CN105680016B - One kind contains addition of C o3O4Lithium sulfur battery anode material and preparation method - Google Patents
One kind contains addition of C o3O4Lithium sulfur battery anode material and preparation method Download PDFInfo
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- CN105680016B CN105680016B CN201610079319.7A CN201610079319A CN105680016B CN 105680016 B CN105680016 B CN 105680016B CN 201610079319 A CN201610079319 A CN 201610079319A CN 105680016 B CN105680016 B CN 105680016B
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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
- H01M4/362—Composites
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 invention discloses one kind to contain addition of C o3O4Lithium sulfur battery anode material, by KS 6, Co3O4Formed with sulfur doping, Co therein3O4It is uniformly filled in sulphur in KS 6 lamella, KS 6 and Co3O4Mass ratio be 1：0.1~0.25, Co3O4The mass ratio of KS 6 and sulphur is 1：1~2.The invention also discloses this kind to contain addition of C o3O4Lithium sulfur battery anode material preparation method.The preparation method of the present invention, using wet-mixing, Co is can obtain after high-temperature calcination3O4The combination products of KS 6, itself and sulphur mixed grinding are obtained into anode composite material of lithium sulfur battery, cost is cheap, simple to operate, is easy to improve production efficiency, beneficial to realizing industrialized production；Anode composite material specific discharge capacity prepared by the present invention is high, and cyclical stability is strong, can be widely used in energy storage field as lithium sulfur battery anode material.
Description
Technical field
The invention belongs to lithium-sulfur cell preparing technical field, is related to one kind and contains addition of C o3O4Lithium-sulphur cell positive electrode material
Material, the invention further relates to this kind to contain addition of C o3O4Lithium sulfur battery anode material preparation method.
Background technology
At present, fossil fuel accounts for leading role in the energy demand of the mankind, however, the resource-constrained of fossil fuel, and
And combustion of fossil fuels environmental pollution is serious.So cleaning and regenerative resource, as the exploitation of wind energy and solar energy is compeled in eyebrow
Eyelash, and these energy needs could be utilized after electrochemical energy storage converts by people, this just need it is reliable, inexpensive,
Environment amenable extensive energy storage system.The theoretical specific capacity of elemental sulfur is 1675mAh/g, and theory reaches than energy
2600Wh/kg, is highest in all known anode material for lithium-ion batteries, and sulphur rich reserves, cheap, low
It is malicious, environmentally friendly, thus sulfenyl material be in anode material for lithium-ion batteries in have development potentiality.
But lithium-sulfur cell is applied in practice process and still suffers from problems with：First, sulphur is that electronics and ion are highly exhausted
Edge material；Second, in battery discharge procedure, more lithium sulfides that sulphur generates during lithiumation can dissolve in the electrolytic solution, cause
Shuttle effect；3rd, due to sulphur and Li2S density is different, and sulphur positive pole has serious volumetric expansion (80% during lithiumation
Left and right).This series of problems can all cause that electrode active material utilization rate is low, cycle performance of battery is poor.
In the last few years, researchers took different measures to suppress shuttle effect, improved lithium-sulfur cell performance.
Sulphur is limited in the duct of conductive material, turns into method the most direct and effective.Such as using different methods, sulphur is limited
Make in the duct of mesoporous carbon, CNT, hollow carbon sphere, graphene or conducting polymer spherical shell, limitation electric discharge intermediate product
The dissolving and shuttle of more lithium sulfides in the electrolytic solution.The above method can improve battery performance to a certain extent, but exist and carry
Body material prepare it is difficult, it is expensive the shortcomings of., can be with using metal nano oxide self character and high-specific surface area feature
More lithium sulfides are adsorbed, prevent it from dissolving and shuttling in the electrolytic solution.Therefore metal nano oxide is prepared into combination electrode material with sulphur
Material can play a part of improving sulphur electric conductivity to a certain extent, suppress shuttle effect, improve cycle performance.Co3O4It is a kind of
Positive electrode, its chemical stability is good, can suppress the oxidation activity of battery surface, and the interface for reducing electrode and electrolyte is anti-
Should, while Co3O4There is no the CoS of shuttle effect with reaction of Salmon-Saxl generationX, so as to improve the cyclical stability of lithium-sulfur cell and electric discharge
Specific capacity, improve the chemical property of cell positive material, extend battery life.
The content of the invention
It is an object of the invention to provide one kind to contain addition of C o3O4Lithium sulfur battery anode material, solve prior art
When middle elemental sulfur makees positive electrode, the problem of electrode active material utilization rate is low, cycle performance of battery is poor be present.
