CN106935773A - A kind of interlayer for lithium-sulfur cell - Google Patents
A kind of interlayer for lithium-sulfur cell Download PDFInfo
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- CN106935773A CN106935773A CN201511008719.0A CN201511008719A CN106935773A CN 106935773 A CN106935773 A CN 106935773A CN 201511008719 A CN201511008719 A CN 201511008719A CN 106935773 A CN106935773 A CN 106935773A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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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
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Abstract
The present invention relates to a kind of interlayer for lithium-sulfur cell, interlayer is coated in both positive and negative polarity or membrane surface, or is attached between negative or positive electrode and barrier film in the form of independent chip solid battery is protected by.Feature interlayer by three kinds into being grouped into, respectively functional agent, adhesive, conductive agent, wherein functional agent be the carbon material containing Sulfonic Lithium group, polymer or both mixture and they mix formed material by different proportion with metal oxide.Because interlayer component contains Sulfonic Lithium, during circulating battery, improve the concentration of lithium ion in electrolyte, ion mass transfer rate is improved, and the presence of sulfonate radical is not only able to strengthen ionic conductivity, and also the use of cooperation adhesive has obvious chemical barrier suction-operated to many lithium sulfides, its dissolving is effectively inhibited to spread, alleviate cathode of lithium surface because insoluble many lithium sulfides deposit the surface passivation to be formed, meanwhile, the addition of conductive agent can reduce the internal resistance of cell.
Description
Technical field
The present invention relates to a kind of interlayer for lithium-sulfur cell, belong to field of chemical power source.
Background technology
With continuing to develop for science and technology, portable set and electrical source of power develop a kind of small to the performance requirement more and more higher of battery
Type, light-weighted high energy density cells are extremely urgent.Lithium-sulfur cell has height ratio capacity (1675 because of its active material elemental sulfur
MAh/g) and high-energy-density (2600Wh/kg), it is and elemental sulfur aboundresources, with low cost, environment-friendly, safe and reliable
The advantages of, possess wide research and application background.However, lithium-sulfur cell active material poorly conductive, in the middle of charge and discharge process
Product polysulfide easily dissolves in the electrolytic solution, diffusion, and side reaction occurs with positive pole sulphur and negative metal lithium, produces shuttle effect,
The cycle efficieny for reducing lithium-sulfur cell and the loss for causing active material, ultimately result in the rapid decay of cycle performance of battery.
In order to the dissolving for solving lithium-sulfur cell intermediate product polysulfide in cyclic process is spread, suppress " shuttle ", scientific research personnel adopts
Numerous effective methods are taken.Positive electrode aspect, employs sulphur/carbon and is combined, and sulphur/polymer is compound etc., and mode is carried out to sulphur positive pole
It is modified, by improving electric conductivity and solidification to sulphur simple substance improves the cycle performance of lithium-sulfur cell to a certain extent, for example：
Nazar etc. is compound with mesoporous carbon by sulphur, and the migration of polysulfide is limited using mesopore orbit, effectively improves lithium-sulfur cell
Cycle performance (Jix, Lee KT, Nazar LF.Nat Mater.2009；8(6)：500-6.)；Barrier film aspect, applies by positive extreme direction
Cover one layer of conductive carbon, and mix a certain proportion of adhesive and it is reinforced to form protective layer, stop polysulfide, and with aluminium foil shape
Into " double-deck collector ", the internal resistance of cell is effectively reduced, so as to lift the multiplying power and cycle performance of battery, except this, barrier film is carried out
Performance boost of polymer-modified and ion selective separator the application also to lithium-sulfur cell is helpful.Example：Cui et al. (Energy
Environ.Sci., super P, ketjen black, MCNT 2014,7,3381) have been respectively coated with barrier film, and have been mixed a small amount of
PVDF formed coating, three has been lifted to the cycle performance of battery, wherein especially with ketjen black coating results the most
Significantly.Chinese patent CN 104393349A disclose a kind of lithium-sulfur cell protective layer, and the various functional groups of grafting are coated on barrier film
Modified graphene and adhesive mixture, the dissolving that many lithium sulfides are suppressed from physical barriers and chemisorbed repulsive interaction expands
Dissipate, and high conductivity using Graphene reduces the internal resistance of cell, so as to lift circulating battery and high rate performance；Negative pole aspect,
By carry out to metal lithium sheet modification protection or add in the electrolytic solution additive promote negative pole formed the SEI diaphragms of stabilization come
Suppress the dendrite efflorescence of lithium metal, so that cell safety and cycle performance are lifted, such as Jing et al. (J.Mater.Chem.A,
2015,3,12213-12219) Al is utilized2O3Coating protects the metal lithium sheet to improve lithium-sulfur cell performance, and they are by Al2O3, it is viscous
Knot agent PVDF is mixed into slurry, is coated with metal lithium sheet, reaches dendrite inhibition, protects the effect of negative pole.
