CN114105227A - Preparation method of hollow-structure metal sulfide electrode material - Google Patents
Preparation method of hollow-structure metal sulfide electrode material Download PDFInfo
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- CN114105227A CN114105227A CN202111401555.3A CN202111401555A CN114105227A CN 114105227 A CN114105227 A CN 114105227A CN 202111401555 A CN202111401555 A CN 202111401555A CN 114105227 A CN114105227 A CN 114105227A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 23
- 229910052976 metal sulfide Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 2
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical group O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 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 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000126 substance Substances 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 12
- 238000004146 energy storage Methods 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000011232 storage material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- -1 transition metal sulfide Chemical class 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
-
- 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
- H01G11/30—Electrodes characterised by their material
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of materials, and discloses a preparation method of a hollow-structure metal sulfide electrode material. The hollow-structure metal sulfide electrode material is prepared by a simple one-step method. The preparation process is simple and low in cost; the obtained energy storage electrode material has excellent electrochemical performance and is convenient for industrial application. The hollow-structure metal sulfide electrode material prepared by the invention has excellent specific capacitance and rate performance, and can be applied to the fields of electrodes of super capacitors and batteries and electrocatalysis.
Description
Technical Field
The invention belongs to the technical field of materials, and discloses a preparation method of a hollow-structure metal sulfide electrode material.
Background
With the rapid development of consumer electronics products and hybrid electric vehicle markets, the intensive development of environment-friendly high-performance energy storage devices becomes a hot spot of current research. The super capacitor has the advantages of a secondary battery and a traditional physical capacitor, and has the advantages of high power density, quick charging, long service life, wide working temperature range, environmental friendliness and the like. The electrode material is an important factor determining the performance of the super capacitor, so the development of the electrode material with low price, high specific capacitance, long stability, high energy and power density is a key for promoting the development of the super capacitor energy storage technology.
The metal sulfide has rich valence, high conductivity and high electrochemical activity, is widely researched as an electrode material of a super capacitor, and is an electrode material of the super capacitor with application prospect. The electrode material with a hollow structure has good energy storage performance, however, the existing method for synthesizing the transition metal sulfide with the hollow structure or the reaction with a liquid phase causes that the surplus sulfur source is difficult to recover or the synthesis steps are complicated. Hollow spherical cobalt sulfide was synthesized as reported by Phase and composition controlled synthesis of cobalt sulfide nanoparticles for electrochemical water separation by Xiaooping Han et al, by dissolving cobalt acetate in water, adding ethylenediamine with sufficient agitation, adding carbon disulfide with agitation, and transferring to a polytetrafluoroethylene kettle at 200 ℃ for 9 hours. Formation of multi-shelled nickel-based catalysts for rechargeable alkylnickel catalysts published by Dan Wang et al reports that hollow spherical NiO is synthesized as a precursor, and then vulcanized in a tube furnace by using sulfur powder as a sulfur source to synthesize hollow spherical nickel sulfide.
The application provides a brand new preparation scheme aiming at the problems that the sulfur source is not easy to recover and the steps are complicated in the preparation of the sulfide electrode material with the hollow structure.
Disclosure of Invention
In view of the defects in the prior art, the invention aims to disclose a hollow-structure metal sulfide with high quality capacity, excellent rate capability and cycling stability and a preparation method thereof, wherein the sulfide can be used in the field of electrode materials or electrocatalysis of asymmetric supercapacitors or batteries. The sulfide synthesis process is simple, environment-friendly, fully utilizes raw materials and is easy to realize large-scale preparation and industrialization.
The technical scheme of the invention is as follows:
the metal sulfide is a hollow structure metal sulfide synthesized by taking a metal source and sulfur powder as raw materials.
The metal sulfide is nickel sulfide or cobalt sulfide or nickel cobalt bimetallic sulfide;
a preparation method of a hollow structure metal sulfide electrode material comprises the following steps:
firstly, adding a nickel source or a cobalt source or a mixture of the nickel source and the cobalt source into ethanol or an aqueous solution, adding sulfur powder after dissolving, uniformly mixing the mixture, drying for 1-8 hours in vacuum at 40-90 ℃, and removing ethanol or water.
