A kind of all solid state plastic crystals flexible electrolyte film and preparation method thereof
阅读说明：本技术 一种全固态塑性晶体柔性电解质薄膜及其制备方法 (A kind of all solid state plastic crystals flexible electrolyte film and preparation method thereof ) 是由 谢惠东 李明亚 王晓强 朱琳 曲袖杰 吴智升 于 2019-08-30 设计创作，主要内容包括：本发明的一种全固态塑性晶体柔性电解质薄膜及其制备方法,属于固态电解质制备领域,所述电解质薄膜中包含的物质主要为：高分子化合物、增塑剂、有机塑性晶体基质、锂盐、添加剂、助剂等。制备时相应采用浇铸法或挤出法即可获得相应全固态塑性晶体柔性电解质薄膜。本发明的制备方法具有制备工艺简单、所制得全固态塑性晶体柔性电解质薄膜电导率高、耐太阳辐射、抗老化、超低收缩率、透过性好等优点,在电致变色、太阳能电池、柔性显示屏等领域具有很好的应用前景。(A kind of all solid state plastic crystals flexible electrolyte film of the invention and preparation method thereof, belong to solid electrolyte preparation field, the substance for including in the electrolytic thin-membrane is main are as follows: high-molecular compound, plasticizer, organic plastic crystal matrices, lithium salts, additive, auxiliary agent etc..Casting method or extrusion molding is accordingly used to can be obtained corresponding all solid state plastic crystals flexible electrolyte film when preparation.Preparation method of the invention has many advantages, such as that preparation process is simple, obtained all solid state plastic crystals flexible electrolyte film conductivity is high, resistance to solar radiation, anti-aging, ultralow shrinking percentage, permeability are good, has a good application prospect in fields such as electrochromism, solar battery, flexible display screens.)
1. a kind of all solid state plastic crystals flexible electrolyte film, which is characterized in that high including raw material and proportion in mass ratio Molecular compound: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer: auxiliary agent=1:(0.1-0.3): (0.5- 0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent=1:(0-10), unit g: ml。
2. all solid state plastic crystals flexible electrolyte film according to claim 1, which is characterized in that described is all solid state Plastic crystals flexible electrolyte film raw material further includes auxiliary agent, and the auxiliary agent is one of antioxidant, age resister or several Kind, the mass ratio of the auxiliary agent and high-molecular compound is (0.001-0.005): 1.
3. all solid state plastic crystals flexible electrolyte film according to claim 1, it is characterised in that:
The high-molecular compound is polyvinyl alcohol, polyvinyl butyral, ethylene-vinyl acetate copolymer, poly- methyl-prop E pioic acid methyl ester, Kynoar, polyvinyl chloride, ethylene-vinyl alcohol copolymer, polytetrafluoroethylene (PTFE) or poly- (vinylidene-co- six One or more of fluoropropene), when for several mixing, mixing ratio is any ratio；
The organic plastic crystal matrices are neutral organic plastic crystals matrix；
The neutral organic plastic crystals matrix is acetonitrile, succinonitrile, adiponitrile, neopentane, cyclohexylamine, cyclobutane, 5- first The trifluoromethane sulfonic acid inferior amine salt, polyacrylonitrile or trifluoromethane sulfonic acid of base -5,6,7,8- tetrahydro-pyrazole quinoline (1,2- α) pyridazone are sub- One or more of amine, when for several mixing, mixing ratio is any ratio；
The plasticizer is terephthalic acid (TPA) dibutyl ester, two formic acid esters of dipropylene glycol, polyol benzoate, polyalcohol benzene One or more of formic acid esters or dipropylene glycol, when for several mixing, mixing ratio is any ratio；
The lithium salts is bis trifluoromethyl sulfimide lithium, lithium perchlorate, difluoro lithium borate, double-perfluoroethyl sulfonyl imines Lithium, lithium carbonate, LiBF4, hexafluoroarsenate lithium, lithium hexafluoro phosphate, lithium rhodanate, tetrafluoro lithium aluminate, lithium chloride, lithium iodide, One of lithium bromide, tetrafluoro oxalic acid lithium phosphate, dioxalic acid lithium phosphate, difluorine oxalic acid boracic acid lithium or trifluoromethanesulfonic acid lithium are several Kind, when for several mixing, mixing ratio is any ratio；
The solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dehydrated alcohol, propene carbonate, carbonic acid two One or more of methyl esters, ethyl cellulose, dimethyl acetamide or methyl methacrylate mix when for several mixing Composition and division in a proportion is any ratio；
The electrolyte additive is inorganic nano-particle.