Document above is effectively improved the electric conductivity and reactivity of positive pole elemental sulfur with strategy described in patent, improves elemental sulfur
Utilization rate, and improve circulation and the security performance of battery by being protected to negative pole, but fail fundamentally to solve many lithium sulfides
Dissolving shuttle and the problem of metal Li dendrite efflorescence, the performance of lithium-sulfur cell still have much room for improvement.
The content of the invention
Present invention aim to address the problem of existing lithium-sulfur cell, there is provided a kind of interlayer for lithium-sulfur cell and preparation method thereof.
The interlayer is applied directly to negative or positive electrode surface, or is coated on protective layer is formed on barrier film, or the independent slabbing as carbon paper
Solid is attached between barrier film and both positive and negative polarity and battery is protected by.Feature interlayer by three kinds into being grouped into, respectively functional agent,
Adhesive, conductive agent, wherein functional agent be the carbon material containing Sulfonic Lithium group, polymer or both mixture and they
With metal oxide by the formed material of different proportion collocation.Because interlayer component contains Sulfonic Lithium, during circulating battery,
The concentration of lithium ion in electrolyte is improved, ion mass transfer rate is improved, and the presence of sulfonate radical is not only able to strengthen ion-conductance
Conductance, and the use of cooperation adhesive has obvious chemical barrier suction-operated to many lithium sulfides, effectively inhibits the molten of it
Solution diffusion, alleviates cathode of lithium surface because insoluble many lithium sulfides deposit the surface passivation to be formed, meanwhile, the addition of conductive agent can
The internal resistance of cell is reduced, circulation and the high rate performance of lithium-sulfur cell is effectively improved.
The technical solution adopted by the present invention：For the interlayer in lithium-sulfur cell by three kinds into being grouped into, respectively functional agent, bonding
Agent, conductive agent, interlayer functional agent be containing the sulfonic carbon material of lithiumation, containing the sulfonic polymer of lithiumation and they with oxidation
Thing mixes formed composition, interlayer be coated in both positive and negative polarity or membrane surface or be attached in the form of independent chip solid positive pole or
Battery is protected by between negative pole and barrier film, interlayer preparation method step is as follows：
Weigh functional agent, adhesive, conductive agent that mass ratio is 1: 0.01~1: 0.01~1 to be put into reaction bulb, by solid-to-liquid ratio 1: 2~5
Add dispersant to size mixing, finely dispersed slurry is formed after stirring, then slurry is coated thickness is just formed on barrier film, both positive and negative polarity
The interlayer for 100nm~100 μm is spent, is coated on glass plate for the preferable slurry of film forming, removed after drying and be placed directly against
Protection is formed between negative or positive electrode and barrier film；
The carbon material of interlayer functional agent is constituted for microporous carbon, activated carbon, biological carbon, mesoporous carbon, mesoporous carbon, macropore carbon, mesoporous
Microporous carbon, macropore microporous carbon, macropore mesoporous carbon, the mesoporous microporous carbon of macropore, graphite, Graphene, fibrous carbon, carbon black, carbon are received
Mitron or acetylene black；Constitute interlayer functional agent polymer be polyaniline, polythiophene, poly-dopamine, polypyrrole, polypyridine or
Polyacrylonitrile；Mass fraction of the lithiumation sulfonic group in modified carbonaceous components or polymer is 0.01%~20%；Composition interlayer function
The oxide of agent is aluminum oxide, silica, zinc oxide, titanium oxide, sodium oxide molybdena, calcium oxide, magnesia, barium monoxide, oxidation
Iron, ferrous oxide, ferroso-ferric oxide or manganese oxide；The adhesive for constituting interlayer is Kynoar, polytetrafluoroethylene (PTFE), poly- second
Enol, sodium cellulose glycolate, butadiene-styrene rubber, gelatin, sodium alginate, LA132 or cyclodextrin；Conductive agent be acetylene black,
Super P, carbon fiber, CNT, Ketjen black, graphite or Graphene.
