CN104600357A - Polymer composite material solid electrolyte and preparation method thereof - Google Patents
Polymer composite material solid electrolyte and preparation method thereof Download PDFInfo
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- CN104600357A CN104600357A CN201410745343.0A CN201410745343A CN104600357A CN 104600357 A CN104600357 A CN 104600357A CN 201410745343 A CN201410745343 A CN 201410745343A CN 104600357 A CN104600357 A CN 104600357A
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a polymer composite material solid electrolyte and a preparation method thereof. The method employs an inorganic nano-particle and a lithium salt to fill an aqueous polymer and enables the polymer to be crosslinked with polyisocyanate for preparing the solid electrolyte, and belongs to the technical field of lithium ion batteries. The technical scheme is characterized in that the method is based on a water solution pouring process, 60%-80% by mass of the aqueous polymer, 10%-40% by mass of a lithium salt, 2.0%-8.0% by mass of an inorganic nanometer filling material and 2.0%-8.0% by mass of a polyisocyanate cross-linking agent are employed for obtaining the electrolyte. The polymer composite material prepared by utilizing the method has the characteristics of high ion conductivity, excellent mechanical properties and short relaxation time, and the forming technology of the material is simple and accords with green environment-protection requirements.
Description
Technical field
The present invention relates to a kind of electrolyte and preparation method thereof, particularly a kind of composite material solid electrolyte and preparation method thereof, is applied to technical field of lithium ion secondary.
Background technology
Lithium ion battery is as a kind of green high-efficient new forms of energy, there is high voltage, high-energy-density, have extended cycle life and the advantage such as memory-less effect, be widely used on the mancarried electronic aids such as mobile communication, notebook computer and microcam, and also show good application prospect in electric powered motor power supply, intelligent grid energy-storage system, the micro-electro-mechanical systems fields such as Aero-Space that unify.Electrolyte is one of core parts of lithium battery, not only between positive and negative electrode, play a part conduction current and transport ions, and determine the working mechanism of battery to a great extent, be the key factor affecting battery specific energy, fail safe, cycle performance and high rate performance etc.
The electrolyte of lithium ion battery can be divided into liquid electrolyte, solid electrolyte and solid-liquid composite electrolyte three major types.Although liquid electrolyte or the compound gel polymer electrolyte of solid-liquid are commercial on a large scale, but all containing the carbonate based organic solvent of easy to leak, make the huge potential safety hazards such as battery existence is caught fire, blast, particularly particularly serious under abuse state, as thermal shock, overcharge/put with short circuit time, battery use time may there is security incident.Because of not containing any organic solvent, and there is safety, low with the reactivity of electrode material, cycle performance good, be easy to process and the remarkable advantage such as encapsulation, high performance polymer composite material solid electrolyte is the indispensable part of lithium battery of new generation.
Full solid state polymer electrolyte battery have energy density high, manufacture the advantages such as easy, safe and reliable and flexible design, become the Developing mainstream of new chemical industry power supply.But, ionic conductivity and the mechanical property of existing polyethylene glycol oxide (PEO), polyacrylonitrile (PAN) and polymethyl methacrylate (PMMA) base solid polymer electrolyte are all lower, and need in forming process to use a large amount of organic solvents, become the principal element of its development of restriction.
Summary of the invention
In order to overcome the deficiency that prior art exists, the invention provides a kind of polymer composites solid electrolyte and preparation method thereof, made composite material not only has that ionic conductivity is high, the advantage of good mechanical performance, and slack time is short, its moulding process is simple and meet environment protection requirement.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
A kind of polymer composites solid electrolyte, combined by all material components of waterborne polymeric, lithium salts, inorganic nano-particle and polyisocyanates, each material component is as follows according to component dry mass percentage proportioning:
Waterborne polymeric 40.0-80.0 wt%
Lithium salts 15.0-40.0 wt%
Inorganic nano-filler 2.0-10.0 wt%
Polyisocyanates 3.0-10.0 wt%
Above-mentioned waterborne polymeric preferably adopts any one or mixtures several arbitrarily in polyvinyl alcohol, polyvinyl acetate-ethene latex powder and carboxymethyl cellulose.
Above-mentioned lithium salts preferably adopts any one or mixtures several arbitrarily in lithium perchlorate, lithium carbonate, lithium sulfate and lithium nitrate.
