CN108134034B - A method of lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism - Google Patents
A method of lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/14—Homopolymers or copolymers of vinyl fluoride
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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
- H01M50/411—Organic material
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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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Abstract
The present invention discloses a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism, it include: that the PVDF-HFP of certain mass is dissolved by heating in the first solvent of certain mass, the PVDF-HFP of certain mass normal-temperature dissolution in the first solvent of certain mass, above-mentioned two parts are added to the second solvent of certain mass after mixing, it is coated on substrate after mixing, just obtains lithium battery diaphragm after dry.PVDF-HFP is added in two portions in the first solvent the present invention, the cross-linked structure with link is formed, the second solvent is added, is partly dissolved link, the part of dissolution chains to form cross-linked structure, and be centered around around link, after dry, the first solvent volatilizees to form main lithium ion transport hole, the volatilization of second solvent, cross-linked structure around link forms hole, is conducive to reinforce the intensity around lithium battery film link, then strengthens the intensity of lithium battery diaphragm.
Description
Technical field
The present invention relates to lithium battery diaphragm technical fields, more particularly to a kind of mixed solvent multistage Volatilization mechanism that is based on to prepare
The method of lithium battery diaphragm.
Background technique
In recent years, as the continuous development of new energy, the demand of lithium battery are also being continuously increased, the entirety of battery is improved
Safety and chemical property are the current emphasis for developing lithium battery.Diaphragm is the important component of lithium battery, affects boundary
Face structure and internal driving, to the thermal stability of battery, cycle performance, high rate performance and safety play vital
Effect.
Phase inversion method is a kind of common method for preparing lithium battery membrane for polymer, its advantage is that simple process and low cost,
Easily operated, film obtained has higher imbibition rate, good conductivity, and can be dissolved in many organic solvents, is considered
It is ideal membrane material, but the disadvantage is that mechanical strength, high rate performance etc. are not so good as common Celgard diaphragm.
Therefore, the prior art is defective, needs to improve.
Summary of the invention
The technical problem to be solved by the present invention is provide it is a kind of based on mixed solvent multistage Volatilization mechanism prepare lithium battery every
The method of film promotes mechanical strength, the high rate performance of the lithium battery diaphragm of phase inversion method preparation.
Technical scheme is as follows: providing and a kind of prepares lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism
Method includes the following steps,
S1: Kynoar-hexafluoropropene (PVDF-HFP) of certain mass is weighed, the first solvent of certain mass is added
In, heating stirring forms the first uniform colloidal solution, the range of the mass ratio of PVDF-HFP and the first solvent are as follows: 0.08-
0.15.PVDF-HFP is dissolved completely in the first solvent in the step, forms a cross-linked structure.
S2: the PVDF-HFP for weighing certain mass is added in the first solvent of certain mass, and stirring at normal temperature is formed uniformly
The suspension is added in the first colloidal solution simultaneously stirring at normal temperature, obtains uniform second colloidal solution, PVDF- by suspension
The range of the mass ratio of HFP and the first solvent are as follows: 0.1-0.6；PVDF-HFP is added in step sl to be added with this step
The range of the mass ratio of PVDF-HFP are as follows: 3.0-4.2.PVDF-HFP in the step is not dissolved completely in stirring at normal temperature
In solvent, form the second colloidal solution after being mixed evenly with the first colloidal solution, second colloidal solution be containing
The cross-linked structure of link, the PVDF-HFP being completely dissolved in step S1 serve as main cross-linked network in the second colloidal solution
Shape structure, the PVDF-HFP not being completely dissolved in this step serve as link in the second colloidal solution.
S3: the second solvent of certain mass being added in the second colloidal solution, stirring at normal temperature, and it is gluey to form uniform third
The range of the mass ratio of solution, second solvent and the second colloidal solution are as follows: 0-0.5.In the step, the second solvent is to second
The PVDF-HFP not being completely dissolved in colloidal solution is partly dissolved, and rear shape is mixed evenly with the second colloidal solution
At third colloidal solution, the third colloidal solution is also the cross-linked structure containing link, and step S1 and step S2 pass through
The PVDF-HFP of first solvent dissolution serves as main cross-linked structure in third colloidal solution, passes through second in step S3
The PVDF-HFP of solvent dissolution serves as secondary cross-linked structure in third colloidal solution, the PVDF-HFP not being completely dissolved
Link is served as in third colloidal solution, and the cross-linked structure master that the PVDF-HFP that the second solvent dissolves in step S3 is formed
It is centered around around link.
