CN106876777A - A kind of lithium-sulfur cell - Google Patents
A kind of lithium-sulfur cell Download PDFInfo
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- CN106876777A CN106876777A CN201510930374.8A CN201510930374A CN106876777A CN 106876777 A CN106876777 A CN 106876777A CN 201510930374 A CN201510930374 A CN 201510930374A CN 106876777 A CN106876777 A CN 106876777A
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The present invention relates to a kind of lithium-sulfur cell, by solvent molecule, solute cation, solute cation composition, solute molar concentration in the electrolytic solution is 0.1~10M to its electrolyte.The solute cation includes：Alkali metal cation, alkaline earth metal cation, season ammonium ion, pridylamino ion, imidazoles amino ion, quaternary phosphonium base cation, pyrimidine cation, than azoles cation, pyridazine cation, thiazolium cation, oxazoles cation, triazole Yi Ji one or two or more kinds in Phosphonium, ammonium cation, its molar concentration 0.1-10M.Charging process of the invention is opposite with traditional lithium-sulfur cell.Fundamentally solve the problems, such as that many lithium sulfides are dissolved into electrolyte and are spread to negative pole.Be not in the problem of the electrode interface mass transfer that all solid state electrolyte faces because electrolyte is liquid.
Description
Technical field
Generality of the present invention relates to the electrode that active material is done with sulphur, is more particularly to the application of lithium-sulfur cell.
Background technology
1962, Herbert et al. applied for the patent using elemental sulfur as anode, and the research and development of lithium-sulfur cell have formally pulled open prelude.As shown by data, sulphur abundance in nature is about 0.048wt%, and belongs to the natural resources for not yet making full use of.Sulphur in nature is mainly with thermodynamically stable elemental sulfur (S under normal temperature8) form is present, the features such as with hypotoxicity, big cheap, storage and low-density, specific capacity is up to 1,675mAh/g, is the specific capacity highest positive electrode being currently known.Lithium is also that current potential is most negative in nature, and energy density highest metal, lithium has theoretical energy density very high with the battery (Li/S) of sulphur composition, and specific energy is more up to 2,600Wh/kg, makes research staff very excited.But the problems such as dissolving deposition inhomogeneities of the electrons/ions insulating properties, the dissolving animal migration of many lithium sulfides of intermediate product and lithium metal due to lithium-sulphur cell positive electrode elemental sulfur, cause the cyclicity of lithium-sulfur cell and security all very poor.The study limitation in 20th century is in the reactivity that elemental sulfur is improved by regulating and controlling temperature and solubility, it is difficult to solve the spontaneous reaction and potential safety hazard of many lithium sulfides and lithium metal, lithium-sulfur cell does not attain full development, and people are also therefore by the shift of the work focus to the more stable sodium-sulphur battery system of high-temperature behavior and the more excellent lithium-ion battery system of cycle performance.Until in recent years, under the dual-pressure of energy crisis and environmental crisis, human society is further urgent to the demand of high specific energy batteries, and lithium-sulfur cell has regained highest attention because of its potential high specific energy advantage (theoretical specific energy 2600Wh/kg).The developed countries such as the U.S., Japan support that lithium-sulfur cell energy storage technology is developed energetically.New Energy and Industrial Technology Development Organization (NEDO) put into 30,000,000,000 yen of development budgets of (being roughly equal to 2,400,000,000 RMB) every year from 2009, and target is the energy density of lithium-sulfur cell is reached 500Wh/kg in the year two thousand twenty.European Union opened " horizon 2020 " research and development plan in 2015, and 7,600,000 dollars of plan input is used for the research and development of lithium-sulfur cell used for electric vehicle.USDOE also puts into the exploitation that substantial amounts of manpower and materials support lithium-sulfur cell.Meanwhile, international business has Sion Power, Polyplus, the Moltech in the U.S., the Oxis and the magnitude of South Korea three of Britain also achieving impressive progress, representative firm in recent years to the research and development of lithium-sulfur cell.2010, Sion Power companies applied on unmanned plane lithium-sulfur cell (350Wh/kg) together with solar cell, create the record of non-stop flight 14 days.Oxis companies declared the 200Wh/kg lithium-sulfur cells cycle life developed in 2013 up to 700 times, had assembled electric motor car, and planned to enable regenerative resource to stablize the lithium-sulfur cell for exporting in production in 2016.When being charged to lithium-sulfur cell, lithium ion is reduced into lithium metal at anode, while lithium sulfide material is oxidized to form polysulfide and sulphur at negative electrode, lithium ion is released into the electrolyte of connection negative electrode and anode.During electric discharge, lithium metal is oxidized to lithium ion at anode, and the lithium ion is released into electrolyte, while lithium ion and sulphur participate in reduction reaction and forms lithium sulfide material at negative electrode.
