CN105070919A - Preparation method of flexible and foldable all-organic secondary battery - Google Patents
Preparation method of flexible and foldable all-organic secondary battery Download PDFInfo
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/058—Construction or manufacture
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
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Abstract
The invention relates to a preparation method of a flexible and foldable all-organic secondary battery, and belongs to the technical field of electrochemical power sources. The preparation method of the flexible and foldable all-organic secondary battery comprises the following steps: (1) preparation of an anode material and a thin film, namely adding naphthalenetetracarboxylic dianhydride and 4,4'-diaminodiphenyl ether to an n-methyl pyrrolidone (NMP) solution, adding a graphene conducting agent and carrying out reflux reaction in an argon atmosphere to prepare the film; (2) preparation of a cathode material and the thin film, namely putting ferrocene, tetramethylethylenediamine and n-butyl lithium into a Schlenk reaction bottle, adding petroleum ether, reacting and precipitating the mixture, cleaning the sediment with a solvent, adding the petroleum ether, dropwise adding hydrogen methyl dichlorosilane, and carrying out thermochemical polymerization on solid to prepare the film; (3) preparation of polymer gel electrolyte, namely mixing polyvinyl pyrrolidone with NaCl/H2O liquid; and (4) battery assembly, assembling the cathode material film, the anode material film and the gel electrolyte into the battery. The preparation method has the advantages that the process is stable; the product is ultrathin, controllable, flexible, foldable, easy to design, safe and nontoxic, and can meet the requirements of human body fitting comfort and special occasions.
Description
Technical field
The invention belongs to technical field of chemical power, particularly relate to a kind of preparation method of flexible foldable full stress-strain secondary cell.
Background technology
At present, wearable electronic is one of current electronics Hot spots for development, and the key technology of restriction wearable device fast development will be the power supply module matched.Occurred the various wearable device of hundreds of money on the market, but the breakthrough development of wearable power technology is few.Based on the reason of human body structure, how better wearable power supply laminating human limb is problem demanding prompt solution, and the thin film flexible of power-supply system changes into the outlet for addressing this problem.
The current main film power supply for meeting wearable electronic is film lithium ion battery, but this battery is the filming of conventional lithium ion battery, the key components such as both positive and negative polarity composition and energy storage mechnism all identical with traditional commerce lithium secondary battery.Be limited to essential structure and the main material character of lithium ion battery, film lithium ion battery cannot meet for a long time, at random, significantly foldingly and bending to use, especially there is the character of use that clothing is the same.And existing film lithium ion battery, owing to adopting organic system electrolyte or transition metal electrode material, there is certain murder by poisoning performance to human body, if once leakage, will produce the health of human body and threaten.
Summary of the invention
The present invention provides a kind of preparation method of flexible foldable full stress-strain secondary cell for solving in known technology the technical problem that exists.
The object of this invention is to provide one to have and can meet comfort requirement characteristic of fitting with human body, and some special occasions demands can the preparation method of flexible foldable full stress-strain secondary cell of the feature such as stochastic larger amplitude folded bent use.
The flexible secondary cell of full stress-strain thin polymer film, for the folding functional realizing flexible thin-film battery future provides a very promising solution, because polymer has good plasticity, can film forming, become silk also can be woven into cloth.Full stress-strain polymer secondary battery, its positive electrode, the battery that negative material and electrolyte three parts all adopt organic polymer material and are assembled into.
The flexible secondary cell preparation process of full stress-strain thin polymer film:
1, the preparation of negative material and film:
The material adopting polyimide is main body, by regulating drawing electronics and obtaining suitable operating voltage to electronic functional group on imines, and adopt nonactive main chain functional group to regulate polyimides or the intermediate polymer solubility property in Conventional solvents, come and conductive carbon composite membrane-forming with this.
2, the preparation of positive electrode and film:
Be all take carbonyl as the material of reactive functionality due to the existing polymer that can be used for negative material, be in complete Charging state.Therefore, the conveniently design of battery and assembling, the selection of positive pole polymeric material just needs the polymer looking for a kind of state of discharging completely.In addition, polymer also needs to be easy to synthesis and preserves, and when with material with carbon element compound, also can film forming keep redox property.Based on this, it is positive electrode that the present invention have chosen ferrocene silane polymer.
3, gel-form solid polymer electrolyte preparation
Because both positive and negative polarity needs to stick together, therefore adopt the sticking water system polymer of a kind of tool to be used as gel electrolyte, play the effect of conducting ion and bonding.
4, the positive and negative pole material film obtained and gel electrolyte are assembled into battery.
