Preparation method and application of Mn-Co-S/Co-MOF nano material |
| CN114094115A (en) * | 2021-10-13 | 2022-02-25 | 中国长江三峡集团有限公司 | Columnar copper array current collector and preparation method and application thereof |
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Application publication date: 20190101 |