Above-mentioned inorganic nano-filler preferably adopts particle diameter to be less than the mixture of any one nanoparticulate fillers in the silicon dioxide of 100 nanometers, titanium dioxide and calcium carbonate or any several nanoparticulate fillers.
Above-mentioned polyisocyanates preferably adopt water dispersible polymeric multi isocyanate and average functionality be not less than in the high functionality polymeric multi isocyanate of 2.85 any one or its both mixture.
A kind of preparation method of Inventive polymers composite material solid electrolyte, based on aqueous solution casting method, each material component is according to component dry mass percentage proportioning, use the polyisocyanate crosslinker of the waterborne polymeric of 60 ~ 80wt%, the lithium salts of 10 ~ 40wt%, the inorganic nano-filler of 2.0 ~ 8.0 wt% and 2.0 ~ 8.0 wt% to prepare polymer composites solid electrolyte as raw material, concrete steps are:
A. waterborne polymeric and deionized water are added in reactor according to the quality proportioning of 1:10, be slowly warming up to 60-95 DEG C, the aqueous polymer solution making it become in mechanical agitation 1-2 hour to be evenly distributed;
B. be cooled to 50 DEG C, and add lithium salts in the aqueous polymer solution prepared in step a, further mechanical agitation 2-3 hour, make lithium salts be dissolved completely in aqueous polymer solution;
C. continue to be cooled to 30-40 DEG C, the nano particle aqueous liquid dispersion being 20 wt % by the solid content containing inorganic nano-filler slowly adds in the aqueous polymer solution of the dissolving lithium salts prepared in stepb, under ultrasonic wave and churned mechanically acting in conjunction, mixing 2-3 hour, makes inorganic nano-filler be scattered in mixed liquor;
D. in the mixed liquor prepared in step c, drip polymeric isocyanate, and stir 15-30 minute;
E. the mixed liquor prepared in steps d is poured in polytetrafluorethylecoatings coatings mould, at room temperature leaves standstill after 48 hours, in vacuum drying chamber at 30-40 DEG C dry 72 hours, obtain dielectric film;
F. will in step e dried dielectric film, under 140 DEG C of conditions, hot setting is after at least 24 hours, eliminates isocyanate groups residual in dielectric film, and final obtained thickness is the solid electrolyte film of 20-60 μm.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. not simply blended between lithium salts and waterborne polymeric segment in the solid electrolyte that prepared by the present invention, but define effective ligand, by this complexing-solution complexing process implementation migration of lithium ion of coordination, lithium salts have impact on the regularity of polymer molecule segment, reduce polymer dielectric degree of crystallinity and fusing point, thus molecule segment warm-up movement ability is strengthened;-the NCO of polymeric isocyanate can with the hydroxyl generation chemical reaction in waterborne polymeric, electrolyte inside is made to form spatial network, then make remaining NCO group be cross-linked further by " reprocessing " heating, change the regularity of segment arrangement, improve the locomitivity of segment further; And nano inorganic particle can reduce the crystallizing power of macromolecular material, increase amorphous region content;
2. the polymer composites solid electrolyte that the inventive method obtains has the feature of ionic conductivity height and good mechanical performance;
3. the method that the present invention uses is compared with existing solid polyelectrolyte preparation method, and not only the performance of product is more superior, avoids the release of organic solvent, and significantly can reduce production cost.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment one:
In the present embodiment, the preparation method of polymer composites solid electrolyte, based on aqueous solution casting method, step is as follows:
A. 600 parts of cold water are injected reactor, start mixer, add the polyvinyl alcohol of 60 parts of alcoholysis degrees 88%, be slowly warming up to 90 DEG C, mechanical mixture obtains homogeneous solution in 2 hours;
B. be cooled to 50 DEG C, add 30 parts of lithium perchlorates, stir 2.5 hours, make it be dissolved completely in polyvinyl alcohol water solution;
C. continue to be cooled to 40 DEG C, the aqueous liquid dispersion (solid content 20%) of 25 parts of Nano particles of silicon dioxide is slowly added, under ultrasonic wave and churned mechanically acting in conjunction, mix 3 hours;
D. drip 5 parts of water dispersible polymeric isocyanate, and stir 15-30 minute;
E. room temperature in above-mentioned solution casting to polytetrafluorethylecoatings coatings mould was left standstill after 48 hours, in vacuum drying chamber at 40 DEG C dry 72 hours;
F. dried dielectric film is solidified 24 hours in 140 DEG C, eliminate wherein residual-NCO, obtain the solid electrolyte film that thickness is 25 μm.
