CN108598339A - A kind of smart polymer lithium battery diaphragm - Google Patents
A kind of smart polymer lithium battery diaphragm Download PDFInfo
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- CN108598339A CN108598339A CN201810305626.1A CN201810305626A CN108598339A CN 108598339 A CN108598339 A CN 108598339A CN 201810305626 A CN201810305626 A CN 201810305626A CN 108598339 A CN108598339 A CN 108598339A
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- Prior art keywords
- lithium battery
- battery diaphragm
- polymer lithium
- smart polymer
- diaphragm
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- 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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- 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
-
- 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
- H01M50/411—Organic material
-
- 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
- H01M50/431—Inorganic material
-
- 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 provides a kind of smart polymer lithium battery diaphragm, including substrate layer and polymeric layer, the polymeric layer are located on two surfaces of the substrate layer, and the substrate layer is porous copper foil, and the polymeric layer is fluoropolymer particles layer.The present invention also provides the preparation methods of the smart polymer lithium battery diaphragm.Smart polymer lithium battery diaphragm provided by the invention not only has many advantages, such as that punctured resistance is high, imbibition lock liquid energy power is strong, can also prejudge the growing state of dendrite in advance, dangerous battery is detected and is investigated, provide safeguard for the security performance of lithium battery.
Description
Technical field
The invention belongs to lithium battery diaphragm technical fields, and in particular to a kind of intelligent lithium ion battery diaphragm and its preparation
Method.
Background technology
Lithium battery because high with operating voltage, energy density is big, memory-less effect, have extended cycle life it is low with self discharge etc. excellent
Point is currently widely used for the fields such as electronic equipment mobile power, and great expectations is also sent in new-energy automobile field.Country formulates
's《Energy saving and new-energy automobile industrial development planning》, the fast development even more for lithium ion battery and associated materials plays by force
Big impetus.
In the structure of lithium battery, diaphragm is one of the interior layer assembly of key, and playing prevents anode direct with cathode
The effect of short circuit occurs for contact, is the key component for influencing battery safety.Since new-energy automobile power battery is frequent
Need powerful carry out charge and discharge, lithium metal inevitably forms dendrite in anode, Li dendrite can penetrate polyolefin every
Film causes short circuit, even burns so as to cause battery-heating.Therefore, power battery carries the punctured resistance of used diaphragm
Higher requirement is gone out.
In order to improve the punctured resistance of the security performance of lithium battery, especially lithium battery diaphragm, method at this stage is removed
Other than the thickness of diaphragm is improved, one layer of ceramic particle mainly is coated in membrane surface, to play the role of stopping dendrite.
As Chinese patent CN106684292A discloses a kind of high performance ion conductor Ceramic Composite diaphragm, including organic polymer layers
With the ion conductor ceramic fiber layer for being bonded in the organic polymer layer surface, the ion conductor ceramic fiber layer is by ion
Conductive ceramic fiber is constituted, and composite diaphragm can be improved while enhancing the heat resistanceheat resistant performance and punctured resistance of composite diaphragm
Lithium ion conductivity.But ceramic coating is very limited to the barrier effect of dendrite, the above method can not completely solve every
The problem of film is punctured by dendrite.In recent years, various safety accidents related with battery or again and again appearance.
Therefore, it is necessary to develop a kind of diaphragm of punctured resistance bigger.
Invention content
The purpose of the present invention is low primarily directed to the above-mentioned punctured resistance of lithium battery diaphragm in the prior art, safety is poor etc.
The problem of aspect, provides a kind of smart polymer lithium battery diaphragm, and on the one hand the diaphragm has punctured resistance height, imbibition
The advantages that liquid energy power is strong is locked, on the other hand, the diaphragm can prejudge the growing state of dendrite, be examined to dangerous battery in advance
It surveys and investigates, provide safeguard for the security performance of lithium battery.
In order to achieve the above objectives, the technical solution adopted by the present invention is as follows：
On the one hand, the present invention provides a kind of smart polymer lithium battery diaphragm comprising substrate layer and polymeric layer, institute
It states polymeric layer to be located on two surfaces of the substrate layer, the substrate layer is porous copper foil, and the polymeric layer is fluorine-containing
Polymer particles layers.