Beneficial effects of the present invention：The interlayer of offer, by lithiumation sulfonate functional groups and carbon material, polymer, conductive agent,
The respective synergy such as adhesive, polysulfide is adsorbed to ionic conductivity is improved from physical barrier and chemical barrier, reduces electricity
Pond internal resistance, the circulation of many-side lifting battery and high rate performance, the industrialization to realizing lithium-sulfur cell have important reference value.
Brief description of the drawings
Fig. 1 lithium-sulfur cell spacer structure schematic diagrames
In figure：1. battery case negative pole, 2. lithium piece, 3. protective coating barrier film, 4. positive plate, 5. battery case positive pole.
Cycle performance under the made lithium-sulfur cell 0.1C multiplying powers of Fig. 2
Specific embodiment
Embodiment 1
The multi-walled carbon nano-tubes of 0.4g sulfonic acid lithiumations is added in reaction bulb, 0.05g acetylene blacks, 0.05gLA132 adhesives, 2g is different
Propyl alcohol prepares mixed solution at 1: 3 by volume with water, after the 24h that sizes mixing is stirred at room temperature, polypropylene diaphragm is uniformly coated on coating device
On, to dry to form protection interlayer naturally, the mode for being then affixed to positive pole according to interlayer is assembled into lithium-sulfur cell and carries out chemical property
Test, battery structure is as shown in Figure 1.In 0.1C (1C=1675mA h g-1) charge-discharge magnification under, it is modified using sulfonic acid lithiumation
The barrier film of coating modification assembles battery first discharge specific capacity and reaches 1259mA h g-1, 100 circle circulation volume stabilizations are in 1048mA
hg-1, individual pen attenuation rate is about 0.15%, and far below the lithium-sulfur cell (0.35%) of common diaphragm, its cyclic curve is as shown in Figure 2.
Embodiment 2
The Graphene of 0.4g sulfonic acid lithiumations, 0.02g sections qin carbon, 0.08g polytetrafluoroethylene (PTFE), 2g normal propyl alcohols and water are added in reaction bulb
It is by volume 1: 3 mixed solution prepared, after the 24h that sizes mixing is stirred at room temperature, is uniformly coated on anode pole piece by spraying process,
Protection interlayer is formed after drying, being then assembled into lithium-sulfur cell by normal assembling mode carries out electrochemical property test.
Embodiment 3
The activated carbon of 0.3g sulfonic acid lithiumations, 0.1g aluminum oxide, 0.05g Super P, 0.05g gelatin, 2g positive third are added in reaction bulb
Alcohol and water prepare mixed solution at 1: 3 by volume, and the 24h that sizes mixing is stirred at room temperature, and are uniformly coated on by spraying process in glove box negative
Protection interlayer is formed in the lithium piece of pole, after drying, being then assembled into lithium-sulfur cell by normal assembling mode carries out electrochemical property test.
Embodiment 4
Microporous carbon BP2000, the 0.05g acetylene black of 0.4g sulfonic acid lithiumations, 0.05g Kynoar, 2g N, N- are added in reaction bulb
Dimethyl pyrrolidone solvent, after the 24h that sizes mixing is stirred at room temperature, is uniformly coated on clean glass plate with coating device, is taken after drying
, then be attached to interlayer between positive pole and barrier film and be assembled into lithium-sulfur cell and carry out electrochemical property test by lower formation independent protective interlayer.
Embodiment 5
The multi-walled carbon nano-tubes of 0.2g sulfonic acid lithiumations, 0.2g titanium oxide, 0.05g acetylene blacks, 0.05g alginic acids are added in reaction bulb
The mixed solution of sodium, 2g isopropanols and water 1: 3 preparation by volume, after the 24h that sizes mixing is stirred at room temperature, by spraying process even spread
Protection interlayer is formed on anode pole piece, after drying, being assembled into lithium-sulfur cell by normal assembling mode carries out electrochemical property test.
Embodiment 6
The acetylene black of 0.4g sulfonic acid lithiumations is added in reaction bulb, 0.05g carbon blacks, 0.05g polyvinyl alcohol, 2g isopropanols press body with water
Product after the 24h that sizes mixing is stirred at room temperature, is uniformly coated on anode pole piece than being 1: 3 mixed solution prepared by spraying process, is dried
Protection interlayer is formed afterwards, and being then assembled into lithium-sulfur cell by normal assembling mode carries out electrochemical property test.
