CN106169561A - A kind of sulfur system anode composite pole piece, the battery comprising it and preparation method thereof - Google Patents
A kind of sulfur system anode composite pole piece, the battery comprising it and preparation method thereof Download PDFInfo
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- CN106169561A CN106169561A CN201610875539.0A CN201610875539A CN106169561A CN 106169561 A CN106169561 A CN 106169561A CN 201610875539 A CN201610875539 A CN 201610875539A CN 106169561 A CN106169561 A CN 106169561A
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of sulfur system anode composite pole piece, the battery comprising it and preparation method thereof.Sulfur system provided by the present invention combination electrode is the positive pole of binder free, its preparation process is as follows: disperseed in a solvent by lamella class carbon, form dispersion liquid, then sulfur based material, perfluorocarbon, polyacrylonitrile are added in this dispersion liquid, mix homogeneously, make anode active material slurry to be coated in current collector aluminum foil, drying, be prepared as sulfur system cell composite anode pole piece.The advantage of the sulfur system anode composite of the binder free that the present invention provides is: lamella class material with carbon element is coated on sulfur based material, perfluorocarbon surface, forms cushion；Stable structure constructed in positive pole by polyacrylonitrile, and (1) can be with the expansion of buffer electrode material and contraction；(2) can be by positive pole 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, be specifically related to the sulfur system anode pole piece of binder free, its preparation method
And the battery applied.
Background technology
Lithium ion battery, since last century, the nineties realized industrialization, has become the electrochmical power source of most practicality,
And the trend of expansion range of application further is had in the field such as electrokinetic cell and energy-storage battery.But lithium ion battery is by existing electricity
Storage lithium capacity limit (cobalt acid lithium actual capacity about 140mAh/g, the theoretical appearance of graphite-like Carbon anode that pole particularly positive pole is relatively low
Amount 372mAh/g), improve energy density spatial further limited.Along with New Generation of Electric Vehicle, unmanned vehicle, electronics produce
The development in the fields such as product, militay space flight airborne vehicle, the army and the people's every profession and trade is the most urgent to the demand of the energy-storage battery of high specific energy.
Sulfur is the solid-state positive electrode that theoretical specific capacity is higher, the light metal negative pole of coupling higher capacity, it is possible to obtain relatively
High battery theory specific energy.Arranging in pairs or groups such as lithium and sulfur and form lithium-sulfur cell, theoretical specific energy reaches ~ 2600Wh/kg, is specific energy
One of secondary cell system of the highest solid state electrode.And use other light metals and sulfur to arrange in pairs or groups, it is possible to obtain higher theory
Specific energy.Perfluorocarbon is as positive electrode, and its specific capacity is high, have stable discharge platform, storage life length, use temperature model
Enclose width, be solid positive pole lithium battery as commodity at first with it as the lithium primary battery of positive electrode.In sode cell
Application, has widened the range of application of fluorinated carbon material greatly.
And both materials, although all having higher specific capacity, but have a common problem, active substance is following
Easily diffuse in liquid electrolyte during ring.For sulfur system positive pole, use liquid electrolyte can cause the electric discharge of sulfur
The many lithium sulfides of product are dissolved in electrolyte, and are diffused into negative pole and react, and shuttle effect occurs during charging, causing charging effect
Rate is low, self discharge is big.The most also can deposit one layer of insulant in negative terminal surface, make battery performance deteriorate, especially capacity declines
Subtract fast.For perfluorocarbon positive pole, in sode cell during circulation, the active fluorine having part is dissolved in electrolyte, causes capacity attenuation
Comparatively fast.If build a kind of electrode, the advantage utilizing the height ratio capacity of sulfur system positive pole and perfluorocarbon positive pole simultaneously, can will circulate again
During generate effective active matter confinement, be effectively improved the cyclical stability of this type of battery, development potentiality space is huge.
Summary of the invention
It is an object of the invention to dissolve in the electrolytic solution for existing sulfur system positive pole polysulfide in cyclic process, formed
Shuttle effect, the problem that coulombic efficiency is low, and the perfluorocarbon positive pole problem that active substance dissolves in sode cell, it is provided that
The preparation method of the sulfur system anode composite pole piece of a kind of binder free, and the battery related to by it.