The technical scheme that the preparation method of flexible foldable full stress-strain secondary cell of the present invention takes is:
A preparation method for flexible foldable full stress-strain secondary cell, is characterized in: the positive electrode of flexible foldable full stress-strain secondary cell, negative material and electrolyte all adopt organic polymer material, and its preparation process comprises the following steps:
1) preparation of negative material and film:
Naphthalenetetracarbacidic acidic acid anhydride and 4, the ratio of 4 '-diaminodiphenyl ether 1:0.5-10 in molar ratio adds in nmp solution, graphene conductive agent is added by the mass ratio of theoretical target product 5-20%, back flow reaction 1-12 hour under argon atmosphere, obtain the solution of target product, solution is formed film, evaporating solvent, then at N
2negative material film is obtained by reacting at 200-350 DEG C of temperature in atmosphere;
2) preparation of positive electrode and film:
Ferrocene, tetramethylethylenediamine and n-BuLi be (1-5) in molar ratio: (1-5): (1-15) puts into Schlenk reaction bulb, adds benzinum, stirring reaction 1-72h, obtains yellow ferrocene dilithium salt precipitation; Under the condition of anhydrous and oxygen-free, precipitating solvent is cleaned, add benzinum, be placed in the cryosel water-bath of-5 DEG C to-25 DEG C; Then drip hydrogen dimethyl dichlorosilane (DMCS), temperature is raised to room temperature; Mixed liquor stirring 2-48h crosses and filters salt, and filtrate removes solvent, solid heat polymerization 1-10h at 100-200 DEG C of the Chinese red obtained; Purify with oxolane dissolution solvent and methanol solvate and precipitate, obtain crocus fibre solid compound; Then dissolve crocus fibre solid compound with oxolane, by solution film-forming, room temperature moves down to desolventize and obtains positive electrode film;
3) gel-form solid polymer electrolyte preparation:
Polyvinylpyrrolidone is adopted to be electrolytical polymer, 1-6MNaCl/H
2o liquid, according to the ratio of mass ratio 1:0.5-50 by solution and polymer mixed;
4) battery assembling:
The positive electrode film obtained, negative material film and gel-form solid polymer electrolyte are assembled into battery.
The preparation method of flexible foldable full stress-strain secondary cell of the present invention can also adopt following technical scheme:
The preparation method of described flexible foldable full stress-strain secondary cell, be characterized in: when negative material and film preparation, naphthalenetetracarbacidic acidic acid anhydride and 4, when 4 '-diaminodiphenyl ether adds nmp solution, naphthalenetetracarbacidic acidic acid anhydride, 4, when 4 '-diaminodiphenyl ether and Graphene add nmp solution, nmp solution be good just to flood powder.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in: when negative material and film preparation, and the solution of target product is added drop-wise to aluminium thin surface and forms film, and 30-70 DEG C of evaporating solvent, at N
2in atmosphere, the reaction time is 1-10h, finally removes aluminum foil substrate.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in: when positive electrode and film preparation, and the amount adding benzinum is powder volume 3-10 times; Obtain under yellow ferrocene dilithium salt is deposited in the condition of anhydrous and oxygen-free, precipitating solvent being cleaned 2-5 time.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in: when positive electrode and film preparation, and in mixed liquor, slowly drip hydrogen dimethyl dichlorosilane (DMCS) by constant pressure funnel, the mol ratio of hydrogen dimethyl dichlorosilane (DMCS) and ferrocene is 1:1-5.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in: when positive electrode and film preparation, and filtrate adopts vacuum mode to remove solvent, finally removes aluminum foil substrate.
The advantage that the present invention has and good effect are:
The preparation method of flexible foldable full stress-strain secondary cell is owing to have employed the brand-new technical scheme of the present invention, and compared with prior art, the advantage of full stress-strain polymer thin film battery of the present invention is mainly manifested in following several aspect:
1) one is difunctional:
Polymer has plasticity, directly electrospinning can become cloth, and inorganic matter is not all right, is thus easy to fabric power supply integration, structoure of the human body of more fitting, and has huge application potential;
2) ultra-thin controlled:
Because electrode material is polymer, be dissolved in structure and chemical property that specific solvent also remains intact, can obtain slimline battery by simple casting mode, inorganic material cannot be accomplished.Its thickness can regulate and control arbitrarily, until the slimline battery of nanometer grade thickness;
3) flexible foldable:
The material adopted due to hull cell is polymer, has good plasticity, by being woven into the electrode of cloth or these types of film forming, makes battery have the flexible foldable feature of picture clothing or plastics;
4) design is easy to:
Due to miniature high-tech electronic equipment, to have volume little, powerful feature, is difficult to reserve enough places to battery, and this battery can by the mode of casting, just small space can need not be utilized fully, for micromodule equipment provides more electric energy by complicated design;
5) safety non-toxic:
Polymeric material composition is non-toxic, also can adopt multiple electrolyte system, for traditional lithium secondary battery is incomparable.Particularly can be designed as brine system (NaCl/H
2o), simple sweat just can realize discharge and recharge, realize truly to human body environmental protection, safety non-toxic.