embodiment two:
The present embodiment is substantially identical with embodiment one, and special feature is:
In the present embodiment, the preparation method of polymer composites solid electrolyte, step is as follows:
A. 600 parts of cold water are injected reactor, start mixer, add 55 parts of polyvinyl acetate-ethene breast (VAE) rubber powder, be slowly warming up to 60 DEG C, mechanical mixture obtains homogeneous solution in 2 hours;
B. be cooled to 50 DEG C, add 35 parts of lithium carbonates, stir 3 hours, make it be dissolved completely in VAE solution;
C. continue to be cooled to 30-40 DEG C, 30 parts of nano-calcium carbonate aqueous liquid dispersions (solid content 20%) are slowly added, under ultrasonic wave and churned mechanically acting in conjunction, mix 2.5 hours;
D. drip 4 parts of water dispersible polymeric multi isocyanates, and stir 15-30 minute;
E. this step is identical with embodiment one;
F. dried dielectric film is solidified 24 hours in 140 DEG C, eliminate wherein residual-NCO, obtain the solid electrolyte film that thickness is 35 μm.
embodiment three:
The present embodiment and previous embodiment are substantially identical, and special feature is:
In the present embodiment, the preparation method of polymer composites solid electrolyte, step is as follows:
A. 600 parts of cold water are injected reactor, start mixer, add polyvinyl alcohol and 10 parts of carboxymethyl celluloses of 50 parts of alcoholysis degrees 99%, be slowly warming up to 95 DEG C, mechanical mixture obtains homogeneous solution in 2 hours;
B. be cooled to 50 DEG C, add 30 parts of lithium sulfates, stir 2.5 hours, make it be dissolved completely in the mixed aqueous solution of polyvinyl alcohol and carboxymethyl cellulose;
C. continue to be cooled to 30-40 DEG C, 20 parts of nano titanium dioxide water-dispersion liquids (solid content 20%) are slowly added, under ultrasonic wave and churned mechanically acting in conjunction, mix 3 hours;
D. drip 6 parts of high functionality polymeric multi isocyanates, and stir 15-30 minute;
E. this step is identical with embodiment one;
F. dried dielectric film is solidified 24 hours in 140 DEG C, eliminate wherein residual-NCO, obtain the solid electrolyte film that thickness is 30 μm.
material property analytical test:
Main performance according to the made solid electrolyte of embodiment one ~ embodiment three detects, and is compared as follows table 1.
the main physico-mechanical performance of table 1. embodiment of the present invention solid electrolyte
From table 1, polymer composites solid electrolyte of the present invention has good normal temperature ionic conductivity and mechanical property, and what is more important is less for its slack time, can guarantee service ability steady in a long-term.The present invention utilizes inorganic nano-particle, lithium salts, modified polyisocyanate waterborne polymeric to prepare total solids electrolyte, can be widely used in lithium rechargeable battery industrial circle.
Above the embodiment of the present invention is illustrated; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of innovation and creation of the present invention; change, the modification made under all Spirit Essences according to technical solution of the present invention and principle, substitute, combination, to simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept of Inventive polymers composite material solid electrolyte and preparation method thereof, all protection scope of the present invention is belonged to.
Claims (6)
1. a polymer composites solid electrolyte, is characterized in that, is combined by all material components of waterborne polymeric, lithium salts, inorganic nano-particle and polyisocyanates, and each material component is as follows according to component dry mass percentage proportioning:
Waterborne polymeric 40.0-80.0 wt%
Lithium salts 15.0-40.0 wt%
Inorganic nano-filler 2.0-10.0 wt%
Polyisocyanates 3.0-10.0 wt%.
2. polymer composites solid electrolyte according to claim 1, is characterized in that: waterborne polymeric is any one or mixtures several arbitrarily in polyvinyl alcohol, polyvinyl acetate-ethene latex powder and carboxymethyl cellulose.
3. polymer composites solid electrolyte according to claim 1 or 2, is characterized in that: lithium salts is any one or mixtures several arbitrarily in lithium perchlorate, lithium carbonate, lithium sulfate and lithium nitrate.
4. polymer composites solid electrolyte according to claim 1 or 2, is characterized in that: inorganic nano-filler is the mixture that particle diameter is less than any one nanoparticulate fillers in the silicon dioxide of 100 nanometers, titanium dioxide and calcium carbonate or any several nanoparticulate fillers.