For reaching above-mentioned purpose, the invention provides the preparation method of a kind of sulfur system anode composite pole piece: first by lamella
Class material with carbon element disperses in a solvent, forms lamella class carbon dispersion liquid；Then sulfur based material, perfluorocarbon, polyacrylonitrile are joined
In described lamella class carbon dispersion liquid, it is prepared as anode sizing agent；Finally above-mentioned slurry is coated in collection liquid surface, dries
Obtain sulfur system anode composite pole piece.This lamella class material with carbon element is coated on sulfur based material, perfluorocarbon surface, forms cushion, permissible
The expansion of buffer electrode material and contraction；Stable structure constructed in positive pole by polyacrylonitrile, can be by positive pole effective active thing
Matter confinement.Lamella class carbon, in positive pole, is coated on the surface of positive active material, forms the structure of similar " sandwich ", and gathers
Then by component each in positive pole effective " gluing " together, the two has synergism to acrylonitrile.
Preferably, described lamella class material with carbon element select Graphene (GNS), graphene oxide (GO), nitrogen-doped graphene,
One or more in sulfur doping Graphene or phosphorus sulfur doping Graphene etc..
Preferably, in lamella class carbon dispersion liquid, the mass fraction of carbon is 3 ~ 6%.
Preferably, described solvent is dimethylformamide (DMF), N,N-dimethylacetamide (DMAC), dimethyl Asia
One in sulfone (DMSO), N-Methyl pyrrolidone (NMP) etc..
Preferably, in positive active material, sulfur based material selects elemental sulfur and sulfur carbon composite, organic sulfur compound, nothing
One or more in machine sulfide etc., in positive pole, its mass fraction is 30 ~ 80%.
Preferably, the fluorinated carbon material of positive active material is fluorographite, carbon fluoride nano-tube, fluorinated graphene, fluorine
Changing one or more in carbon fiber, perfluorocarbon nanometer disk, fluorination coke etc., fluorine carbon mol ratio is 0.33 ~ 1.2, at positive pole
In, its mass ratio is 30 ~ 80%.
Preferably, polyacrylonitrile (PAN) be particle diameter be 20nm ~ 40 μm, mass fraction is 3 ~ 5%.
Preferably, the sulfur system anode composite pole piece prepared is vacuum dried 12 ~ 24h under the conditions of 70 ~ 90 DEG C.
Present invention also offers the battery that a kind of sulfur system anode composite using method provided by the present invention to prepare assembles,
Including:
Negative pole: selected from periodic table of elements group ia, Group IIA, aluminum and alloy thereof or intermetallic compound.
Electrolyte: electrolyte comprises organic solvent and electrolytic salt.This organic solvent is selected from dimethyl carbonate (DMC), carbon
Diethyl phthalate (DEC), 1,2-dimethoxy-ethane (DME), oxolane (THF), methyl acetate (MA), diethylene glycol dimethyl ether,
Triethylene glycol dimethyl ether., tetraethylene glycol dimethyl ether, propylene carbonate (PC), carbonic acid ethylidene ester (EC), acetonitrile, dimethyl sulfoxide, two
Methylformamide, dimethyl acetylamide, gamma-butyrolacton (GBL), N-methyl-pyrrolidon (NMP), Ethyl methyl carbonate, carbonic acid are sub-
Vinyl acetate, dioxolanes, dioxane, dimethoxy-ethane or its mixture.Electrolytic salt is selected from MM ' F6Or MM ' F4Salt,
Wherein M is the metal identical with at least one metal in described negative pole, and M ' is the unit 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 the salt of mixture, other batteries
Analogize.In organic solvent, the concentration of salt is 0.3 ~ 2M.
Barrier film: polypropylene, polyethylene, polyamide, Vingon (PVC), Kynoar (PVDF), glass fibre,
One in non-woven fabrics etc..
The beneficial effect comprise that (1) prepares the pole piece of binder free, improve the energy density of battery, (2) can
Using as different metal base battery positive electrode, lamella class material with carbon element that (3) use and polyacrylonitrile, in charge and discharge process,
Because of polyacrylonitrile firm, " " effect, and the coating function that lamella class material with carbon element is to sulfur system positive electrode, can alleviate gluing
Shuttle effect in cyclic process, promotes cycle performance (4) low raw-material cost of battery.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of the sulfur system anode composite pole piece of the present invention.
