CN108183191A - A kind of porous dickite coating non-woven fabrics lithium ion battery separator and preparation method thereof - Google Patents
A kind of porous dickite coating non-woven fabrics lithium ion battery separator and preparation method thereof Download PDFInfo
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- CN108183191A CN108183191A CN201810010167.4A CN201810010167A CN108183191A CN 108183191 A CN108183191 A CN 108183191A CN 201810010167 A CN201810010167 A CN 201810010167A CN 108183191 A CN108183191 A CN 108183191A
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- ion battery
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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
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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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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Cell Separators (AREA)
- Secondary Cells (AREA)
Abstract
The present invention relates to a kind of porous dickite coating non-woven fabrics lithium ion battery separators and preparation method thereof, belong to diaphragm material field.This method is prepared first to be penetrated through with duct, porous dickite powder of the pore size in 0.1 1 μ ms, again using the powder as coating material, coating slurry is mixed and made into binding agent, modifying agent and water, then the composite diaphragm that PET nonwoven surfaces are made lithium ion battery and use is coated in by infusion process.This method goes out uniform macroporous structure using the unique pore property of porous dickite in PET nonwoven fabric base reflector surface configurations, improves the porosity of diaphragm；Wetability of the composite diaphragm to electrolyte is improved, and reduce the internal resistance of cell using dickite surface functional group and the good compatibility of electrolyte, so as to improve lithium ion battery charge and discharge cycles stability.Preparation method that the present invention illustrates is simple, equipment requirement is low, cost of material is low, has the stronger market competitiveness.
Description
Technical field：
The invention belongs to lithium ion battery separator technical fields, are related to a kind of high temperature resistant, are suitble to the dynamic of high current charge-discharge
Power type lithium ion battery separator and preparation method thereof.
Background technology：
With the rapid development of power vehicle, battery will become future development core, and as battery core component every
Film is just welcoming the development peak of a new round.Had using the diaphragm in power lithium-ion battery with conventional lithium-ion battery diaphragm bright
Aobvious difference, the former provides power for vehicles such as automobiles, it is desirable to provide higher voltage, the power of bigger and more electricity
Amount, therefore, proposes diaphragm higher requirement.For example, power battery diaphragm should have heat resistance higher, gas permeability is more
Greatly, the features such as security performance is more preferable.At present, the lithium battery diaphragm material of commercialization is mainly porous polyolefin such as polyethylene
(PE), polypropylene, polyethylene (PP/PE) film etc., although polyalkene diaphragm has many advantages, such as lithium ion battery, polyolefin
The problems such as film high-temp. shrinking percentage is big, poor to electrolyte wetability, also only uses reluctantly in power lithium-ion battery.Therefore,
Develop the task of top priority that the novel separator product suitable for power lithium-ion battery has been Development of EV.
Lithium ion battery separator of the PET non-woven fabrics because making current primary study exploitation with good heat-resisting quantity
One of material.But the excessive pore structure size of PET non-woven fabrics is unfavorable for the holding of the insulation and electrolyte of positive and negative anodes, therefore is making
For lithium ion battery separator before use, needing to carry out composite modified to control non-woven fabrics membrane pore size.Common mode has nanometer
Granule modified nonwoven cloth diaphragm, micro porous coating coating modification nonwoven cloth diaphragm, electrostatic spinning diaphragm.Nano-particles filled non-woven fabrics
Diaphragm can effectively improve the pore property of nonwoven cloth diaphragm, improve the security performance of battery.In such diaphragm it is most typical just
It is the Separion ceramic membranes of Degussa companies.Degussa companies point out in patent US20050255769A1, with positive silicic acid
Ethyl ester or tetraisopropoxy titanium are silicon source or titanium source, and SiO is generated by sol-gel process2Or TiO2Gel, and with nanometer
Al2O3Slurry is mixed and made into, coated in PET non-woven fabrics matrix surfaces, raising cycle can be prepared after cured, hot rolling, drying
Property and durothermic novel lithium ion battery diaphragm.United States Patent (USP) US6447958BI also reports a kind of composite diaphragm for preparing
Method.By aramid fiber solution and nanometer Al2O3It is coated to after particle mixed pulp on PET non-woven fabrics, then polyethylene wax is coated to
Film surface is stated, can be prepared with the composite battery separator film for closing performance and good thermal stability.Chinese patent
Week, justice equality reported a kind of diaphragm of power lithium ion battery in CN206401415U, inorganic using PET non-woven fabrics as base material
Oxide is coating, and PVDF is coating, realizes membrane pore size size Control between hundreds of nanometers, and with certain guarantor
Wet function.
