CN105514325A - Composite film for lithium-sulfur battery - Google Patents
Composite film for lithium-sulfur battery Download PDFInfo
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- CN105514325A CN105514325A CN201410494484.XA CN201410494484A CN105514325A CN 105514325 A CN105514325 A CN 105514325A CN 201410494484 A CN201410494484 A CN 201410494484A CN 105514325 A CN105514325 A CN 105514325A
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Abstract
A composite film for a lithium-sulfur battery is composed of: one or more than two polymers having film-forming property, and one or more than two salts containing nitrate. The mass percentage of the salts containing nitrate in the composite film is 0.1-90%. Because the film is rich in nitrate, better utilization on the nitrate in the composite film can be achieved and further quick uncontrollable consumption of the nitrate is avoided, thereby delaying consumption of the nitrate and further increasing capacity retention ratio of the battery.
Description
Technical field
The present invention relates to lithium-sulfur cell field, specifically, the lithium-sulfur cell related to comprises negative metal lithium, containing element sulphur positive pole, barrier film and electrolyte solution.
Background technology
Lithium-sulfur cell, because it has very high theoretical specific energy density (2600Wh.kg-1) and low price, becomes the study hotspot of lithium battery of future generation.Particularly last decade comes, and along with the development of the positive electrode of the ripe nanometer technology of application, greatly advances the process that lithium-sulfur cell is practical.
But some intrinsic shortcomings of lithium-sulfur cell.The dissolving of such as discharging product polysulfide and shuttle back and forth between both positive and negative polarity, lithium sulfide/curing lithium is all improve the obstacle of lithium-sulfur cell cyclical stability further in the irreversible deposition of both positive and negative polarity.
In order to solve the problem, people mainly study from three aspects battery.1), positive electrode aspect, charcoal is carried out coated mixing with sulphur by physical method or chemical method and is stoped polysulfide to spread to negative pole.2), electrolyte aspect, by reducing polysulfide dissolving in the electrolytic solution.3), negative pole aspect, by adding material in the electrolytic solution, make its method forming diaphragm in negative terminal surface suppress the effect of shuttling back and forth of polysulfide.People have done a lot of work in this respect.ZhanLin etc. (Adv.Funct.Mater.2012.DOI:10.1002/adfm.201200696) propose and add phosphoric sulfide in the electrolytic solution; not only can form diaphragm in lithium sheet negative terminal surface; and the lithium sulfide of irreversible deposition can be dissolved; stability test improves, but phosphoric sulfide also may increase " flying shuttle " effect of battery to the dissolving of polysulfide.YuriyV.Mikhaylik etc. (Pub.No.:US2011/0059350Al) propose nitrate can suppress shuttling back and forth of polysulfide.Its mechanism of action forms diaphragm in lithium sheet negative terminal surface, effectively improves the coulombic efficiency of battery.The SEI film formed due to nitrate ion is also unstable, can carry out along with discharge and recharge, and occur to decompose or avalanche, newly exposed lithium can react again with nitrate anion.Under zhang etc. report low-voltage in addition can there is irreversible reaction at positive pole and consume lithium nitrate in nitrate anion.To sum up, the content can saying nitrate ion in battery and the use how managing nitrate ion better will determine coulombic efficiency and the capacity stability of battery.
Summary of the invention
The object of this invention is to provide the composite membrane being rich in nitrate ion.This composite membrane has the advantages such as cost is low, nitrate anion utilance is high, stability test is good.
Composite membrane provided by the invention comprises:
(1), one or more contain the salt of nitrate anion;
The described salt containing acid group include, but are not limited to following one or more: lithium nitrate, ammonium nitrate, guanidine nitrate, cesium nitrate, rubidium nitrate.Wherein preferably lithium nitrate, guanidine nitrate, cesium nitrate etc.
The mass fraction of the described salt containing acid group is 0.1%-90%.Preferably 10%-70%.
(2), one or more have the polymer of film forming.
The described polymer with film forming include but not limited to following one or more: Kynoar, polysulfones, polypropylene, polyethylene, polyurethane, poly epoxy resin, polybenzimidazoles, polyphenylene oxide, shitosan, sodium carboxymethylcellulose etc.