Further, the thickness of the porous copper foil is 10-20 μm.
Further, the porosity of the porous copper foil is 40-90%.
Further, the grain size of the fluoropolymer particles is 0.1-0.8 μm.
Further, the fluoropolymer in the fluoropolymer particles is Kynoar (PVDF), polyvinylidene fluoride
One or both of alkene-hexafluoropropene (PVDF-HFP).
On the other hand, the present invention also provides the preparation methods of above-mentioned smart polymer lithium battery diaphragm, including：
S11：It is prepared by coating liquid：In parts by weight, by 10~30 parts of fluoropolymer resins, 1~5 part of binder and 0.1~1 part
Dispersant is added in 70~90 parts of solvents, and heating stirring dispersion obtains coating liquid through deaeration；
S12：It is prepared by diaphragm：Above-mentioned coating liquid is coated on to the two sides of porous copper foil base material through extrusion coated method, it is dry, it obtains
To separator product.
Further, fluoropolymer resin described in step S11 is in Kynoar, Kynoar-hexafluoropropene
It is one or two kinds of.
Further, binder described in step S11 is one kind in carboxymethyl cellulose, butadiene-styrene latex, polyvinyl alcohol
Or more than one.
It is further preferred that binder described in step S11 is the mixture of carboxymethyl cellulose and butadiene-styrene latex, it is described
The mass ratio of carboxymethyl cellulose and butadiene-styrene latex is 1:1.
Further, dispersant described in step S11 is cetyl trimethylammonium bromide, octadecyl trimethyl chlorination
One or more in ammonium, ammonium lauryl sulfate, alkylnaphthalene sulfonate formaldehyde condensation products.
It is further preferred that dispersant described in step S11 is alkylnaphthalene sulfonate formaldehyde condensation products.
Further, solvent described in step S11 is the one or more in deionized water, ethyl alcohol, n-butanol.
Further, the grain size of fluoropolymer resin described in step S11 is 0.1-0.8 μm.
Further, the wet-film thickness that the two sides of porous copper foil base material is coated on described in step S12 is respectively 20-60 μ
m。
Further, drying temperature described in step S12 is 50-80 DEG C, drying time 1-12h.
Unless explicitly stated otherwise in contrast, otherwise, all ranges that the present invention quotes include end value.For example, " 10-30
Part fluoropolymer resin " indicates that the value range of polymer resin content is 10 parts≤fluorine resin≤30 part.
Terminology used in the present invention "one" or "an" describes element and component described herein.It does so only
It is for convenience, and to provide general meaning to the scope of the present invention.This description should be read to include one or extremely
It is one few, and the odd number also includes plural number, is anticipated unless significantly separately referring to him.
Number in the present invention is approximation, no matter whether uses the wordings such as " about " or " about ".The numerical value of number has
It is possible that the differences such as 1%, 2%, 5%, 7%, 8%, 10%.It is any to have whenever disclosing a number with N values
The number of N+/- 1%, N+/- 2%, N+/- 3%, N+/- 5%, N+/- 7%, N+/- 8% or the values of N+/- 10% can be by clearly public
It opens, wherein " +/- " refers to adding deduct, and the range between N-10% to N+10% is also disclosed.
Unless otherwise defined, the otherwise meaning of all scientific and technical terminologies used herein and common skill of the art
As art personnel are generally understood.Although similar or equivalent method and material also can be used with approach described herein and material
In the implementation or test of embodiment of the present invention, but suitable method and material is described below.What is be mentioned above is all
Publication, patent application, patent and other bibliography are incorporated herein in a manner of being cited in full text, and remove non-quoted physical segment
It falls.If conflict occurs, it is subject to this specification and its included definition.In addition, material, method and embodiment are only illustrative
, it is no intended to it is limited.