S4: obtained uniform third colloidal solution is coated on substrate with coating machine, after dry, obtains different-thickness
Lithium battery diaphragm diaphragm, thickness range are as follows: 10 μm -120 μm.First solvent volatilizees to form main lithium ion transport hole,
The volatilization of second solvent, the cross-linked structure around link form hole, are conducive to reinforce around lithium battery film link
Intensity then strengthens the intensity of lithium battery diaphragm.
Further, in step s3, organic and/or inorganic materials, inorganic material and the second solvent are added in second solvent
The range of mass ratio is 0-0.15, the particle size range of the inorganic material are as follows: 15nm-5000nm, the inorganic material are Al2O3、
SiO2、TiO2One of or at least two mixture.The reunion of the inorganic material can be conducive to the transmission of lithium ion,
Meanwhile inorganic material particles limit the free movement of PVDF-HFP chain, further promote the structural strength of lithium battery diaphragm.
Further, the volatilization intensity of first solvent is greater than the volatilization intensity of the second solvent.First solvent can be prior to
Second solvent vapors away, and the second solvent has part and remains in PVDF-HFP film, can play the role of plasticizer, add
The toughness of strong PVDF-HFP film；Remaining second solvent is conducive to the infiltration of electrolyte simultaneously.
Further, first solvent is acetone, and second solvent is N-Methyl pyrrolidone (NMP), dimethyl
Acetamide (DMAc), dimethylformamide (DMF), dimethyl sulfoxide (DMSO), diethyl acetamide (DEAc), trimethyl phosphate
(TMP), one of triethyl phosphate (TEP), hexamethyl ammonium phosphate (HMPA) and tetramethyl urine (TMU).
Preferably, first solvent is acetone, and the second solvent is NMP.
Further, in step sl, the temperature range of heating is 45 DEG C -55 DEG C, the range of viscosities of the first colloidal solution
Are as follows: 1000cp-5000cp.In step s 2, the temperature range of room temperature is 15 DEG C -30 DEG C, the range of viscosities of the second colloidal solution
Are as follows: 1000cp-4500cp.In step s3, the temperature range of room temperature is 15 DEG C -30 DEG C, the range of viscosities of third colloidal solution
Are as follows: 2000cp-5500cp.In step s 4, the thickness range of the lithium battery diaphragm are as follows: 10 μm -120 μm.
Further, the substrate is the substrate that can be reused, and using reusable substrate, reduction is produced into
This.
Further, the substrate is aluminium foil or copper foil or glass plate.
Using the above scheme, the present invention provides a kind of side that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism
Method forms the cross-linked structure with link, it is molten to be added second by the way that PVDF-HFP to be added in two portions in the first solvent
Agent is partly dissolved link, and the part of dissolution chains to form cross-linked structure, and is centered around around link, after dry, first
Solvent volatilizees to form main lithium ion transport hole, and the second solvent volatilization, the cross-linked structure around link forms hole
Hole is conducive to reinforce the intensity around lithium battery film link, then strengthens the intensity of lithium battery diaphragm.Further, exist
Inorganic material is added in second solvent, the reunion of the inorganic material can be conducive to the transmission of lithium ion, meanwhile, inorganic material
Particle limits the free movement of PVDF-HFP chain, further promotes the structural strength of lithium battery diaphragm.Moreover, the second solvent portion
Divide and remain in PVDF-HFP film, plasticizer can be played the role of, reinforces the toughness of PVDF-HFP film；While remaining second
Solvent is conducive to the infiltration of electrolyte.