4. all solid state plastic crystals flexible electrolyte film according to claim 3, which is characterized in that described inorganic to receive Rice corpuscles is Nano-meter SiO_22, nano-TiO2, nanometer Al2O3, nano-ZnO, nanometer ZrO2, nanometer Ta2O5, nano Ce O2, nanometer MoO3, nano-MgO or nanometer Nb2O5One or more of, when for several mixing, mixing ratio is any ratio.
5. all solid state plastic crystals flexible electrolyte film according to claim 1, which is characterized in that described is all solid state Plastic crystals flexible electrolyte film has 10-3-10-6Ionic conductivity, service life cycle-index reach 100000- 1000000 times, at applied voltage -3V~3V: initial volt-ampere circulation peak point current is 3.4-28mA, recycles 100000- After 1000000 times, peak point current is stablized in 3.3-27mA, and decaying is no more than 10%；In the UV lamp after Continuous irradiation 15 days, follow Ring 100000-1000000 times, peak point current are stablized in 3-25.5mA, and decaying is no more than 15%.
6. all solid state plastic crystals flexible electrolyte film according to claim 1, which is characterized in that described is all solid state Electrolytic thin-membrane with a thickness of 50-1000 μm, surface roughness is less than 10nm.
7. the preparation method of all solid state electrolyte film described in claim 1, which is characterized in that use casting method or extrusion Method, comprising the following steps:
Step 1, stock:
In mass ratio, high-molecular compound: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer=1: (0.1- 0.3): (0.5-0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent=1: (0- 10), unit g:ml, stock；
Step 2, film preparation:
When preparing film using casting method, steps are as follows:
1, electrolyte precursor preparation:
Load weighted high-molecular compound, organic plastic crystal matrices, lithium salts, solvent, electrolyte additive and plasticizer are mixed It closes, the solvent of respective volume is added, be uniformly mixed, obtain electrolyte precursor；
2, casting:
Electrolyte precursor is cast to release film, it is dry after natural levelling, all solid state electrolyte film is made；
When preparing film using extrusion by melting, steps are as follows:
After high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive and plasticizer are mixed, it is heated to melting After melting state, after extrusion, all solid state electrolyte film is made.
8. the preparation method of all solid state electrolyte film according to claim 7, which is characterized in that the step two In, high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive, plasticizer and auxiliary agent are intended to do before use Non-aqueous processing.
9. the preparation method of all solid state electrolyte film according to claim 7, which is characterized in that the step two In, when using casting method, mass volume ratio is pressed in raw material, high-molecular compound: solvent=1: (7-10), unit g:ml are used When extrusion by melting, quantity of solvent is 0 in raw material.
Technical field:
The invention belongs to technical field of inorganic nonmetallic materials, and in particular to a kind of all solid state plastic crystals flexible electrolyte Film and preparation method thereof.
Background technique:
Laminated safety glass with its safety, sound insulation, heat-insulated, uvioresistant, etc. excellent properties be widely used in construction industry； And the property and preparation method of the laminating layer among laminated glass also gradually cause the attention and research of people.
The solid polymer gel electrolyte being made of polymer and salt etc. is because that need not encapsulate liquid, avoid leakage and safety The advantages such as performance height cause exploration deep both at home and abroad.Many scholars are for solid polymer gel electrolyte in recent years Research is concentrated mainly on the electrolyte of design different structure and makes great efforts to improve two aspect of ionic conductivity；It is solidifying according to solid polymer The conductivity principle of glue electrolyte, it is main from poly- in order to increase ionic conductivity when designing composite solid state polymer dielectric Object matrix, alkali metal salt are closed, the several respects such as additive consider.
The present invention uses the high-molecular compounds such as polyvinyl alcohol, polyvinyl butyral for matrix, and lithium salts is alkali metal salt, Inorganic nano-particle is electrolyte additive, while using two kinds of preparation methods of casting method and extrusion by melting, one prepared The all solid state plastic crystals flexible electrolyte film of kind has bigger ionic conductivity, and performance is more stable, time that can be recycled Number is more, anti-aging to use the longer time, also more preferable for the attached performance of parent of glass, while having longer service life.
Summary of the invention:
The purpose of the present invention is overcoming above-mentioned the shortcomings of the prior art, a kind of simple process, low in cost, property are provided The stable all solid state plastic crystals flexible electrolyte film and preparation method thereof of energy, mainly solving the technical problems that solid state electrolysis The stability problem of matter film.
