CN106784557A - A kind of composite diaphragm for lithium battery - Google Patents
A kind of composite diaphragm for lithium battery Download PDFInfo
- Publication number
- CN106784557A CN106784557A CN201710043795.8A CN201710043795A CN106784557A CN 106784557 A CN106784557 A CN 106784557A CN 201710043795 A CN201710043795 A CN 201710043795A CN 106784557 A CN106784557 A CN 106784557A
- Authority
- CN
- China
- Prior art keywords
- barrier film
- diamond alkene
- nanometer diamond
- lithium battery
- composite diaphragm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- 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
-
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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
Abstract
The present invention discloses a kind of composite diaphragm for lithium battery, including barrier film base material and the polymer solution for being coated on barrier film base material surface, and the polymer solution is made up of following methods：In at 20 30 DEG C, PVDF HFP micro mists and polyoxyethylene polyoxypropylene polyoxyethylene copolymer F127 are dissolved in organic solvent, nanometer diamond alkene, mixing are added after stirring；The weight ratio of the PVDF HFP micro mists, polyoxyethylene polyoxypropylene polyoxyethylene copolymer F127 and organic solvent three is（0.5‑1）:0.1:（9‑10）, the addition of the nanometer diamond alkene is 2% the 10% of PVDF HFP micropowder weights.Its preparation method is provided simultaneously.The present invention carries out surface to nanometer diamond alkene and is modified by silane coupler, strengthen the compatibility of its dispersiveness and polymer substrate, soilless sticking phenomenon, with good imbibition and liquid-keeping property, pick up, percent thermal shrinkage, raising barrier film ionic conductivity and the charge-discharge performance of barrier film are improve.
Description
Technical field
The present invention relates to lithium battery manufacture field, and in particular to a kind of composite diaphragm for lithium battery.
Background technology
At present, lithium ion battery is applied widely in daily life, and barrier film is the important composition of lithium ion battery
One of part, because barrier film is located between positive pole and negative pole, its Main Function is to separate both positive and negative polarity active material, is prevented
Only the two poles of the earth short circuit because of contact, while can pass through electrolyte ion, therefore, have vital to the performance of battery
Influence.
Lithium ion battery separator is broadly divided into polyolefin film and polymer matrix gel electrolyte membrane, and polyolefin film absorbency is poor
And ionic conductivity is low；Polymer matrix gel electrolyte membrane fusing point and mechanical strength be not high, when using, easily deforms upon or dendrite
Pierce through, so as to cause battery short circuit.In recent years, people have studied polyacrylonitrile (PAN), polymethyl methacrylate again
(PMMA) and the polymer such as polyethylene glycol oxide (PEO) is applied to battery diaphragm material, but there is room-temperature ion conductance again in them
The deficiencies such as rate is relatively low, bad mechanical strength.
The content of the invention
Present invention aim at providing, a kind of ionic conductivity is high and the good composite diaphragm for lithium battery of charge-discharge performance.
Based on above-mentioned purpose, the present invention takes following technical scheme：
A kind of composite diaphragm for lithium battery, including barrier film base material and the polymer solution for being coated on barrier film base material surface, the polymerization
Thing solution is made up of following methods：In at 20-30 DEG C, PVDF-HFP micro mists and polyoxyethylene-poly-oxypropylene polyoxyethylene are total to
Polymers F127 is dissolved in organic solvent, and nanometer diamond alkene, mixing are added after stirring；The PVDF-HFP micro mists, polyoxy second
Alkene-polyoxypropylene polyoxyethylene copolymer F127 is with the weight ratio of organic solvent three（0.5-1）:0.1:（9-10）, it is described
The addition of nanometer diamond alkene is the 2%-10% of PVDF-HFP micropowder weights.
