CN103779603A - Preparation method of composite electrolyte film - Google Patents
Preparation method of composite electrolyte film Download PDFInfo
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- CN103779603A CN103779603A CN201310754555.0A CN201310754555A CN103779603A CN 103779603 A CN103779603 A CN 103779603A CN 201310754555 A CN201310754555 A CN 201310754555A CN 103779603 A CN103779603 A CN 103779603A
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- solution
- composite
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- composite electrolyte
- organic solvent
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
-
- 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
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Dispersion Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
Abstract
The invention relates to a preparation method of a composite electrolyte film. The preparation method comprises the main steps: soaking a polyethylene diaphragm in a chromium oxidation solution for three minutes, then rinsing with deionized water and drying for later use; dissolving 1-35 percent by mass of polymer in 30-98 percent by mass of organic solvent, and stirring to obtain a gel solution; adding 1-35 percent by mass of ceramic particles to the gel solution and stirring so that the particle oxides are uniformly dispersed to form a coating solution; uniformly coating the treated polyethylene diaphragm with the coating solution by adopting steps of dipping, coating and the like; enabling the organic solvent to be evaporated at normal temperature or by heating, so that a composite film is basically formed; and soaking the basically formed composite film in absolute ethyl alcohol, standing, then taking out, and carrying out vacuum drying to obtain the composite electrolyte film meeting production requirements.
Description
Technical field
The present invention is the method during lithium electricity is produced, and that concrete is the preparation method of a kind of composite electrolyte membrane during lithium electricity is produced.
Background technology
The features such as green secondary lithium battery is with its excellent electrical property and nuisanceless, and security performance is good, development is exceedingly fast, and becomes the focus of novel power supply technical research in recent years.Common lithium rechargeable battery is made up of positive/negative material, electrolyte, barrier film and battery case packaging material.Barrier film is the important component part of liquid lithium ion secondary cell, in battery, play and prevent positive/negative short circuit, the effect of ion transportation electric channel is provided simultaneously in charge and discharge process, its performance has determined interfacial structure, the internal resistance etc. of battery, the characteristic such as capacity, cycle performance and security performance that directly affects battery, the barrier film of excellent performance has important effect to the combination property that improves battery
The lithium ion battery separator of existing market still, take polyethylene, polypropylene as main polyalkene diaphragm, comprises individual layer PE, individual layer PP, three layers of PP/PE/PP composite membrane.The patent US Patent3426754 in 1970 of Celanse company of the U.S., for the production of the polypropylene porous film of individual layer.This technique is very ripe in the U.S., Japan through the development of decades, and Celgard company of the U.S., Japanese UBE company adopt this kind of explained hereafter individual layer PP, PE and three layers of PP/PE/PP composite membrane now.But in Celgard method, be difficult to obtain the film of aperture homogeneous and interelectrode distance is increased, the internal resistance that has increased battery.Generally speaking, polyethylene, polypropylene diaphragm are poor to electrolyte compatibility, and imbibition ability is low, causes battery conductance rate low.
Summary of the invention
The object of the invention provides a kind of preparation method of composite electrolyte membrane, and dielectric film is coated on polyethylene barrier film and is prepared from by polymer and ceramic particle.This method comprises the following steps:
(1) polyethylene barrier film soaks three minutes in chromium oxidation solution, then uses deionized water rinsing, dry for standby.
(2) mass ratio 1%-35% polymer is dissolved in mass ratio 30%-98% organic solvent, stirs into gel solution.
(3) mass ratio 1%-35% ceramic particle is added in gel solution and stirs 3-5 hour, make the dispersed formation coating solution of particulate oxide thing.
(4) dipping for coating solution, the methods such as coating are evenly coated on treated polyethylene barrier film, and ventilation normal temperature or heating make organic solvent volatilization, composite membrane basic forming.
(5) composite membrane of basic forming is immersed in absolute ethyl alcohol, leaves standstill and take out vacuumize 4 hours after 12 hours, be met the composite electrolyte membrane of production.
Described polymer is Kynoar, and organic solvent is N-methyl 2-pyrrolidone N-solution, and ceramic micro-ceramic particle is alumina in Nano level, a kind of or their mixtures among zirconia.