A kind of all solid state plastic crystals flexible electrolyte film of the present invention and preparation method thereof specifically includes that high score The Non-aqueous processing of the drugs such as sub- compound, plasticizer, organic plastic crystal matrices, lithium salts, electrolyte additive, auxiliary agent, colloidal sol The preparation of electrolyte precursor, the casting of film layer, drying and the test of film layer of film layer etc..
To achieve the above object, the invention adopts the following technical scheme:
A kind of all solid state plastic crystals flexible electrolyte film, including raw material and proportion are macromolecule chemical combination in mass ratio Object: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer: auxiliary agent=1:(0.1-0.3): (0.5-0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent=1:(0-10), unit g:ml.
The all solid state plastic crystals flexible electrolyte film raw material further includes auxiliary agent, the auxiliary agent be antioxidant, The mass ratio of one or more of age resister, the auxiliary agent and high-molecular compound is (0.001-0.005): 1.
The high-molecular compound is polyvinyl alcohol, polyvinyl butyral, ethylene-vinyl acetate copolymer, poly- first Base methyl acrylate, Kynoar, polyvinyl chloride, ethylene-vinyl alcohol copolymer, polytetrafluoroethylene (PTFE) or poly- (vinylidene- One or more of co- hexafluoropropene), when for several mixing, mixing ratio is any ratio.
The organic plastic crystal matrices are neutral organic plastic crystals matrix.
The neutral organic plastic crystals matrix be acetonitrile, succinonitrile, adiponitrile, neopentane, cyclohexylamine, cyclobutane, The trifluoromethane sulfonic acid inferior amine salt, polyacrylonitrile or trifluoromethyl sulphur of 5- methyl -5,6,7,8- tetrahydro-pyrazole quinoline (1,2- α) pyridazone One or more of acid imide, when for several mixing, mixing ratio is any ratio.
The plasticizer is terephthalic acid (TPA) dibutyl ester, two formic acid esters of dipropylene glycol, polyol benzoate, polynary One or more of alcohol benzoic ether or dipropylene glycol, when for several mixing, mixing ratio is any ratio.
The lithium salts is bis trifluoromethyl sulfimide lithium, lithium perchlorate, difluoro lithium borate, double-perfluoroethyl sulfonyl Imine lithium, lithium carbonate, LiBF4, hexafluoroarsenate lithium, lithium hexafluoro phosphate, lithium rhodanate, tetrafluoro lithium aluminate, lithium chloride, iodine Change one of lithium, lithium bromide, tetrafluoro oxalic acid lithium phosphate, dioxalic acid lithium phosphate, difluorine oxalic acid boracic acid lithium or trifluoromethanesulfonic acid lithium Or it is several, when for several mixing, mixing ratio is any ratio.
The solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dehydrated alcohol, propene carbonate, carbon One or more of dimethyl phthalate, ethyl cellulose, dimethyl acetamide or methyl methacrylate, when for several mixing When, mixing ratio is any ratio.
The electrolyte additive is inorganic nano-particle.
The inorganic nano-particle is Nano-meter SiO_22, nano-TiO2, nanometer Al2O3, nano-ZnO, nanometer ZrO2, nanometer Ta2O5, nano Ce O2, nanometer MoO3, nano-MgO or nanometer Nb2O5One or more of, when for several mixing, mixing ratio Arbitrarily to compare.
The all solid state plastic crystals flexible electrolyte film has 10-3-10-6Ionic conductivity, service life circulation Number reaches 100000-1000000 times, at applied voltage -3V~3V: initial volt-ampere circulation peak point current is 3.4-28mA, After circulation 100000-1000000 times, peak point current is stablized in 3.3-27mA, and decaying is no more than 10%；It is continuous in the UV lamp to shine It after penetrating 15 days, recycles 100000-1000000 times, peak point current is stablized in 3-25.5mA, and decaying is no more than 15%.
The all solid state electrolyte film with a thickness of 50-1000 μm, use different manufacture crafts or drying time Film thickness can be had some impact on temperature difference, it is bigger compared to casting method film thickness using extrusion by melting, it does The higher film thickness of dry time longer temperature is smaller, and film thickness is uniform, and flatness is high, and surface roughness is less than 10nm.
