CN106532115A - Gel electrolyte and lithium-sulfur secondary battery - Google Patents
Gel electrolyte and lithium-sulfur secondary battery Download PDFInfo
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- CN106532115A CN106532115A CN201611055541.XA CN201611055541A CN106532115A CN 106532115 A CN106532115 A CN 106532115A CN 201611055541 A CN201611055541 A CN 201611055541A CN 106532115 A CN106532115 A CN 106532115A
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- gel electrolyte
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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
- H01M10/056—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
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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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- 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
Abstract
The invention relates to a gel electrolyte and a lithium-sulfur secondary battery. The gel electrolyte comprises a liquid electrolyte, a polymerizable monomolecular organic matter and an initiator, wherein the liquid electrolyte comprises an ether organic solvent and a lithium salt; the polymerizable monomolecular organic matter is one or combination of more than one selected from the following structural formula: the formula is as shown in the specification, wherein R1, R2 and R3 are independently selected from an alkyl group or an alkyl acrylate group. According to the gel electrolyte disclosed by the invention, the probability of a monomolecular reaction can be effectively increased when a polymerization reaction occurs, so that the degree of polymerization of a polymer is improved; the gel electrolyte disclosed by the invention has high electrochemical performance and safety, so that, according to the lithium-sulfur secondary battery prepared by the gel electrolyte, the charging and discharging efficiency of the battery can be improved, and the battery has relatively high first-week discharging capacitance; and the preparation technology of the lithium-sulfur secondary battery is simple, and mass production is easily realized.
Description
Technical field
The invention belongs to technical field of electrochemistry, and in particular to a kind of gel electrolyte and lithium-sulfur rechargeable battery.
Background technology
Lithium rechargeable battery is because having big running voltage height, energy density, memory-less effect, having extended cycle life and nothing
The advantages of pollution.Since commercialization in 1991, lithium rechargeable battery has become the first-selected power supply of each electronic product.But
As electric bicycle, electric automobile, large-scale energy-accumulating power station enter extensive development and application stage, to lithium rechargeable battery
Propose the requirement of more height ratio capacity.At this stage, low (the actual ratio of positive electrode of the capacity of lithium rechargeable battery positive and negative pole material
Capacity<300mAh/g；Negative material specific capacity<400mAh/g) become the principal element of its development of restriction.Lithium-sulfur rechargeable battery must
So become the first-selection of battery of new generation.As positive electrode, the theoretical specific capacity of elemental sulfur reach 1675mAh/g and hypotoxicity,
Amount of storage is big, it is cheap the advantages of.
At this stage, it is that lithium polysulfide is dissolved in nonaqueous electrolytic solution that lithium-sulfur rechargeable battery has one of subject matter.Lithium sulfur
The middle discharging product of secondary cell can be dissolved in organic electrolyte, increase the viscosity of electrolyte, reduce ionic conductivity.Sulfur
Many sulphions that electrode occurs reduction reaction generation can be migrated between lithium battery both positive and negative polarity, cause the loss of active substance；Together
When, the polysulfide of dissolving can be diffused into negative pole across barrier film, with negative reaction, destroy anolyte interfacial film.In addition,
Lithium-sulfur rechargeable battery uses lithium metal as negative pole, and in addition to the high activity of lithium metal itself, lithium anode is in discharge and recharge
Li dendrite is formed in journey easily.Therefore, one of main solution is started with terms of electrolyte, is made using ether compound in early days
For the electrolyte solvent of lithium-sulfur cell, some additives in electrolyte, are added, the problems of dissolution of lithium polysulfide can be alleviated.
The content of the invention
The technical problem to be solved is to provide a kind of gel with good chemical property and safety
Electrolyte and lithium-sulfur rechargeable battery.
To reach above-mentioned purpose, the technical solution used in the present invention is：
It is an object of the present invention to provide a kind of gel electrolyte, including liquid electrolyte, polymerizable unimolecule are organic
Thing and initiator, described liquid electrolyte include ether organic solvent and lithium salts, and described polymerizable unimolecule Organic substance is
The combination of one or more in following structural formula：Wherein, R1、R2、R3Independently selected from
Alkyl or alkyl acrylic ester group.
Acrylate-based functional group in the polymerizable unimolecule Organic substance of the present invention primarily forms the net of gel electrolyte
Shape structure, makes gel electrolyte have certain mechanical strength and hardness；Alkyl functional group in polymerizable unimolecule Organic substance
Lithium ion mobility passage is primarily formed, lithium ion is moved freely in gel electrolyte under electric field action.
