CN106169561B - A kind of sulphur system anode composite pole piece includes its battery and preparation method thereof - Google Patents
A kind of sulphur system anode composite pole piece includes its battery and preparation method thereof Download PDFInfo
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- CN106169561B CN106169561B CN201610875539.0A CN201610875539A CN106169561B CN 106169561 B CN106169561 B CN 106169561B CN 201610875539 A CN201610875539 A CN 201610875539A CN 106169561 B CN106169561 B CN 106169561B
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M4/366—Composites as layered products
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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
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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 a kind of sulphur system anode composite pole piece, include its battery and preparation method thereof.Sulphur system provided by the present invention combination electrode is the anode of binder free, its preparation process is as follows: in a solvent by the dispersion of lamella class carbon, form dispersion liquid, then sulphur based material, fluorocarbons, polyacrylonitrile are added in the dispersion liquid, it is uniformly mixed, anode active material slurry is made coated in current collector aluminum foil, through drying, is prepared into sulphur system cell composite anode pole piece.The advantage of the sulphur system anode composite of binder free provided by the invention is: lamella class carbon material is coated on sulphur based material, fluorination carbon surface, forms buffer layer；Polyacrylonitrile constructs stable structure in anode, and (1) can be with the expansion and contraction of buffer electrode material；It (2) can be by positive effective active matter confinement；(3) positive-active ratio is high；(4) low raw-material cost can be mass-produced.
Description
Technical field
The invention belongs to technical field of chemical power, and in particular to sulphur system anode pole piece, the preparation method of binder free
And its applied battery.
Background technique
Lithium ion battery is since the nineties in last century realizes industrialization, at the electrochmical power source of most practicability,
And has the tendency that further expansion application range in the fields such as power battery and energy-storage battery.But lithium ion battery is by existing electricity
(cobalt acid lithium actual capacity about 140mAh/g, the theoretical of graphite-like Carbon anode hold the especially positive lower storage lithium capacity limit in pole
Measure 372mAh/g), it is limited to further increase energy density spatial.As New Generation of Electric Vehicle, unmanned vehicle, electronics produce
The development in the fields such as product, militay space flight aircraft, demand of the army and the people's every profession and trade to the energy-storage battery of high specific energy are more urgent.
Sulphur is the higher solid-state positive electrode of theoretical specific capacity, matches the light metal cathode of higher capacity, can obtain compared with
High battery theory specific energy.Such as lithium and sulphur collocation composition lithium-sulfur cell, it is specific energy that theoretical specific energy, which reaches ~ 2600Wh/kg,
One of secondary cell system of highest solid state electrode.And other light metals and sulphur is used to arrange in pairs or groups, it also can get higher theory
Specific energy.For fluorocarbons as positive electrode, specific capacity is high, has stable discharge platform, storage life length, uses temperature model
Enclose width, use its as the lithium primary battery of positive electrode be the solid anode lithium battery as commodity at first.In sode cell
Using greatly having widened the application range of fluorinated carbon material.
And both materials have a common problem although specific capacity all with higher, active material is following
It is easy to diffuse in liquid electrolyte during ring.For sulphur system anode, the electric discharge of sulphur will lead to using liquid electrolyte
The more lithium sulfides of product are dissolved in electrolyte, and are diffused into cathode and are reacted, and shuttle effect occurs when charging, and charging is caused to imitate
Rate is low, self discharge is big.Also one layer of insulant can be deposited in negative terminal surface simultaneously, deteriorate battery performance, especially capacity declines
Subtract fast.For fluorocarbons anode, when recycling in sode cell, the active fluorine for having part is dissolved in electrolyte, causes capacity attenuation
Comparatively fast.If the advantages of constructing a kind of electrode, while utilizing the height ratio capacity of sulphur system anode and fluorocarbons anode, and can will recycle
The effective active matter confinement generated in the process, effectively improves the cyclical stability of such battery, and development potentiality space is huge.
Summary of the invention
The purpose of the present invention is for existing sulphur system anode, polysulfide dissolution in the electrolytic solution, is formed in cyclic process
Shuttle effect, the low problem of coulombic efficiency and fluorocarbons anode the problem of active material dissolution, provide in sode cell
A kind of preparation method of the sulphur system anode composite pole piece of binder free, the battery that Ji Youqi is related to.
