CN108091874A - A kind of preparation method of the nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode - Google Patents
A kind of preparation method of the nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode Download PDFInfo
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- CN108091874A CN108091874A CN201711352912.5A CN201711352912A CN108091874A CN 108091874 A CN108091874 A CN 108091874A CN 201711352912 A CN201711352912 A CN 201711352912A CN 108091874 A CN108091874 A CN 108091874A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of preparation method of the nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode, including：Cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate and sodium acetate are dissolved in solvent, add in potassium peroxydisulfate or ammonium persulfate, stirring, it pours into reaction kettle and reacts, cool down, washing, centrifugation, it is dry, it is dissolved in solvent, ultrasound adds in nine hydrated sodium sulfides, pours into reaction kettle and react, cooling is washed, centrifugation, it is dry to get.The present invention is simple and practicable, and safety and environmental protection, raw material is easy to get, at low cost, suitable for large-scale production；The nanometer nickel-cobalt sulphur particle size being prepared is small, improves specific surface area, has good fixation to polysulfide, it will be apparent that weaken the shuttle effect of battery.In addition, compared to commonly used to solid sulfur oxide, binary sulfide, nickel cobalt sulphur has good electric conductivity.The cyclical stability of battery is improved in the case where ensureing certain specific capacity, is solving the problems, such as that lithium-sulfur cell there are huge potentiality presently, there are this aspect.
Description
Technical field
The invention belongs to the preparation field of ion battery electrode materials, more particularly to a kind of receiving as lithium-sulphur cell positive electrode
The preparation method of rice nickel cobalt sulphur particle.
Background technology
The efficient of the energy utilizes and stores always advancing one big difficult scientific problems of energy development.During this period, lithium from
Sub- battery gets their way into people's lives as a kind of high load, portable equipment, and lithium-sulfur cell has very high theoretical specific volume
It measures (1675mAh/g), is much higher by the lithium ion battery (372mAh/g) that current graphite makees cathode, therefore as there is very much prospect
Next-generation energy storage device.However, lithium-sulfur cell in addition to having the shortcomings that conventional lithium ion battery, also has even more serious ask
Topic：Lithium metal can increasingly generate Li dendrite in charge and discharge process, and the final membrane that pierces through causes battery short circuit；Due to the use of be
Lithium metal, thus it is very high to the sealing performance requirement of battery；The electric discharge more lithium sulfides of intermediate product can be dissolved in electrolyte, and in charge and discharge
It reacts in electric process as electrolyte reaches cathode with lithium metal, causes battery performance deep fades；Sulphur simple substance is insulation
Body, the internal resistance of cell are very big；Final product lithium sulfide density is less than sulphur simple substance, this causes anode volume to expand, and destroys battery structure.
Sulphur is mainly coated in the nano material with captured sulfur result by current solution；Diagram modification；Electrolyte is modified；Make
Use solid electrolyte.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode
Preparation method, this method is simple and practicable, and safety and environmental protection, raw material is easy to get, at low cost, and suitable for large-scale production, what is be prepared receives
The lithium-sulphur cell positive electrode that rice nickel cobalt sulphur particle can be used as load emerging makes up sulphur simple substance on electric conductivity the defects of and subtracts
The dissolving of few intermediate product promotes the high rate performance and cyclical stability of battery.
A kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode of the present invention, concretely comprises the following steps：
(1) by cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate and sodium acetate using mass ratio as 1-2:1-2:20-60 is dissolved in molten
Mixed solution is formed in agent, adds in potassium peroxydisulfate or ammonium persulfate, stirring obtains solution, wherein sodium acetate is dense in mixed solution
It is 10-30 to spend for the mass ratio of 0.025-0.075g/mL, sodium acetate and potassium peroxydisulfate or ammonium persulfate:1-2；
(2) solution in step (1) is poured into reaction kettle and reacted, cooled down, washed, centrifuged, it is dry, obtain nanometer cobalt acid
Nickel；
(3) nano nickel cobalt oxide in step (2) is dissolved in formation nano nickel cobalt oxide solution in solvent, ultrasound adds in nine hydrations
Vulcanized sodium is poured into reaction kettle and reacted, and is cooled down, and is washed, and is centrifuged, dry, obtains nanometer nickel-cobalt sulphur particle, wherein nano nickel cobalt oxide
Solution concentration is 0.75-2.25mg/mL, and the mass ratio of nano nickel cobalt oxide and nine hydrated sodium sulfides is 1-3:24-32.
Mixing time is 30-60min in the step (1).
Solvent is deionized water in the step (1), (3).