And secondly, transferring the mixture obtained in the first step into a tubular furnace, heating for 1-8 hours at the temperature of 100-400 ℃ in the atmosphere of inert gas, adding a sulfur gas recovery device at the tail part of the tubular furnace, recovering the residual sulfur for recycling, washing by using deionized water, and keeping the temperature in a vacuum drying oven at 50-80 ℃ for 1-10 hours to obtain the metal sulfide with the hollow structure.
In the first step, the nickel source is nickel nitrate hexahydrate or nickel chloride hexahydrate; the cobalt source is cobalt nitrate hexahydrate or cobalt chloride hexahydrate.
In the first step, the amount of the added sulfur powder is 2 times or more of the amount of the added metal ion.
The invention has the beneficial effects that:
1) the invention provides a novel method for preparing a hollow-structure metal sulfide electrode material, which is characterized in that a large amount of sulfur powder is added into a solution containing a metal source, so that the metal source and the sulfur powder generate a hollow-structure metal sulfide through a one-step method and are prevented from agglomerating.
2) The preparation process is simple and easy to operate; the surplus sulfur source can be recycled, and is suitable for large-scale preparation and convenient for industrial application.
Drawings
FIG. 1 is a flow chart of the preparation of the hollow structure metal sulfide electrode material of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that all of the following examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
A hollow structure metal sulfide electrode material and a preparation method thereof comprise the following steps:
in the first step, 0.5mmoL Ni (NO) is added3)2·6H2O is added to absolute ethyl alcohol to be fully dissolved, and then 5g of sulfur powder is added. The mixture was mixed well and dried at 80 ℃ for 5 hours.
Secondly, transferring the mixture obtained in the first step into a tubular furnace, heating for 4 hours at 350 ℃ in a nitrogen atmosphere, adding a sulfur gas recovery device at the tail of the tubular furnace to recover the excessive sulfur,
the metal sulfide is recycled, washed by deionized water and kept at the constant temperature of 60 ℃ for 8 hours in a vacuum drying oven to obtain the metal sulfide with the hollow structure.
The electrode material prepared in the embodiment is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, 2mol/L potassium hydroxide is used as electrolyte to form a three-electrode system, and constant current charge and discharge tests are carried out within a voltage range of-0.2-0.6V. When the current density is 1A/g, the specific mass capacity of the material is 1830F/g; when the current density reaches 20A/g, the specific mass capacity of the material can still reach 1020F/g, which shows that the material has excellent rate capability as an energy storage material.
The electrode material prepared in the embodiment is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, 2mol/L potassium hydroxide is used as electrolyte to form a three-electrode system, and repeated constant current charge and discharge tests are carried out within a voltage range of 0-0.6V under the condition that the current density is 10A/g. After 2000 cycles of charge and discharge, the mass specific capacitance of the material still remained 75% of the initial capacity, indicating that the material has excellent stability as an energy storage material.
Example 2
In the first step, 0.5mmoL Ni (NO) is added3)2·6H2O and 0.5mmoL Co (NO)3)2·6H2O was added to an aqueous solution containing 75% ethanol to dissolve it sufficiently, and then 8g of sulfur powder was added. The mixture was mixed well and dried at 70 ℃ for 5 hours.
Secondly, transferring the mixture obtained in the first step into a tubular furnace, heating for 4 hours at 350 ℃ in a nitrogen atmosphere, adding a sulfur gas recovery device at the tail of the tubular furnace to recover the excessive sulfur,
the mixture is recycled, washed by deionized water and kept at the constant temperature of 60 ℃ for 8 hours in a vacuum drying oven to obtain the transition metal sulfide with the hollow structure.