In order to achieve the above objectives, the present invention provides a kind of preparation methods of sulphur system anode composite pole piece: first by lamella
Class carbon material disperses in a solvent, to form lamella class carbon dispersion liquid；Then sulphur based material, fluorocarbons, polyacrylonitrile are added to
In the lamella class carbon dispersion liquid, it is prepared into anode sizing agent；Above-mentioned slurry is finally coated in collection liquid surface, drying
Obtain sulphur system anode composite pole piece.The lamella class carbon material is coated on sulphur based material, fluorination carbon surface, forms buffer layer, can be with
The expansion and contraction of buffer electrode material；Polyacrylonitrile constructs stable structure in anode, can be by positive effective active object
Matter confinement.Lamella class carbon is coated on the surface of positive active material in anode, forms the structure of similar " sandwich ", and gathers
Acrylonitrile then by each component in anode effective " gluing " together, the two has synergistic effect.
Preferably, described lamella class carbon material selection graphene (GNS), graphene oxide (GO), nitrogen-doped graphene,
One of sulfur doping graphene or phosphorus sulfur doping graphene etc. are a variety of.
Preferably, the mass fraction of carbon is 3 ~ 6% in lamella class carbon dispersion liquid.
Preferably, the solvent be dimethylformamide (DMF), n,N-dimethylacetamide (DMAC), dimethyl it is sub-
One of sulfone (DMSO), N-Methyl pyrrolidone (NMP) etc..
Preferably, sulphur based material selection elemental sulfur and its sulphur carbon composite, organic sulfur compound, nothing in positive active material
One of machine sulfide etc. is a variety of, and in anode, mass fraction is 30 ~ 80%.
Preferably, the fluorinated carbon material of positive active material is fluorographite, carbon fluoride nano-tube, fluorinated graphene, fluorine
Change one of carbon fiber, fluorocarbons nanometer disk, fluorination coke etc. or a variety of, fluorine carbon molar ratio is 0.33 ~ 1.2, in anode
In, mass ratio is 30 ~ 80%.
Preferably, it is 20nm ~ 40 μm that polyacrylonitrile (PAN), which is partial size, and mass fraction is 3 ~ 5%.
Preferably, the sulphur system anode composite pole piece prepared is dried in vacuo 12 under the conditions of 70 ~ 90 DEG C ~ for 24 hours.
The battery of the sulphur system anode composite assembling prepared using method provided by the present invention the present invention also provides a kind of,
Include:
Cathode: periodic table of elements group ia, Group IIA, aluminium and its alloy or intermetallic compound are selected from.
Electrolyte: electrolyte includes organic solvent and electrolytic salt.The organic solvent is selected from dimethyl carbonate (DMC), carbon
Diethyl phthalate (DEC), 1,2- dimethoxy-ethane (DME), tetrahydrofuran (THF), methyl acetate (MA), diethylene glycol dimethyl ether,
Triglyme, tetraethylene glycol dimethyl ether, propylene carbonate (PC), carbonic acid ethylidene ester (EC), acetonitrile, dimethyl sulfoxide, two
Methylformamide, dimethyl acetamide, gamma-butyrolacton (GBL), N- methyl-pyrrolidon (NMP), methyl ethyl carbonate, carbonic acid are sub-
Vinyl acetate, dioxolanes, dioxane, dimethoxy-ethane, or mixtures thereof.Electrolytic salt is selected from MM ' F6Or MM ' F4Salt,
Wherein M is metal identical at least one of cathode metal, and M ' is the member selected from three valent phosphors, arsenic, antimony and boron
Element, such as lithium salts LiPF6、LiAsF6、LiSbF6、LiBF4、LiClO4、LiAlCl4、LiGaCl4、LiC(SO2CF3)3、LiB
(C6H4O2)2、LiN(SO2CF3)2、LiN(SO2C2F5)2、LiB(C2O4)2、Li(SO3CF3) and its mixture salt, other batteries
Analogize.The concentration of salt is 0.3 ~ 2M in organic solvent.
Diaphragm: polypropylene, polyethylene, polyamide, Vingon (PVC), Kynoar (PVDF), glass fibre,
One of non-woven fabrics etc..
The beneficial effect comprise that (1) prepares the pole piece of binder free, the energy density of battery is improved, (2) can
Using as different metal base battery positive electrode, the lamella class carbon material and polyacrylonitrile that (3) use, in charge and discharge process,
Secured " gluing " effect and lamella class carbon material because of polyacrylonitrile can alleviate the coating function of sulphur system positive electrode
Shuttle effect in cyclic process promotes cycle performance (4) low raw-material cost of battery.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of sulphur system anode composite pole piece of the invention.