Described composite film thickness is 0.01mm-5mm, is preferably 0.05mm-1mm.
Described composite membrane preparation method can be:
Be dissolved in one or several solvents by the salt containing acid group and the polymer with film forming, by spraying, blade coating, dip-coating, from methods such as curtain coatings, oven dry or natural drying form certain thickness composite membrane.Described solvent include but not limited to following one or more: 1-METHYLPYRROLIDONE (NMP), N, dinethylformamide (DMF), DMA (DMAc), acetone, oxolane, acetonitrile, dimethyl sulfoxide (DMSO), water etc.Namely can be applicable in battery after abundant for the composite membrane of preparation drying is dewatered.
The concentration of film forming solution is 2%-70%, wherein even more preferably 5%-50%.
Beneficial effect of the present invention
Adopt the lithium-sulfur cell being rich in the composite membrane of nitrate ion.There is better capacity stability.Because be rich in by nitrate anion in film, nitrate anion can be utilized better, avoid nitrate anion by quick uncontrollable consumption, delay the use of nitrate anion, and then improve the capability retention of battery.
Embodiment
The present invention is set forth further below by embodiment, instead of restriction the present invention.
Embodiment 1
Be rich in the preparation of the composite membrane of nitrate ion: Kynoar (PVDF) and lithium nitrate mixed according to mass ratio 1:1 and be dissolved in 1-METHYLPYRROLIDONE (NMP), be made into the film forming solution that concentration is 10%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 2
Be rich in the preparation of the composite membrane of nitrate ion: Kynoar (PVDF) and cesium nitrate mixed according to mass ratio 1:2 and be dissolved in 1-METHYLPYRROLIDONE (NMP), be made into the film forming solution that concentration is 15%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 3
Be rich in the preparation of the composite membrane of nitrate ion: polysulfones (PSF) and lithium nitrate mixed according to mass ratio 1:1 and be dissolved in DMF (DMF), be made into the film forming solution that concentration is 20%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 4
Be rich in the preparation of the composite membrane of nitrate ion: polysulfones (PSF) and guanidine nitrate mixed according to mass ratio 1:0.7 and be dissolved in DMA (DMAc), be made into the film forming solution that concentration is 15%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 5
Be rich in the preparation of the composite membrane of nitrate ion: sodium carboxymethylcellulose and ammonium nitrate mixed according to mass ratio 1:1 and be dissolved in deionized water, be made into the film forming solution that concentration is 25%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 6
Be rich in the preparation of the composite membrane of nitrate ion: sodium carboxymethylcellulose and rubidium nitrate mixed according to mass ratio 1:2 and be dissolved in deionized water, be made into the film forming solution that concentration is 30%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Embodiment 7
Be rich in the preparation of the composite membrane of nitrate ion: shitosan and lithium nitrate mixed according to mass ratio 1:0.6 and be dissolved in deionized water (containing 5% acetic acid), be made into the film forming solution that concentration is 30%.By film forming solution casting film.Naturally dry for 70 DEG C, for subsequent use after 70 DEG C of vacuum dryings dewater.
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Comparative example
Comparative example film: the polyethylene polypropylene composite membrane (2325) that Celgard company produces
The negative pole of lithium-sulfur cell to be thickness the be lithium paper tinsel of 20 microns, positive pole adopts following methods preparation: blended in 1-METHYLPYRROLIDONE (NMP) of the Kynoar (PVDF) of the SuperP charcoal of 20 mass fractions, the elemental sulfur of 70 mass fractions, 10 mass fractions, is coated on aluminium foil.Sulfur content after drying in positive-active layer is 1.0 millis gram/cm.The electrolyte of lithium-sulfur cell is the dioxolanes/glycol dimethyl ether (volume ratio 1:1) of 1 mol/L trimethyl fluoride sulfonyl amine lithium.
Above-mentioned assembly is fitted together with the layer structure of positive pole/barrier film/negative pole, and seals after 20 microlitres/every square centimeter of positive pole area adds electrolyte.After static 1 hour, relative to the quality of positive active material sulphur, carry out battery charging and discharging with 0.1C, 1C respectively.The cut-ff voltage of charging is 2.8V, and the cut-ff voltage of electric discharge is 1.88V.Carry out 100 circulations.Investigate the initial specific capacity of battery, specific capacity and battery coulombic efficiency after 100 circulations.Experimental result is as shown in table 1.