The electrode material prepared in the embodiment is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, 2mol/L potassium hydroxide is used as electrolyte to form a three-electrode system, and constant current charge and discharge tests are carried out within a voltage range of-0.2-0.6V. When the current density is 1A/g, the specific mass capacity of the material is 2040F/g; when the current density reaches 20A/g, the specific mass capacity of the material can still reach 1320F/g, which shows that the material has excellent rate capability as an energy storage material.
The electrode material prepared in the embodiment is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, 2mol/L potassium hydroxide is used as electrolyte to form a three-electrode system, and repeated constant current charge and discharge tests are carried out within a voltage range of 0-0.6V under the condition that the current density is 10A/g. After 2000 cycles of charge and discharge, the mass specific capacitance of the material still remained 80% of the initial capacity, indicating that the material has excellent stability as an energy storage material.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning or limited experiments based on the prior art according to the concepts of the present invention should be within the scope of protection defined by the claims.
Claims (3)
1. A preparation method of a hollow structure metal sulfide electrode material is characterized by comprising the following steps:
firstly, adding a metal source into ethanol or water, dissolving, adding sulfur powder, uniformly mixing the mixture, carrying out vacuum drying at 40-90 ℃ for 1-8 hours, and removing ethanol and water;
secondly, transferring the mixture obtained in the first step into a tubular furnace, heating for 1-8 hours at the temperature of 100-400 ℃ in the atmosphere of inert gas, additionally arranging a sulfur gas recovery device at the tail part of the tubular furnace, recovering excess sulfur for recycling, washing by using deionized water, and keeping the temperature in a vacuum drying oven at 50-80 ℃ for 1-10 hours to obtain the metal sulfide with the hollow structure;
wherein the metal source is a nickel source or/and a cobalt source.
2. The production method according to claim 1, wherein the nickel source is nickel nitrate hexahydrate or nickel chloride hexahydrate; the cobalt source is cobalt nitrate hexahydrate or cobalt chloride hexahydrate.
3. The production method according to claim 1 or 2, wherein the amount of the substance added to the sulfur powder is not less than 2 times the amount of the substance added to the metal ion.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101058437A (en) * | 2007-04-10 | 2007-10-24 | 安徽大学 | Liquid state preparation method for nano cadmium sulfide hollow sphere |
CN105720250A (en) * | 2016-02-21 | 2016-06-29 | 钟玲珑 | Preparation method of graphene/zirconium dioxide hollow sphere/sulfur composite material |
CN110444404A (en) * | 2019-04-24 | 2019-11-12 | 金华莱顿新能源科技有限公司 | A kind of preparation and application of iron cobalt dual-metal sulfide hollow micron ball |
CN110581026A (en) * | 2019-09-03 | 2019-12-17 | 滨州学院 | Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof |
CN110575842A (en) * | 2019-10-12 | 2019-12-17 | 福州大学 | Preparation method of adjustable and controllable yolk-shell structure nitrogen-carbon-doped cobalt molybdenum sulfide counter electrode catalyst |
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- 2021-11-24 CN CN202111401555.3A patent/CN114105227A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101058437A (en) * | 2007-04-10 | 2007-10-24 | 安徽大学 | Liquid state preparation method for nano cadmium sulfide hollow sphere |
CN105720250A (en) * | 2016-02-21 | 2016-06-29 | 钟玲珑 | Preparation method of graphene/zirconium dioxide hollow sphere/sulfur composite material |
CN110444404A (en) * | 2019-04-24 | 2019-11-12 | 金华莱顿新能源科技有限公司 | A kind of preparation and application of iron cobalt dual-metal sulfide hollow micron ball |
CN110581026A (en) * | 2019-09-03 | 2019-12-17 | 滨州学院 | Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof |
CN110575842A (en) * | 2019-10-12 | 2019-12-17 | 福州大学 | Preparation method of adjustable and controllable yolk-shell structure nitrogen-carbon-doped cobalt molybdenum sulfide counter electrode catalyst |
Non-Patent Citations (1)
Title |
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JIWEI ZHANG ET AL.: "Targeted synthesis of NiS and NiS2 nanoparticles for high−performance hybrid supercapacitor via a facile green solid−phase synthesis route" * |
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