Reaction in reaction kettle is poured into the step (2) is specially：140- is warming up to the heating rate of 5-10 DEG C/min
180 DEG C of reaction 6-8h；Drying temperature is 60 DEG C, drying time 12h.
The filling rate poured into the step (2), (3) in reaction kettle is 80%；Washing is first to be washed with deionized water
It washs and is washed again with ethyl alcohol.
Ultrasonic time is 15-30min in the step (3)；Pouring into reaction in reaction kettle is specially：With 5-10 DEG C/min's
Heating rate is warming up to 90-120 DEG C of reaction 6-14h；Drying temperature is 60 DEG C, drying time 12-24h.
Nanometer nickel-cobalt sulphur particle size is in 5nm or so in the step (3).
Nanometer nickel-cobalt sulphur particle is used as lithium-sulphur cell positive electrode in the step (3), is specially：
(1) by nanometer nickel-cobalt sulphur and sublimed sulfur using mass ratio as 1:2-5 is mixed, and is reacted under inert gas shielding, is cooled down,
Obtain sulphur/nickel cobalt sulphur composite material；
(2) by sulphur/nickel cobalt sulphur composite material in step (1) and Kynoar PVDF, acetylene black using mass ratio as 6-7:
1-2:2-3 is mixed, and grinding is dissolved in solvent, coated on being handled on clean aluminium foil, obtains positive pole plate of lithium-sulfur cell.
Inert gas is nitrogen or argon gas in the step (1)；Reaction time is 15-24h, reaction temperature 150-160
℃。
Solvent is NMP in the step (2)；Processing is specially：It is placed in 12-24h in 60 DEG C of vacuum drying ovens.
Positive pole plate of lithium-sulfur cell, by the use of lithium metal as cathode assembled battery, is tested in glove box in the step (2)
Cycle performance and high rate performance.
The present invention prepares nanometer nickel-cobalt sulphur particle using a kind of simple hydro-thermal method, and nanometer nickel-cobalt sulphur particle is as solid sulphur material
Material improves the cycle performance of lithium-sulfur cell.
Advantageous effect
(1) present invention is simple and practicable, and safety and environmental protection, raw material is easy to get, at low cost, suitable for large-scale production；
(2) nano-particles size that the present invention is prepared is small, has been correspondingly improved specific surface area, and nickel cobalt sulphur is to more
Sulfide has good fixation, can significantly weaken the shuttle effect of battery.In addition, compared to commonly used to solid sulphur
Oxide, binary sulfide, nickel cobalt sulphur have good electric conductivity.Battery is improved in the case where ensureing certain specific capacity
Cyclical stability is solving the problems, such as that lithium-sulfur cell has huge potentiality presently, there are this aspect.
Description of the drawings
Fig. 1 is nanometer nickel-cobalt sulphur particle low power field emission scanning electron microscope figure prepared by embodiment 1；
Fig. 2 is nanometer nickel-cobalt sulphur particle high power Flied emission transmission electron microscope picture prepared by embodiment 1；
Fig. 3 be in embodiment 4 nanometer nickel-cobalt sulphur particle be used as lithium-sulphur cell positive electrode when respectively 0.1C, 0.2C, 0.5C,
High rate performance test chart under 1C, 2C, 1C, 0.5C, 0.2C, 0.1C；
Fig. 4 is that stable circulation performance when nanometer nickel-cobalt sulphur particle is used as lithium-sulphur cell positive electrode in embodiment 4 under 1C is surveyed
Attempt.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
(1) 75mg cabaltous nitrate hexahydrates, 75mg Nickelous nitrate hexahydrates and 3g sodium acetates are weighed and is dissolved in 40mL deionized waters
In, it adds 0.2g potassium peroxydisulfates or ammonium persulfate and stirs 30min, obtain pink solution.
(2) pink solution that step (1) obtains is poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal
Be placed in constant temperature oven, with the heating rate of 10 DEG C/min be warming up to 180 DEG C reaction 6h, spent respectively after natural cooling from
Sub- water and ethyl alcohol washing, centrifuge repeatedly to no heteroion, are placed in 12h in 60 DEG C of vacuum drying ovens, obtain fluffy dry
Dry black cobalt acid nickel nanometer powder.
(3) black cobalt acid nickel nanometer powder in 30mg steps (2) is taken, adds in 40mL deionized waters and ultrasonic disperse 30min,
Nine hydrated sodium sulfides of 0.96g are added in, mixed liquor are poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal is placed on
In constant temperature oven, 120 DEG C of reaction 6-14h are warming up to the heating rate of 10 DEG C/min, use deionization respectively after natural cooling
Water and ethyl alcohol washing are centrifuged repeatedly to no heteroion, are placed in 60 DEG C of vacuum drying ovens for 24 hours, obtaining receiving for black
Rice nickel cobalt sulphur particle powder (Ni1.5Co1.5S4)。
Fig. 1 and Fig. 2 show：Product nanometer nickel-cobalt sulphur particle granules are uniform in size, and size is 5 rans.
