CN105789557B - A kind of lithium sulphur pole piece and the preparation method and application thereof with function and protecting layer - Google Patents
A kind of lithium sulphur pole piece and the preparation method and application thereof with function and protecting layer Download PDFInfo
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- CN105789557B CN105789557B CN201610357591.7A CN201610357591A CN105789557B CN 105789557 B CN105789557 B CN 105789557B CN 201610357591 A CN201610357591 A CN 201610357591A CN 105789557 B CN105789557 B CN 105789557B
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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
- 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
- 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
- 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
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- Y02E60/10—Energy storage using batteries
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Abstract
A kind of lithium sulphur pole piece and the preparation method and application thereof with function and protecting layer, is related to lithium-sulfur cell.The lithium sulphur pole piece with function and protecting layer is equipped with lithium sulphur pole piece, armor coated in lithium sulphur pole piece, and the protective layer is bear electron ion compound protective layer or bear electron ion compound and ionic conduction type blend polymer protective layer.The preparation method of the lithium sulphur pole piece with function and protecting layer, includes the following steps：(1) ball milling after mixing the blend of bear electron ion compound or bear electron ion compound and ionic conduction type polymer, binder and solvent, obtains slurries；(2) slurries are coated on lithium sulphur pole piece, to get the lithium sulphur pole piece with function and protecting layer after drying.The lithium sulphur pole piece with function and protecting layer can be applied in preparing lithium-sulfur cell.
Description
Technical field
The present invention relates to lithium-sulfur cells, are specifically related to a kind of lithium sulphur pole piece and preparation method thereof with function and protecting layer
With application.
Background technology
With the development in the fields such as electric vehicle, capacity and power for the electrochmical power sources system such as lithium ion battery propose
Higher requirement, therefore the safety of battery also more and more paid attention to.Lithium-sulfur cell is one kind of lithium battery, lithium sulphur
Battery is a kind of lithium battery of the lithium metal as cathode using element sulphur as anode.Specific capacity is up to 1675mAh/g, far
Far above commercial widely applied cobalt acid lithium battery capacity (<150mAh/g).And sulphur is a kind of environment amenable member
Element does not pollute environment substantially, is a kind of very promising lithium battery.
At present lithium-sulfur cell there are the problem of mainly have：
The first, the electron conduction of elemental sulfur and ionic conductivity are poor, the conductivity of sulfur materials at room temperature extremely low (5.0
×10-30S·cm-1), the final product Li of reaction2S2And Li2S is also electronic body, is unfavorable for the high rate capability of battery.
The second, the intermediate discharging product of lithium-sulfur cell can be dissolved into organic electrolyte, increase the viscosity of electrolyte, be reduced
Ionic conductivity.More sulphions can migrate (Shuttle effects) between positive and negative anodes, lead to the wave of active material loss and electric energy
Take.The polysulfide of dissolving can be diffused into cathode across diaphragm, with negative reaction, destroy the solid electrolyte interface film of cathode
(SEI films).
The final discharging product Li of third, lithium-sulfur cell2Sn(n=1~2) electronic isolation and do not dissolve in electrolyte, be deposited on
The surface of conducting matrix grain；Partial vulcanization lithium is detached from conducting matrix grain, can not be reacted by reversible charging process and become sulphur or more
The polysulfide of high-order causes the significant attenuation of capacity.
4th, the density of sulphur and lithium sulfide is respectively 2.07 and 1.66gcm-3, there is up to 79% in charge and discharge process
Volume expansion/contraction, this expansion can lead to the change of positive pattern and structure, lead to the disengaging of sulphur and conducting matrix grain, from
And cause the decaying of capacity；This bulk effect is not notable under button cell, but bulk effect can amplify in large-sized battery,
It will produce significant capacity attenuation, it is possible to cause the damage of battery, huge volume change that can destroy electrode structure.
5th, lithium-sulfur cell uses lithium metal as cathode, and in addition to the high activity of lithium metal itself, lithium anode is filling
Volume change can occur for discharge process, and be easy to form dendrite.
6th, the research of lithium-sulfur cell laboratory scale is carried out more, and sulphur carrying capacity is generally all in 3.0mg on unit area
cm-2Hereinafter, the research for carrying out high load amount pole piece has important value for obtaining high-performance lithium-sulfur cell.
