CN108777284A - A kind of preparation method of lithium ion battery composite separation membrane - Google Patents
A kind of preparation method of lithium ion battery composite separation membrane Download PDFInfo
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- CN108777284A CN108777284A CN201810593321.5A CN201810593321A CN108777284A CN 108777284 A CN108777284 A CN 108777284A CN 201810593321 A CN201810593321 A CN 201810593321A CN 108777284 A CN108777284 A CN 108777284A
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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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- 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
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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
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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Abstract
The present invention relates to a kind of preparation methods of lithium ion battery composite separation membrane, belong to field of new energy technologies.The present invention utilizes the unique surface nature of pure silica zeolites particle and internal gutter structure, it is inorganic in conjunction with a kind of kernel, outer layer is organically-modified cage-type silsesquioxane, pass through ethylenediamine tetra-acetic acid pore-creating, improve the lyophily group on the surface of zeolite particles, the compatibility of composite membrane and electrolyte can be enhanced, composite membrane has flourishing porous structure simultaneously, including the micropore of the macropore and zeolite itself formed after Kynoar inversion of phases, higher porosity enhances imbibition/liquid-keeping property of composite membrane, improve the charge-discharge performance of battery, with higher porosity and superior chemical property；The present invention possesses higher ionic conductivity using polyacrylonitrile, improves the mechanical property of Electrospun diaphragm, while improving the charge-discharge performance of battery, improves the interface stability of diaphragm, reduces side reaction, improves coulombic efficiency.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery composite separation membrane, belong to field of new energy technologies.
Background technology
Lithium ion battery separator is present between lithium ion battery plus-negative plate, and permissible ion stream passes through, and is prevented positive and negative
The perforated membrane that pole connects.From various diaphragms such as cellulose, glassine paper to non-woven fabrics, proton exchange membrane, high molecular materials
It is applied in lithium ion battery.In the early 1990s, lithium ion battery separator realizes industrialization, and preferable hair is obtained
Exhibition.With the development of Study on Li-ion batteries, the requirement to lithium ion battery separator also becomes increasingly harsher and complicated.Diaphragm
Very crucial effect is played in the battery, and major function is to maintain positive and negative electrode separation to prevent electric short circuit, and at the same time permitting
Perhaps the quick transmission of lithium ion.Diaphragm should have preferable ionic conductivity and electronic isolation, not influence the effect of battery
The performances such as rate and specific capacity.
According to the physics and chemical property of diaphragm, diaphragm can be divided into different types.As woven fabric, non-woven fabrics, microporous barrier,
Woven fabric class etc..The lithium ion battery to work at room temperature is general to select organic material fiber element, polymer or inorganic material stone
Cotton, glass fibre etc. are used as diaphragm.In alkaline battery, the diaphragm material generally selected is renewable cellulose or polymer
Microporous barrier.In order to facilitate discussion, diaphragm is divided into following several types by we：Micro-pore septum, nonwoven cloth diaphragm, composite diaphragm.
Lithium ion battery is because energy density height is widely used in every field, but lithium ion battery is used with inflammable
Property organic electrolyte, and be easy to happen and overcharge or generated in cyclic process heat, cause internal short-circuit of battery, occur
Fire or explosion.Therefore, security performance is one of important performance of lithium ion battery, and diaphragm is to ensure lithium ion battery peace
One of the critical material of full performance, the following performance of diaphragm play highly important work to the safety of lithium ion battery
With.
Invention content
The technical problems to be solved by the invention：It is poor for now septate electrochemical stability, it is also easy to produce metachromatism,
Lead to battery performance difference and lead to the problem of security risk, provides a kind of preparation side of lithium ion battery composite separation membrane
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Pure silica zeolites, ethylenediamine tetra-acetic acid, Ludox, cage-type silsesquioxane is taken to be fitted into 2~3h of ball milling in ball mill, then
Alcohol is washed after high-temperature calcination, and dry at 110~120 DEG C, obtains composite conductor powder；
（2）It takes acetone, n,N-Dimethylformamide to be uniformly mixed, adds Kynoar and stir to being completely dissolved, must gather partially
Vinyl fluoride spray coating liquor；
（3）Take n,N-Dimethylformamide, tetrahydrofuran that polyacrylonitrile, composite conductor powder are added after mixing, 40~
It is stirred evenly at 50 DEG C, 1~2h of re-ultrasonic dispersion obtains spinning solution；
（4）Polyethylene film is successively immersed in absolute ethyl alcohol and acetone, taking-up is dry after draining, then by the polyethylene after drying
Film is laid in electrostatic spinning reception device, and spinning solution is fitted into the syringe of electrostatic spinning apparatus and carries out continuous spinning,
It is dried in vacuo after spinning, obtains semi-finished product film；
（5）Semi-finished product film is placed on coating machine, then Kynoar spray coating liquor even application has been sprayed on semi-finished product film
It is dry after finishing and hot-forming, obtain lithium ion battery composite separation membrane.
