CN105070919B - A kind of preparation method of flexible foldable full stress-strain secondary cell - Google Patents
A kind of preparation method of flexible foldable full stress-strain secondary cell Download PDFInfo
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- CN105070919B CN105070919B CN201510403948.6A CN201510403948A CN105070919B CN 105070919 B CN105070919 B CN 105070919B CN 201510403948 A CN201510403948 A CN 201510403948A CN 105070919 B CN105070919 B CN 105070919B
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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
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- 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
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- 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
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Abstract
The present invention relates to a kind of preparation method of flexible foldable full stress-strain secondary cell.The invention belongs to technical field of chemical power.The preparation method of flexible foldable full stress-strain secondary cell：1) preparation of negative material and film：Naphthalenetetracarbacidic acidic acid anhydride and 4,4 ' diaminodiphenyl ethers add nmp solution, plus graphene conductive agent, back flow reaction under argon atmosphere, masking；2) preparation of positive electrode and film：Ferrocene, tetramethylethylenediamine and n-BuLi are put into Schlenk reaction bulbs, add petroleum ether, reaction, precipitation；Solvent is cleaned, plus petroleum ether, and hydrogen dimethyl dichlorosilane (DMCS) is added dropwise；Solid heat polymerization；Masking；3) prepared by gel-form solid polymer electrolyte：Polyvinylpyrrolidone and NaCl/H2O liquid mixes；4) battery assembling：Positive and negative pole material film is assembled into battery with gel electrolyte.The present invention has process stabilizing, and product is ultra-thin controllable, flexible foldable, it is easy to design, safety non-toxic, disclosure satisfy that the advantages of comfortable and special occasions demand is fitted with human body.
Description
Technical field
The invention belongs to technical field of chemical power, more particularly to a kind of system of flexible foldable full stress-strain secondary cell
Preparation Method.
Background technology
At present, wearable electronic is one of current electronics Hot spots for development, and restriction wearable device is fast-developing
Key technology will be matching power supply module.The various wearable devices of hundreds of moneys have been occurred in that on the market,
But the breakthrough development of wearable power technology is few.Based on the reason for human body is constructed, how more preferable wearable power supply is
Laminating human limb be problem demanding prompt solution, and the thin film flexible of power-supply system chemical conversion outlet to solve this problem.
It is currently used in that to meet the main film power supply of wearable electronic be film lithium ion battery, but this battery
The key components such as the simply filming of conventional lithium ion battery, both positive and negative polarity composition and energy storage mechnism are all secondary with traditional commerce lithium
Battery is identical.Essential structure and the main material property of lithium ion battery are limited to, film lithium ion battery cannot meet
For a long time, at random, significantly fold used with bending, especially with the character of use that clothing is the same.And existing film
Lithium ion battery, due to using organic system electrolyte or transition metal electrode material, there is certain murder by poisoning performance to human body,
Once if leakage, threat will be produced to the health of human body.
The content of the invention
The present invention provides a kind of secondary electricity of flexible foldable full stress-strain to solve technical problem present in known technology
The preparation method in pond.
Have it is an object of the invention to provide one kind and disclosure satisfy that comfort requirement characteristic of being fitted with human body, and some are special
Occasion demand can be the features such as significantly folded bent be used at random flexible foldable full stress-strain secondary cell preparation method.
Full stress-strain thin polymer film flexibility secondary cell, for future realizes that the folding functional of flexible thin-film battery provides one
Individual very promising solution because polymer has good plasticity, can film forming, can also be woven into cloth into silk.Quan You
Machine polymer secondary battery, its positive electrode, negative material and electrolyte three parts use organic polymer material
And the battery being assembled into.
Full stress-strain thin polymer film flexibility secondary cell preparation process：
1st, the preparation of negative material and film：
The material for using polyimide is main body, is obtained by adjusting the drawing electronics on imines and electron functional group
Suitable operating voltage, and polyimides or intermediate polymer are adjusted using nonactive main chain functional group in Conventional solvents
Solubility property, come and conductive carbon composite membrane-forming with this.