Detailed description of the invention
Fig. 1 is flow chart of the invention；
Fig. 2 is 1 gained of 2400 diaphragm of business Celgard, the made PVDF-HFP diaphragm of single solvent acetone and embodiment
The scanning electron microscope (SEM) photograph of PVDF-HFP-NMP diaphragm；
Fig. 3 is obtained by 2400 diaphragm of business Celgard, the made PVDF-HFP diaphragm of single solvent acetone and embodiment 1
The cycle performance of battery that is showed in 1C of PVDF-HFP-NMP diaphragm；
Fig. 4 is PVDF-HFP-Al obtained by embodiment 42O3Diaphragm is in the 1C cycle performance for being and coulombic efficiency；
Fig. 5 is showed by 2400 diaphragm of business Celgard and 1 gained PVDF-HFP-NMP diaphragm of embodiment in 10C
Cycle performance of battery.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Referring to Fig. 1, the present invention provides a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism,
The following steps are included:
S1: weighing the PVDF-HFP of certain mass, be added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.1, and in 45 DEG C of -55 DEG C of heating stirrings of water-bath, form the first uniform colloidal solution, viscosity are as follows: 1500cp.
S2: the PVDF-HFP for weighing certain mass is added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.6, stirring at normal temperature forms uniform suspension, and stirring at normal temperature in the first colloidal solution is then added, and obtains uniform second
Colloidal solution, viscosity are: 2000cp.It is added in PVDF-HFP and this step in step sl and the mass ratio of PVDF-HFP is added
Are as follows: 3.0.
S3: a certain amount of NMP is added in the second colloidal solution, the mass ratio of NMP and the second colloidal solution are as follows: 0.2, after
Continuous stirring, obtains uniform third colloidal solution, viscosity is 2500cp.
S4: obtained uniform third glue coating machine is coated on aluminium foil, after natural air drying, obtains PVDF-
HFP-NMP diaphragm, with a thickness of 25 μm.
Embodiment 2
Referring to Fig. 1, the present invention provides a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism,
The following steps are included:
S1: weighing the PVDF-HFP of certain mass, be added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
It is yes: 0.12, and in 45-55 DEG C of heating stirring of water-bath, the first uniform colloidal solution is formed, viscosity is: 2000cp.
S2: the PVDF-HFP for weighing certain mass is added in the acetone of certain mass, mass ratio are as follows: and 0.4, stirring at normal temperature shape
At uniform suspension, stirring at normal temperature in the first colloidal solution is then added, obtains uniform second colloidal solution, viscosity are as follows:
3000cp.It is added in PVDF-HFP and this step in step sl and the mass ratio of PVDF-HFP is added are as follows: 3.5.
S3: a certain amount of NMP is added in the second colloidal solution, the mass ratio of NMP and solution are as follows: 0.4, continue to stir,
Uniform third colloidal solution is obtained, viscosity is 3500cp.
S4: obtained uniform third glue glue coating machine is coated on aluminium foil, after natural air drying, is obtained
PVDF-HFP-NMP diaphragm, with a thickness of 30 μm.
Embodiment 3
Referring to Fig. 1, the present invention provides a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism,
The following steps are included:
S1: weighing the PVDF-HFP of certain mass, be added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.14, and in 45-55 DEG C of heating stirring of water-bath, form the first uniform colloidal solution, viscosity are as follows: 2200cp；
S2: the PVDF-HFP for weighing certain mass is added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.3, stirring at normal temperature forms uniform suspension, and stirring at normal temperature in the first colloidal solution is then added, and obtains uniform second
Colloidal solution, viscosity are as follows: 3000cp.It is added in PVDF-HFP and this step in step sl and the mass ratio of PVDF-HFP is added
Are as follows: 3.8.
S3: a certain amount of DMF is added in the second colloidal solution, the mass ratio of DMF and the second colloidal solution are as follows: 0.45,
Continue to stir, obtains uniform third colloidal solution, viscosity is: 4800cp.
S4: obtained uniform third colloidal solution coating machine is coated on aluminium foil, after natural air drying, is obtained
PVDF-HFP-NMP diaphragm, with a thickness of 25 μm.
Embodiment 4
Referring to Fig. 1, the present invention provides a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism,
The following steps are included:
S1: weighing the PVDF-HFP of certain mass, be added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.12, and in 45-55 DEG C of heating stirring of water-bath, the first uniform colloidal solution is formed, viscosity is: 2000cp.
