CN106920698A - A kind of ultracapacitor NixCo3‑xS4/NiCo2O4Composite and preparation method thereof - Google Patents
A kind of ultracapacitor NixCo3‑xS4/NiCo2O4Composite and preparation method thereof Download PDFInfo
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- CN106920698A CN106920698A CN201710183093.XA CN201710183093A CN106920698A CN 106920698 A CN106920698 A CN 106920698A CN 201710183093 A CN201710183093 A CN 201710183093A CN 106920698 A CN106920698 A CN 106920698A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000002131 composite material Substances 0.000 claims abstract description 27
- 229910005949 NiCo2O4 Inorganic materials 0.000 claims abstract description 26
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- 239000006260 foam Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000003491 array Methods 0.000 claims abstract description 10
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 6
- 229910002567 K2S2O8 Inorganic materials 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims abstract description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 241000080590 Niso Species 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 4
- 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 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- 239000007772 electrode material Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002023 wood Substances 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- 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
- H01G11/46—Metal oxides
-
- 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)
- Inorganic Compounds Of Heavy Metals (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of ultracapacitor NixCo3‑xS4/NiCo2O4Composite and preparation method thereof, composite is NixCo3‑xS4/NiCo2O4Composite.Prepare:By NiSO4·6H2O、CoSO4·6H2O and K2S2O8It is well mixed, above-mentioned length then there is into NixCo3‑xS4The nickel foam of nano-chip arrays is vertically put into mixed solution and adds ammonia spirit, keeps 3 20min, and calcining is obtained final product.The Ni that the present invention is designed and synthesizedxCo3‑xS4@NiCo2O4Composite shows excellent chemical property, with critically important application prospect.
Description
Technical field
The invention belongs to super capacitor material and its preparation field, more particularly to a kind of ultracapacitor NixCo3-xS4/
NiCo2O4Composite and preparation method thereof.
Background technology
With the fast development of global economy, the continuous consumption of fossil energy, environmental pollution it is increasingly serious, research is a kind of
Efficiently, inexpensive, environment-friendly, high performance energy conversion and stocking system have seemed more and more important.Ultracapacitor
Under due to power density high, the advantages of fast charging and discharging speed and cycle life long being considered as most promising
Generation energy is changed and storage facilities.However, being compared with battery with fuel cell, the low energy density of ultracapacitor is seriously made
About its following large-area applications.It is that the one kind for improving super capacitor energy density has to develop new, high performance electrode material
Efficacious prescriptions method.Transient metal sulfide is due to being considered as excellent with the specific capacitance higher than carbon material and conducting polymer
Electrode material.In numerous transient metal sulfides, NiCo2S4Due to there is more excellent electricity than single metal sulfide
Conductance and can for faraday's reversible reaction provides multiple oxidation state and be considered as new class high performance electrode material.Therefore, structure
Build based on NiCo2S4The combination electrode material of material is significant to improving ultracapacitor chemical property.The present invention sets
The Ni for counting and synthesizingxCo3-xS4@NiCo2O4Composite shows excellent chemical property, preceding with critically important application
Scape.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of ultracapacitor NixCo3-xS4/NiCo2O4Composite
And preparation method thereof, the ultracapacitor Ni prepared by the present inventionxCo3-xS4/NiCo2O4Composite shows excellent electrification
Performance is learned, with actual application prospect.
A kind of ultracapacitor Ni of the inventionxCo3-xS4/NiCo2O4Composite, it is characterised in that:The composite wood
Expect be
NixCo3-xS4/NiCo2O4Composite, wherein x=0-1.
A kind of ultracapacitor Ni of the inventionxCo3-xS4/NiCo2O4The preparation method of composite, including:
(1) Nickelous nitrate hexahydrate Ni (NO3)2·6H2O, cabaltous nitrate hexahydrate Co (NO3)2·6H2O and hexamethylenetetramine
HMT is dissolved in solvent, and is sufficiently stirred for, and obtains mixed solution;
(2) above-mentioned mixed solution is poured into reactor and is put into nickel foam, reactor is put into air dry oven,
3-12h is reacted under 90-120 DEG C of hydrothermal condition, reaction cools down reactor to room temperature, washing after terminating, and dries, obtaining length has
NixCo3-xS4The nickel foam of presoma;
(3) above-mentioned length there is into NixCo3-xS4The nickel foam of presoma is put into reactor and adds sodium sulfide solution,
Reacted 2-12 hours under 100-150 DEG C of hydrothermal condition, reaction cools down reactor to room temperature after terminating, washing is dried, and obtaining length has
NixCo3-xS4The nickel foam of nano-chip arrays;
(4) by NiSO4·6H2O、CoSO4·6H2O and K2S2O8Solution be well mixed, above-mentioned length is then had into NixCo3- xS4The nickel foam of nano-chip arrays is vertically put into mixed solution and adds ammoniacal liquor, keeps 3-20min, and calcining is obtained final product.