Solution in view of the above problems is usually from the modification of electrode material and structure design and electrolysis additive
Two aspects are started with.Such as the micron order sulfur granules that the graphene oxide of the patent CN104852025A modifications announced coats, nano-sulfur
Particle and hollow sulfur granules, prepared combination electrode electrode material have good cycle, and high rate performance is high, in energy storage field
It has broad application prospects.In patent CN104485449A carbon packet is formed with elemental sulfur with the polymer of unsaturated carbon-carbon double bond
The sulfur content of the sulfur materials covered, composite material prepared by the method is relatively high, and simple process and low cost is honest and clean.Patent
The one or more as electrolysis additive of silane ethers are used in CN103855425A, this electrolyte has viscosity low, electric
The characteristics such as conductance is high, inhibition sulphion shuttle is good.Therefore it is to improve lithium sulphur to hinder migration of the polysulfide ion between positive and negative anodes
The effective way of battery capacity.
Invention content
The purpose of the present invention is to provide a kind of lithium sulphur pole pieces with function and protecting layer.
Another object of the present invention is to provide the preparation methods of the lithium sulphur pole piece with function and protecting layer.
It is still another object of the present invention to provide the applications of the lithium sulphur pole piece with function and protecting layer.
The lithium sulphur pole piece with function and protecting layer is equipped with lithium sulphur pole piece, institute armor coated in lithium sulphur pole piece
It is that bear electron ion compound protective layer or bear electron ion compound and ionic conduction type blend polymer are protected to state protective layer
Sheath；The bear electron ion compound is selected from perfluor fluorinated sulfonic resin, partially fluorinated sulfonate resin, graphene oxide, band
Sulfonic polyether-ketone, with sulfonic ether ketone copolymers, the polyether-ketone with carboxylic acid group, the ether ketone copolymers with carboxylic acid group, band
The polyether-ketone of phosphonic acid base, the ether ketone copolymers with phosphonic acid base, polyimides, polyimide copolymer, polystyrene, polystyrene
At least one of copolymer etc.；It is total that the ion-conducting polymers can be selected from Kynoar, biasfluoroethylene-hexafluoropropylene
At least one of polymers, Pluronic F-127, polyethylene oxide, polymethacrylates, polyacrylonitrile etc..
The thickness of the function and protecting layer can be 10nm~20 μm.
The mass ratio of the bear electron ion compound protective layer and binder can be (19~4): 1, the bear ionization
Sub- compound and the mass ratio of ionic conduction type blend polymer protective layer and binder can be (19~4): 1.
The solvent and the mass ratio of binder and bear electron ion compound protective layer gross mass can be (199~4): 1；
The solvent and binder and the matter of bear electron ion compound and ionic conduction type blend polymer protective layer gross mass
It can be (199~4) to measure ratio: 1.
The binder can be selected from Kynoar (Polyvinylidene fluoride, PVDF), Kynoar-
Hexafluoropropylene copolymer (Polyvinylidene fluoride-hexafluoropropylene, PVDF-HFP), poly- methyl-prop
E pioic acid methyl ester (polymethyl methacrylate, PMMA), polyacrylonitrile (Polyacrylonitrile, PAN), polyamides are sub-
Amine (Polyimide, PI), polyvinylpyrrolidone (Polyvinylpyrrolidone, PVP), polyethylene oxide
(Polyethylene oxide, PEO), polyvinyl alcohol (Polyving akohol, PVA), sodium carboxymethylcellulose
In (Polymethyl methacrylate, CMC), butadiene-styrene rubber (Styrene-butadiene rubber, SBR), gelatin etc.
At least one.
The preparation method of the lithium sulphur pole piece with function and protecting layer, includes the following steps：
(1) by the blend of bear electron ion compound or bear electron ion compound and ionic conduction type polymer, viscous
Ball milling after knot agent and solvent mixing, obtains slurries；
(2) slurries are coated on lithium sulphur pole piece, to get the lithium sulphur pole piece with function and protecting layer after drying.
In step (2), the drying can be dried in vacuo at 50~60 DEG C.
The lithium sulphur pole piece with function and protecting layer can be applied in preparing lithium-sulfur cell.
The lithium-sulfur cell includes anode, diaphragm and cathode etc., and the anode is using the lithium with function and protecting layer
Sulphur pole piece.
When the lithium sulphur pole piece with function and protecting layer is used to constitute the anode of non-aqueous electrolyte secondary lithium-sulfur cell,
Conductive auxiliary agent and adhesive etc. can be properly added in positive active material, carbon black, acetylene black etc. can be used in the conductive auxiliary agent
In one kind, one kind in Kynoar, polyethylene oxide etc. can be used in described adhesive, by it with aluminium foil, copper foil etc.