The beneficial effects of the present invention are：
(1) smart polymer lithium battery diaphragm provided by the invention uses porous copper foil for base material, can effectively hinder
The growth for keeping off dendrite, improves the anti-puncture intensity of diaphragm, enhances the security performance of lithium battery；
(2) smart polymer lithium battery diaphragm provided by the invention is coated with poly- inclined fluorine on the two sides of porous copper foil base material
Ethylene and its copolymer pellet, the particle can form polymer gel in lithium battery with Electolyte-absorptive, on the one hand can be with
The imbibition liquid-keeping property of membrane for polymer is improved, on the other hand improving ionic conductivity can also lock when lithium battery is punctured
Firmly electrolyte does not flow out, and enhances the security performance of lithium battery；
(3) since there is porous copper foil electric action can form electricity when dendrite punctures the polymeric layer with cathode contact
Circuit, the growing state of dendrite can be prejudged using this principle in advance, and dangerous battery is detected and is investigated, and be the peace of lithium battery
Full performance provides safeguard.
Description of the drawings
Fig. 1：Smart polymer lithium battery diaphragm provided by the invention.
Wherein：1, substrate layer；2, polymeric layer.
Specific implementation mode
As described below is the preferred embodiment of the present invention, and what the present invention was protected is not limited to following preferred implementation side
Formula.It should be pointed out that for those skilled in the art on the basis of this innovation and creation conceive, several deformations for making with
It improves, belongs to protection scope of the present invention, in order to further describe the present invention, illustrate with reference to specific embodiment.
Embodiment 1
(1) in parts by weight, by 30 parts of Kynoar, 2 parts of carboxymethyl celluloses, 2 parts of butadiene-styrene latexes and 0.2 part of alkyl
Naphthalenesulfonate formaldehyde condensation compound is added in 70 parts of deionized waters, and heating stirring dispersion, deaeration obtains coating liquid；
(2) by above-mentioned coating liquid by extrusion coated on the two sides of porous copper foil base material, control coating thickness is 40 μm, is done
Dry temperature is 70 DEG C, and drying time 4h obtains separator product.
2 performance test of embodiment and evaluation
The separator product that embodiment 1 is obtained and commercially available diaphragm commodity Celgard2325 carry out following performance test：
1, membrane thicknesses are tested：Calibrator is divided directly to measure using hand formula digital display thousand, 0~1mm of measurement range, accuracy≤
0.001mm.Test result is shown in Table 1.
2, tensile strength is tested：It is tested in omnipotent mechanical test testing machine, standard uses《GB/T1040.32-
The experiment of 2006 plastic tensile performances》.Test result is shown in Table 1.
3, puncture strength is tested：Testing standard is《The general then 6.5.5 of GB/T 21302-2007 composite packing films, bag》,
Using the needle of a not no a diameter of 1mm for sharp edge, cyclic annular fixation is stabbed with 3m/min speed on puncture strength tester
Film, record puncture the required maximum, force of film.Test result is shown in Table 1.
4, porosity test：Diaphragm is impregnated into 2h in n-butanol, the positive fourth of membrane surface absorption is blotted in taking-up with filter paper
Alcohol, with electronic balance weighing diaphragm impregnate before and after n-butanol of poor quality (Δ m), porosity (P) are calculated by following formula
It arrives：Porosity P=Δs m/ (ρ × V), wherein ρ is the density of n-butanol, and V is the volume of diaphragm.Test result is shown in Table 1.
5, imbibition rate is tested：It is that m films are immersed in LiPF by quality6/ EC/DMC/DEC (EC/DMC/DEC=1/1/1, quality
Than) 2h in electrolyte solution, the electrolyte of membrane surface is blotted after taking-up with filter paper, nanometer is calculated with electronic balance weighing
Tunica fibrosa impregnate before and after electrolyte solution of poor quality (Δ m), imbibition rate (K) are calculated by following formula：K=(Δ m/
M) × 100%, wherein m is the quality before diaphragm impregnates.Whole operation process is completed in vacuum glove box.Test result is shown in
Table 1.
6, lock liquid rate test：It is that m films are immersed in 2h in electrolyte solution by quality, film surface is blotted with filter paper after taking-up
It is placed in 30 DEG C of baking oven dry 4h after electrolyte, then obtains m2 with scales/electronic balance weighing, then diaphragm is placed on 100 DEG C
Dry 4h, then obtains m3 with scales/electronic balance weighing in baking oven.Lock liquid rate (H) is calculated by following formula：H=((m3-
M2)/m) × 100%.Test result is shown in Table 1.