Fig. 2 is the microscopic appearance figure of the sulfur system anode composite pole piece of the present invention.
Fig. 3 is the discharge curve of the sulfur system anode composite/lithium battery of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is described further.Embodiments of the invention,
It it is the protection domain in order to the present invention further illustrates rather than limits the claims in the present invention.
As it is shown in figure 1, the preparation technology flow process of the sulfur system anode composite pole piece of the present invention comprises:
Step 1, disperses lamella class material with carbon element in a solvent, forms lamella class carbon dispersion liquid；
Step 2, joins sulfur based material, perfluorocarbon, polyacrylonitrile in described lamella class carbon dispersion liquid, is prepared as positive pole slurry
Material；
Step 3, is coated in collection liquid surface by described anode sizing agent, is vacuum dried 12 ~ 24h, obtains sulfur under the conditions of 70 ~ 90 DEG C
It it is anode composite pole piece.
Embodiment 1
Prepared by sulfur system anode composite pole piece: weigh 50mg GO, is dispersed in 40ml NMP, and after stirring 1h, more ultrasonic 1h is formed all
Even dispersion liquid.It is sequentially added into 460mg fluorographite (fluorine carbon ratio is 0.8), 30mg PAN, 460mg elemental sulfur, stirs 8h, i.e. shape
Become sulfur system anode composite slurry.Use scraper to be coated in aluminum foil current collector by this slurry, dry 2h for 70 DEG C, until nmp solvent
Volatilize completely, it is thus achieved that sulfur system anode composite pole piece, its microscopic appearance is as shown in Figure 2.
Prepared by Metal Substrate battery: the sulfur system anode composite of preparation is die-cut into the circular pole piece of Φ 14mm, true at 85 DEG C
Empty drying baker dries 12h.Under dry air or inert atmosphere conditions, with metal lithium sheet as negative pole, Celgard 2325 is
Barrier film, double (trifluoromethane sulfonic acid acyl group) imine lithium (the LiTFSI)/dioxolanes (DOL)+1 of 1mol/L, 2-dimethoxy-ethane
(DME) (volume ratio is 1:1) is electrolyte, is assembled into CR2016 button cell.Battery discharges with the electric current density of 50mA/g, warp
Crossing calculating, this sulfur system anode composite specific discharge capacity is 853mAh/g.
Embodiment 2
Prepared by sulfur system anode composite pole piece: weigh 30mg GO and 20mg GNS, is dispersed in 40ml DMF, after stirring 1h, then surpasses
Sound 1h forms uniform dispersion.Be sequentially added into 300mg fluorographite (fluorine carbon ratio is 1.0), 50mg PAN, 600mg sulfur carbon is combined
Material, stirs 8h, i.e. forms sulfur system anode composite slurry.Scraper is used to be coated in aluminum foil current collector by this slurry, 70 DEG C of bakings
Dry 2h, until nmp solvent volatilizees completely.
Prepared by Metal Substrate battery: the sulfur system anode composite of preparation is die-cut into the circular pole piece of Φ 14mm, true at 85 DEG C
Empty drying baker dries 24h.Under dry air or inert atmosphere conditions, with metal lithium sheet as negative pole, Celgard 2325 is
Barrier film, double (trifluoromethane sulfonic acid acyl group) imine lithium (the LiTFSI)/dioxolanes (DOL)+1 of 1mol/L, 2-dimethoxy-ethane
(DME) (volume ratio is 1:1) is electrolyte, is assembled into CR2016 button cell.Battery is with the electric current density discharge and recharge of 50mA/g
Circulation, discharge curve is as shown in Figure 3 first.Through calculating, this sulfur system anode composite specific discharge capacity is 947mAh/g, circulates 10
After secondary, because of the on-reversible cycle in lithium battery of perfluorocarbon positive pole, capacity is 557mAh/g.