In sum, full stress-strain polymer thin film battery has boundless application prospect and foreseeable huge advantage, can make very large progradation to the battery technology of wearable technology and variform and occupation mode.
Accompanying drawing explanation
Fig. 1 is the model structure schematic diagram of flexible foldable full stress-strain polymer secondary battery of the present invention;
In figure, 1 is anode portion, containing active material/carbon film layer and conductive carbon thin layer; 2 is gel electrolyte part, containing polymer and saline electrolysis liquid; 3 is cathode portion, containing active material/carbon film layer and conductive carbon thin layer.
Fig. 2 is the typical charging and discharging curve figure of flexible foldable full stress-strain polymer secondary battery of the present invention.
Embodiment
For summary of the invention of the present invention, Characteristic can be understood further, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
Accompanying drawings 1 and Fig. 2.
Embodiment 1
A preparation method for flexible foldable full stress-strain secondary cell, its positive electrode, negative material and electrolyte three parts all adopt organic polymer material, and preparation process comprises following processing step:
1, the preparation of negative material and film:
The material adopting polyimide is main body, by regulating drawing electronics and obtaining suitable operating voltage to electronic functional group on imines, and adopt nonactive main chain functional group to regulate polyimides or the intermediate polymer solubility property in Conventional solvents, come and conductive carbon composite membrane-forming with this.
Concrete manufacturing step is as follows:
The preparation of polyamide
Adopt naphthalenetetracarbacidic acidic acid anhydride and 4,4 '-diaminodiphenyl ether (4,4 '-Diaminodiphenylether, ODA) is as raw material.Be that the ODA of 1:1.05 and naphthalenetetracarbacidic acidic acid anhydride successively add in nmp solution by mol ratio, graphene conductive agent is being added by 10% of theoretical target product quality, back flow reaction 6 hours under argon atmosphere, the solution of target product is added drop-wise to aluminium thin surface and forms film, 50 DEG C of evaporating solvents, 120 DEG C of constant pressure and dry 10h, then at N
2isothermal reaction 5h at the temperature of 200 DEG C in atmosphere;
2, the preparation of positive electrode and film:
Be all take carbonyl as the material of reactive functionality due to the existing polymer that can be used for negative material, be in complete Charging state.Therefore, the conveniently design of battery and assembling, the selection of positive pole polymeric material just needs the polymer looking for a kind of state of discharging completely.In addition, polymer also needs to be easy to synthesis and preserves, and when with material with carbon element compound, also can film forming keep redox property.Based on this, it is positive electrode that the present invention have chosen ferrocene silane polymer.
Concrete manufacturing step is as follows:
1:1:2.2 gets ferrocene in molar ratio, tetramethylethylenediamine (TMEDTA) and n-BuLi (solvent is benzinum) put into Schlenk reaction bulb, and add benzinum, stirred at ambient temperature reaction 24h, obtain yellow ferrocene dilithium salt precipitation.Under the condition of anhydrous and oxygen-free, precipitating solvent is cleaned 3 times, then add benzinum in the yellow solid obtained, and be placed in the cryosel water-bath of about-20 DEG C.Then in mixed liquor, slowly drip hydrogen dimethyl dichlorosilane (DMCS) by constant pressure funnel, slow subsequently temperature is raised to room temperature.Cross after mixed liquor stirs 20h and filter salt, the filter vacuum obtained is removed solvent, the solid of the Chinese red obtained.Then the solid heat polymerization 5h at 150 DEG C will obtained.Finally collect the material of cooling gained, repeatedly to purify precipitation more than three times with oxolane dissolution solvent and methanol solvate, obtain crocus fibre solid compound.Then dissolve crocus fibre solid compound with oxolane, solution is added drop-wise to aluminium thin surface, room temperature moves down to desolventize and obtains film
3, gel-form solid polymer electrolyte preparation:
Because both positive and negative polarity needs to stick together, therefore adopt the sticking water system polymer of a kind of tool to be used as gel electrolyte, play the effect of conducting ion and bonding.
Concrete manufacturing step is as follows:
Polyvinylpyrrolidone (polyvinylpyrrolidone, PVP) is adopted to be electrolytical polymer, 5MNaCl/H
2the O aqueous solution is liquid, is mixed by polymer according to the ratio of mass ratio 1:2 with solution.