Claims (1)
1. a kind of interlayer for lithium-sulfur cell, it is characterised in that the interlayer is made up of three kinds of compositions, respectively functional agent, bonding
Agent, conductive agent, interlayer functional agent be containing the sulfonic carbon material of lithiumation, containing the sulfonic polymer of lithiumation and they with oxidation
Thing mixes formed composition, interlayer be coated in both positive and negative polarity or membrane surface or be attached in the form of independent chip solid positive pole or
Battery is protected by between negative pole and barrier film, interlayer preparation method is as follows：
Weigh functional agent, adhesive, conductive agent that mass ratio is 1: 0.01~1: 0.01~1 to be put into reaction bulb, by solid-to-liquid ratio 1: 2~5
Dispersant is added to size mixing, stirring forms finely dispersed slurry, slurry then is coated into formation thickness on barrier film, both positive and negative polarity is
The interlayer of 100nm~100 μm, is coated on glass plate for the preferable slurry of film forming, is removed after drying and is placed directly against positive pole
Or protection is formed between negative pole and barrier film；
It is described composition interlayer functional agent carbon material for microporous carbon, activated carbon, biological carbon, mesoporous carbon, mesoporous carbon, macropore carbon,
Mesoporous microporous carbon, macropore microporous carbon, macropore mesoporous carbon, the mesoporous microporous carbon of macropore, graphite, Graphene, fibrous carbon, carbon black,
CNT or acetylene black；
The polymer of the composition interlayer functional agent is polyaniline, polythiophene, poly-dopamine, polypyrrole, polypyridine or polypropylene
Nitrile；
Mass fraction of the lithiumation sulfonic group in modified carbonaceous components or polymer is 0.01%~20%；
It is described composition interlayer functional agent oxide for aluminum oxide, silica, zinc oxide, titanium oxide, sodium oxide molybdena, calcium oxide,
Magnesia, barium monoxide, iron oxide, ferrous oxide, ferroso-ferric oxide or manganese oxide；
The adhesive of the composition interlayer is Kynoar, polytetrafluoroethylene (PTFE), polyvinyl alcohol, sodium cellulose glycolate, butylbenzene
Rubber, gelatin, sodium alginate, LA132 or cyclodextrin；
The conductive agent is acetylene black, Super P, carbon fiber, CNT, Ketjen black, graphite or Graphene.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673350A (en) * | 2017-09-04 | 2018-02-09 | 北京化工大学 | A kind of polyethyleneimine-modified biomass carbon material, preparation method and the application in lithium-sulfur cell diagram modification |
| CN107706337A (en) * | 2017-11-13 | 2018-02-16 | 桑顿新能源科技有限公司 | A kind of composite coated barrier film for nickelic ternary lithium ion battery and preparation method thereof |
| CN108461691A (en) * | 2018-02-08 | 2018-08-28 | 深圳锂硫科技有限公司 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
| CN108987648A (en) * | 2018-06-28 | 2018-12-11 | 肇庆市华师大光电产业研究院 | A kind of preparation method applied to the functional interlayer of anode in lithium-sulfur cell |
| CN109065800A (en) * | 2018-07-03 | 2018-12-21 | 华南师范大学 | A kind of preparation method of metal organic frame carbon nano tube compound material |
| CN109103399A (en) * | 2018-08-22 | 2018-12-28 | 武汉大学 | A kind of lithium-sulfur cell functional diaphragm and preparation method thereof and the application in lithium-sulfur cell |
| CN109273649A (en) * | 2018-09-25 | 2019-01-25 | 合肥先杰新能源科技有限公司 | Lithium battery micro-pore septum and preparation method thereof |
| CN110364660A (en) * | 2018-04-10 | 2019-10-22 | 中国科学院上海硅酸盐研究所 | A kind of water system Zinc ion battery composite diaphragm and preparation method |
| CN110731021A (en) * | 2018-02-19 | 2020-01-24 | 株式会社Lg化学 | Separator for lithium-sulfur battery, method for preparing same, and lithium-sulfur battery comprising same |