Step（1）The pure silica zeolites, ethylenediamine tetra-acetic acid, Ludox, cage-type silsesquioxane parts by weight be 50~
60 parts of pure silica zeolites, 30~40 parts of ethylenediamine tetra-acetic acids, 10~20 parts of Ludox, 5~10 parts of cage-type silsesquioxanes.
Step（1）The high-temperature burning process is that 3~5h is calcined at 800~1000 DEG C.
Step（2）The acetone, n,N-Dimethylformamide, the parts by weight of Kynoar be 30~40 parts of acetone, 20
~25 parts of n,N-Dimethylformamide, 1.2~1.5 parts of Kynoar.
Step（3）The n,N-Dimethylformamide, tetrahydrofuran, polyacrylonitrile, composite conductor powder parts by weight be
60~90 parts of n,N-Dimethylformamide, 40~60 parts of tetrahydrofurans, 16~32 parts of polyacrylonitrile, 3~6 parts of composite conductor powder
End.
Step（4）The continuous spinning parameter is to receive 25~30cm of distance, 25~30kV of spinning voltage, fltting speed
0.6~0.8mL/h, 300~500r/min of drum rotation speed.
Step（5）The spray rate is 2~4mL/dm2。
Step（5）The hot pressing is 10~15min of hot pressing at 100~120 DEG C.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention utilize the unique surface nature of pure silica zeolites particle and internal gutter structure, in conjunction with a kind of kernel be it is inorganic,
Outer layer is organically-modified cage-type silsesquioxane improves the lyophily on the surface of zeolite particles by ethylenediamine tetra-acetic acid pore-creating
Group can enhance the compatibility of composite membrane and electrolyte, while composite membrane has flourishing porous structure, including poly- inclined fluorine
The micropore of the macropore and zeolite itself formed after ethylene inversion of phases, higher porosity enhance imbibition/guarantor's liquid energy of composite membrane
Power improves the charge-discharge performance of battery, has higher porosity and superior chemical property；
（2）The present invention is interfered using the track of continuous electrostatic spinning jet stream by the high rotating speed of rotary drum, close to the fibre bundle of rotary drum
Drum surface can be adsorbed onto because of electrostatic interaction, the fibre bundle being wound up on rotary drum can stretch follow-up spinning because of higher rotating speed
Silk jet stream, and be aligned on rotary drum along orbit orientation, while possessing higher ionic conductivity, and imbibition using polyacrylonitrile
Performance is good, and the preferable feature with the compatibility of electrode compounds conductor powder, destroys the entanglement between polymer, reduce fiber
Fineness, while enhancing the adhesive property between nanofiber, improve the mechanical property of Electrospun diaphragm, while improving ionic conductance
Rate improves the charge-discharge performance of battery, improves the interface stability of diaphragm, reduces side reaction, improves coulombic efficiency, significantly carries
The cycle performance and security performance of high-lithium ion battery, improve high voltage withstanding performance.