Current-collecting member as on the band-like formed body of core material be coated with after use.But positive production method is not limited only to example.
In the nonaqueous electrolytic solution secondary battery, using nonaqueous solvents (organic solvent) as nonaqueous electrolytic solution.It is non-aqueous
Agent includes carbonates, ethers etc..
The beneficial effects of the invention are as follows：
1, of the invention in lithium-sulfur cell pole piece coating function protective layer, function and protecting layer is by bear electron ion chemical combination
Object is made of the blend of bear electron ion compound and ionic conduction type polymer.Due to its electrostatic repulsion and micropore
Filter membrane acts on, and function and protecting layer can effectively prevent polysulfide ion from being dissolved into entire battery system, polysulfide ion is obstructed
In sulfur electrode side, the capacity holding capacity of lithium-sulfur cell is improved.
2, the region of the inactive substance of 0.1~5mm, coating organic matter protection are reserved in lithium-sulfur cell pole piece of the present invention edge
, cannot be from the edge leakage of agent piece after the polysulfide ion generation of lithium-sulfur cell after layer, it can be effectively by the polysulfide ion of generation
It is fixed on the surface of pole piece.
Description of the drawings
Fig. 1 is 1 elemental sulfur pole piece stereoscan photograph of the embodiment of the present invention.
Fig. 2 is the surface scan Electronic Speculum of the elemental sulfur pole piece with perfluorinated sulfonic resin protective layer in the embodiment of the present invention 2
Figure.
Fig. 3 is the profile scanning electron microscope of the copper sulfide pole piece in the embodiment of the present invention 2.
Fig. 4 is the scanning electron microscope (SEM) photograph that the present invention is the copper sulfide pole piece with graphene oxide protective layer in embodiment 2.
Fig. 5 be the embodiment of the present invention 1 lithium sulphur pole piece with perfluorinated sulfonic resin function and protecting layer and comparative example 1 it is general
Logical the assembled lithium-sulfur cell cycle performance comparison of lithium sulphur pole piece.
Specific implementation mode
Technical scheme of the present invention is further detailed and is described below by way of specific embodiment combination attached drawing.
Embodiment 1
Perfluorinated sulfonic resin 0.45g made of polytetrafluoroethylene (PTFE) is grafted and sodium cellulose glycolate (CMC) and butylbenzene and
Rubber (SBR) (2: 3, w: w) 0.05g hybrid adhesives are put into deionized water and ethyl alcohol (1: 1, v: v) mixed solution 20g magnetic force stirs
Mix 5h.Using elemental sulfur as active material, makes elemental sulfur: acetylene black: Kynoar mass ratio is 7: 2: 1, be collection with aluminium foil
The area of fluid is the pole piece of 5cm × 5cm, and the inactive Physical Zone of 0.5mm is reserved at pole piece edge, is used for subsequent experiment.
By the coating slurries of above-mentioned making, uniformly blade coating is in pole piece, and it is 1 μm to control the thickness of coat, and equal solvent largely volatilizees
After be put into 60 DEG C of drying of vacuum drying oven and remove solvent overnight, (elemental sulfur is swept for the elemental sulfur pole piece that obtains having function and protecting layer
Electromicroscopic photograph is retouched as shown in Figure 1, the elemental sulfur pole piece stereoscan photograph with perfluorinated sulfonic acid protective layer is as shown in Figure 2).
Embodiment 2
By graphene oxide 0.9g and polyethylene glycol oxide (PEO) binder 0.1g be put into deionized water and ethyl alcohol (1: 1, v:
V) mixed solution 50g magnetic agitations 10h.Using copper sulfide as active material, copper sulfide: acetylene black: Kynoar quality is made
Take afflux bulk area as the pole piece of 10cm × 10cm of copper foil than being 6: 3: 1, the inactive substance area of 1mm is reserved at pole piece edge
Domain is used for subsequent experiment.By the coating slurries of above-mentioned making, uniformly in pole piece, the thickness for controlling coat is blade coating
3 μm, equal solvent is put into 60 DEG C of drying of vacuum drying oven and thoroughly removes solvent overnight after largely volatilizing, obtain with graphene oxide
The copper sulfide pole piece of protective layer.