Preferably, described R1、R2、R3It is 1 independently selected from the carbon number of the alkyl or alkyl that carbon number is 1～5
～5 alkyl acrylic ester group.For example, R1、R2、R3Independently selected from methyl, ethyl, propyl group, butyl, amyl group,
CH3CH2COOCH2-、CH3CH2COOCH2CH2-、CH3CH2COOCH2CH2CH2- etc..
Preferably, the acrylate-based molecular weight in described polymerizable unimolecule Organic substance accounts for described polymerizable list
The 20～90% of molecular organic total molecular weight.
Preferably, the molecular weight of alkyl accounts for the 10～80% of described polymerizable unimolecule Organic substance total molecular weight.
It is further preferred that the acrylate-based molecular weight in described polymerizable unimolecule Organic substance account for it is described can
The 65～85% of polymerization unimolecule Organic substance total molecular weight.
It is further preferred that the molecular weight of alkyl account for described polymerizable unimolecule Organic substance total molecular weight 15～
35%.
Most preferably, described polymerizable unimolecule Organic substance is selected from trimethylolpropane trimethacrylate, Ji Wusi
The combination of one or more in alcohol tetraacrylate, neopentylglycol diacrylate.
Preferably, the addition quality of described polymerizable unimolecule Organic substance is the 1 of described gel electrolyte gross mass
～10%, more preferably 1～3%.
Preferably, the addition quality of described initiator is the 0.001～3% of described gel electrolyte gross mass, is entered
One step is preferably 0.05～0.1%.
Preferably, described initiator is the one kind or several in organic peroxide, inorganic peroxide, azo
The combination planted.
Preferably, described ether organic solvent is selected from glycol dimethyl ether, 1,3- dioxolanes, Isosorbide-5-Nitrae-dioxane
The combination of one or more in four (ethylene glycol) dimethyl ether, three (ethylene glycol) dimethyl ether.
Preferably, described lithium salts is the one kind in two (trimethyl fluoride sulfonyl) imine lithium, double fluorine sulfimide lithiums
Or several combinations.
It is further preferred that concentration of the described lithium salts in described liquid electrolyte is 0.9～1.1mol/L.
Preferably, described liquid electrolyte also includes additive, and described additive is selected from LiNO3、CrNO3、
RbNO3In the combination of one or more.
It is further preferred that the addition quality of described additive be described gel electrolyte gross mass 0.01～
5%, more elect 0.5～2% as.
It is a further object to provide a kind of lithium-sulfur rechargeable battery, using described gel electrolyte.
Third object of the present invention is to provide a kind of preparation method of described lithium-sulfur rechargeable battery, by positive pole, negative pole,
Barrier film and shell are assembled into battery core, and by described gel electrolyte injection described battery core, then sealing causes polymerization anti-
Should, battery carries out successively again being melted into, circulates, deflates, seal lithium-sulfur rechargeable battery described in obtaining.
Preferably, cause described polyreaction at a temperature of 20～100 DEG C or cause under the action of uv light
Described polyreaction.
It is further preferred that causing described polyreaction at a temperature of 60～80 DEG C.
It is outer that the lithium-sulfur rechargeable battery of the present invention is not limited to monetary apparatus, cylindrical steel shell-type, square aluminum shell type, Soft Roll polymer etc.
See feature.
As above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
The gel electrolyte of the present invention can be effectively increased the probability of monomolecular reaction when there is polyreaction, improve poly-
The degree of polymerization of compound, the gel electrolyte of the present invention have good chemical property and safety, thus gel electrolyte system
Standby lithium-sulfur rechargeable battery, can lift the efficiency for charge-discharge of battery and with higher head weeks discharge capacity, and the present invention
Preparation process is simple, easily realize producing in enormous quantities.
Specific embodiment
The present invention and its effectively result are described in detail with reference to specific embodiment, but embodiment of the present invention
Not limited to this.
Comparative example 1：
Prepare liquid electrolyte：Weighed, mixed stand-by by following volume ratio relation：Glycol dimethyl ether (is write a Chinese character in simplified form：
DME):1,3- dioxolane (is write a Chinese character in simplified form：DOL) volume ratio is 50：50, (the letter of two (trimethyl fluoride sulfonyl) imine lithium is added afterwards
Write：LiTFSI), obtain the liquid electrolyte E1 that LiTFSI concentration is 1mol/L.
Fluid injection battery core is treated in preparation：By elemental sulfur, conductive agent and bonding agent, it is agitated, coat, cold pressing, slitting, the work such as welding
Sequence obtains positive plate；Sulfur positive plate, lithium cathode sheet and barrier film prepare naked battery core together, are sealed for packaging bag using aluminum plastic film
Dress, is toasted afterwards.