The surface-modified treatment of nanometer diamond alkene, concretely comprises the following steps：In at 20-30 DEG C, by 10-15g nanometer diamonds
Alkene is added in 150-200mL absolute ethyl alcohols, ultrasonic disperse 30-40min, then adds 10-15g Silane coupling reagent KH-570s, in
N2Under protection, after ultrasonic disperse 30-40min, 120-130 DEG C, isothermal reaction 4-5h, successively using absolute ethyl alcohol and first are warming up to
Benzene washing, filtering, vacuum drying.
The organic solvent is acetone and N,N-dimethylformamide（DMF）Mixture, acetone and N, N- dimethyl methyl
The weight ratio of acid amides is（8-9）:（1-2）.
The barrier film base material is polypropylene（PP）Non-woven fabrics.
The barrier film base material upper and lower surface is coated with polymer solution.
Nanometer diamond alkene of the invention is disclosed in 201510749250X, and it is lamellar mono-crystalline structures, same lamella
It is sp between carbon atom3Orbital hybridization carbon is bonded and connects, and is sp between carbon atom between layers2Hydridization carbon is bonded and connects；The nanometer
The average grain diameter of diamond alkene is R, 20 nm≤R≤500nm；The C content of the nanometer diamond alkene is 99~100%.
Compared with prior art, the invention has the advantages that：
Nanometer diamond alkene is a kind of good inorganic material of chemical stability, can improve mechanics, calorifics and the electricity of polymeric material
Performance is learned, the present invention carries out surface to nanometer diamond alkene and is modified by silane coupler, strengthens its dispersiveness and polymer substrate
Compatibility, soilless sticking phenomenon, with good imbibition and liquid-keeping property, improves pick up, percent thermal shrinkage, the raising of barrier film
Barrier film ionic conductivity and charge-discharge performance.
Brief description of the drawings
Fig. 1 be nanometer diamond alkene surface before modified after thermogravimetric curve figure；
Fig. 2 is charge and discharge cycles curve map.
Specific embodiment
Embodiment 1
A kind of composite diaphragm for lithium battery, including barrier film base material is molten with the polymer for being coated on barrier film base material upper and lower surface
Liquid, the barrier film base material is polypropylene non-woven fabric, and the polymer solution is made up of following methods：In at 20 DEG C, by PVDF-
HFP micro mists and polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer F127 are dissolved in organic solvent, nanometer is added after stirring and is bored
Stone alkene, mixing；The PVDF-HFP micro mists, polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer F127 and organic solvent
The weight ratio of three is 1:0.1:10, the addition of the nanometer diamond alkene is the 6% of PVDF-HFP micropowder weights, described organic
Solvent is acetone and N,N-dimethylformamide（DMF）Mixture, the weight ratio of acetone and DMF is 9:
1。
The surface-modified treatment of nanometer diamond alkene, concretely comprises the following steps：In at 20 DEG C, 15g nanometer diamonds alkene is added
In 200ml absolute ethyl alcohols, then ultrasonic disperse 30min adds 10g Silane coupling reagent KH-570s, in N2Under protection, ultrasonic disperse
After 30min, 120 DEG C are warming up to, isothermal reaction 5h, successively using vacuum drying at absolute ethyl alcohol and toluene washing, filtering, 20 DEG C
, drying time is 24h.
Embodiment 2
A kind of composite diaphragm for lithium battery, including barrier film base material is molten with the polymer for being coated on barrier film base material upper and lower surface
Liquid, the barrier film base material is polypropylene non-woven fabric, and the polymer solution is made up of following methods：In at 30 DEG C, by PVDF-
HFP micro mists and polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer F127 are dissolved in organic solvent, nanometer is added after stirring and is bored
Stone alkene, mixing；The PVDF-HFP micro mists, polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer F127 and organic solvent
The weight ratio of three is 0.5:0.1:9, the addition of the nanometer diamond alkene is the 8% of PVDF-HFP micropowder weights, described to have
Machine solvent is acetone and N,N-dimethylformamide（DMF）Mixture, the weight ratio of acetone and DMF is
8:2。
The surface-modified treatment of nanometer diamond alkene, concretely comprises the following steps：In at 30 DEG C, 10g nanometer diamonds alkene is added
In 150ml absolute ethyl alcohols, then ultrasonic disperse 40min adds 15g Silane coupling reagent KH-570s, in N2Under protection, ultrasonic disperse
After 40min, 130 DEG C are warming up to, isothermal reaction 5h, successively using vacuum drying at absolute ethyl alcohol and toluene washing, filtering, 30 DEG C
, drying time is 24h.