2nd, the preparation of positive electrode and film：
Because the existing polymer that can be used for negative material is all the material with carbonyl as reactive functionality, in filling completely
Electric state.Therefore, the design of battery and assembling for convenience, the selection of positive pole polymeric material is accomplished by looking for a kind of state of discharging completely
Polymer.In addition, polymer also need to be readily synthesized with preservation, and with carbon material it is compound in the case of, also can
Enough film forming simultaneously keep redox property.Based on this, the present invention have chosen ferrocene silane polymer for positive electrode.
3rd, prepared by gel-form solid polymer electrolyte
Because both positive and negative polarity needs to stick together, therefore gel electrolyte is used as using a kind of sticking water system polymer of tool
Matter, plays a part of conduction ion and bonding.
4th, the positive and negative pole material film and gel electrolyte that will be obtained are assembled into battery.
The preparation method of flexible foldable full stress-strain secondary cell of the present invention is adopted the technical scheme that：
A kind of preparation method of flexible foldable full stress-strain secondary cell, is characterized in：Flexible foldable full stress-strain is secondary
The positive electrode of battery, negative material and electrolyte use organic polymer material, its preparation process to comprise the following steps：
1) preparation of negative material and film：
Naphthalenetetracarbacidic acidic acid anhydride and 4,4 '-diaminodiphenyl ether in molar ratio 1:The ratio of 0.5-10 is added in nmp solution, according to reason
Graphene conductive agent is added by the mass ratio of target product 5-20%, back flow reaction 1-12 hours under argon atmosphere, mesh is obtained
The solution of product is marked, solution is formed into film, evaporation solvent, then in N2Reaction is born at a temperature of 200-350 DEG C in atmosphere
Pole material film；
2) preparation of positive electrode and film：
Ferrocene, tetramethylethylenediamine and n-BuLi are in molar ratio (1-5):(1-5):It is anti-that (1-15) is put into Schlenk
Answer in bottle, add petroleum ether, stirring reaction 1-72h to obtain the ferrocene dilithium salt precipitation of yellow；Under conditions of anhydrous and oxygen-free
Precipitating solvent is cleaned, petroleum ether is added, is placed in -5 DEG C to -25 DEG C of ice salt bath；Then hydrogen methyl dichloro silicon is added dropwise
Alkane, temperature is raised to room temperature；Mixed liquor stirring 2-48h is filtered to remove salt, and filtrate removes solvent, and the solid of the Chinese red for obtaining exists
Heat polymerization 1-10h at 100-200 DEG C；Precipitation is purified with tetrahydrofuran dissolution solvent and methanol solvate, crocus is obtained fine
Dimension solid chemical compound；Then crocus fibre solid compound is dissolved with tetrahydrofuran, by solution film-forming, solvent is removed at room temperature
Obtain positive electrode film；
3) prepared by gel-form solid polymer electrolyte：
It is the polymer of electrolyte, 1-6M NaCl/H to use polyvinylpyrrolidone2O liquid, according to mass ratio 1:0.5-
50 ratio is by solution and mixed with polymers；
4) battery assembling：
Positive electrode film, negative material film and the gel-form solid polymer electrolyte that will be obtained are assembled into battery.
The preparation method of flexible foldable full stress-strain secondary cell of the present invention can also be adopted the following technical scheme that：
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in：Negative material and film preparation
When, naphthalenetetracarbacidic acidic acid anhydride and 4,4 '-diaminodiphenyl ether add nmp solution when, naphthalenetetracarbacidic acidic acid anhydride, 4,4 '-diaminodiphenyl ether with
And Graphene, when adding nmp solution, nmp solution is preferred with just flooding powder.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in：Negative material and film preparation
When, the solution of target product is added drop-wise to aluminium thin surface and forms film, 30-70 DEG C of evaporation solvent, in N2The reaction time is in atmosphere
1-10h, finally removes aluminum foil substrate.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in：Positive electrode and film preparation
When, the amount for adding petroleum ether is 3-10 times of powder volume；The ferrocene dilithium salt for obtaining yellow is deposited in the condition of anhydrous and oxygen-free
It is lower to clean precipitating solvent 2-5 times.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in：Positive electrode and film preparation
When, with constant pressure funnel to the mol ratio that hydrogen dimethyl dichlorosilane (DMCS), hydrogen dimethyl dichlorosilane (DMCS) and ferrocene are slowly added dropwise in mixed liquor
It is 1:1-5.