It is a further object of the present invention to provide this kind to contain addition of C o3O4Lithium sulfur battery anode material preparation method.
The technical solution adopted in the present invention is that one kind contains addition of C o3O4Lithium sulfur battery anode material, by KS-6,
Co3O4Formed with sulfur doping, Co therein3O4It is uniformly filled in sulphur in KS-6 lamella, KS-6 and Co3O4Mass ratio be 1：
0.1~0.25, Co3O4The mass ratio of-KS-6 and sulphur is 1：1~2.
Another technical scheme of the present invention is that one kind contains addition of C o3O4Lithium sulfur battery anode material system
Preparation Method, specifically implement according to following steps：
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：0.5~1 mass ratio is put into ball grinder, adds appropriate second
Alcohol, after wet-mixing 1.5-2 hours, in 70 DEG C of oven drying 12-15h；
Step 2) is by mixture high-temperature calcination 4 under the conditions of 250 DEG C~400 DEG C protective gas in tube furnace obtained by step 1)
~7 hours, KS-6 and Co in the product obtained after calcining3O4Mass ratio be 1：0.1~0.25；
Step 3) is by the calcined product of step 2) and sulphur with 1：1~2 mixed grinding is uniform, is placed in hydrothermal reaction kettle, leads to
After entering 20-30 minute argon gas, reactor is placed in 150-160 DEG C of insulation 10-12 hour, obtained containing addition of C o3O4Lithium sulphur
Cell positive material.
The invention has the advantages that using wet-mixing, Co is can obtain after high-temperature calcination3O4- KS-6 combination products,
Itself and sulphur mixed grinding are obtained into anode composite material of lithium sulfur battery, cost is cheap, simple to operate, is easy to improve production efficiency,
Beneficial to realizing industrialized production；Addition of C o3O4Chemical stability is good, can suppress electrode surface oxidation activity, reduce electrode with
The interfacial reaction of electrolyte, so as to improve the cyclical stability of lithium-sulfur cell and actual specific capacity, improve battery material electrochemistry
Performance, extend battery life.Anode composite material specific discharge capacity prepared by the present invention is high, and cyclical stability is strong, can be used as lithium
Sulphur cell positive electrode material is widely used in energy storage field.
Brief description of the drawings
Fig. 1 is Co prepared by embodiment 13O4The scanning electron microscope (SEM) photograph of-KS-6/S anode composite materials；
Fig. 2 is Co prepared by embodiment 13O4The X-ray diffractogram of-KS-6/S anode composite materials；
Fig. 3 is Co prepared by embodiment 13O4- KS-6/S anode composite materials and no added Co3O4KS-6/S positive poles answer
First charge-discharge curve of the condensation material under 0.1C；
Fig. 4 is Co prepared by embodiment 13O4Cycle performance and coulombic efficiency of-the KS-6/S anode composite materials under 0.1C
Figure.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The present invention contains addition of C o3O4Lithium sulfur battery anode material (abbreviation anode composite material), by KS-6, Co3O4
Formed with sulfur doping, Co therein3O4It is uniformly filled in sulphur in KS-6 lamella, KS-6 and Co3O4Mass ratio be 1：
(0.1~0.25), Co3O4The mass ratio of-KS-6 and sulphur is 1：(1~2).
The present invention contains addition of C o3O4Lithium sulfur battery anode material preparation method, it is specifically real according to following steps
Apply：
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：The mass ratio of (0.5~1) is put into ball grinder, is added appropriate
Ethanol, after wet-mixing 1.5-2 hours, in 70 DEG C of oven drying 12-15h.
Step 2) is by mixture high-temperature calcination 4 under the conditions of 250 DEG C~400 DEG C protective gas in tube furnace obtained by step 1)
~7 hours, KS-6 and Co in the product obtained after calcining3O4(by Co (NO3)2·6H2O decompose produce) mass ratio be 1：(0.1
~0.25).
Step 3) is by the calcined product of step 2) and sulphur with 1：(1~2) mixed grinding is uniform, is placed in hydrothermal reaction kettle,
After being passed through 20-30 minute argon gas, reactor is placed in 150-160 DEG C of insulation 10-12 hour, obtained containing addition of C o3O4Lithium
Sulphur cell positive electrode material.
Above-mentioned steps 1) in wet ball grinding solvent from one of water, ethanol or acetone low boiling point solvent.
Above-mentioned steps 2) in tube furnace calcining protective gas from nitrogen, at least one of inert gas.