Embodiment 3
Prepared by sulfur system anode composite pole piece: weigh 60mg N-GNS, is dispersed in 40ml NMP, after stirring 1h, more ultrasonic 1h shape
Uniformly dispersion liquid.It is sequentially added into 400mg fluorographite (fluorine carbon ratio is 1.0), 40mg PAN, 500mg sulfur carbon composite, stirs
Mix 8h, i.e. form sulfur system anode composite slurry.Use scraper to be coated in aluminum foil current collector by this slurry, dry 2h, directly for 70 DEG C
Volatilize completely to nmp solvent.
Prepared by Metal Substrate battery: the perfluorocarbon positive pole of preparation is die-cut into the circular pole piece of Φ 14mm, in the vacuum of 85 DEG C
Drying baker is dried 24h.Under dry air or inert atmosphere conditions, with metallic sodium sheet as negative pole, 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 is to circulate under the electric current density of 50mA/g, and first discharge specific capacity is 907mAh/g, and after circulating 10 times, discharge specific volume
Amount is 865mAh/g, and cyclical stability is good.
The positive plate that the present invention provides can use lithium metal, sodium etc. as negative pole, is assembled into battery.When lithium is as negative pole
Time, because wherein there being perfluorocarbon, this is the material of one-shot battery, so relative to discharge capacity first, show for cyclicity
Can be bad.And in embodiment 3, metallic sodium is as negative pole, now perfluorocarbon is that secondary is reversible, and show is cyclicity
Can be preferably.
In sum, the sulfur system anode composite pole piece that the present invention provides, it is not necessary to binding agent, the energy that can improve battery is close
Degree, cycle performance is good.
Although present disclosure has been made to be discussed in detail by 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 foregoing, for the present invention's
Multiple amendment and replacement all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the preparation method of a sulfur system anode composite pole piece, it is characterised in that the method comprises:
Step 1, disperses lamella class material with carbon element in a solvent, forms lamella class carbon dispersion liquid；
Step 2, joins sulfur based material, perfluorocarbon, polyacrylonitrile in described lamella class carbon dispersion liquid, is prepared as positive pole slurry
Material；
Step 3, is coated in collection liquid surface by described anode sizing agent, dries, obtains sulfur system anode composite pole piece.
2. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described lamella class carbon material
It is any one that material selects in Graphene, graphene oxide, nitrogen-doped graphene, sulfur doping Graphene or phosphorus sulfur doping Graphene
Plant or multiple.
3. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described lamella class carbon divides
Dissipating the mass fraction of carbon in liquid is 3 ~ 6%.
4. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described solvent selects
At least one in DMF, DMAC, DMSO, NMP.
5. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described sulfur based material choosing
Select any one or more in elemental sulfur, sulfur carbon composite, organic sulfur compound, inorganic sulphide, in positive pole, its quality
Mark is 30 ~ 80%.
6. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described perfluorocarbon selects
Fluorographite, carbon fluoride nano-tube, fluorinated graphene, fluorinated carbon fiber, perfluorocarbon nanometer disk and fluorination coke in any
One or more, fluorine carbon mol ratio is 0.33 ~ 1.2, and in positive pole, its mass ratio is 30 ~ 80%.
7. the preparation method of sulfur system as claimed in claim 1 anode composite pole piece, it is characterised in that described polyacrylonitrile
Particle diameter is 20nm ~ 40 μm, and mass fraction is 3 ~ 5%.
8. the sulfur system anode composite pole piece prepared according to the method described in any one in claim 1-7.
9. the battery of the sulfur system anode composite pole piece that a kind comprises described in claim 8, it is characterised in that this battery comprises described
Sulfur system anode composite, negative pole, electrolyte, barrier film.
10. battery as claimed in claim 9, it is characterised in that negative pole be selected from periodic table of elements group ia, Group IIA, aluminum and
Its alloy or intermetallic compound.
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| 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 |
| 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 |
| 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 |
| CN109167040A (en) * | 2018-08-28 | 2019-01-08 | 南京工业大学 | Method for applying carbon fluoride additive to lithium-sulfur battery and application of carbon fluoride additive |
| 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 |
| 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 |
| 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 |
| CN114628670A (en) * | 2020-12-11 | 2022-06-14 | 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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| 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 |
| CN114628670A (en) * | 2020-12-11 | 2022-06-14 | 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 |
| 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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