The preparation method of described flexible foldable full stress-strain secondary cell, is characterized in：Positive electrode and film preparation
When, filtrate removes solvent using vacuum mode, finally removes aluminum foil substrate.
The present invention has the advantages and positive effects that：
The preparation method of flexible foldable full stress-strain secondary cell is and existing as a result of the brand-new technical scheme of the present invention
There is technology to compare, the advantage of full stress-strain polymer thin film battery of the present invention is mainly manifested in following aspects：
1) one is difunctional：
Polymer has plasticity, can directly electrospinning into cloth, and inorganic matter is not all right, thus be easy to fabric power supply integrally
Change, structoure of the human body of more fitting, with huge application potential；
2) it is ultra-thin controllable：
Because electrode material is polymer, structure and chemical property that specific solvent is also remained intact are dissolved in, can
Slimline battery is obtained with by simple casting mode, inorganic material cannot accomplish.Its thickness can arbitrarily regulate and control, until nanometer
The slimline battery of level thickness；
3) flexible foldable：
By the material that hull cell is used is polymer, with good plasticity, by being woven into cloth or film forming
The electrode of these types so that battery has the flexible foldable feature as clothing or plastics；
4) it is easily designed：
Because miniature high-tech electronic equipment has small volume, powerful feature, it is difficult to reserve enough places to
Battery, this battery just can sufficiently utilize small space by way of casting without by complicated design,
For micromodule equipment provides more electric energy；
5) safety non-toxic：
Polymeric material composition is non-toxic, can also use various electrolyte systems, is that traditional lithium secondary battery is incomparable.
Particularly can be designed as brine system (NaCl/H2O), simple sweat can be achieved with 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 excellent
Gesture, can make very big progradation to the battery technology of wearable technology and variform and occupation mode.
Brief description of the drawings
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 poly-
Compound 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.
Specific embodiment
For the content of the invention of the invention, feature and effect can be further appreciated that, following examples are hereby enumerated, and coordinate accompanying drawing
Describe in detail as follows：
Refering to accompanying drawing 1 and Fig. 2.
Embodiment 1
A kind of preparation method of flexible foldable full stress-strain secondary cell, its positive electrode, negative material and electrolysis
Matter three parts use organic polymer material, preparation process to comprise the following steps that：
1st, the preparation of negative material and film：
The material for using polyimide is main body, is obtained by adjusting the drawing electronics on imines and electron functional group
Suitable operating voltage, and polyimides or intermediate polymer are adjusted using nonactive main chain functional group in Conventional solvents
Solubility property, come and conductive carbon composite membrane-forming with this.
Specific manufacturing step is as follows：
The preparation of polyamide
Using naphthalenetetracarbacidic acidic acid anhydride and 4,4 '-diaminodiphenyl ether (4,4 '-Diaminodiphenyl ether, ODA) conduct
Raw material.It is 1 by mol ratio:1.05 ODA is successively added in nmp solution with naphthalenetetracarbacidic acidic acid anhydride, by theoretical target product matter
10% addition graphene conductive agent of amount, the solution of target product is added drop-wise to aluminium thin by back flow reaction 6 hours under argon atmosphere
Surface forms film, 50 DEG C of evaporation solvents, 120 DEG C of constant pressure and dry 10h, then in N2Constant temperature is anti-at a temperature of 200 DEG C in atmosphere
Answer 5h；
2nd, the preparation of positive electrode and film：
Because the existing polymer that can be used for negative material is all the material with carbonyl as reactive functionality, in filling completely
Electric state.Therefore, the design of battery and assembling for convenience, the selection of positive pole polymeric material is accomplished by looking for a kind of state of discharging completely
Polymer.In addition, polymer also need to be readily synthesized with preservation, and with carbon material it is compound in the case of, also can
Enough film forming simultaneously keep redox property.Based on this, the present invention have chosen ferrocene silane polymer for positive electrode.