7, thermal contraction test：The circular sample for taking an a diameter of 18mm calculates the area S1 of sample；It is placed in vacuum drying chamber
In 200 DEG C heating 12h；Sample is taken out, the area S2 after sample heating is calculated；Percent thermal shrinkage (S) is calculated by following formula
It arrives：S=((S1-S2)/S1) × 100%.It the results are shown in Table 1.
8, dendritic growth detects：It, then will be in red gauge outfit and diaphragm by universal meter switch rotary to DC voltage shelves
Between porous copper foil contact and fix, then use black gauge outfit pierce through diaphragm, see whether to form current path, the results are shown in Table 1.
The property test result of 1 separator product of table
By the test result of table 1 it is found that the puncture for the smart polymer lithium battery diaphragm that the embodiment of the present invention 1 provides is strong
Degree is 1.5 times or more of commercially available diaphragm commodity Celgard2325, and imbibition liquid-keeping property is relatively strong, can also form electrical circuit, examines
The presence of measuring stick crystalline substance provides safeguard for the security performance of lithium battery, has preferable market application prospect.
Claims (10)
1. a kind of smart polymer lithium battery diaphragm, including substrate layer and polymeric layer, the polymeric layer is located at the base
On two surfaces of material layer, which is characterized in that the substrate layer is porous copper foil, and the polymeric layer is fluoropolymer particles
Layer.
2. smart polymer lithium battery diaphragm as described in claim 1, which is characterized in that the thickness of the porous copper foil is
10-20μm。
3. smart polymer lithium battery diaphragm as described in claim 1, which is characterized in that the porosity of the porous copper foil
For 40-90%.
4. smart polymer lithium battery diaphragm as described in claim 1, which is characterized in that the fluoropolymer particles
Grain size is 0.1-0.8 μm.
5. smart polymer lithium battery diaphragm as described in claim 1, which is characterized in that in the fluoropolymer particles
Fluoropolymer be Kynoar, one or both of Kynoar-hexafluoropropene.
6. a kind of preparation method of claim 1-5 any one of them smart polymer lithium battery diaphragm, which is characterized in that
Including：
S11：It is prepared by coating liquid：In parts by weight, by 10~30 parts of fluoropolymer resins, 1~5 part of binder and 0.1~1 part of dispersion
Agent is added in 70~90 parts of solvents, and heating stirring dispersion obtains coating liquid through deaeration；
S12：It is prepared by diaphragm：Above-mentioned coating liquid is coated on to the two sides of porous copper foil base material through extrusion coated method, it is dry, obtain every
Film product.
7. the preparation method of smart polymer lithium battery diaphragm as claimed in claim 6, which is characterized in that in step S11
The binder is the one or more in carboxymethyl cellulose, butadiene-styrene latex, polyvinyl alcohol.
8. the preparation method of smart polymer lithium battery diaphragm as claimed in claim 6, which is characterized in that in step S11
The dispersant is cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride, ammonium lauryl sulfate, alkylnaphthalene sulphur
One or more in hydrochlorate formaldehyde condensation products.
9. the preparation method of smart polymer lithium battery diaphragm as claimed in claim 6, which is characterized in that in step S11
The solvent is the one or more in deionized water, ethyl alcohol and n-butanol.
10. the preparation method of smart polymer lithium battery diaphragm as claimed in claim 6, which is characterized in that in step S12
The wet-film thickness on the two sides for being coated on porous copper foil base material is respectively 20-60 μm.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2017111356070 | 2017-11-16 | ||
| CN201711135607 | 2017-11-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108598339A true CN108598339A (en) | 2018-09-28 |
Family
ID=63621108
Family Applications (1)
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|---|---|---|---|
| CN201810305626.1A Pending CN108598339A (en) | 2017-11-16 | 2018-04-08 | A kind of smart polymer lithium battery diaphragm |
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2018
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Application publication date: 20180928 |