Although having as above advantage, lithium-sulfur cell also has with a distance from suitable from practical, and current subject matter includes：(1) lithium metal of negative pole reacts with the polysulfide for being dissolved in electrolyte, and then little by little generation polysulfide enters electrolyte to the elemental sulfur of side of the positive electrode, and then is reacted with lithium metal, ultimately causes both positive and negative polarity active material and is lost in and is caved in region；(2) in lithium-sulfur cell discharge process, after the polysulfide of formation enters electrolyte, highly enriched polysulfide causes electrolysis fluid viscosity to raise, and causes electrolyte conductivity to reduce, and battery performance is remarkably decreased；(3) operating temperature of lithium-sulfur cell system is up to 300~400 DEG C, and this needs exotic material costly prevents battery from burning with the preparation technology of complexity.In addition, because elemental sulfur is non-conductive at room temperature, it is impossible to used separately as positive electrode, so generally it is mixed with a certain amount of conductive material to improve positive pole zone electric conductivity when lithium-sulfur cell is prepared, but excessive hybrid conductive material, can significantly reduce the specific energy of lithium-sulfur cell again.Recent years, correlative study work both domestic and external was rather active, at present on the occasion of the key stage of technological break-through.This kind of typical rechargeable battery is included using lithium metal as active material, using lithium metal alloy as active material or using lithium metal/carbon complex as the anode of active anode material.This battery includes the negative electrode as active material containing sulphur.
For " shuttle " effect that polysulfide dissolving migration is caused, current solution is very limited, and people are more to set about from the angle of electrolysis additive and barrier film.1)《Electrochemistry journal》(ElectrochimicaActa70; 2012; 344-348) work that Sheng S.Zhang add additive lithium nitrate in the electrolytic solution is reported; the addition of lithium nitrate can make cathode of lithium surface form protective layer; but the protective layer can be gradually used up, by will gradually be failed after ten several times charge and discharge cycles.2)《Power source magazine》(Journal of Power Sources 183,2008,441-445) describes another method, i.e., add toluene, methyl acetate etc. in the electrolytic solution to suppress the dissolving of polysulfide, but this method easily causes the decline of electrolytic conductivity.3) the third method is to use composite polymer gel electrolyte separator, as Chinese invention patent 201110110093.X and《Power source magazine》(Journal of Power Sources 212,2012,179-185) disclosed report, gel electrolyte is the gel polymeric network with appropriate microporous structure formed by certain method by polymer, plasticizer (lithium salts solvent, ionic liquid etc.) and lithium salts, ionic conduction is realized by the polymer network system of solvent swell using the liquid electrolyte molecule being fixed in micro-structural, and its unique network structure makes gel while having the cohesiveness of solid and the dispersion conductibility of liquid.Because electrolyte solution quilt " cladding " is in polymer network, it is suppressed the dissolving of polysulfide, consequently, it is possible to solving the problems, such as that sulphur active material is lost in a certain extent；But gel electrolyte separator electrical conductivity and intensity are all relatively low.4) the 4th kind of method is the electrolyte membrance for preparing macroion selectivity, as《Power and energy magazine》(253-259 of Journal of Power Sources 246 (2014)) disclosed report, there is the obstructing capacity of lithium ion selective penetrated property and polysulfide higher with barrier film of the Nafion perfluorosulfonic acid ion conductive membranes as representative, such that it is able to effectively suppress diffusion of the polysulfide from positive pole to negative pole.But the material cost of this kind of barrier film is higher, and ionic conductivity is relatively low, it is difficult to meet real requirement.5) fifth method is to deposit one layer of lithium ion permselective membrane of one layer of SEI film or sputtering in negative terminal surface, and this film is inorganic ceramic membrane, with larger fragility.And be Volume Changes the characteristics of lithium-sulfur cell than larger, the dissolving of lithium ion and the pattern of deposition are not fixed, therefore this solid ceramic film is difficult to tolerate the investigation of battery longtime running.In sum, although above method plays the role of positive to the shuttle effect for organizing many lithium sulfides, the dissolving of many lithium sulfides cannot be inherently limited, also just cannot inherently organizes the possibility that many lithium sulfides spread to negative pole.Show that the coulombic efficiency of developed lithium-sulfur cell is difficult to reach 100%, best level is also only capable of between 95%~99%.