5. polymer composites solid electrolyte according to claim 1 or 2, is characterized in that: polyisocyanates for water dispersible polymeric multi isocyanate and average functionality be not less than in the high functionality polymeric multi isocyanate of 2.85 any one or its both mixture.
6. the preparation method of polymer composites solid electrolyte described in a claim 1, it is characterized in that, based on aqueous solution casting method, each material component is according to component dry mass percentage proportioning, use the polyisocyanate crosslinker of the waterborne polymeric of 60 ~ 80wt%, the lithium salts of 10 ~ 40wt%, the inorganic nano-filler of 2.0 ~ 8.0 wt% and 2.0 ~ 8.0 wt% to prepare polymer composites solid electrolyte as raw material, concrete steps are:
A. waterborne polymeric and deionized water are added in reactor according to the quality proportioning of 1:10, be slowly warming up to 60-95 DEG C, the aqueous polymer solution making it become in mechanical agitation 1-2 hour to be evenly distributed;
B. be cooled to 50 DEG C, and add lithium salts in the aqueous polymer solution prepared in described step a, further mechanical agitation 2-3 hour, make lithium salts be dissolved completely in aqueous polymer solution;
C. continue to be cooled to 30-40 DEG C, the nano particle aqueous liquid dispersion being 20 wt % by the solid content containing inorganic nano-filler is slowly added in the aqueous polymer solution of the dissolving lithium salts prepared in described step b, under ultrasonic wave and churned mechanically acting in conjunction, mixing 2-3 hour, makes inorganic nano-filler be scattered in mixed liquor;
D. in the mixed liquor prepared in described step c, drip polymeric isocyanate, and stir 15-30 minute;
E. the mixed liquor prepared in described steps d is poured in polytetrafluorethylecoatings coatings mould, at room temperature leaves standstill after 48 hours, in vacuum drying chamber at 30-40 DEG C dry 72 hours, obtain dielectric film;
F. will in described step e dried dielectric film, under 140 DEG C of conditions, hot setting is after at least 24 hours, eliminates isocyanate groups residual in dielectric film, and final obtained thickness is the solid electrolyte film of 20-60 μm.
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Cited By (12)
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| CN105860114A (en) * | 2016-03-21 | 2016-08-17 | 青岛科技大学 | Preparation method for cellulose nanofiber solid electrolyte membrane |
| CN107925126A (en) * | 2015-08-17 | 2018-04-17 | 地方独立行政法人大阪产业技术研究所 | Additive, all solid state secondary battery and its manufacture method of all solid state secondary battery |
| CN108475808A (en) * | 2016-01-04 | 2018-08-31 | 纳米技术仪器公司 | solid electrolyte for lithium secondary battery |
| CN108469388A (en) * | 2018-02-01 | 2018-08-31 | 上海大学 | The prediction technique of high polymer dynamic storage modulus under wet heat condition |
| CN108520959A (en) * | 2018-03-20 | 2018-09-11 | 上海大学 | Waterborne polymeric-isocyanate group electrode composite material and preparation method thereof |
| CN109004280A (en) * | 2018-07-11 | 2018-12-14 | 珠海光宇电池有限公司 | A kind of preparation method and full solid state polymer battery of full solid state polymer electrolyte |
| CN109326822A (en) * | 2018-11-05 | 2019-02-12 | 珠海光宇电池有限公司 | A kind of preparation method and lithium ion battery of all solid state fluoropolymer electrolyte film |
| CN110268573A (en) * | 2016-12-12 | 2019-09-20 | 纳米技术仪器公司 | Hybrid solid-state electrolyte for lithium secondary battery |
| CN111786017A (en) * | 2020-04-17 | 2020-10-16 | 中国科学院青岛生物能源与过程研究所 | High-cohesiveness solid electrolyte prepared by in-situ curing, preparation method and application |
| CN111969245A (en) * | 2020-04-17 | 2020-11-20 | 中国科学院青岛生物能源与过程研究所 | High-safety solid electrolyte and preparation method and application thereof |
| CN112234314A (en) * | 2020-09-28 | 2021-01-15 | 佛山市金辉高科光电材料股份有限公司 | Composite slurry, lithium battery diaphragm and preparation method and application of lithium battery diaphragm |
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