Specific manufacturing step is as follows：
In molar ratio 1:1:2.2 take ferrocene, tetramethylethylenediamine (TMEDTA) and n-BuLi (solvent is petroleum ether)
It is put into Schlenk reaction bulbs, and adds petroleum ether, at room temperature stirring reaction 24h, the ferrocene dilithium salt for obtaining yellow sinks
Form sediment.Precipitating solvent is cleaned 3 times under conditions of anhydrous and oxygen-free, then to adding petroleum ether in the yellow solid for obtaining, and will
It is placed in -20 DEG C or so of ice salt bath.Then with constant pressure funnel to being slowly added dropwise hydrogen dimethyl dichlorosilane (DMCS) in mixed liquor, with
Temperature is slowly raised to room temperature afterwards.Salt is filtered to remove after mixed liquor stirring 20h, the filter vacuum that will be obtained removes solvent, obtains
Chinese red solid.Then the solid that will be obtained heat polymerization 5h at 150 DEG C.The material obtained by cooling is finally collected,
Precipitation is purified repeatedly more than three times, obtain crocus fibre solid compound with tetrahydrofuran dissolution solvent and methanol solvate.So
Crocus fibre solid compound is dissolved with tetrahydrofuran afterwards, solution is added drop-wise to aluminium thin surface, solvent removed at room temperature and is obtained
Film
3rd, prepared by gel-form solid polymer electrolyte：
Because both positive and negative polarity needs to stick together, therefore gel electrolyte is used as using a kind of sticking water system polymer of tool
Matter, plays a part of conduction ion and bonding.
Specific manufacturing step is as follows：
It is the polymer of electrolyte, 5M using polyvinylpyrrolidone (polyvinyl pyrrolidone, PVP)
NaCl/H2The O aqueous solution is liquid, according to mass ratio 1:2 ratio mixes polymer with solution.
4th, battery assembling：
Positive electrode film, negative material film and the gel electrolyte that will be obtained are assembled into battery, and carry out discharge and recharge
Test, charging and discharging curve such as Fig. 2.
Claims (6)
1. a kind of preparation method of flexible foldable full stress-strain secondary cell, it is characterized in that：The secondary electricity of flexible foldable full stress-strain
The positive electrode in pond, negative material and electrolyte use organic polymer material, its preparation process to comprise the following steps：
1) preparation of negative material and film：
Naphthalenetetracarbacidic acidic acid anhydride and 4,4 '-diaminodiphenyl ether in molar ratio 1:The ratio of 0.5-10 is added in nmp solution, by theoretical mesh
The mass ratio of mark product 5-20% adds graphene conductive agent, back flow reaction 1-12 hours under argon atmosphere, obtains target product
The solution of thing, film, evaporation solvent, then in N are formed by solution2Reaction obtains negative pole material at a temperature of 200-350 DEG C in atmosphere
Material film；
2) preparation of positive electrode and film：
Ferrocene, tetramethylethylenediamine and n-BuLi are in molar ratio (1-5):(1-5):(1-15) is put into Schlenk reaction bulbs
In, add petroleum ether, stirring reaction 1-72h to obtain the ferrocene dilithium salt precipitation of yellow；Will be heavy under conditions of anhydrous and oxygen-free
Shallow lake is cleaned with solvent, adds petroleum ether, is placed in -5 DEG C to -25 DEG C of ice salt bath；Then hydrogen dimethyl dichlorosilane (DMCS), temperature is added dropwise
Degree is raised to room temperature；Mixed liquor stirring 2-48h is filtered to remove salt, and filtrate removes solvent, and the solid of the Chinese red for obtaining is in 100-200
Heat polymerization 1-10h at DEG C；Precipitation is purified with tetrahydrofuran dissolution solvent and methanol solvate, crocus fibre solid is obtained
Compound；Then crocus fibre solid compound is dissolved with tetrahydrofuran, by solution film-forming, solvent is removed at room temperature and obtains positive pole
Material film；
3) prepared by gel-form solid polymer electrolyte：
It is the polymer of electrolyte, 1-6M NaCl/H to use polyvinylpyrrolidone2O liquid, according to mass ratio 1:0.5-50's
Ratio is by solution and mixed with polymers；
4) battery assembling：
Positive electrode film, negative material film and the gel-form solid polymer electrolyte that will be obtained 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：Negative material
And during Film synthesis preparation, naphthalenetetracarbacidic acidic acid anhydride, 4, when 4 '-diaminodiphenyl ether and Graphene add nmp solution, nmp solution
Amount be preferred with just flooding powder.
3. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1 and 2, it is characterized in that：Negative pole
When material and film preparation, the solution of target product is added drop-wise to aluminium foil surface and forms film, 30-70 DEG C of evaporation solvent, in N2Gas
The reaction time is 1-10h in atmosphere.
4. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1, it is characterized in that：Positive electrode
And during film preparation, ferrocene, tetramethylethylenediamine and n-BuLi are put into the amount of addition petroleum ether in Schlenk reaction bulbs
For 3-10 times of powder volume；The ferrocene dilithium salt precipitation of yellow is obtained, it is under conditions of anhydrous and oxygen-free that precipitating solvent is clear
Wash 2-5 times.
5. the preparation method of flexible foldable full stress-strain secondary cell according to claim 1, it is characterized in that：Positive electrode
And during film preparation, with constant pressure funnel to being slowly added dropwise hydrogen dimethyl dichlorosilane (DMCS) in mixed liquor, hydrogen dimethyl dichlorosilane (DMCS) and two cyclopentadienyls
The mol ratio of iron is 1:1-5.
6. the preparation method of the flexible foldable full stress-strain secondary cell according to claim 1,4 or 5, it is characterized in that：Just
When pole material and film preparation, filtrate removes solvent using vacuum mode.
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| CN107644996B (en) * | 2017-08-08 | 2020-06-16 | 曲靖师范学院 | Preparation method of pure organic polymer lithium ion battery electrode material |
| TWI670882B (en) * | 2018-06-15 | 2019-09-01 | 沈明東 | Lithium ion secondary battery |
| CN113574699A (en) * | 2019-03-14 | 2021-10-29 | 赢创运营有限公司 | Method for manufacturing shaped organic charge storage unit |
| CN111430718B (en) * | 2020-04-08 | 2021-07-27 | 西北工业大学 | Lithium-based battery electrode slurry, preparation method and application thereof |
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| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
| WO2012140709A1 (en) * | 2011-04-11 | 2012-10-18 | パナソニック株式会社 | Flexible battery and manufacturing method thereof |
| CN103682368A (en) * | 2012-09-20 | 2014-03-26 | 中国科学院金属研究所 | Rapidly charged flexible lithium ion battery and preparation method of electrodes of rapidly charged flexible lithium ion battery |
| CN103715380A (en) * | 2013-12-30 | 2014-04-09 | 深圳市格瑞普电池有限公司 | Flexible wearable lithium battery |
| CN104143655A (en) * | 2014-07-31 | 2014-11-12 | 天津力神电池股份有限公司 | Flexible and pliable lithium ion secondary battery and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012140709A1 (en) * | 2011-04-11 | 2012-10-18 | パナソニック株式会社 | Flexible battery and manufacturing method thereof |
| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
| CN103682368A (en) * | 2012-09-20 | 2014-03-26 | 中国科学院金属研究所 | Rapidly charged flexible lithium ion battery and preparation method of electrodes of rapidly charged flexible lithium ion battery |
| CN103715380A (en) * | 2013-12-30 | 2014-04-09 | 深圳市格瑞普电池有限公司 | Flexible wearable lithium battery |
| CN104143655A (en) * | 2014-07-31 | 2014-11-12 | 天津力神电池股份有限公司 | Flexible and pliable lithium ion secondary battery and manufacturing method thereof |
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