Fig. 2 is the microscopic appearance figure of sulphur system anode composite pole piece of the invention.
Fig. 3 is sulphur system anode composite/lithium battery discharge curve of the invention.
Specific embodiment
Below in conjunction with drawings and examples, the following further describes the technical solution of the present invention.The embodiment of the present invention,
It is rather than to limit the protection scope of the claims in the present invention in order to further explanation of the invention.
As shown in Figure 1, the preparation process flow of sulphur system anode composite pole piece of the invention includes:
Step 1, in a solvent by the dispersion of lamella class carbon material, lamella class carbon dispersion liquid is formed；
Step 2, sulphur based material, fluorocarbons, polyacrylonitrile are added in the lamella class carbon dispersion liquid, are prepared into anode
Slurry；
Step 3, by the anode sizing agent be coated in collection liquid surface, under the conditions of 70 ~ 90 DEG C be dried in vacuo 12 ~ for 24 hours, obtain
To sulphur system anode composite pole piece.
Embodiment 1
The preparation of sulphur system anode composite pole piece: weighing 50mg GO, be dispersed in 40ml NMP, after stirring 1h, then ultrasound 1h shape
At uniform dispersion.460mg fluorographite (fluorine carbon ratio 0.8), 30mg PAN, 460mg elemental sulfur are sequentially added, 8h is stirred,
Form sulphur system anode composite slurry.This slurry is coated in aluminum foil current collector using scraper, 70 DEG C of drying 2h, until NMP
Solvent volatilizees completely, obtains sulphur system anode composite pole piece, and microscopic appearance is as shown in Figure 2.
The sulphur system anode composite of preparation: being punched into the round pole piece of Φ 14mm by the preparation of metal base battery, true at 85 DEG C
12h is dried in empty drying box.Under dry air or inert atmosphere conditions, using metal lithium sheet as cathode, Celgard 2325 is
Diaphragm, bis- (trifluoromethane sulfonic acid acyl group) imine lithiums (LiTFSI) of 1mol/L/dioxolanes (DOL)+1,2- dimethoxy-ethane
(DME) (volume ratio 1:1) is electrolyte, is assembled into CR2016 button cell.Battery is discharged with the current density of 50mA/g, warp
Calculating is crossed, which is 853mAh/g.
Embodiment 2
The preparation of sulphur system anode composite pole piece: weighing 30mg GO and 20mg GNS, be dispersed in 40ml DMF, after stirring 1h,
Ultrasound 1h forms uniform dispersion again.Sequentially add 300mg fluorographite (fluorine carbon ratio 1.0), 50mg PAN, 600mg sulphur carbon
Composite material stirs 8h, that is, forms sulphur system anode composite slurry.This slurry is coated in aluminum foil current collector using scraper, 70
DEG C drying 2h, until nmp solvent volatilizees completely.
The sulphur system anode composite of preparation: being punched into the round pole piece of Φ 14mm by the preparation of metal base battery, true at 85 DEG C
It is dried for 24 hours in empty drying box.Under dry air or inert atmosphere conditions, using metal lithium sheet as cathode, Celgard 2325 is
Diaphragm, bis- (trifluoromethane sulfonic acid acyl group) imine lithiums (LiTFSI) of 1mol/L/dioxolanes (DOL)+1,2- dimethoxy-ethane
(DME) (volume ratio 1:1) is electrolyte, is assembled into CR2016 button cell.Battery is with the current density charge and discharge of 50mA/g
Circulation, discharge curve is as shown in Figure 3 for the first time.By calculating, which is 947mAh/g, circulation 10
After secondary, because of the on-reversible cycle in lithium battery of fluorocarbons anode, capacity 557mAh/g.
Embodiment 3
The preparation of sulphur system anode composite pole piece: weighing 60mg N-GNS, be dispersed in 40ml NMP, after stirring 1h, then ultrasound
1h forms uniform dispersion.Sequentially add 400mg fluorographite (fluorine carbon ratio 1.0), 40mg PAN, 500mg sulphur carbon composite wood
Material stirs 8h, that is, forms sulphur system anode composite slurry.This slurry is coated in aluminum foil current collector using scraper, 70 DEG C of drying
2h, until nmp solvent volatilizees completely.