The content of the invention
It is an object of the invention to solve the above problems, there is provided a kind of method of lithium-sulfur cell negative pole protection.
To achieve the above object, the technical solution adopted by the present invention is：It is made up of the polarity of the lithium-sulfur cell electrolyte and functional group, make many lithium sulfides of the intermediate product in discharge process that disproportionation (unconventional from S82- to S62- to the reaction of S42- to S22- and S2-) directly to occur, generation sulphur and lithium sulfide are attached to positive electrode (mainly carbon material) surface, so as to stop its continued dissolution in the electrolytic solution and be spread to negative pole.
Wherein, the traditional discharge process of sulphur is as follows：
S8→S8→ S → S → S → S,
Charging process is in contrast.
The discharge process of sulphur of the invention is as follows:
S/Sn4~8.Wherein, first step reaction is transformation of the elemental sulfur to soluble many lithium sulfides, is long response time；Second step is the process that many lithium sulfides change to elemental sulfur and curing lithium/lithium sulfide, is fast response.Because elemental sulfur and curing lithium/lithium sulfide are solids of sedimentation, will not dissolve in the electrolytic solution, it is possible to fundamentally solving the problems, such as many lithium sulfide diffusions.From apparent, course of reaction is such：S/S,
With solvent molecule, solute anion, solute cation composition, solute molar concentration in the electrolytic solution is 0.1~10M to this kind of electrolyte.
The solute cation includes：Alkali metal cation, alkaline earth metal cation, season ammonium ion, pridylamino ion, imidazoles amino ion, quaternary phosphonium base cation, pyrimidine cation, than azoles cation, pyridazine cation, thiazolium cation, oxazoles cation, triazole Yi Ji one or two or more kinds in Phosphonium, ammonium cation, its molar concentration 0.1-10M.
The preferred season ammonium ion of solute cation or/and quaternary phosphonium base cation.
The molecular structure of the cation is as follows：
R1-R10 is respectively-H ,-C6H6 ,-CH3 ,-CH2CH2CH3 ,-CH (CH3) CH3 ,-OH ,-OCH3 ,-OCH2CH3 ,-CH2CH3 ,-OC6H6.
Alkali metal cation and alkaline earth metal cation are one or two or more kinds in lithium, sodium, potassium, rubidium, caesium, calcium, magnesium, barium.
The cation dispersion exists in solvent, and/or with the complex form that cation and solvent are formed.
The solute anion can include：1) acid ion, such as sulfate radical, nitrate anion, acetate, perchlorate, chlorate anions, chlorion, fluorine ion, bromide ion, iodide ion；2) 1) described in ion and its complex ion with solvent；3) sulfoamido, sulfimide base, bis trifluoromethyl sulfimide base, trifluorosulfonimide base；4) 3) described in anion and solvent complex compound；5) combination of above-mentioned anion.
The solvent includes：Silicon ethers (such as dimethoxy silicon ether, 1,2- dimethoxy silicon ether), polyoxy ethers (such as tetraethyleneglycol dimethyl ether, six glycol dimethyl ethers, eight glycol dimethyl ethers), polyethylene glycols (molecular weight is below 1000), alcohols (polyvinyl alcohol molecule amount is below 1000), sulfone class (dimethyl sulfoxide (DMSO), sulfolane), and various solvents mixture.