The invention has the beneficial effects as follows: the composite electrolyte membrane pick up of producing by this method is more than 120%, exceed more than 40% compared with traditional polyethylene barrier film, the reticulated cell even structure forming, is conducive to electrolyte and keeps ion concentration stable, promotes the cycle performance of battery.
Embodiment
Embodiment 1
Polyethylene barrier film is soaked three minutes in chromium oxidation solution, use again deionized water rinsing, dry for standby, be dissolved in 50 grams of N-methyl 2-pyrrolidone N-solution poly-1 gram of Kynoar, 50 degree water-bath magnetic stirrings become gel solution for 2 hours, add 2 grams of alumina in Nano level to stir 3-5 hour, make the dispersed formation coating solution of particulate oxide thing, polyethylene barrier film is immersed, put 60 degree true temp casees into and after 5 minutes, take out just film of formation, the composite membrane of basic forming is immersed in absolute ethyl alcohol, leave standstill and after 12 hours, take out vacuumize ventilation in 4 hours, be met the composite electrolyte membrane of production.
Under high-power microscope, observe the micro-nano structure of its formation; It is weighed, film is placed in electrolyte, to activate 2 hours and take out dabs the unnecessary electrolyte calculating pick up of weighing; Become battery finished product to carry out performance test take composite diaphragm as Raw material processing.Relevant data is in table 1.
Embodiment 2
Polyethylene barrier film is soaked three minutes in chromium oxidation solution, use again deionized water rinsing, dry for standby, be dissolved in 50 grams of N-methyl 2-pyrrolidone N-solution poly-2 grams of Kynoar, 50 degree water-bath magnetic stirrings become gel solution in 2 hours, add 1 gram of alumina in Nano level to stir 3-5 hour, make the dispersed formation coating solution of particulate oxide thing, polyethylene barrier film is immersed, puts 60 degree true temp casees into and after 5 minutes, take out and form just film, by basic forming
Composite membrane is immersed in absolute ethyl alcohol, leaves standstill and after 12 hours, takes out vacuumize ventilation in 4 hours, is met the composite electrolyte membrane of production.
Under high-power microscope, observe the micro-nano structure of its formation; It is weighed, film is placed in electrolyte, to activate 2 hours and take out dabs unnecessary electrolyte, the calculating pick up of weighing; Become battery finished product to carry out performance test take composite diaphragm as Raw material processing.Relevant data is in table 1.
Embodiment 3
Polyethylene barrier film is soaked three minutes in chromium oxidation solution, then use deionized water rinsing, dry for standby, by 1.5 grams of poly-being dissolved in 50 grams of N-methyl 2-pyrrolidone N-solution of Kynoar, 50 degree water-bath magnetic stirrings become gel solution for 2 hours, add 1.5 grams of alumina in Nano level to stir 3-5 hour, make the dispersed formation coating solution of particulate oxide thing, polyethylene barrier film is immersed, puts 60 degree true temp casees into and after 5 minutes, take out just film of formation, the composite membrane of basic forming is immersed in absolute ethyl alcohol, leave standstill and after 12 hours, take out vacuumize ventilation in 4 hours, be met the composite electrolyte membrane of production.
Under high-power microscope, observe the micro-nano structure of its formation; It is weighed, film is placed in electrolyte, to activate 2 hours and take out dabs the unnecessary electrolyte calculating pick up of weighing; Become battery finished product to carry out performance test take composite diaphragm as Raw material processing.Relevant data is in table 1.
Table 1
Claims (3)
1. a preparation method for composite electrolyte membrane, the steps include:
(1) polyethylene barrier film is soaked three minutes in chromium oxidation solution, then use deionized water rinsing, dry for standby;
(2) mass ratio 1%-35% polymer is dissolved in to mass ratio 30%-98% organic solvent and stirs into gel solution;
(3) mass ratio 1%-35% ceramic particle is added in gel solution and stirs 3-5 hour, make the dispersed formation coating solution of particulate oxide thing;
(4) dipping for coating solution, the methods such as coating are evenly coated on treated ethene barrier film, and ventilation normal temperature or heating make organic solvent volatilization, composite membrane basic forming;
(5) composite membrane of basic forming is immersed in absolute ethyl alcohol, leaves standstill and take out vacuumize 4 hours after 12 hours, be met the composite electrolyte membrane of production.