S2: the PVDF-HFP for weighing certain mass is added in the acetone of certain mass, the mass ratio of PVDF-HFP and acetone
Are as follows: 0.2, stirring at normal temperature forms uniform suspension, and stirring at normal temperature in the first colloidal solution is then added, and obtains uniform second
Colloidal solution, viscosity are as follows: 3000cp.It is added in PVDF-HFP and this step in step sl and the mass ratio of PVDF-HFP is added
Are as follows: 4.0.
S3: by a certain amount of Al2O3It is added in a certain amount of NMP, Al2O3Mass ratio with NMP is 0.12, stirring at normal temperature,
Uniform suspension is formed, is added in the second colloidal solution, is continued to stir, obtain uniform third colloidal solution, viscosity is:
3200cp；The Al2O3Particle size range are as follows: 18nm-50nm.
S4: obtained uniform third colloidal solution coating machine is coated on aluminium foil, after natural air drying, is obtained
PVDF-HFP-Al2O3Diaphragm, with a thickness of 30 μm.
Gained lithium battery diaphragm assembled battery is tested, uses LiFePO4 as positive electrode, cathode uses lithium piece.
Referring to Fig. 2, (a) in Fig. 2, (b), (c) are respectively that 2400 diaphragm of business Celgard, single solvent acetone are made
The scanning electron microscope (SEM) photograph of 1 gained PVDF-HFP-NMP diaphragm of PVDF-HFP diaphragm and embodiment.As can be seen that mixed solvent institute in figure
The PVDF-HFP-NMP diaphragm micro-hole of system is more, and material is evenly distributed, and is conducive to the imbibition rate and conductivity that improve diaphragm, has
Conducive to the transmission of lithium ion, to improve battery performance.
Referring to Fig. 3, Fig. 3 is 2400 diaphragm of business Celgard, the made PVDF-HFP diaphragm of single solvent acetone and reality
The cycle performance of battery that PVDF-HFP-NMP diaphragm is showed in 1C obtained by example 1 is applied, it can be seen from the figure that embodiment
Cycle performance of battery of the 1 PVDF-HFP-NMP diaphragm obtained in 1C is better than 2400 diaphragm of business Celgard, single
The made PVDF-HFP diaphragm of solvent acetone.
Fig. 3 and Fig. 4 are please referred to, Fig. 4 is PVDF-HFP-Al obtained by embodiment 42O3The cycle performance that diaphragm is in 1C
And coulombic efficiency, it demonstrates on the basis of the method with Fig. 3 comparison, can further be improved by adding other inorganic material
Membrane properties.
Referring to Fig. 5, Fig. 5 is 2400 diaphragm of business Celgard and 1 gained PVDF-HFP-NMP diaphragm of embodiment in 10C
When the cycle performance of battery that is showed.It can be seen from the figure that the PVDF-HFP-NMP diaphragm obtained of embodiment 1 is in 10C
Cycle performance of battery be better than 2400 diaphragm of business Celgard.
In conclusion the present invention provides a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism,
By the way that PVDF-HFP to be added in two portions in the first solvent, the cross-linked structure with link is formed, the second solvent is added, makes
Link is partly dissolved, and the part of dissolution chains to form cross-linked structure, and is centered around around link, after dry, the first solvent
Volatilization forms main lithium ion transport hole, the volatilization of the second solvent, and the cross-linked structure around link forms hole, has
Conducive to the intensity reinforced around lithium battery film link, the intensity of lithium battery diaphragm is then strengthened.Further, molten second
Inorganic material is added in agent, the reunion of the inorganic material can be conducive to the transmission of lithium ion, meanwhile, inorganic material particles limit
The free movement of PVDF-HFP chain has been made, the structural strength of lithium battery diaphragm is further promoted.Moreover, the second solvent portion remains
In PVDF-HFP film, plasticizer can be played the role of, reinforce the toughness of PVDF-HFP film；Remaining second solvent has simultaneously
Conducive to the infiltration of electrolyte.