Fluid injection and anode ring forming：In the battery core that above-mentioned liquid electrolyte E1 is injected after baking, stand until electrolysis immersion
Moisten whole diaphragm, then carry out being melted into, shaping, the operation such as degasification, finally give lithium-sulfur cell comparative example B1.
Comparative example 2：
After preparing by liquid electrolyte E1, plus 1%LiNO3As additive, liquid electrolyte E2 is obtained；
Fluid injection and anode ring forming：(battery core prepares same comparative example to the battery core that above-mentioned liquid electrolyte E2 is injected after baking
1), in, stand until electrolyte infiltrates whole diaphragm, then carry out being melted into, shaping, the operation such as degasification, finally give lithium-sulfur cell ratio
Compared with example B2.
Comparative example 3：
After preparing by liquid electrolyte E2, add 5% methyl methacrylate and 0.05% perbenzoic acid initiator,
Obtain gel electrolyte E3；
Fluid injection and anode ring forming：(battery core prepares same comparative example to the battery core that above-mentioned liquid electrolyte E3 is injected after baking
1), in, stand until electrolyte infiltrates whole diaphragm, after 80 DEG C of high temperature shelves 6 hours, then carry out being melted into, shaping, the work such as degasification
Sequence, finally gives lithium-sulfur cell comparative example B3.
Embodiment 1：
After preparing by liquid electrolyte E1, add 2% trimethylolpropane trimethacrylate (No. CAS：15625-89-
5) He 0.05% perbenzoic acid initiator, obtains gel electrolyte ES1；
Fluid injection and anode ring forming：(battery core prepares same comparative example to the battery core that above-mentioned gel electrolyte ES1 is injected after baking
1), in, stand until electrolyte infiltrates whole diaphragm, after 80 DEG C of high temperature shelves 4 hours, then carry out being melted into, shaping, the work such as degasification
Sequence, finally gives lithium-sulfur cell embodiment BS1.
Embodiment 2：
After preparing by liquid electrolyte E2, add 2% trimethylolpropane trimethacrylate (No. CAS：15625-89-
5) He 0.05% perbenzoic acid initiator, obtains gel electrolyte ES2；
Fluid injection and anode ring forming：The battery core that above-mentioned electrolyte ES2 is injected after baking (preparation of battery core is with comparative example 1)
In, stand until electrolyte infiltrates whole diaphragm, after 65 DEG C of high temperature shelves 6 hours, then carry out being melted into, shaping, the operation such as degasification,
Finally give lithium-sulfur cell embodiment BS2.
Embodiment 3：
After preparing by liquid electrolyte E1, add 2% tetramethylol methane tetraacrylate (No. CAS：4986-89-4) and
0.05% perbenzoic acid initiator, obtains gel electrolyte ES3；
Fluid injection and anode ring forming：The battery core that above-mentioned electrolyte ES3 is injected after baking (preparation of battery core is with comparative example 1)
In, stand until electrolyte infiltrates whole diaphragm, after 80 DEG C of high temperature shelves 4 hours, then carry out being melted into, shaping, the operation such as degasification,
Finally give lithium-sulfur cell embodiment BS3.
Embodiment 4：After preparing by liquid electrolyte E2, add 2% tetramethylol methane tetraacrylate (No. CAS：4986-
89-4) He 0.05% perbenzoic acid initiator, obtains gel electrolyte ES4；
Fluid injection and anode ring forming：The battery core that above-mentioned electrolyte ES4 is injected after baking (preparation of battery core is with comparative example 1)
In, stand until electrolyte infiltrates whole diaphragm, after 65 DEG C of high temperature shelves 6 hours, then carry out being melted into, shaping, the operation such as degasification,
Finally give lithium-sulfur cell embodiment BS4.
Embodiment 5：After preparing by liquid electrolyte E1, add 2% neopentylglycol diacrylate (No. CAS：2223-
82-7) He 0.08% perbenzoic acid initiator, obtains gel electrolyte ES5；
Fluid injection and anode ring forming：The battery core that above-mentioned electrolyte ES5 is injected after baking (preparation of battery core is with comparative example 1)
In, stand until electrolyte infiltrates whole diaphragm, after 80 DEG C of high temperature shelves 4 hours, then carry out being melted into, shaping, the operation such as degasification,
Finally give lithium-sulfur cell embodiment BS5.