Embodiment 2
(1) 100mg cabaltous nitrate hexahydrates, 50mg Nickelous nitrate hexahydrates and 3g sodium acetates are weighed and is dissolved in 40mL deionized waters
In, it adds 0.2g potassium peroxydisulfates or ammonium persulfate and stirs 60min, obtain pink solution.
(2) pink solution that step (1) obtains is poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal
Be placed in constant temperature oven, with the heating rate of 10 DEG C/min be warming up to 180 DEG C reaction 6h, spent respectively after natural cooling from
Sub- water and ethyl alcohol washing are centrifuged repeatedly to no heteroion, are placed in 12h in 60 DEG C of vacuum drying ovens, are obtained fluffy dry
Dry black cobalt acid nickel nanometer powder.
(3) black cobalt acid nickel nanometer powder in 30mg steps (2) is taken, adds in 40mL deionized waters and ultrasonic disperse 30min,
Nine hydrated sodium sulfides of 0.96g are added in, mixed liquor are poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal is placed on
In constant temperature oven, 120 DEG C of reaction 6h are warming up to the heating rate of 10 DEG C/min, after natural cooling respectively with deionized water and
Ethyl alcohol washing is centrifuged repeatedly to no heteroion, is placed in 60 DEG C of vacuum drying ovens for 24 hours, obtaining the nano nickel of black
Cobalt sulphur particle powder (NiCo2S4)。
Embodiment 3
(1) 50mg cabaltous nitrate hexahydrates, 100mg Nickelous nitrate hexahydrates and 3g sodium acetates are weighed and is dissolved in 40mL deionized waters
In, it adds 0.2g potassium peroxydisulfates or ammonium persulfate and stirs 60min, obtain pink solution.
(2) pink solution that step (1) obtains is poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal
Be placed in constant temperature oven, with the heating rate of 10 DEG C/min be warming up to 180 DEG C reaction 6h, spent respectively after natural cooling from
Sub- water and ethyl alcohol washing are centrifuged repeatedly to no heteroion, are placed in 12h in 60 DEG C of vacuum drying ovens, are obtained fluffy dry
Dry black cobalt acid nickel nanometer powder.
(3) black cobalt acid nickel nanometer powder in 30mg steps (2) is taken, adds in 40mL deionized waters and ultrasonic disperse 30min,
Nine hydrated sodium sulfides of 0.96g are added in, mixed liquor are poured into 50mL polytetrafluoroethylene (PTFE) autoclave liners, good seal is placed on
In constant temperature oven, 120 DEG C of reaction 6h are warming up to the heating rate of 5-10 DEG C/min, use deionized water respectively after natural cooling
With ethyl alcohol washing, centrifugation repeatedly to no heteroion, it is placed in 60 DEG C of vacuum drying ovens for 24 hours, obtaining the nanometer of black
Nickel cobalt sulphur particle powder (Ni2CoS4)。
Embodiment 4
(1) nanometer nickel-cobalt sulphur particle powder 40mg in embodiment 2 and sublimed sulfur 80mg is mixed, in temperature under nitrogen protection
For 155 DEG C of heat preservations for 24 hours, cooled to room temperature obtains sulphur/nickel cobalt sulphur composite material.
(2) by sulphur in step (1)/nickel cobalt sulphur composite material 42mg and Kynoar PVDF 6mg, acetylene black 12mg mixes
It closes, grinding is uniform, coated on clean aluminium foil after being dissolved with NMP, is subsequently placed in 60 DEG C of vacuum drying ovens for 24 hours, obtains
To positive pole plate of lithium-sulfur cell.
(3) by pole piece in step (2) in glove box, by the use of lithium metal as cathode assembled battery, test high rate performance and
Cyclical stability.Fig. 3 shows：Battery charge and discharge under low range 0.1C, 0.2C, 0.5C have higher capacity, and in high magnification
Charge and discharge electric energy keeps capacity to stablize under 1C, 2C.
Fig. 4 shows：Battery is under 1C after the circle of charge and discharge 1000, and specific capacity is reduced to 200mAh/g from 550mAh/g, quite
In each charge-discharge cycle capacity attenuation 0.064%, coulombic efficiency about 97% illustrates that the battery has preferable cyclical stability.