The above is merely preferred embodiments of the present invention, be not intended to restrict the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (7)
1. a kind of method for preparing lithium battery diaphragm based on mixed solvent multistage Volatilization mechanism, which is characterized in that including following step
Suddenly,
S1: weighing Kynoar-hexafluoropropene (PVDF-HFP) of certain mass, be added in the first solvent of certain mass,
Heating stirring, forms the first uniform colloidal solution, the range of the mass ratio of PVDF-HFP and the first solvent are as follows: 0.08-0.15；
S2: the PVDF-HFP for weighing certain mass is added in the first solvent of certain mass, and stirring at normal temperature forms uniform suspended
The suspension is added in the first colloidal solution and stirring at normal temperature, obtains uniform second colloidal solution by liquid, PVDF-HFP with
The range of the mass ratio of first solvent are as follows: 0.1-0.6；It is added in PVDF-HFP and this step in step sl and PVDF-HFP is added
Mass ratio range are as follows: 3.0-4.2；
S3: the second solvent of certain mass is added in the second colloidal solution, it is molten to form uniform third glue for stirring at normal temperature
The quality of liquid, second solvent and the second colloidal solution compares range are as follows: is greater than 0 and is less than or equal to 0.5；
S4: obtained uniform third colloidal solution is coated on substrate with coating machine, after dry, obtains the lithium of different-thickness
Battery diaphragm；
In step s 2, the temperature range of room temperature is 15 DEG C -30 DEG C；
In step s3, the temperature range of room temperature is 15 DEG C -30 DEG C.
2. a kind of method that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism according to claim 1,
It is characterized in that, in step s3, organic and/or inorganic materials, inorganic material and the mass ratio of the second solvent is added in second solvent
Range is greater than 0 and to be less than or equal to 0.15, the particle size range of the inorganic material are as follows: 15nm-5000nm, the inorganic material are
Al2O3、SiO2、TiO2One of or at least two mixture.
3. a kind of method that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism according to claim 1,
It is characterized in that, the volatilization intensity of first solvent is greater than the volatilization intensity of the second solvent.
4. according to claim 1 or 3 described in any item one kind are based on mixed solvent multistage Volatilization mechanism and prepare lithium battery diaphragm
Method, which is characterized in that first solvent be acetone, second solvent be N-Methyl pyrrolidone (NMP), dimethyl
Acetamide (DMAc), dimethylformamide (DMF), dimethyl sulfoxide (DMSO), diethyl acetamide (DEAc), trimethyl phosphate
(TMP), one of triethyl phosphate (TEP), hexamethyl ammonium phosphate (HMPA) and tetramethyl urine (TMU).
5. a kind of method that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism according to claim 1,
It is characterized in that, in step sl, the temperature range of heating is 45 DEG C -55 DEG C, the range of viscosities of the first colloidal solution are as follows:
1000cp-5000cp, the range of viscosities of the second colloidal solution are as follows: 1000cp-4500cp, the range of viscosities of third colloidal solution
Are as follows: 2000cp-5500cp, in step s 4, the thickness range of the lithium battery diaphragm are as follows: 10 μm -120 μm.
6. a kind of method that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism according to claim 1,
It is characterized in that, the substrate is the substrate that can be reused.
7. a kind of method that lithium battery diaphragm is prepared based on mixed solvent multistage Volatilization mechanism according to claim 6,
It is characterized in that, the substrate is aluminium foil or copper foil or glass plate.
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| CN111341975B (en) * | 2020-03-16 | 2022-11-15 | 四川优源新能源有限公司 | Diaphragm for high-efficiency lithium ion secondary battery and preparation method thereof |
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| CN102324481A (en) * | 2011-09-23 | 2012-01-18 | 江苏华富储能新技术发展有限公司 | Composite diaphragm for lithium ion battery and preparation method thereof |
| CN103840112B (en) * | 2012-11-19 | 2017-04-12 | 东莞东阳光科研发有限公司 | PVDF-HFP-based composite porous polymer diaphragm and preparation method thereof |
| US9991514B2 (en) * | 2013-08-29 | 2018-06-05 | Lg Chem, Ltd. | Method of manufacturing lithium nickel complex oxide, lithium nickel complex oxide manufactured thereby, and cathode active material including the same |
| CN103545476B (en) * | 2013-10-30 | 2016-03-02 | 中国第一汽车股份有限公司 | There is PVDF-HFP micropore polymer diaphragm and the preparation method of grappling humidification |
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