Specific implementation mode
Take 50~60g pure silica zeolites, 30~40g ethylenediamine tetra-acetic acids, 10~20g Ludox, 5~10g cage model sesquialter silicon
Oxygen alkane is fitted into ball mill, and with 200~300r/min, 2~3h of ball milling, ball milling terminates to be transferred in Muffle furnace, at 800~1000 DEG C
3~5h of lower calcining, is washed 2~3 times after being cooled to room temperature with absolute ethyl alcohol, and is dried to constant weight at 110~120 DEG C, must be answered
Conductor powder is closed, 30~40g acetone, 20~25gN, dinethylformamide is taken to be uniformly mixed, 1.2~1.5g is added and gathers inclined fluorine
Ethylene is stirred to powder with 300~400r/min and is completely dissolved under 50~55 DEG C of water bath with thermostatic control, obtains Kynoar spraying
Liquid, takes 60~90gN, dinethylformamide, 40~60g tetrahydrofurans, is added 16~32g polyacrylonitrile after mixing, and 3
~6g composite conductor powder stirs 20~30min, then super with 150W under 40~50 DEG C of waters bath with thermostatic control with 300~400r/min
Sound wave 1~2h of ultrasonic disperse, obtains spinning solution, and polyethylene film is successively immersed in 15~20min in absolute ethyl alcohol and acetone, is taken out
It drains and is placed in 60~65 DEG C of drying boxes dry 2~3h, then the polyethylene film after drying is laid in electrostatic spinning and receives dress
It sets, and spinning solution is fitted into the syringe of electrostatic spinning apparatus and carries out spinning, it is 25~30cm, spinning that setting, which receives distance,
Voltage be 25~30kV, fltting speed be 0.6~0.8mL/h, drum rotation speed be 300~500r/min, continuous spinning 10~
12h is transferred to after spinning in vacuum drying chamber, and dry 10~12h, obtains semi-finished product film, by semi-finished product film at 50~60 DEG C
It is placed on coating machine, then by Kynoar spray coating liquor with 2~4mL/dm2Even application is on semi-finished product film, after spraying
Be transferred in drying box, dry 5~6h at 70~80 DEG C, then be transferred on hot press, at 100~120 DEG C hot pressing 10~
15min obtains lithium ion battery composite separation membrane.
Taking 50g pure silica zeolites, 30g ethylenediamine tetra-acetic acids, 10g Ludox, 5g cage-type silsesquioxanes are fitted into ball mill,
With 200r/min ball milling 2h, ball milling terminates to be transferred in Muffle furnace, and 3h is calcined at 800 DEG C, and absolute ethyl alcohol is used after being cooled to room temperature
Washing 2 times, and dried to constant weight at 110 DEG C, composite conductor powder is obtained, 30g acetone, 20gN, dinethylformamide is taken to mix
It closes uniformly, 1.2g Kynoar is added and is stirred to powder and is completely dissolved with 300r/min under 50 DEG C of waters bath with thermostatic control, obtains poly-
Vinylidene spray coating liquor takes 60gN, dinethylformamide, 40g tetrahydrofurans that 16g polyacrylonitrile, 3g are added after mixing
Composite conductor powder stirs 20min with 300r/min, then disperse 1h with 150W ultrasonic echographies, obtains under 40 DEG C of waters bath with thermostatic control
Polyethylene film is successively immersed in 15min in absolute ethyl alcohol and acetone by spinning solution, and taking-up is drained to be placed in 60 DEG C of drying boxes and be done
Dry 2h, then the polyethylene film after drying is laid in electrostatic spinning reception device, and spinning solution is packed into electrostatic spinning apparatus
Syringe in carry out spinning, it is 25cm, spinning voltage 25kV, fltting speed 0.6mL/h that setting, which receives distance, and roller turns
Speed is 300r/min, and continuous spinning 10h is transferred to after spinning in vacuum drying chamber, and dry 10h, obtains semi-finished product at 50 DEG C
Semi-finished product film is placed on coating machine by film, then by Kynoar spray coating liquor with 2mL/dm2Even application on semi-finished product film,
It is transferred in drying box, the dry 5h at 70 DEG C, then is transferred on hot press after spraying, hot pressing 10min, obtains lithium at 100 DEG C
Ion battery composite diaphragm.