The preparation of metal base battery: the fluorocarbons anode of preparation is punched into the round pole piece of Φ 14mm, in 85 DEG C of vacuum
It is dried for 24 hours in drying box.Under dry air or inert atmosphere conditions, using metallic sodium piece as cathode, Glass Fiber be every
Film, 0.5mol/L sodium hexafluoro phosphate (NaPF6)/1,2- dimethoxy-ethane (DME) is electrolyte, is assembled into CR2016 button electricity
Pond.Battery under the current density of 50mA/g to recycle, first discharge specific capacity 907mAh/g, and after circulation 10 times, discharge specific volume
Amount is 865mAh/g, and cyclical stability is good.
Lithium metal, sodium etc. can be used as cathode in positive plate provided by the invention, is assembled into battery.When lithium is as cathode
When, because wherein there is fluorocarbons, this is the material of one-shot battery, so showing to be cyclicity relative to discharge capacity for the first time
It can be bad.And in embodiment 3, metallic sodium is secondary reversible as cathode, at this time fluorocarbons, and what is shown is cyclicity
It can be preferably.
In conclusion sulphur system anode composite pole piece provided by the invention, is not necessarily to binder, the energy that can improve battery is close
Degree, cycle performance are good.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (6)
1. a kind of preparation method of sulphur system anode composite pole piece, which is characterized in that this method includes:
Step 1, in a solvent by the dispersion of lamella class carbon material, lamella class carbon dispersion liquid is formed；The lamella class carbon material choosing
Select in graphene, graphene oxide, nitrogen-doped graphene, sulfur doping graphene or phosphorus sulfur doping graphene any one or
It is a variety of；At least one of described solvent selection DMF, DMAC, DMSO, NMP；
Step 2, sulphur based material, fluorocarbons, polyacrylonitrile are added in the lamella class carbon dispersion liquid, are prepared into positive slurry
Material；
Step 3, the anode sizing agent is coated in collection liquid surface, drying obtains sulphur system anode composite pole piece；
Wherein, the mass fraction of carbon is 3~6% in the lamella class carbon dispersion liquid；The partial size of the polyacrylonitrile is
20nm~40 μm, mass fraction are 3~5%.
2. the preparation method of sulphur system anode composite pole piece as described in claim 1, which is characterized in that the sulphur based material choosing
Select elemental sulfur, sulphur carbon composite, organic sulfur compound, any one or more in inorganic sulphide, in anode, quality
Score is 30~80%.
3. the preparation method of sulphur system anode composite pole piece as described in claim 1, which is characterized in that the fluorocarbons selection
It is any in fluorographite, carbon fluoride nano-tube, fluorinated graphene, fluorinated carbon fiber, fluorocarbons nanometer disk and fluorination coke
One or more, fluorine carbon molar ratio is 0.33~1.2, and in anode, mass ratio is 30~80%.
4. a kind of sulphur system anode composite pole piece of the preparation of method described in any one of -3 according to claim 1.
5. a kind of battery comprising sulphur system anode composite pole piece as claimed in claim 4, which is characterized in that the battery includes described
Sulphur system anode composite, cathode, electrolyte, diaphragm.
6. battery as claimed in claim 5, which is characterized in that cathode is lithium piece or sodium piece.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895794A (en) * | 2017-11-23 | 2018-04-10 | 中国航发北京航空材料研究院 | A kind of high specific energy lithium fluorocarbon battery |
| CN108054352A (en) * | 2017-11-23 | 2018-05-18 | 中国航发北京航空材料研究院 | A kind of high power lithium battery positive electrode and preparation method thereof |
| CN108039469A (en) * | 2017-12-06 | 2018-05-15 | 贵州梅岭电源有限公司 | The preparation method of fluorographite-sulfur electrode |
| CN109167040A (en) * | 2018-08-28 | 2019-01-08 | 南京工业大学 | A kind of fluorination carbonaceous additive is used for the method and its application of lithium-sulfur cell |
| CN111106309A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院大连化学物理研究所 | Carbon-sulfur composite electrode with carbon fluoride as additive, preparation and application thereof |
| CN109698365A (en) * | 2018-12-05 | 2019-04-30 | 上海空间电源研究所 | A kind of lithium metal battery with elastic buffer structure |
| CN112038589A (en) * | 2019-06-04 | 2020-12-04 | 中国科学院物理研究所 | High energy density aluminum secondary battery, positive electrode material thereof and preparation method |
| CN114628670B (en) * | 2020-12-11 | 2023-11-10 | 中国科学院大连化学物理研究所 | Application of nitrogen doped-carbon coated carbon fluoride in lithium/carbon fluoride battery |
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