Ni (NO in the step (1)3)2·6H2O、Co(NO3)2·6H2The ratio of O, HMT is 1-10mmol:1-
10mmol:0.1-10g.
Solvent is the mixed solution of water and ethanol in the step (1).
Reactor is polytetrafluoroethylene (PTFE) hydrothermal reaction kettle in the step (2), (3).
Nickelous nitrate hexahydrate Ni (NO in step (1)3)2·6H2The molal weight ratio of vulcanized sodium is 1- in O and step (3)
10mmol:0.1-2g.
The quality of vulcanized sodium is 0.1-2g in the step (3).
Washing is to be washed with deionized water and alcohol solvent respectively in the step (2), (3).
NiSO in the step (4)4·6H2O, CoSO4·6H2O and K2S2O8Mol ratio be 1:2:0.4.
The volume ratio of mixed solution and ammoniacal liquor is 180 in the step (4):5-100.
Ammonia volume is 5-100mL in the step (4).
It is preferred that ammonia vol is 5-50ml.
To be calcined in tube furnace, calcining heat is 350-550 DEG C for calcining in the step (4), and the time is 1-10 hours.
Beneficial effect
The ratio of present invention research Ni and Co is to NixCo3-xS4The Electrochemical Performances of electrode material, and with electrochemistry
Ni that can be most excellentxCo3-xS4Electrode material builds combination electrode material, due to having cooperative effect to improve whole therebetween
The chemical property of individual electrode, can meet the growth requirement of following practical application.
Brief description of the drawings
Fig. 1 is the Ni of the preparation of embodiment 1 in the present inventionxCo3-xS4@NiCo2O4(x=1.8) ESEM of composite
Figure (a, b);Fig. 2 is the Ni of the preparation of embodiment 1 in the present inventionxCo3-xS4@NiCo2O4(x=1.8) composite and NixCo3-xS4
(x=1.8) cyclic voltammetric (a) of material, discharge and recharge (b), area specific capacitance (c) and cyclical stability (d) figure.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
1)NixCo3-xS4The preparation of nano-chip arrays
A () weighs raw material 1.8mmol Nickelous nitrate hexahydrates (Ni (NO3)2·6H2O), 1.2mmol cabaltous nitrate hexahydrates (Co
(NO3)2·6H2O) it is dissolved into water (30ml) and ethanol (20ml) mixed solution with 0.8g hexamethylenetetramines (HMT), and is filled
Divide stirring.
B above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and is put into one piece of foam being cleaned by ()
Nickel, reactor is put into air dry oven, is reacted 8 hours under 95 DEG C of hydrothermal conditions, and reaction cools down reactor to room after terminating
Temperature, and take out length have NixCo3-xS4The nickel foam of presoma, is washed with deionized water and alcohol solvent respectively, and is dried.
C the length of above-mentioned preparation is had Ni by ()xCo3-xS4The nickel foam of presoma is put into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle simultaneously
0.5g sodium sulfide solutions are added, reactor is put into air dry oven, reacted 8 hours under 120 DEG C of hydrothermal conditions, reaction knot
Reactor is cooled down after beam to room temperature, and takes out length has NixCo3-xS4The nickel foam of nano-chip arrays, respectively with deionized water and second
Alcoholic solvent is washed, and is dried.
2)NixCo3-xS4/NiCo2O4The preparation of composite:By the 1M NiSO of 50mL4·6H2The 2M of O, 50mL
CoSO4·6H2The 0.25M K of O and 80mL2S2O8It is well mixed, above-mentioned length then there is into NixCo3-xS4The foam of nano-chip arrays
Nickel is vertically put into mixed solution, and adds ammonia spirit (20mL), is taken out after being kept for 8 minutes.Finally the sample of taking-up is put
Enter calcining (calcining heat is 300 DEG C, and the time is 2 hours) in the tube furnace of argon gas protection, obtain NixCo3-xS4/NiCo2O4It is multiple
Condensation material.
NiCo2O4Nanometer sheet uniform fold is in NixCo3-xS4Material surface, forms high porosity.Above-mentioned composite
Area specific capacitance be up to 4.44F/cm2。
Embodiment 2
1)NixCo3-xS4The preparation of nano-chip arrays
A () weighs raw material 1.2mmol Nickelous nitrate hexahydrates (Ni (NO3)2·6H2O), 1.8mmol cabaltous nitrate hexahydrates (Co
(NO3)2·6H2O) it is dissolved into water (30ml) and ethanol (20ml) mixed solution with 0.8g hexamethylenetetramines (HMT), and is filled
Divide stirring.