Embodiment 6：After preparing by liquid electrolyte E2, add 2% neopentylglycol diacrylate (No. CAS：2223-82-
7) He 0.08% perbenzoic acid initiator, obtains gel electrolyte ES6；
Fluid injection and anode ring forming：The battery core that above-mentioned electrolyte ES6 is injected after baking (preparation of battery core is with comparative example 1)
In, stand until electrolyte infiltrates whole diaphragm, after 65 DEG C of high temperature shelves 6 hours, then carry out being melted into, shaping, the operation such as degasification,
Finally give lithium-sulfur cell embodiment BS6.
Table 1 is the battery performance contrast of comparative example and embodiment.
Table 1
From experimental result, using the gel state lithium-sulfur rechargeable battery of the present invention, the capacity in its cyclic process in 10 weeks
Conservation rate and efficiency for charge-discharge are above lithium-sulfur rechargeable battery and adopt liquid electrolyte.Illustrate that the gel state lithium-sulfur rechargeable battery has
There is more excellent chemical property.
Above-described embodiment technology design only to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this, all according to the present invention
Equivalence changes or modification that spirit is made, should all be included within the scope of the present invention.
Claims (11)
1. a kind of gel electrolyte, it is characterised in that：Including liquid electrolyte, polymerizable unimolecule Organic substance and initiator, institute
The liquid electrolyte stated includes ether organic solvent and lithium salts, and described polymerizable unimolecule Organic substance is selected from following structural formula
In the combination of one or more：Wherein, R1、R2、R3Independently selected from alkyl or alkyl
Perester radical.
2. gel electrolyte according to claim 1, it is characterised in that：Described R1、R2、R3Independently selected from carbon atom
Number for 1～5 alkyl or alkyl carbon number be 1～5 alkyl acrylic ester group.
3. gel electrolyte according to claim 1, it is characterised in that：In described polymerizable unimolecule Organic substance third
The molecular weight of olefin(e) acid ester group accounts for the 20～90% of described polymerizable unimolecule Organic substance total molecular weight, and the molecular weight of alkyl accounts for institute
The 10～80% of the polymerizable unimolecule Organic substance total molecular weight stated.
4. gel electrolyte according to claim 3, it is characterised in that：In described polymerizable unimolecule Organic substance third
The molecular weight of olefin(e) acid ester group accounts for the 65～85% of described polymerizable unimolecule Organic substance total molecular weight, and the molecular weight of alkyl accounts for institute
The 15～35% of the polymerizable unimolecule Organic substance total molecular weight stated.
5. gel electrolyte according to claim 4, it is characterised in that：Described polymerizable unimolecule Organic substance be selected from
One or more in trimethylolpropane trimethacrylate, tetramethylol methane tetraacrylate, neopentylglycol diacrylate
Combination.
6. gel electrolyte according to any one of claim 1 to 5, it is characterised in that：Described polymerizable unimolecule
The addition quality of Organic substance is the 1～10% of described gel electrolyte gross mass；The addition quality of described initiator is institute
The 0.001～3% of the gel electrolyte gross mass stated.
7. gel electrolyte according to any one of claim 1 to 5, it is characterised in that：Described initiator be selected from
The combination of one or more in organic peroxide, inorganic peroxide, azo；
Described ether organic solvent is selected from glycol dimethyl ether, 1,3- dioxolanes, Isosorbide-5-Nitrae-dioxane four (ethylene glycol)
The combination of one or more in dimethyl ether, three (ethylene glycol) dimethyl ether；
Described lithium salts is the group of one or more in two (trimethyl fluoride sulfonyl) imine lithium, double fluorine sulfimide lithiums
Close.
8. gel electrolyte according to any one of claim 1 to 5, it is characterised in that：Described liquid electrolyte is also
Including additive, described additive is selected from LiNO3、CrNO3、RbNO3In the combination of one or more.
9. a kind of lithium-sulfur rechargeable battery, it is characterised in that：Using the gel electrolyte any one of claim 1 to 8.
10. a kind of preparation method of lithium-sulfur rechargeable battery as claimed in claim 9, it is characterised in that：By positive pole, negative pole, every
Film and shell are assembled into battery core, by described gel electrolyte injection described battery core, seal, then initiated polymerization,
Battery carries out successively again being melted into, circulates, deflates, seal and obtain described lithium-sulfur rechargeable battery.
The preparation method of 11. lithium-sulfur rechargeable batteries according to claim 10, it is characterised in that：In 20～100 DEG C of temperature
Degree is lower to be caused described polyreaction or causes described polyreaction under the action of uv light.
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| CN108933275A (en) * | 2017-05-26 | 2018-12-04 | 北京师范大学 | It is a kind of for lithium-sulfur cell can gelling system and its preparation method and application |
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| CN111106382A (en) * | 2018-10-29 | 2020-05-05 | 北京师范大学 | Gelable system containing cross-linking agent and preparation method and application thereof |
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