Embodiment 3
Difference with embodiment 1 is：The addition of nanometer diamond alkene is the 2% of PVDF-HFP micropowder weights, and other are with real
Apply example 1.
Embodiment 4
Difference with embodiment 2 is：The addition of nanometer diamond alkene is the 10% of PVDF-HFP micropowder weights, and other are same
Embodiment 1.
Embodiment 5
Difference with embodiment 2 is：The addition of nanometer diamond alkene is the 4% of PVDF-HFP micropowder weights, and other are with real
Apply example 2.
The preparation method of embodiment 1-5：Polymer solution is evenly applied to the upper and lower surface of PP non-woven fabrics, in
At 60 DEG C, 8h is vacuum dried, obtains final product composite diaphragm for lithium battery of the invention.
The nanometer diamond alkene surface of embodiment 6 before modified after thermogravimetic analysis (TGA)
To the nanometer diamond alkene of long time without surface modification（Labeled as a）Thermal weight loss point is carried out with surface-modified nanometer diamond alkene
Analysis, the addition of nanometer diamond alkene is 2%, 6% and 10%, is labeled as b, c, d successively respectively, and the addition of nanometer diamond alkene is to receive
The quality of rice diamond alkene and the mass ratio of Silane coupling reagent KH-570, draw thermogravimetric curve as shown in Figure 1.
As shown in Figure 1, the nanometer diamond alkene of long time without surface modification 800 DEG C fugitive constituent be 5.01%, it is surface-modified
Nanometer diamond alkene is respectively 10.71%, 11.32% and 12.51% in 800 DEG C of fugitive constituents, therefore can learn, long time without surface modification
The quality of nanometer diamond alkene loss should be the quality of its surface-bonded water, and be grafted on the silane coupler on nanometer diamond alkene surface
The mass ratio of KH-570 should be respectively 5.70%, 6.31%, 7.50%.This also illustrates that Silane coupling reagent KH-570 is successfully grafted
To the surface of nanometer diamond alkene.
Influence of the nanometer diamond alkene consumption of embodiment 7 to composite diaphragm pick up
Addition to not surface-modified and surface-modified nanometer diamond alkene is variable, and addition is respectively PVDF-HFP
0,2%, 4%, 6%, 8%, the 10% of micropowder weight, other conditions carry out pick up survey with embodiment 1 to made composite diaphragm
Examination, test result is as shown in table 1.Current pick up is measured using imbibition priting, and normative reference is《SJ-247-10171.7
The measure of barrier film alkali absorbing rate》, the method is alkaline battery standard, and the solvent for using is alkali lye, for measuring during lithium ion battery
Electrolyte should be replaced with, due to electrolyte volatilization the problems such as it is most of using to the preferable organic solvent of barrier film wellability at present
It is measured, conventional solvent is hexadecane, n-butanol, hexamethylene etc..
As shown in Table 1, the pick up of the composite diaphragm containing nanometer diamond alkene is significantly greater than the mark of commercial barrier film Celgard 2400
It is accurate.With the increase of nanometer diamond alkene addition, the porosity of barrier film increases such that it is able to improve guarantor's liquid measure and the imbibition of barrier film
Rate；But when nanometer diamond alkene addition is more than 6%, pick up has downward trend, and reason may is that, the addition of nanometer diamond alkene
Amount increases, and slight agglomeration occurs in polymer solution, so as to cause barrier film pick up to decline.And nanometer diamond alkene is added
Amount is identical, and the pick up of the surface-modified made barrier film of nanometer diamond alkene is significantly greater than the barrier film of long time without surface modification, former
Because being that to carry out surface to nanometer diamond alkene modified, its dispersiveness is improved, so as to increased the pick up of barrier film.