Beneficial effect
The sulphur of present invention offer, electrolyte combination electrode have the characteristics that and beneficial effect：
(1) sulphur, electrolyte compound system make it be changed in the reaction mechanism of positive electrode surface, and many lithium sulfides directly occur disproportionation and produce sulphur and lithium sulfide, and the existence time of intermediate product is very of short duration, therefore does not diffuse into electrolyte body and negative terminal surface.
(2) charging process of the invention is opposite with traditional lithium-sulfur cell.Fundamentally solve the problems, such as that many lithium sulfides are dissolved into electrolyte and are spread to negative pole.Be not in the problem of the electrode interface mass transfer that all solid state electrolyte faces because electrolyte is liquid.Meanwhile, because polysulfide root ion is alkalescent, highly polar anion, by selecting the electrolyte containing highly acid, low pole cation paired, the unstability of polysulfide root ion can be increased, make it easy to disproportionation.This can be as the guiding theory for developing such electrolyte.
(3) divergent question of the sulfur electrode that the innovation makes is solved, and has fabulous application prospect in the battery system in addition to lithium-sulfur cell.
Brief description of the drawings
Fig. 1 is sulfur-bearing, the lithium-sulfur cell performance of electrolyte combination electrode assembling prepared by embodiment 1；
Fig. 2 is common carbon sulphur combination electrode and common glycol dimethyl ether/dioxy ring amyl ether (1：1) the lithium-sulfur cell performance of assembling；
Fig. 3 is sulfur-bearing, the lithium-sulfur cell performance of electrolyte combination electrode assembling prepared by embodiment 2；
Fig. 4 is sulfur-bearing, the lithium-sulfur cell performance of electrolyte combination electrode assembling prepared by embodiment 3；
Fig. 5 a) it is the XRD spectra of elemental sulfur；B) it is the XRD spectra of lithium sulfide；C) XRD spectra of the sediment obtained for disproportionation in the electrolyte of embodiment 1, is the mixture of sulphur and lithium sulfide.
Specific embodiment
The protection of lithium-sulfur cell negative pole additive and its application method of the present invention are further described by the following examples.
Embodiment 1：
By 0.25g1,1,2,2- tetrafluoro ethyl sulfonic acid 1- ethyl-3-methylimidazoles are added in 10g sulfolane solvents, add bis trifluoromethyl sulfimide lithium, make the concentration of lithium ion for 1M, and strong agitation obtains clarifying electrolyte.Positive pole is impregnated using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 100 circulations, average coulombic efficiencies are 99.9% to battery, and capability retention is 89% (Fig. 1)；
And when using additive-free electrolyte, other conditions are constant, the average coulombic efficiencies of battery only have 48%, and capability retention is 40% ((Fig. 2).
Embodiment 2：
5g bromination triethyl group pyridines are added in 10g sulfolane solvents, bis trifluoromethyl sulfimide lithium is added, make the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 100 circulations, average coulombic efficiencies are 99.9% to battery, and capability retention is 90% (Fig. 3).
Embodiment 3：
0.504 gram of dialkyl group bromination phosphonium salt of tributyl ten is added in 10g sulfolane solvents, bis trifluoromethyl sulfimide lithium is added, makes the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 37 circulations, average coulombic efficiencies are 100% to battery, and capability retention is 80% (Fig. 4).
Embodiment 4：
1 gram of dialkyl group bromination phosphonium salt of tributyl ten is added in 10g sulfolane solvents, bis trifluoromethyl sulfimide lithium is added, makes the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 37 circulations, average coulombic efficiencies are 100% to battery, and capability retention is 85%.
Embodiment 5：
1 gram of dialkyl group bromination phosphonium salt of tributyl ten is added in 10g sulfolane solvents, bis trifluoromethyl sulfimide lithium is added, makes the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 100 circulations, average coulombic efficiencies are 100% to battery, and capability retention is 90%.
Embodiment 6：
0.64 gram of dialkyl group bromination phosphonium salt of tributyl ten is added in 10g dimethyl sulfoxide solvents, bis trifluoromethyl sulfimide lithium is added, makes the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 37 circulations, average coulombic efficiencies are 90% to battery, and capability retention is 70%.