The cross-section diagram of copper sulfide pole piece is as shown in figure 3, the section of the copper sulfide pole piece with graphene oxide protective layer is swept
It is as shown in Figure 4 to retouch electron microscope.
Embodiment 3
By the sulfonate resin 1.9g and sodium cellulose glycolate (CMC) and butylbenzene of part fluoro and rubber (SBR) (2: 3, w:
W) 0.1g hybrid adhesives are put into deionized water and ethyl alcohol (1: 1, v: v) mixed solution 100g magnetic agitations 20h.With how thio pyrrole
It coughs up as active material, the how thio pyrroles of making: acetylene black: Kynoar mass ratio is 7: 2: 1, using aluminium foil as afflux bulk area
For the pole piece of 15cm × 15cm, the inactive Physical Zone of 1.5mm is reserved at pole piece edge, is used for subsequent experiment.By above-mentioned system
Uniformly blade coating is in pole piece for the coating slurries of work, and it is 5 μm to control the thickness of coat, and equal solvent is put into after largely volatilizing
60 DEG C of drying of vacuum drying oven thoroughly remove solvent overnight, obtain the how thio pyrroles electricity with part flurosulphonic acid resin protective layer
Pond pole piece.
Embodiment 4
Sulfonated polyimide 0.9g and Kynoar (PVDF) binder 0.1g are put into N-methyl pyrrolidones and third
Ketone (1: 1, v: v) mixed solution 10g magnetic agitations 10h.Using cobalt sulfide as active material, cobalt sulfide: acetylene black is made: gathering inclined fluorine
Ethylene mass ratio is 7: 2: 1, take afflux bulk area as the pole piece of 10cm × 10cm of aluminium foil, and the nothing of 0.5mm is reserved at pole piece edge
Active material region is used for subsequent experiment.By the coating slurries of above-mentioned making, uniformly blade coating is coated in pole piece, control
The thickness of layer is 1 μm, and equal solvent is put into 60 DEG C of drying of vacuum drying oven and thoroughly removes solvent overnight after largely volatilizing, had
The cobalt sulfide battery pole piece of sulfonated polyimide protective layer.
Embodiment 5
Graphene oxide 0.5g and Kynoar-hexafluoropropene (PVDF-HFP) ionic conduction type polymer 0.5g are put
Enter nitrogen nitrogen dimethylacetylamide and acetone (1: 1, v: v) mixed solution 20g magnetic agitations 5h.It is active matter with how thio thiophene
Matter makes how thio thiophene: acetylene black: Kynoar mass ratio is 6: 3: 1, is 5cm × 5cm by afflux bulk area of copper foil
Pole piece, pole piece edge reserve 0.5mm inactive Physical Zone, be used for subsequent experiment.By the coating slurries of above-mentioned making
Uniform blade coating is 3 μm in pole piece, the thickness for controlling coat, and equal solvent is put into 60 DEG C of vacuum drying oven after largely volatilizing
Drying thoroughly removes solvent overnight, obtains the how thio thiophene with graphene oxide and Kynoar-hexafluoropropene protective layer
Pheno pole piece.
Comparative example 1
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is common lithium-sulfur cell pole
Piece.
Embodiment 6
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is tool prepared by embodiment 1
The lithium sulphur pole piece of functional protective layer.The cycle performance of battery that testing example 6 is obtained with comparative example 1, as shown in Figure 5.It can be with
Find out, using the cycle performance of battery for the lithium sulphur pole piece with function and protecting layer that the present invention obtains, than using prior art system
The cycle performance of battery of standby common lithium sulphur pole piece is obviously improved.
Embodiment 7
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is tool prepared by embodiment 2
The lithium sulphur pole piece of functional protective layer.
Embodiment 8
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is tool prepared by embodiment 3
The lithium sulphur pole piece of functional protective layer.
Embodiment 9
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is tool prepared by embodiment 4
The lithium sulphur pole piece of functional protective layer.
Embodiment 10
Lithium-sulfur cell, including positive electrode, negative material, electrolyte and diaphragm.Positive electrode is tool prepared by embodiment 5
The lithium sulphur pole piece of functional protective layer.