The performance test of embodiment 8
The physical property of 8.1 composite diaphragms
Nanometer diamond alkene, PP non-woven fabrics, the non-modified and modified made composite diaphragm of nanometer diamond alkene will be free of（Other
Condition is with embodiment 1）, test group 1,2,3,4 is respectively labeled as, the tensile strength and shrinkage factor to the barrier film of test group 1-4 are entered
Row test, test result is as shown in table 2.The tensile strength project accepted standard is《GB/T 1040.3-2006 plastic tensiles
The test of performance》；The percent thermal shrinkage of barrier film refers to the size changing rate of barrier film before and after barrier film heating, and Primary Reference standard has《GB/
T 12027-2004 plastic films and thin slice-heated dimensions rate of change test method》.
As shown in Table 2, the barrier film tensile strength of test group 1 only has 1.6MPa, and the tensile strength of test group 2 is 2.8 MPa, is relatively tried
The barrier film for testing group 1 improves 75%, and the tensile strength of the barrier film of test group 3 and 4 is more slightly worse than test group 2, but its percent thermal shrinkage is obvious
Reduce, i.e., hot property is significantly improved, and reason is that the thermal deformation coefficient of nanometer diamond alkene is small, being added in barrier film can be with
Play a part of to reduce percent thermal shrinkage, by contrast, shrinkage factors of the commercial barrier film Celgard 2400 at 150 DEG C is up to
50.2%, hot property is poor.
The ionic conductivity of 8.2 composite diaphragms
Nanometer diamond alkene will be not added with, composite diaphragm made by non-modified nanometer diamond alkene is added（Other conditions are with real
Apply example 1）With the composite diaphragm of embodiment 1, test group 1,2,3 is respectively labeled as, to the barrier film and Celgard of test group 1-3
The ionic conductivity of 2400 barrier films is tested, and test result is as shown in table 3.Electrical conductivity is the ability that object conducts electric current, with
Resistivity is reciprocal each other.The measurement apparatus of ionic conductivity can refer to the measurement apparatus of closed pore temperature, and method uses AC impedance
Method, in order to eliminate the influence of electrode resistance and contact resistance etc., the repeatedly resistance value under test laminated diaphragm, an and test
Result carries out linear fit, and slope value is the membrane electrical resistance value.
As shown in Table 3, after addition nanometer diamond alkene, the ionic conductivity of barrier film is improved, because the pore structure of barrier film
Influenceed by nanometer diamond alkene, aperture becomes than larger, and barrier film is smaller to the resistance that lithium ion is moved, so ionic conductivity is carried
Height, and nanometer diamond alkene is dispersed more preferable after modified, dispersed drop of the modified Nano diamond alkene in PVDF-HFP films
Low its inhibition to ion, and then improve the ionic conductivity of composite membrane.
The chemical property of 8.3 composite diaphragms
Composite diaphragm, the barrier films of Celgard 2400 to embodiment 1, add compound made by non-modified nanometer diamond alkene
Barrier film（Other conditions are with embodiment 1）The lithium battery being assembled into, is respectively labeled as a, b, c, carries out charge and discharge cycles experiment, experiment
Carried out under the conditions of voltage 2.5V-4.2V, multiplying power 0.2C, circulated 100 times, draw charge and discharge cycles curve, as shown in Figure 2.
As shown in Figure 2, specific discharge capacity is higher at the beginning for the lithium battery of the commercial assemblings of barrier film Celgard 2400, but is following
Ring is decreased obviously for 70 times later, and uses the lithium battery of the composite diaphragm assembling of addition nanometer diamond alkene, charge-discharge cycle ratio
Relatively stablize, especially add the lithium battery of the composite diaphragm assembling of modified Nano diamond alkene, specific discharge capacity obtains larger carrying
Height, after cycle charge-discharge 100 times, specific discharge capacity is still maintained at 145.5mAh/g or so, by barrier film group of the invention
The chemical property of the lithium battery dressed up is excellent.