Embodiment 1
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：1 mass ratio is put into ball grinder, adds ethanol in proper amount, wet
After method mixes 1.5 hours, in 70 DEG C of oven drying 12h.
Step 2) high-temperature calcination 5 hours under 300 DEG C of condition of nitrogen gas in tube furnace by mixture obtained by step 1), after calcining
KS-6 and Co in obtained product3O4(by Co (NO3)2·6H2O decompose produce) mass ratio be 1：0.25.
Step 3) is by the calcined product of step 2) and sulphur with 1：1 mixed grinding is uniform, is placed in hydrothermal reaction kettle, is passed through 20
After minute argon gas, reactor is placed in 156 DEG C and is incubated 10 hours, is obtained containing addition of C o3O4Lithium sulfur battery anode material.
Embodiment 2
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：0.5 mass ratio is put into ball grinder, adds ethanol in proper amount,
After wet-mixing 2 hours, in 70 DEG C of oven drying 15h.
Step 2) high-temperature calcination 4 hours under 400 DEG C of condition of nitrogen gas in tube furnace by mixture obtained by step 1), after calcining
KS-6 and Co in obtained product3O4(by Co (NO3)2·6H2O decompose produce) mass ratio be 1：0.1.
Step 3) is by the calcined product of step 2) and sulphur with 1：1.5 mixed grindings are uniform, are placed in hydrothermal reaction kettle, are passed through
After 25 minutes argon gas, reactor is placed in 155 DEG C and is incubated 12 hours, is obtained containing addition of C o3O4Lithium-sulphur cell positive electrode material
Material.
Embodiment 3
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：0.75 mass ratio is put into ball grinder, adds proper amount of acetone,
After wet-mixing 1.5 hours, in 70 DEG C of oven drying 12h.
Step 2) high-temperature calcination 7 hours under 250 DEG C of condition of nitrogen gas in tube furnace by mixture obtained by step 1), after calcining
KS-6 and Co in obtained product3O4(by Co (NO3)2·6H2O decompose produce) mass ratio be 1：0.23.
Step 3) is by the calcined product of step 2) and sulphur with 1：2 mixed grindings are uniform, are placed in hydrothermal reaction kettle, are passed through 30
After minute argon gas, reactor is placed in 156 DEG C and is incubated 12 hours, is obtained containing addition of C o3O4Lithium sulfur battery anode material.
Summary embodiment, battery assembling is further carried out using the sample prepared by embodiment 1-3, by the lithium of gained
Sulphur cell positive electrode composite is with KS-6, Kynoar (PVDF) according to mass ratio 7：2：1 is weighed, with N- methylpyrroles
Alkanone is that solvent is modulated into uniform pulpous state, and drying tabletting is carried out after coating, and positive plate is made in cut-parts, and lithium piece is as negative plate, electricity
It is containing 1%LiNO to solve liquid31mol/L LiTFSI/DOL-DME (1：1, V%), barrier film Celgard2300, it is assembled into button
CR2025 batteries.
Fig. 1 is Co prepared by embodiment 13O4The scanning electron microscope (SEM) photograph of-KS-6/S anode composite materials, can be clearly from Fig. 1
See sulphur and Co3O4Uniformly cover between KS-6 lamellas.
Fig. 2 is Co prepared by embodiment 13O4The X-ray diffractogram of-KS-6/S anode composite materials, as can be seen from Figure 2
Composite has Co3O4With S characteristic diffraction peak.
Fig. 3 is Co prepared by embodiment 13O4- KS-6/S anode composite materials and no added Co3O4KS-6/S positive poles answer
First charge-discharge curve of the condensation material under 0.1C.Co3O4- KS-6/S anode composite material first discharge specific capacities are
1260mAh/g, because electrolyte initial insult is bad, therefore discharge platform is relatively low first, discharge platform 2.0V, and no added
Co3O4KS-6/S anode composite materials first discharge specific capacity be 676mAh/g, it was demonstrated that addition Co3O4Electricity can be significantly improved
The first discharge specific capacity in pond.
Fig. 4 is Co prepared by embodiment 13O4Cycle performance and coulomb of-the KS-6/S anode composite materials under the conditions of 0.1C
Efficiency chart.As seen from Figure 4, discharge capacity 539mAh/g after circulating 50 times, capability retention 42.8%, coulombic efficiency is 95%
Left and right, mix Co3O4There is remarkable result to the capability retention and coulombic efficiency of battery.