Claims (9)
1. a kind of preparation method of the nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode, concretely comprises the following steps：
(1) by cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate and sodium acetate using mass ratio as 1-2:1-2:20-60 is dissolved in solvent
Mixed solution is formed, adds in potassium peroxydisulfate or ammonium persulfate, stirring obtains solution, wherein sodium acetate concentration is in mixed solution
0.025-0.075g/mL, sodium acetate are 10-30 with the mass ratio of potassium peroxydisulfate or ammonium persulfate:1-2；
(2) solution in step (1) is poured into reaction kettle and reacted, cooled down, washed, centrifuged, it is dry, obtain nano nickel cobalt oxide；
(3) nano nickel cobalt oxide in step (2) is dissolved in formation nano nickel cobalt oxide solution in solvent, ultrasound adds in nine hydration vulcanizations
Sodium is poured into reaction kettle and reacted, and is cooled down, and is washed, and is centrifuged, dry, obtains nanometer nickel-cobalt sulphur particle, wherein nano nickel cobalt oxide solution
Concentration is 0.75-2.25mg/mL, and the mass ratio of nano nickel cobalt oxide and nine hydrated sodium sulfides is 1-3:24-32.
2. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that mixing time is 30-60min in the step (1).
3. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that solvent is deionized water in the step (1), (3).
4. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that reaction in reaction kettle is poured into the step (2) is specially：140- is warming up to the heating rate of 5-10 DEG C/min
180 DEG C of reaction 6-8h；Drying temperature is 60 DEG C, drying time 12h.
5. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that the filling rate poured into the step (2), (3) in reaction kettle is 80%；Washing is first to be washed with deionized
It is washed again with ethyl alcohol.
6. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that ultrasonic time is 15-30min in the step (3)；Pouring into reaction in reaction kettle is specially：With 5-10 DEG C/min's
Heating rate is warming up to 90-120 DEG C of reaction 6-14h；Drying temperature is 60 DEG C, drying time 12-24h.
7. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 1, special
Sign is that nanometer nickel-cobalt sulphur particle is used as lithium-sulphur cell positive electrode in the step (3), is specially：
(1) by nanometer nickel-cobalt sulphur and sublimed sulfur using mass ratio as 1:2-5 is mixed, and is reacted under inert gas shielding, is cooled down, is obtained
Sulphur/nickel cobalt sulphur composite material；
(2) by sulphur/nickel cobalt sulphur composite material in step (1) and Kynoar PVDF, acetylene black using mass ratio as 6-7:1-2:
2-3 is mixed, and grinding is dissolved in solvent, coated on being handled on clean aluminium foil, obtains positive pole plate of lithium-sulfur cell.
8. a kind of preparation method of nanometer nickel-cobalt sulphur particle as lithium-sulphur cell positive electrode according to claim 7, special
Sign is that inert gas is nitrogen or argon gas in the step (1)；Reaction time is 15-24h, reaction temperature 150-160
℃。
9. a kind of lithium-sulphur cell positive electrode according to claim 7 preparation method of sulphur/nickel cobalt sulphur composite material, feature
It is, solvent is NMP in the step (2)；Processing is specially：It is placed in 12-24h in 60 DEG C of vacuum drying ovens.
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| CN114149032A (en) * | 2021-12-06 | 2022-03-08 | 安徽师范大学 | Nano-hierarchical nickel cobaltous oxide material, preparation method thereof, semi-solid dual-ion battery anode slurry and semi-solid dual-ion battery |
| US11335900B2 (en) * | 2018-11-12 | 2022-05-17 | Zhejiang A & F University | Nanosheet composite for cathode of lithium-sulfur battery, preparation method thereof and electrode and battery comprising the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109378449A (en) * | 2018-09-13 | 2019-02-22 | 天津大学 | NiCo for lithium sulfur battery anode material2S4The preparation method of coated porous carbon skeleton |
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| US11335900B2 (en) * | 2018-11-12 | 2022-05-17 | Zhejiang A & F University | Nanosheet composite for cathode of lithium-sulfur battery, preparation method thereof and electrode and battery comprising the same |
| CN114149032A (en) * | 2021-12-06 | 2022-03-08 | 安徽师范大学 | Nano-hierarchical nickel cobaltous oxide material, preparation method thereof, semi-solid dual-ion battery anode slurry and semi-solid dual-ion battery |
| CN114149032B (en) * | 2021-12-06 | 2024-01-16 | 安徽师范大学 | Nano hierarchical structure nickel thiocobalt material, preparation method thereof, semi-solid double-ion battery anode slurry and semi-solid double-ion battery |
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