The preparation method of all solid state electrolyte film, using casting method or extrusion molding, comprising the following steps:
Step 1, stock:
In mass ratio, high-molecular compound: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer=1: (0.1-0.3): (0.5-0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent= 1:(0-10), unit g:ml, stock；
Step 2, film preparation:
When preparing film using casting method, steps are as follows:
Using first preparing electrolyte precursor, concrete operations scheme when casting method are as follows:
1, electrolyte precursor preparation:
By load weighted high-molecular compound, organic plastic crystal matrices, lithium salts, solvent, electrolyte additive and plasticising Agent mixing, is added the solvent of respective volume, is uniformly mixed, and obtains electrolyte precursor；
2, casting:
Electrolyte precursor is cast to release film, it is dry after natural levelling, all solid state electrolyte film is made；
When preparing film using extrusion by melting, steps are as follows:
After high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive and plasticizer are mixed, heating To molten condition, after slowly squeezing out, all solid state electrolyte film is made.
In the step two, high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive, plasticizer It is intended to do Non-aqueous processing, specific processing method before use with auxiliary agent are as follows: each substance is put into sealed environment, passes through vacuum pump Environment is evacuated to vacuum state, is then heated to 50-90 DEG C, keeps the temperature 24-28h.
In the step two 1, when using casting method, electrolyte precursor is cast under water-less environment.
In the step two 1, when using casting method, mass volume ratio is pressed in raw material, high-molecular compound: solvent=1: (7-10), unit g:ml.
In the step 21,
Each uniform detailed process of material mixing are as follows: after each material mixing is sealed, and start to be heated in stirring, Agitating mode is mechanical stirring or magnetic agitation, and mixing time 20-26h, heating temperature is 40-60 DEG C, heating time 1- 3h is uniformly mixed, and obtains electrolyte precursor.
In the step 22, detailed process of casting are as follows:
(1) release film is attached on glass substrate or ptfe substrate, with alcohol swab wiped clean；
(2) glass substrate or ptfe substrate of having release film are leveled with level meter；
(3) part electrolyte precursor drop is drawn on release film with rubber head dropper, repeatedly after 2-4 times, natural levelling；
(4) electrolyte precursor of levelling is covered with clean culture dish, after spontaneously drying 20-28h, is put into vacuum environment Middle heat drying 20-26h, heating temperature are 45-60 DEG C, and all solid state electrolyte film is made.
In the step two 2, when using extrusion by melting, quantity of solvent is 0 in raw material.
In the step two, when film raw material contains auxiliary agent, when using casting method, it is added and helps after heating 1-3h Agent is uniformly mixed, and obtains electrolyte precursor；When using extrusion by melting, auxiliary agent directly with high-molecular compound, organic plastic Crystal substrate, lithium salts, electrolyte additive and plasticizer mixing, after being heated to molten condition, slowly squeeze out.
Beneficial effects of the present invention:
All solid state plastic crystals flexible electrolyte film prepared by the present invention is compared to used in doubling glass on the market Electrolyte performance is more stable, and the number that can be recycled is more, anti-aging to use the longer time, attached simultaneously for the parent of glass Performance is also more preferable.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
The used raw material of solid plastics crystal flexible electrolyte film is prepared in following example is purchased from lark prestige reagent Company.
Ultraviolet lamp model ZF-7；Illumination wavelength is 365nm；
The auxiliary agent is antioxidant or age resister；
The high-molecular compound is polyvinyl alcohol (molecular formula: [- CH2CHOH-] n, molecular weight: 44.05), polyethylene Butyral (MW25000-40000), ethylene-vinyl acetate copolymer (vinyl acetate 40wt.%, melt index 52g/10min (190 DEG C/2.16kg)) polymethyl methacrylate (molecular formula [C5H8O2] n, molecular weight Beilstein), Kynoar (molecular formula: (CH2CF2) n, purity: Mn~107,000 average MW~275,000by GPC, average, Pellets), polyvinyl chloride (MW80000-100000), ethylene-vinyl alcohol copolymer (ethylene 60wt.%), polytetrafluoroethylene (PTFE) (molecular formula-[- CF2-CF2-] n-, molecular weight 5000-15000) or poly- (vinylidene-co- hexafluoropropene) (average Mw ~400,000 (bimodal distribution), average Mn~130,000, pellets)；