2. the preparation method of composite electrolyte membrane according to claim 1, is characterized in that: described polymer is Kynoar, organic solvent is N-methyl 2-pyrrolidone N-solution.
3. the preparation method of composite electrolyte membrane according to claim 1, is characterized in that: described ceramic particle is alumina in Nano level, a kind of or their mixtures among zirconia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310754555.0A CN103779603A (en) | 2013-12-25 | 2013-12-25 | Preparation method of composite electrolyte film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310754555.0A CN103779603A (en) | 2013-12-25 | 2013-12-25 | Preparation method of composite electrolyte film |
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| CN103779603A true CN103779603A (en) | 2014-05-07 |
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| CN201310754555.0A Pending CN103779603A (en) | 2013-12-25 | 2013-12-25 | Preparation method of composite electrolyte film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016201757A1 (en) * | 2015-06-19 | 2016-12-22 | 深圳市星源材质科技股份有限公司 | High dielectric constant nano-composite coating separator and manufacturing method thereof |
| CN110212141A (en) * | 2019-06-18 | 2019-09-06 | 林雨露 | It is a kind of based on the lithium battery of polyethene microporous membrane new types of diaphragm material |
| CN112670662A (en) * | 2020-12-02 | 2021-04-16 | 乐凯胶片股份有限公司 | Method for coating ceramic particles with polymer and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101552359A (en) * | 2009-05-12 | 2009-10-07 | 湖南大学 | Micro-nano porous structure polymer electrolyte membrane used for lithium ion battery and method of producing the same |
| CN101621134A (en) * | 2009-06-23 | 2010-01-06 | 华南师范大学 | Gel polymer lithium ion battery electrolyte, preparation method and application thereof |
| CN101872853A (en) * | 2010-04-21 | 2010-10-27 | 东莞新能源电子科技有限公司 | Polymer lithium ion secondary battery and isolating membrane thereof |
| CN102867931A (en) * | 2012-10-11 | 2013-01-09 | 山东天阳新能源有限公司 | Separation membrane for gel-state polymer lithium-ion battery |
| CN103296239A (en) * | 2012-02-29 | 2013-09-11 | 第一毛织株式会社 | Separator including density-controlled coating layer and battery including the same |
| CN103400959A (en) * | 2013-08-19 | 2013-11-20 | 天津力神特种电源科技有限公司 | Diaphragm for lithium ion battery, production method thereof, and battery core |
-
2013
- 2013-12-25 CN CN201310754555.0A patent/CN103779603A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101552359A (en) * | 2009-05-12 | 2009-10-07 | 湖南大学 | Micro-nano porous structure polymer electrolyte membrane used for lithium ion battery and method of producing the same |
| CN101621134A (en) * | 2009-06-23 | 2010-01-06 | 华南师范大学 | Gel polymer lithium ion battery electrolyte, preparation method and application thereof |
| CN101872853A (en) * | 2010-04-21 | 2010-10-27 | 东莞新能源电子科技有限公司 | Polymer lithium ion secondary battery and isolating membrane thereof |
| CN103296239A (en) * | 2012-02-29 | 2013-09-11 | 第一毛织株式会社 | Separator including density-controlled coating layer and battery including the same |
| CN102867931A (en) * | 2012-10-11 | 2013-01-09 | 山东天阳新能源有限公司 | Separation membrane for gel-state polymer lithium-ion battery |
| CN103400959A (en) * | 2013-08-19 | 2013-11-20 | 天津力神特种电源科技有限公司 | Diaphragm for lithium ion battery, production method thereof, and battery core |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016201757A1 (en) * | 2015-06-19 | 2016-12-22 | 深圳市星源材质科技股份有限公司 | High dielectric constant nano-composite coating separator and manufacturing method thereof |
| CN110212141A (en) * | 2019-06-18 | 2019-09-06 | 林雨露 | It is a kind of based on the lithium battery of polyethene microporous membrane new types of diaphragm material |
| CN112670662A (en) * | 2020-12-02 | 2021-04-16 | 乐凯胶片股份有限公司 | Method for coating ceramic particles with polymer and application thereof |
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Application publication date: 20140507 |