B above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and is put into one piece of foam being cleaned by ()
Nickel, reactor is put into air dry oven, is reacted 8 hours under 95 DEG C of hydrothermal conditions, and reaction cools down reactor to room after terminating
Temperature, and take out length have NixCo3-xS4The nickel foam of presoma, is washed with deionized water and alcohol solvent respectively, and is dried.
C the length of above-mentioned preparation is had Ni by ()xCo3-xS4The nickel foam of presoma is put into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle simultaneously
1g sodium sulfide solutions are added, reactor is put into air dry oven, reacted 8 hours under 120 DEG C of hydrothermal conditions, reaction terminates
Reactor is cooled down afterwards to room temperature, and takes out length has NixCo3-xS4The nickel foam of nano-chip arrays, respectively with deionized water and ethanol
Solvent is washed, and is dried.
2)NixCo3-xS4/NiCo2O4The preparation of composite:By the 1M NiSO of 50mL4·6H2The 2M of O, 50mL
CoSO4·6H2The 0.25M K of O and 80mL2S2O8It is well mixed, above-mentioned length then there is into NixCo3-xS4The foam of nano-chip arrays
Nickel is vertically put into mixed solution, and adds ammonia spirit (50mL), is taken out after being kept for 8 minutes.Finally the sample of taking-up is put
Enter calcining (calcining heat is 300 DEG C, and the time is 2 hours) in the tube furnace of argon gas protection, obtain NixCo3-xS4/NiCo2O4It is multiple
Condensation material.
Claims (8)
1. a kind of ultracapacitor NixCo3-xS4/NiCo2O4Composite, it is characterised in that:The composite is NixCo3- xS4/NiCo2O4Composite, wherein x=0-1.
2. a kind of ultracapacitor Ni as claimed in claim 1xCo3-xS4/NiCo2O4The preparation method of composite, including:
(1) Nickelous nitrate hexahydrate Ni (NO3)2·6H2O, cabaltous nitrate hexahydrate Co (NO3)2·6H2O and hexamethylenetetramine HMT are molten
In solvent, and it is sufficiently stirred for, obtains mixed solution;
(2) above-mentioned mixed solution is poured into reactor and is put into nickel foam, reactor is put into air dry oven, in 90-
3-12h is reacted under 120 DEG C of hydrothermal conditions, reaction cools down reactor to room temperature, washing after terminating, and dries, obtaining length has
NixCo3-xS4The nickel foam of presoma;
(3) above-mentioned length there is into NixCo3-xS4The nickel foam of presoma is put into reactor and adds sodium sulfide solution, in 100-
Reacted 2-12 hours under 150 DEG C of hydrothermal conditions, reaction cools down reactor to room temperature after terminating, washing is dried, and obtaining length has
NixCo3-xS4The nickel foam of nano-chip arrays;
(4) by NiSO4·6H2O、CoSO4·6H2O and K2S2O8It is well mixed, above-mentioned length then there is into NixCo3-xS4Nanometer sheet battle array
The nickel foam of row is vertically put into mixed solution and adds ammoniacal liquor, keeps 3-20min, and calcining is obtained final product.
3. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:Ni (NO in the step (1)3)2·6H2O、Co(NO3)2·6H2The ratio of O, HMT is 1-10mmol:1-10mmol:
0.1-10g。
4. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:Solvent is the mixed solution of water and ethanol in the step (1).
5. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:The quality of vulcanized sodium is 0.1-2g in the step (3).
6. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:NiSO in the step (4)4·6H2O, CoSO4·6H2O and K2S2O8Mol ratio be 1:2:0.4.
7. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:Ammonia volume is 5-100mL in the step (4).
8. a kind of ultracapacitor Ni according to claim 2xCo3-xS4/NiCo2O4The preparation method of composite, it is special
Levy and be:To be calcined in tube furnace, calcining heat is 350-550 DEG C for calcining in the step (4), and the time is 1-10 hours.
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Cited By (5)
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CN108258238A (en) * | 2018-01-16 | 2018-07-06 | 吉林大学 | A kind of anode material of lithium-ion battery NiCo of flaky nanometer structure2S4And preparation method thereof |
CN108597893A (en) * | 2018-05-28 | 2018-09-28 | 江苏大学 | A kind of preparation method based on the composite electrode material for super capacitor in nickel foam |
CN109119258A (en) * | 2018-08-27 | 2019-01-01 | 江南大学 | A kind of preparation method of electrode material |
CN110330058A (en) * | 2019-06-20 | 2019-10-15 | 东华大学 | A kind of supercapacitor NixCoySzElectrode material and its preparation and application |
CN112863887A (en) * | 2020-12-28 | 2021-05-28 | 沈阳工业大学 | Preparation method of high-performance cabbage-shaped heterostructure electrode material |
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