Taking 55g pure silica zeolites, 35g ethylenediamine tetra-acetic acids, 15g Ludox, 8g cage-type silsesquioxanes are fitted into ball mill,
With 250r/min ball milling 2h, ball milling terminates to be transferred in Muffle furnace, and 4h is calcined at 900 DEG C, and absolute ethyl alcohol is used after being cooled to room temperature
Washing 2 times, and dried to constant weight at 150 DEG C, composite conductor powder is obtained, 35g acetone, 22gN, dinethylformamide is taken to mix
It closes uniformly, 1.3g Kynoar is added and is stirred to powder and is completely dissolved with 350r/min under 52 DEG C of waters bath with thermostatic control, obtains poly-
Vinylidene spray coating liquor takes 75gN, dinethylformamide, 50g tetrahydrofurans that 24g polyacrylonitrile, 5g are added after mixing
Composite conductor powder stirs 25min with 350r/min, then disperse 1h with 150W ultrasonic echographies, obtains under 45 DEG C of waters bath with thermostatic control
Polyethylene film is successively immersed in 18min in absolute ethyl alcohol and acetone by spinning solution, and taking-up is drained to be placed in 62 DEG C of drying boxes and be done
Dry 2h, then the polyethylene film after drying is laid in electrostatic spinning reception device, and spinning solution is packed into electrostatic spinning apparatus
Syringe in carry out spinning, it is 28cm, spinning voltage 28kV, fltting speed 0.7mL/h that setting, which receives distance, and roller turns
Speed is 400r/min, and continuous spinning 11h is transferred to after spinning in vacuum drying chamber, and dry 11h, obtains semi-finished product at 55 DEG C
Semi-finished product film is placed on coating machine by film, then by Kynoar spray coating liquor with 3mL/dm2Even application on semi-finished product film,
It is transferred in drying box, the dry 5h at 75 DEG C, then is transferred on hot press after spraying, hot pressing 12min, obtains lithium at 110 DEG C
Ion battery composite diaphragm.
Take 60g pure silica zeolites, 40g ethylenediamine tetra-acetic acids, 20g Ludox, 10g cage-type silsesquioxanes loading ball mill
In, with 300r/min ball milling 3h, ball milling terminates to be transferred in Muffle furnace, and 5h is calcined at 1000 DEG C, with anhydrous after being cooled to room temperature
Ethyl alcohol washs 3 times, and is dried to constant weight at 120 DEG C, obtains composite conductor powder, takes 40g acetone, 25gN, N- dimethyl formyls
Amine is uniformly mixed, and 1.5g Kynoar is added and is stirred to powder and is completely dissolved with 400r/min under 55 DEG C of waters bath with thermostatic control,
Kynoar spray coating liquor is obtained, takes 90gN, dinethylformamide, 60g tetrahydrofurans that 32g polypropylene is added after mixing
Nitrile, 6g composite conductor powder stir 30min, then disperse with 150W ultrasonic echographies under 50 DEG C of waters bath with thermostatic control with 400r/min
2h obtains spinning solution, polyethylene film is successively immersed in 20min in absolute ethyl alcohol and acetone, taking-up, which drains, is placed on 65 DEG C of dryings
Dry 3h in case, then the polyethylene film after drying is laid in electrostatic spinning reception device, and spinning solution is packed into Static Spinning
Carrying out spinning in the syringe of silk device, it is 30cm, spinning voltage 30kV, fltting speed 0.8mL/h that setting, which receives distance,
Drum rotation speed is 500r/min, and continuous spinning 12h is transferred to after spinning in vacuum drying chamber, and dry 12h, obtains at 60 DEG C
Semi-finished product film is placed on coating machine by semi-finished product film, then by Kynoar spray coating liquor with 4mL/dm2Even application is in semi-finished product
It on film, is transferred in drying box, the dry 6h at 80 DEG C, then is transferred on hot press, the hot pressing 15min at 120 DEG C after spraying,
Obtain lithium ion battery composite separation membrane.
Reference examples：The lithium ion battery composite separation membrane of Dongguan mold materials Co., Ltd production.
The lithium ion battery composite separation membrane of example and reference examples is detected, specific detection is as follows：
Porosity test：By diaphragm punching at the disk of 16.5mm, its quality is referred to as M0, then it is placed on butanol solution
In.After 2h, sample is taken out, is removed the extra n-butanol of membrane surface with filter paper, quality is referred to as M after its imbibition1.Diaphragm sample
Porosity calculated by porosity formula.
Mechanics Performance Testing：Mechanical property mainly tests the tensile strength of diaphragm, and diaphragm is done in 60 DEG C of constant temperature ovens
Sample is cut into 8 × 1cm sizes by dry 1h, and the examination of U.S.'s Instron Corporation Inston-3300 electronic universal materials is selected in experiment
The machine of testing measures, and after clamping each 1cm in sample both ends with fixture, is tested with the tensile speed of 10mm/min, each sample does three
Secondary parallel testing.