Claims (6)
1. a kind of lithium sulphur pole piece with function and protecting layer, it is characterised in that be equipped with lithium sulphur pole piece, coated in lithium sulphur pole piece
Protective layer, the protective layer are bear electron ion compound protective layer or bear electron ion compound and the polymerization of ionic conduction type
Object blend protective layer；The bear electron ion compound protective layer includes bear electron ion compound and binder, the lotus
Negative ion compound and ionic conduction type blend polymer protective layer include bear electron ion compound and ionic conduction type
Blend polymer and binder；The bear electron ion compound is selected from perfluor fluorinated sulfonic resin, partially fluorinated sulfonic acid tree
Fat, graphene oxide, with sulfonic polyether-ketone, with sulfonic ether ketone copolymers, the polyether-ketone with phosphonic acid base, band phosphonic acid base
Ether ketone copolymers, polyimides, polyimide copolymer, polystyrene, at least one of polystyrene copolymer；It is described
Ion-conducting polymers be selected from Kynoar, vinylidene fluoride-hexafluoropropylene copolymer, Pluronic F-127, polyethylene oxide,
At least one of polymethacrylates, polyacrylonitrile；The quality of the bear electron ion compound protective layer and binder
Than for (19~4): 1；The matter of the bear electron ion compound and ionic conduction type blend polymer protective layer and binder
Amount is than being (19~4): 1.
2. a kind of lithium sulphur pole piece with function and protecting layer as described in claim 1, it is characterised in that the function and protecting layer
Thickness is 10nm~20 μm.
3. a kind of lithium sulphur pole piece with function and protecting layer as described in claim 1, it is characterised in that the binder is selected from poly-
Vinylidene, Kynoar-hexafluoropropylene copolymer, polymethyl methacrylate, polyacrylonitrile, polyimides, polyethylene
At least one of pyrrolidones, polyethylene oxide, polyvinyl alcohol, sodium carboxymethylcellulose, butadiene-styrene rubber, gelatin.
4. a kind of preparation method of the lithium sulphur pole piece with function and protecting layer as described in claim 1, it is characterised in that including such as
Lower step：
(1) by blend, the binder of bear electron ion compound or bear electron ion compound and ionic conduction type polymer
Ball milling after being mixed with solvent, obtains slurries；
(2) slurries are coated on lithium sulphur pole piece, to get the lithium sulphur pole piece with function and protecting layer after drying.
5. a kind of preparation method of the lithium sulphur pole piece with function and protecting layer as claimed in claim 4, it is characterised in that in step
(2) in, the drying is dried in vacuo at 50~60 DEG C.
6. a kind of lithium sulphur pole piece with function and protecting layer is applied in preparing lithium-sulfur cell as described in claim 1.
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| CN106450422A (en) * | 2016-09-30 | 2017-02-22 | 上海空间电源研究所 | Lithium-sulfur battery with multi-protection layer structure |
| CN108281659A (en) * | 2018-01-18 | 2018-07-13 | 中国计量大学 | Sulphur anode and lithium-sulfur cell |
| CN109004173B (en) * | 2018-09-06 | 2020-12-25 | 西安建筑科技大学 | Lithium-sulfur battery positive electrode and manufacturing method thereof |
| CN109638284B (en) * | 2018-12-18 | 2020-07-10 | 华中科技大学 | Metallic lithium negative electrode material and preparation method thereof |
| KR102415168B1 (en) * | 2019-05-03 | 2022-07-01 | 주식회사 엘지에너지솔루션 | Functional separator, method for preparing the same and lithium secondary battery including the same |
| CN110098375A (en) * | 2019-05-19 | 2019-08-06 | 中国科学院青岛生物能源与过程研究所 | A kind of modification of cyano sulphur anode and its high-performance lithium-sulfur cell that constitutes |
| CN110911662A (en) * | 2019-11-06 | 2020-03-24 | 华南理工大学 | Lithium cathode with protective layer and preparation method and application thereof |
| CN113206344A (en) * | 2020-02-03 | 2021-08-03 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method and application thereof |
| CN112436151B (en) * | 2020-11-13 | 2023-02-03 | 昆明理工大学 | Preparation method of lithium-sulfur battery current collector |
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| CN104716324B (en) * | 2013-12-15 | 2017-02-01 | 中国科学院大连化学物理研究所 | Lithium-sulfur battery positive electrode making method |
| CN104600251A (en) * | 2014-12-26 | 2015-05-06 | 中南大学 | Lithium-sulfur battery positive electrode and preparation method thereof |
| CN104766967A (en) * | 2015-03-18 | 2015-07-08 | 南京师范大学 | Preparation method of S/C composite material used in positive pole of Li-S battery |
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