Charge and discharge cycles 50 times under the conditions of 0.1C of the gained battery of embodiment 2, first discharge specific capacity 1176mAh/g,
Capacity is maintained at 450mAh/g, capability retention 38.3% after 50 times.
Charge and discharge cycles 50 times under the conditions of 0.1C of the gained battery of embodiment 3, first discharge specific capacity 1054mAh/g,
Capacity is maintained at 432mAh/g, capability retention 41.0% after 50 times.
By method provided by the invention, Co can be reached3O4It is uniformly filled in sulphur in KS-6 lamella, compares ball-milling method
The Co of addition3O4More uniformly, so as to give full play to Co3O4Effect, improve the cyclical stability and specific capacity of lithium-sulfur cell.
Claims (3)
1. one kind contains addition of C o3O4Lithium sulfur battery anode material preparation method, should addition of C o be contained3O4Lithium sulphur electricity
Pond positive electrode, by KS-6, Co3O4Formed with sulfur doping, Co therein3O4It is uniformly filled in sulphur in KS-6 lamella, KS-6
With Co3O4Mass ratio be 1：0.1~0.25, Co3O4The mass ratio of-KS-6 and sulphur is 1：1~2,
Characterized in that, specifically implement according to following steps：
Step 1) is by KS-6 and Co (NO3)2·6H2O presses 1：0.5~1 mass ratio is put into ball grinder, adds ethanol in proper amount, wet
After method mixing 1.5-2 hours, in 70 DEG C of oven drying 12-15h；
Step 2) is by mixture high-temperature calcination 4~7 under the conditions of 250 DEG C~400 DEG C protective gas in tube furnace obtained by step 1)
Hour, KS-6 and Co in the product obtained after calcining3O4Mass ratio be 1：0.1~0.25；
Step 3) is by the calcined product of step 2) and sulphur with 1：1~2 mixed grinding is uniform, is placed in hydrothermal reaction kettle, is passed through 20-
After 30 minutes argon gas, reactor is placed in 150-160 DEG C of insulation 10-12 hour, obtained containing addition of C o3O4Lithium-sulfur cell
Positive electrode.
2. according to claim 1 contain addition of C o3O4Lithium sulfur battery anode material preparation method, its feature exists
In：It is one of water, ethanol or acetone that wet ball grinding solvent, which is selected, in described step 1).
3. according to claim 1 contain addition of C o3O4Lithium sulfur battery anode material preparation method, its feature exists
In：Tube furnace calcining protective gas is from least one of nitrogen, inert gas in described step 2).
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| CN108281633B (en) * | 2018-01-26 | 2020-11-27 | 南开大学 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN108232115B (en) * | 2018-01-26 | 2020-12-15 | 南开大学 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN110993902B (en) * | 2019-11-12 | 2023-02-14 | 东北师范大学 | Lithium-sulfur battery with positively charged organic small molecule positive electrode additive |
| CN112054196B (en) * | 2020-08-11 | 2022-03-08 | 深圳市德创美科技有限公司 | Waste paper-based porous carbon-coated S-Co3O4The positive electrode material of the lithium-sulfur battery and the preparation method thereof |
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| CN102945966A (en) * | 2012-12-07 | 2013-02-27 | 中国科学院上海硅酸盐研究所 | Positive pole composite system of lithium sulphur battery containing catalytic additive |
| CN104577080A (en) * | 2014-12-29 | 2015-04-29 | 中国地质大学（武汉） | Composite cathode material used for lithium-sulfur battery and having high-rate performance and preparation method |
| CN105118972A (en) * | 2015-07-06 | 2015-12-02 | 浙江大学 | Metal hydroxide coated carbon and sulfur lithium-sulfur battery positive electrode material, and preparation method and application thereof |
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| US9203084B2 (en) * | 2013-08-08 | 2015-12-01 | Nanotek Instrurments, Inc. | Cathode active material-coated discrete graphene sheets for lithium batteries and process for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102945966A (en) * | 2012-12-07 | 2013-02-27 | 中国科学院上海硅酸盐研究所 | Positive pole composite system of lithium sulphur battery containing catalytic additive |
| CN104577080A (en) * | 2014-12-29 | 2015-04-29 | 中国地质大学（武汉） | Composite cathode material used for lithium-sulfur battery and having high-rate performance and preparation method |
| CN105118972A (en) * | 2015-07-06 | 2015-12-02 | 浙江大学 | Metal hydroxide coated carbon and sulfur lithium-sulfur battery positive electrode material, and preparation method and application thereof |
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