| CN112768840A (en) * | 2021-01-04 | 2021-05-07 | 长沙矿冶研究院有限责任公司 | Multifunctional diaphragm of lithium-sulfur battery and preparation method thereof |
| CN112952203A (en) * | 2021-02-26 | 2021-06-11 | 大连交通大学 | Intelligent lithium-sulfur battery based on shape memory effect |
| CN113782912A (en) * | 2021-09-15 | 2021-12-10 | 电子科技大学长三角研究院(湖州) | Composite diaphragm modified by rhizopus hypha carbon and preparation method and application thereof |
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| CN115275525A (en) * | 2022-08-23 | 2022-11-01 | 吉林师范大学 | Diaphragm for inhibiting polysulfide shuttling effect, preparation process thereof and lithium-sulfur battery using diaphragm |
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| CN107673350A (en) * | 2017-09-04 | 2018-02-09 | 北京化工大学 | A kind of polyethyleneimine-modified biomass carbon material, preparation method and the application in lithium-sulfur cell diagram modification |
| CN107706337A (en) * | 2017-11-13 | 2018-02-16 | 桑顿新能源科技有限公司 | A kind of composite coated barrier film for nickelic ternary lithium ion battery and preparation method thereof |
| CN108461691A (en) * | 2018-02-08 | 2018-08-28 | 深圳锂硫科技有限公司 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
| US11289770B2 (en) | 2018-02-19 | 2022-03-29 | Lg Energy Solution, Ltd. | Separator including separator base with coating layer including structural unit derived from sulfonic acid containing catechol/pyrogallol and dopamine, manufacturing method therefor, and lithium-sulfur battery comprising same |
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| CN110364660A (en) * | 2018-04-10 | 2019-10-22 | 中国科学院上海硅酸盐研究所 | A kind of water system Zinc ion battery composite diaphragm and preparation method |
| CN108987648A (en) * | 2018-06-28 | 2018-12-11 | 肇庆市华师大光电产业研究院 | A kind of preparation method applied to the functional interlayer of anode in lithium-sulfur cell |
| WO2020006788A1 (en) * | 2018-07-03 | 2020-01-09 | 华南师范大学 | Method for preparing composite material of metal-organic frameworks and carbon nanotubes |
| CN109065800A (en) * | 2018-07-03 | 2018-12-21 | 华南师范大学 | A kind of preparation method of metal organic frame carbon nano tube compound material |
| CN109103399A (en) * | 2018-08-22 | 2018-12-28 | 武汉大学 | A kind of lithium-sulfur cell functional diaphragm and preparation method thereof and the application in lithium-sulfur cell |
| CN109273649A (en) * | 2018-09-25 | 2019-01-25 | 合肥先杰新能源科技有限公司 | Lithium battery micro-pore septum and preparation method thereof |
| CN112768840A (en) * | 2021-01-04 | 2021-05-07 | 长沙矿冶研究院有限责任公司 | Multifunctional diaphragm of lithium-sulfur battery and preparation method thereof |
| CN112952203A (en) * | 2021-02-26 | 2021-06-11 | 大连交通大学 | Intelligent lithium-sulfur battery based on shape memory effect |
| CN112952203B (en) * | 2021-02-26 | 2023-09-01 | 大连交通大学 | Intelligent lithium sulfur battery based on shape memory effect |
| CN113782912A (en) * | 2021-09-15 | 2021-12-10 | 电子科技大学长三角研究院(湖州) | Composite diaphragm modified by rhizopus hypha carbon and preparation method and application thereof |
| CN113937418A (en) * | 2021-10-11 | 2022-01-14 | 中科南京绿色制造产业创新研究院 | Lithium-sulfur battery diaphragm, preparation method thereof and lithium-sulfur battery |
| CN113937418B (en) * | 2021-10-11 | 2023-11-17 | 中科南京绿色制造产业创新研究院 | Lithium-sulfur battery diaphragm, preparation method thereof and lithium-sulfur battery |
| CN115275525A (en) * | 2022-08-23 | 2022-11-01 | 吉林师范大学 | Diaphragm for inhibiting polysulfide shuttling effect, preparation process thereof and lithium-sulfur battery using diaphragm |
| CN115275525B (en) * | 2022-08-23 | 2023-08-22 | 吉林师范大学 | Diaphragm for inhibiting polysulfide shuttle effect, preparation process thereof and lithium sulfur battery using diaphragm |
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