Ionic conductivity is tested：The ionic conductivity of diaphragm or electrolyte is generally by test ac impedance measurement sheet
Body impedance, and be calculated by formula.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Porosity/% | 85 | 86 | 88 | 55 |
| Tensile strength/MPa | 37 | 38 | 39 | 12 |
| Ionic conductivity/Scm﹣ 1 | 1.4×10﹣ 3 | 1.3×10﹣ 3 | 1.5×10﹣ 3 | 6.4×10﹣ 4 |
As shown in Table 1, the lithium ion battery composite separation membrane that prepared by the present invention has good porosity, tensile strength and ion-conductance
Conductance.
Claims (8)
1. a kind of preparation method of lithium ion battery composite separation membrane, which is characterized in that specifically preparation process is：
（1）Pure silica zeolites, ethylenediamine tetra-acetic acid, Ludox, cage-type silsesquioxane is taken to be fitted into 2~3h of ball milling in ball mill, then
Alcohol is washed after high-temperature calcination, and dry at 110~120 DEG C, obtains composite conductor powder；
（2）It takes acetone, n,N-Dimethylformamide to be uniformly mixed, adds Kynoar and stir to being completely dissolved, must gather partially
Vinyl fluoride spray coating liquor；
（3）Take n,N-Dimethylformamide, tetrahydrofuran that polyacrylonitrile, composite conductor powder are added after mixing, 40~
It is stirred evenly at 50 DEG C, 1~2h of re-ultrasonic dispersion obtains spinning solution；
（4）Polyethylene film is successively immersed in absolute ethyl alcohol and acetone, taking-up is dry after draining, then by the polyethylene after drying
Film is laid in electrostatic spinning reception device, and spinning solution is fitted into the syringe of electrostatic spinning apparatus and carries out continuous spinning,
It is dried in vacuo after spinning, obtains semi-finished product film；
（5）Semi-finished product film is placed on coating machine, then Kynoar spray coating liquor even application has been sprayed on semi-finished product film
It is dry after finishing and hot-forming, obtain lithium ion battery composite separation membrane.
2. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（1）Institute
State pure silica zeolites, ethylenediamine tetra-acetic acid, Ludox, cage-type silsesquioxane parts by weight be 50~60 parts of pure silica zeolites, 30~
40 parts of ethylenediamine tetra-acetic acids, 10~20 parts of Ludox, 5~10 parts of cage-type silsesquioxanes.
3. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（1）Institute
It is that 3~5h is calcined at 800~1000 DEG C to state high-temperature burning process.
4. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（2）Institute
It is 30~40 parts of acetone, 20~25 parts of N, N- dimethyl methyls to state acetone, n,N-Dimethylformamide, the parts by weight of Kynoar
Amide, 1.2~1.5 parts of Kynoar.
5. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（3）Institute
State n,N-Dimethylformamide, tetrahydrofuran, polyacrylonitrile, composite conductor powder parts by weight be 60~90 parts of N, N- dimethyl
Formamide, 40~60 parts of tetrahydrofurans, 16~32 parts of polyacrylonitrile, 3~6 parts of composite conductor powder.
6. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（4）Institute
It is to receive 25~30cm of distance, 25~30kV of spinning voltage, 0.6~0.8mL/h of fltting speed to state continuous spinning parameter, and roller turns
300~500r/min of speed.
7. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（5）Institute
It is 2~4mL/dm to state spray rate2。
8. a kind of preparation method of lithium ion battery composite separation membrane as described in claim 1, which is characterized in that step（5）Institute
It is 10~15min of hot pressing at 100~120 DEG C to state hot pressing.
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| CN114256561A (en) * | 2021-11-19 | 2022-03-29 | 国科广化韶关新材料研究院 | Composite diaphragm for lithium metal battery and preparation method thereof |
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| CN107732102A (en) * | 2017-09-19 | 2018-02-23 | 常州市丰瑞电子有限公司 | A kind of preparation method of composite lithium ion cell barrier film |
Cited By (1)
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| CN114256561A (en) * | 2021-11-19 | 2022-03-29 | 国科广化韶关新材料研究院 | Composite diaphragm for lithium metal battery and preparation method thereof |
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