The neutral organic plastic crystals matrix is acetonitrile (purity 99.9%, MW41.05), succinonitrile (purity 99% MW80.09), adiponitrile, neopentane, cyclohexylamine (purity 99.5%, molecular formula C6H13N, molecular weight 99.18), cyclobutane, 5- first The trifluoromethane sulfonic acid inferior amine salt, polyacrylonitrile ((C of base -5,6,7,8- tetrahydro-pyrazole quinoline (1,2- α) pyridazone3H3)n ) or trifluoromethane sulfonic acid imines MW150000；
The plasticizer is terephthalic acid (TPA) dibutyl ester, dipropylene glycol dibenzoate (purity 80%), polyalcohol benzene Formic acid esters or dipropylene glycol (purity 99%)；
The lithium salts is bis trifluoromethyl sulfimide lithium (anhydrous grade 99.99%), lithium perchlorate (anhydrous grade 99.99%), difluoro lithium borate, double-perfluoroethyl sulfonyl imine lithium, lithium carbonate (purity 97%), LiBF4 (purity 99%), hexafluoroarsenate lithium, lithium hexafluoro phosphate (purity > 97%), lithium rhodanate, tetrafluoro lithium aluminate, lithium chloride (purity > 99%), Lithium iodide (anhydrous grade 99.99%), lithium bromide (purity 99.99%), tetrafluoro oxalic acid lithium phosphate, dioxalic acid lithium phosphate, difluoro grass Sour lithium borate (99%, water content≤200ppm) or trifluoromethanesulfonic acid lithium (purity 98%)；
The solvent is N,N-dimethylformamide (AR 99.5%), DMAC N,N' dimethyl acetamide (AR 99%), nothing Water-ethanol (AR), propene carbonate (AR 99.5%), dimethyl carbonate (anhydrous grade, >=99%), ethyl cellulose (18- 22mPa.s, 5% toluene/isopropanol 80:20), dimethyl acetamide or methyl methacrylate (AR 99.0%, contain 30ppmMEHQ stabilizer)；
The inorganic nano-particle is Nano-meter SiO_22(15 ± 5nm of average grain diameter, 250 ± 30m of specific surface area2/ g), nanometer TiO2(average grain diameter 40nm), nanometer Al2O3(γ phase, average grain diameter 20nm), nano-ZnO (30 ± 10nm of average grain diameter), nanometer ZrO2(20 ± 5nm of average grain diameter), nanometer Ta2O5(average grain diameter 25nm), nano Ce O2(30 ± 5nm of average grain diameter), nanometer MoO3(average grain diameter 35nm), nano-MgO (average grain diameter 50nm) or nanometer Nb2O5(average grain diameter 30nm).
A kind of all solid state plastic crystals flexible electrolyte film, including raw material and proportion are macromolecule chemical combination in mass ratio Object: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer: auxiliary agent=1:(0.1-0.3): (0.5-0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent=1:(0-10), unit g:ml.
The all solid state plastic crystals flexible electrolyte film raw material further includes auxiliary agent, the auxiliary agent be antioxidant, The mass ratio of one or more of age resister, the auxiliary agent and high-molecular compound is (0.001-0.005): 1.
The high-molecular compound is polyvinyl alcohol, polyvinyl butyral, ethylene-vinyl acetate copolymer, poly- first Base methyl acrylate, Kynoar, polyvinyl chloride, ethylene-vinyl alcohol copolymer, polytetrafluoroethylene (PTFE) or poly- (vinylidene- One or more of co- hexafluoropropene), when for several mixing, mixing ratio is any ratio.
The organic plastic crystal matrices are neutral organic plastic crystals matrix.
The neutral organic plastic crystals matrix be acetonitrile, succinonitrile, adiponitrile, neopentane, cyclohexylamine, cyclobutane, The trifluoromethane sulfonic acid inferior amine salt, polyacrylonitrile or trifluoromethyl sulphur of 5- methyl -5,6,7,8- tetrahydro-pyrazole quinoline (1,2- α) pyridazone One or more of acid imide, when for several mixing, mixing ratio is any ratio.
The plasticizer is terephthalic acid (TPA) dibutyl ester, two formic acid esters of dipropylene glycol, polyol benzoate, polynary One or more of alcohol benzoic ether or dipropylene glycol, when for several mixing, mixing ratio is any ratio.
The lithium salts is bis trifluoromethyl sulfimide lithium, lithium perchlorate, difluoro lithium borate, double-perfluoroethyl sulfonyl Imine lithium, lithium carbonate, LiBF4, hexafluoroarsenate lithium, lithium hexafluoro phosphate, lithium rhodanate, tetrafluoro lithium aluminate, lithium chloride, iodine Change one of lithium, lithium bromide, tetrafluoro oxalic acid lithium phosphate, dioxalic acid lithium phosphate, difluorine oxalic acid boracic acid lithium or trifluoromethanesulfonic acid lithium Or it is several, when for several mixing, mixing ratio is any ratio.
The solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dehydrated alcohol, propene carbonate, carbon One or more of dimethyl phthalate, ethyl cellulose, dimethyl acetamide or methyl methacrylate, when for several mixing When, mixing ratio is any ratio.
The electrolyte additive is inorganic nano-particle.
The inorganic nano-particle is Nano-meter SiO_22, nano-TiO2, nanometer Al2O3, nano-ZnO, nanometer ZrO2, nanometer Ta2O5, nano Ce O2, nanometer MoO3, nano-MgO or nanometer Nb2O5One or more of, when for several mixing, mixing ratio Arbitrarily to compare.
The all solid state plastic crystals flexible electrolyte film has 10-3-10-6Ionic conductivity, service life circulation Number reaches 100000-1000000 times, at applied voltage -3V~3V: initial volt-ampere circulation peak point current is 3.4-28mA, After circulation 100000-1000000 times, peak point current is stablized in 3.3-27mA, and decaying is no more than 10%；It is continuous in the UV lamp to shine It after penetrating 15 days, recycles 100000-1000000 times, peak point current is stablized in 3-25.5mA, and decaying is no more than 15%, wherein initial Volt-ampere circulation peak point current is the peak point current after volt-ampere recycles 20 times.
The all solid state electrolyte film with a thickness of 50-1000 μm, use different manufacture crafts or drying time Film thickness can be had some impact on temperature difference, it is bigger compared to casting method film thickness using extrusion by melting, it does The higher film thickness of dry time longer temperature is smaller, and film thickness is uniform, and flatness is high, and surface roughness is less than 10nm.
The preparation method of all solid state electrolyte film, using casting method or extrusion molding, comprising the following steps:
Step 1, stock:
In mass ratio, high-molecular compound: organic plastic crystal matrices: lithium salts: electrolyte additive: plasticizer=1: (0.1-0.3): (0.5-0.7): (0.02-0.04): (0.04-0.08), by mass volume ratio, high-molecular compound: solvent= 1:(0-10), unit g:ml, stock；
Step 2, film preparation:
When preparing film using casting method, steps are as follows:
Using first preparing electrolyte precursor, concrete operations scheme when casting method are as follows:
1, electrolyte precursor preparation:
(1) by load weighted high-molecular compound, organic plastic crystal matrices, lithium salts, solvent, electrolyte additive and increasing Agent mixing is moulded, the solvent of respective volume is added, is uniformly mixed；
(2) by the medication containment mixed it is good after be put into magnetic stirring apparatus, magnetic agitation, magnetic force are carried out under heating condition Mixing time is 20-26h, and heating temperature is 40-60 DEG C, heating time 1-3h, is uniformly mixed, obtains electrolyte precursor；
2, casting:
(1) release film is attached on glass substrate or ptfe substrate, with alcohol swab wiped clean；
(2) glass substrate or ptfe substrate of having release film are leveled with level meter；
(3) part electrolyte precursor drop is drawn on release film with rubber head dropper, repeatedly after 2-4 times, natural levelling；
(4) electrolyte precursor of levelling is covered with clean culture dish, after spontaneously drying 20-28h, is put into vacuum environment Middle heat drying 20-26h, heating temperature are 45-60 DEG C, and all solid state electrolyte film is made；
When preparing film using extrusion by melting, steps are as follows:
After high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive and plasticizer are mixed, heating To molten condition, after slowly squeezing out, all solid state electrolyte film is made.
In the step two, high-molecular compound, organic plastic crystal matrices, lithium salts, electrolyte additive, plasticizer It is intended to do Non-aqueous processing, specific processing method before use with auxiliary agent are as follows: each substance is put into sealed environment, passes through vacuum pump Environment is evacuated to vacuum state, is then heated to 50-90 DEG C, keeps the temperature 24-28h.
In the step two, when film raw material contains auxiliary agent, when using casting method, it is added and helps after heating 1-3h Agent is uniformly mixed, and obtains electrolyte precursor；When using extrusion by melting, auxiliary agent directly with high-molecular compound, organic plastic Crystal substrate, lithium salts, electrolyte additive and plasticizer mixing, after being heated to molten condition, slowly squeeze out.
In the step two 1, when using casting method, electrolyte precursor is cast under water-less environment；Matter is pressed in raw material Measure volume ratio, high-molecular compound: solvent=1:(7-10), unit g:ml.
In the step two 2, when using extrusion by melting, quantity of solvent is 0 in raw material.
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