Table 1
Result shows, adopts the lithium-sulfur cell being rich in the composite membrane of nitrate ion.There is better capacity stability.Because be rich in by nitrate anion in film, nitrate anion can be utilized better, avoid nitrate anion by quick uncontrollable consumption, delay the use of nitrate anion, and then improve the capability retention of battery.
Claims (8)
1. for a composite membrane for lithium-sulfur cell, by a kind of or more than the two kinds polymer with film forming, and a kind of or more than the two kinds salt containing nitrate anion;
The mass fraction of the salt containing nitrate anion in composite membrane is 0.1%-90%.
2., according to composite membrane according to claim 1, it is characterized in that:
The described salt containing nitrate anion comprises one in lithium nitrate, ammonium nitrate, guanidine nitrate, cesium nitrate, rubidium nitrate or more than two kinds; One wherein preferably in lithium nitrate, guanidine nitrate, cesium nitrate or more than two kinds.
3., according to the composite membrane described in claim 1 or 2, it is characterized in that:
The mass fraction of the described salt containing nitrate anion is preferably 10%-70%.
4., according to composite membrane according to claim 1, it is characterized in that:
The described polymer with film forming comprises one in Kynoar, polysulfones, polypropylene, polyethylene, polyurethane, poly epoxy resin, polybenzimidazoles, polyphenylene oxide, shitosan, sodium carboxymethylcellulose or more than two kinds.
5., according to composite membrane according to claim 1, it is characterized in that:
Described composite film thickness is 0.01mm-5mm, is preferably 0.05mm-1mm.
6. composite membrane according to claim 1, is characterized in that: composite membrane is prepared from by following process:
Required salt containing nitrate anion and the polymer with film forming are dissolved in solvent, by spraying, blade coating, dip-coating or from casting method, dry or natural drying formation composite membrane;
Described solvent comprises: 1-METHYLPYRROLIDONE (NMP), N, one in dinethylformamide (DMF), DMA (DMAc), acetone, oxolane, acetonitrile, dimethyl sulfoxide (DMSO), water or more than two kinds; The mass concentration of film forming solution is 2%-70%.
7. according to composite membrane described in claim 6, it is characterized in that: the mass concentration preferably 5%-50% of film forming solution.
8. according to composite membrane described in claim 6, it is characterized in that: namely can be applicable in battery after abundant for the composite membrane of preparation drying is dewatered.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111224046A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Application of composite membrane in lithium-sulfur battery |
| CN111755745A (en) * | 2020-06-18 | 2020-10-09 | 合肥国轩高科动力能源有限公司 | Lithium-sulfur battery electrolyte and liquid injection method thereof |
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| CN1930725A (en) * | 2004-01-06 | 2007-03-14 | 赛昂能源有限公司 | Electrolytes for lithium sulfur cells |
| CN102903974A (en) * | 2012-10-22 | 2013-01-30 | 中国电子科技集团公司第十八研究所 | Lithium-sulfur secondary battery |
| CN103855349A (en) * | 2012-12-04 | 2014-06-11 | 中国科学院大连化学物理研究所 | Diaphragm of lithium-sulfur battery |
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- 2014-09-24 CN CN201410494484.XA patent/CN105514325A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1930725A (en) * | 2004-01-06 | 2007-03-14 | 赛昂能源有限公司 | Electrolytes for lithium sulfur cells |
| CN102903974A (en) * | 2012-10-22 | 2013-01-30 | 中国电子科技集团公司第十八研究所 | Lithium-sulfur secondary battery |
| CN103855349A (en) * | 2012-12-04 | 2014-06-11 | 中国科学院大连化学物理研究所 | Diaphragm of lithium-sulfur battery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111224046A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Application of composite membrane in lithium-sulfur battery |
| CN111224046B (en) * | 2018-11-26 | 2023-04-18 | 中国科学院大连化学物理研究所 | Application of composite membrane in lithium-sulfur battery |
| CN111755745A (en) * | 2020-06-18 | 2020-10-09 | 合肥国轩高科动力能源有限公司 | Lithium-sulfur battery electrolyte and liquid injection method thereof |
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