4, battery assembling:
The positive electrode film obtained, negative material film and gel electrolyte are assembled into battery, and carry out charge-discharge test, charging and discharging curve is as Fig. 2.
Claims (6)
1. a preparation method for flexible foldable full stress-strain secondary cell, is characterized in that: the positive electrode of flexible foldable full stress-strain secondary cell, negative material and electrolyte all adopt organic polymer material, and its preparation process comprises the following steps:
1) preparation of negative material and film:
Naphthalenetetracarbacidic acidic acid anhydride and 4, the ratio of 4 '-diaminodiphenyl ether 1:0.5-10 in molar ratio adds in nmp solution, graphene conductive agent is added by the mass ratio of theoretical target product 5-20%, back flow reaction 1-12 hour under argon atmosphere, obtain the solution of target product, solution is formed film, evaporating solvent, then at N
2negative material film is obtained by reacting at 200-350 DEG C of temperature in atmosphere;
2) preparation of positive electrode and film:
Ferrocene, tetramethylethylenediamine and n-BuLi be (1-5) in molar ratio: (1-5): (1-15) puts into Schlenk reaction bulb, adds benzinum, stirring reaction 1-72h, obtains yellow ferrocene dilithium salt precipitation; Under the condition of anhydrous and oxygen-free, precipitating solvent is cleaned, add benzinum, be placed in the cryosel water-bath of-5 DEG C to-25 DEG C; Then drip hydrogen dimethyl dichlorosilane (DMCS), temperature is raised to room temperature; Mixed liquor stirring 2-48h crosses and filters salt, and filtrate removes solvent, solid heat polymerization 1-10h at 100-200 DEG C of the Chinese red obtained; Purify with oxolane dissolution solvent and methanol solvate and precipitate, obtain crocus fibre solid compound; Then dissolve crocus fibre solid compound with oxolane, by solution film-forming, room temperature moves down to desolventize and obtains positive electrode film;
3) gel-form solid polymer electrolyte preparation:
Polyvinylpyrrolidone is adopted to be electrolytical polymer, 1-6MNaCl/H
2o liquid, according to the ratio of mass ratio 1:0.5-50 by solution and polymer mixed;
4) battery assembling:
The positive electrode film obtained, negative material film and gel-form solid polymer electrolyte are assembled into battery.
2. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1, it is characterized in that: time prepared by negative material and Film synthesis, naphthalenetetracarbacidic acidic acid anhydride, 4, when 4 '-diaminodiphenyl ether and Graphene add nmp solution, nmp solution be good just to flood powder.
3. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1 and 2, is characterized in that: when negative material and film preparation, and the solution of target product is added drop-wise to aluminium thin surface and forms film, and 30-70 DEG C of evaporating solvent, at N
2in atmosphere, the reaction time is 1-10h.
4. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1, is characterized in that: when positive electrode and film preparation, and the amount adding benzinum is powder volume 3-10 times; Obtain under yellow ferrocene dilithium salt is deposited in the condition of anhydrous and oxygen-free, precipitating solvent being cleaned 2-5 time.
5. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1, it is characterized in that: when positive electrode and film preparation, in mixed liquor, slowly drip hydrogen dimethyl dichlorosilane (DMCS) by constant pressure funnel, the mol ratio of hydrogen dimethyl dichlorosilane (DMCS) and ferrocene is 1:1-5.
6. the preparation method of the flexible foldable full stress-strain secondary cell according to claim 1,4 or 5, is characterized in that: when positive electrode and film preparation, and filtrate adopts vacuum mode to remove solvent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107644996A (en) * | 2017-08-08 | 2018-01-30 | 曲靖师范学院 | A kind of preparation method of pure organic polymer lithium ion battery electrode material |
| CN110611118A (en) * | 2018-06-15 | 2019-12-24 | 沈明东 | Lithium ion secondary battery |
| CN111430718A (en) * | 2020-04-08 | 2020-07-17 | 西北工业大学 | Lithium-based battery electrode slurry, preparation method and application thereof |
| CN113574699A (en) * | 2019-03-14 | 2021-10-29 | 赢创运营有限公司 | Method for manufacturing shaped organic charge storage unit |
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| CN113574699A (en) * | 2019-03-14 | 2021-10-29 | 赢创运营有限公司 | Method for manufacturing shaped organic charge storage unit |
| CN111430718A (en) * | 2020-04-08 | 2020-07-17 | 西北工业大学 | Lithium-based battery electrode slurry, preparation method and application thereof |
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| Publication number | Publication date |
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| CN105070919B (en) | 2017-06-27 |
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