Claims (5)
1. a kind of composite diaphragm for lithium battery, it is characterised in that including barrier film base material and the polymer for being coated on barrier film base material surface
Solution, the polymer solution is made up of following methods：In at 20-30 DEG C, by PVDF-HFP micro mists and polyoxyethylene-polyoxy third
Alkene-polyoxyethylene copolymer F127 is dissolved in organic solvent, and nanometer diamond alkene, mixing are added after stirring；The PVDF-
The weight ratio of HFP micro mists, polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer F127 and organic solvent three is（0.5-1）:
0.1:（9-10）, the addition of the nanometer diamond alkene is the 2%-10% of PVDF-HFP micropowder weights.
2. composite diaphragm for lithium battery as claimed in claim 1, it is characterised in that the surface-modified place of nanometer diamond alkene
Reason, concretely comprises the following steps：In at 20-30 DEG C, during 10-15g nanometer diamonds alkene added into 150-200mL absolute ethyl alcohols, ultrasonic disperse
30-40min, then adds 10-15g Silane coupling reagent KH-570s, in N2Under protection, after ultrasonic disperse 30-40min, it is warming up to
120-130 DEG C, isothermal reaction 4-5h, successively using absolute ethyl alcohol and toluene washing, filtering, vacuum drying.
3. composite diaphragm for lithium battery as claimed in claim 1, it is characterised in that the organic solvent is acetone and N, N- diformazan
The weight ratio of the mixture of base formamide, acetone and DMF is（8-9）:（1-2）.
4. composite diaphragm for lithium battery as claimed in claim 1, it is characterised in that the barrier film base material is polypropylene non-woven fabric.
5. the composite diaphragm for lithium battery described in claim 1, it is characterised in that the barrier film base material upper and lower surface is applied
It is covered with polymer solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043795.8A CN106784557A (en) | 2017-01-21 | 2017-01-21 | A kind of composite diaphragm for lithium battery |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043795.8A CN106784557A (en) | 2017-01-21 | 2017-01-21 | A kind of composite diaphragm for lithium battery |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108550764A (en) * | 2018-03-16 | 2018-09-18 | 河南力旋科技股份有限公司 | A kind of ultra-fine diamond coated insulation film and the lithium ion battery using this isolation film |
| CN111211277A (en) * | 2020-02-19 | 2020-05-29 | 重庆云天化纽米科技股份有限公司 | Preparation method of PMMA gel coating diaphragm |
| CN113764823A (en) * | 2021-09-17 | 2021-12-07 | 江苏卓高新材料科技有限公司 | High-performance gradient composite gel polymer diaphragm and preparation method thereof |
-
2017
- 2017-01-21 CN CN201710043795.8A patent/CN106784557A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108550764A (en) * | 2018-03-16 | 2018-09-18 | 河南力旋科技股份有限公司 | A kind of ultra-fine diamond coated insulation film and the lithium ion battery using this isolation film |
| CN108550764B (en) * | 2018-03-16 | 2021-06-29 | 河南力旋科技股份有限公司 | Superfine diamond coating isolating membrane and lithium ion battery applying same |
| CN111211277A (en) * | 2020-02-19 | 2020-05-29 | 重庆云天化纽米科技股份有限公司 | Preparation method of PMMA gel coating diaphragm |
| CN113764823A (en) * | 2021-09-17 | 2021-12-07 | 江苏卓高新材料科技有限公司 | High-performance gradient composite gel polymer diaphragm and preparation method thereof |
| CN113764823B (en) * | 2021-09-17 | 2023-06-30 | 江苏卓高新材料科技有限公司 | High-performance gradient composite gel polymer diaphragm and preparation method thereof |
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