Embodiment 7：
By in 0.75g additions 5g polydioxolanes (molecular weight 500) and 5g glycol dimethyl ethers, bis trifluoromethyl sulfimide lithium is added, make the concentration of lithium ion for 1M, strong agitation obtains clarifying electrolyte.Lithium sulphur button cell is assembled using electrolyte obtained above, its just extremely carbon-sulfur compound (58% fills sulfur content, PVDF binding agents).With 0.1 rate charge-discharge, 37 circulations, average coulombic efficiencies are 90% to battery, and capability retention is 70%.
Claims (9)
1. a kind of lithium-sulfur cell, its electrolyte is made up of solvent, solute cation, solute anion, and the solute cation includes：Alkali metal cation, alkaline earth metal cation, season ammonium ion, pridylamino ion, imidazoles amino ion, quaternary phosphonium base cation, pyrimidine cation, than azoles cation, pyridazine cation, thiazolium cation, oxazoles cation, triazole Yi Ji one or two or more kinds in Phosphonium, ammonium cation, its molar concentration 0.1-10M.
2. according to lithium-sulfur cell described in claim 1, it is characterised in that：The molecular structure of the cation be it is as follows in one or two or more kinds：
R1-R10 is respectively-H ,-C6H6 ,-CH3 ,-CH2CH2CH3 ,-CH (CH3) CH3 ,-OH ,-OCH3 ,-OCH2CH3 ,-CH2CH3 ,-OC6H6.
3. according to lithium-sulfur cell described in claim 1, it is characterised in that：
Metal cation is one or two or more kinds in lithium, sodium, potassium, rubidium, caesium, calcium, magnesium, barium.
4. according to lithium-sulfur cell described in claim 1 or 3, it is characterised in that：
The cation dispersion exists in solvent, and/or with the complex form that cation and solvent are formed.
5. according to lithium-sulfur cell described in claim 1, it is characterised in that：
The solute anion includes：Sulfate radical, nitrate anion in acid ion, acetate, perchlorate, chlorate anions, chlorion, fluorine ion, bromide ion, iodide ion, one or two or more kinds in sulfoamido, sulfimide base, bis trifluoromethyl sulfimide base, trifluorosulfonimide base, its molar concentration 0.1-10M.
6. according to lithium-sulfur cell described in claim 1 or 5, it is characterised in that：
The anionic dispersant exists in solvent, and/or with the complex form of anion and solvent.
7. according to lithium-sulfur cell described in claim 1, it is characterised in that：
The solvent includes the mixture of one or two or more kinds in silicon ethers, polyoxy ethers, polyethylene glycols, alcohols, sulfone class.
8. according to lithium-sulfur cell described in claim 7, it is characterised in that：
The silicon ethers is one or two or more kinds in dimethoxy silicon ether, 1,2- dimethoxy silicon ethers；The polyoxy ethers is one or two or more kinds in tetraethyleneglycol dimethyl ether, six glycol dimethyl ethers, eight glycol dimethyl ethers；The molecular weight of the polyethylene glycols is between 100-1000；The alcohols is molecular weight 100-1000 polyvinyl alcohol；The sulfone class is one or two or more kinds in dimethyl sulfoxide (DMSO), sulfolane.
9. according to lithium-sulfur cell described in claim 1, it is characterised in that：The solute cation, solute anion collectively form solute, and solute molar concentration in the electrolytic solution is 0.1~10M.
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| CN109873200A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of dication liquid electrolyte and its preparation and application |
| CN109873199A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of polymer dispersion liquid and its application |
| CN112993406A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Electrolyte for fluorine ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109873199A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of polymer dispersion liquid and its application |
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| CN109873200B (en) * | 2017-12-04 | 2021-04-30 | 中国科学院大连化学物理研究所 | Double-cation liquid electrolyte and preparation and application thereof |
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| CN112993406B (en) * | 2019-12-14 | 2022-02-11 | 中国科学院大连化学物理研究所 | Electrolyte for fluorine ion battery |
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Application publication date: 20170620 |
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