The coating of inorganic nano-particle can effectively modify the pore structure of PET non-woven fabrics, membrane pore size size be reduced, to carry
The insulating properties of high diaphragm positive and negative anodes improves the thermal stability of nonwoven cloth diaphragm.But the meanwhile micropore ruler of nano particle coating construction
The problems such as very little too small, porosity is relatively low, liquid absorption amount is insufficient, limits further improving for lithium ionic mobility, is unfavorable in battery
The reduction of resistance and battery high current charge-discharge, while the use of Nano filling also increases the cost of product.Therefore, PET is utilized
Non-woven fabrics finds novel inorganic filler as matrix, prepares that pore size is larger, porosity is higher, higher, thermostabilization of protecting liquid rate
Property higher compound nonwoven cloth lithium ion battery separator have become the critical issue for solving battery security.
Dickite chemical formula is Al4[Si4O10](OH)8, it is one kind 1:1 type layer aluminosilicate mineral, i.e. structural unit layer
It is made of one layer of oxygen-octahedron layer and one layer of alumina octahedral sheet.Since the intermolecular forces of structural unit layer are relatively weak, lead to
The stripping of dickite lamella can be realized by crossing after organic molecule intercalation-removing is handled, specific oxidant (such as potassium chlorate)
Under effect, the removing of organic molecule (such as urea) can result in the formation of dickite pore structure, that is, form pore size as 0.1-1
μm perforation porous structure.It if can be using the dickite with porous structure as the coating material of PET non-woven fabrics, then will have
Hope using the unique porous connectivity of dickite, non-woven fabrics intrinsic silicon and surface structure go out pore size is larger, duct is flourishing,
The high lithium ion diffusion admittance of porosity.In addition, dickite unit layer surface contain abundant functional group to aqueous electrolyte and
Organic electrolyte is respectively provided with good adaptability, can improve wetability of the diaphragm to different electrolytes, so as to reduce battery resistance
It is anti-, improve the high rate performance and cycle performance of battery.Meanwhile the incombustible characteristic of dickite will also further improve PET without
The thermal stability of woven fabric promotes the safety in utilization of diaphragm.
The unique structure feature of matrix porosity dickite and the application prospect in lithium ion battery separator field.The present invention carries
Go out a kind of side for preparing novel lithium ion battery diaphragm coated in PET non-woven fabrics matrix surfaces by the use of porous dickite as filler
Method, this method process is simple, and raw material is easily obtained, is cheap, effectively facilitates lithium ion battery in large current density electric process
In cyclical stability.
Invention content：
The purpose of the present invention aiming in current application type lithium ion battery separator pore size is too small, porosity compared with
Low, the problems such as liquid absorption amount is insufficient, using dickite as raw material, using the processing of urea, potassium chlorate to dickite, obtain dickite
Porous structure feature, and using porous dickite as coating material, coated on PET non-woven fabrics matrix surfaces, preparation can improve
Diaphragm porosity, wetability reduce the internal resistance of cell, improve the lithium ion battery composite separation membrane of battery charging and discharging cyclical stability.
The present invention is achieved by the following technical solutions：
The preparation of porous dickite coating PET non-woven fabrics lithium ion battery separators, includes the following steps：
A. the preparation of porous dickite
Dickite crushes 5~20 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, urea
Quality is 10~25wt% of dickite quality, and mixture is placed in open glass container, is put into micro-wave oven high fire heating
It 10~20 minutes, is put into later in 70 DEG C of baking ovens and keeps the temperature 50 hours.Again by mixture and potassium chlorate mixed grinding 40 minutes, chloric acid
The dosage of potassium is the 4% of dickite quality.Finally the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and is calcined 15 seconds,
Obtain porous dickite powder.
B. the preparation of porous dickite/PET diaphragms
By porous dickite and binding agent, water, modifying agent 60-80 in mass ratio:33-13:5:After 2 uniformly mix, even
It is stirred in pulp grinder and has just obtained within 1-2 hours coating slurry, then PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken
Go out the dry PET nonwoven cloth diaphragms for just having obtained porous dickite coating in 40 DEG C of vacuum drying chamber.
Above-described dickite is the dickite for originating from the white county of Jilin governor, other siliceous dephasign contents are less than 5%, ground
Stone crystallization index Hinckley index values are opened more than 1；The binding agent for LA132 (the aqueous electrode adhesive of LA types) or
LA132 and SBR (butadiene-styrene rubber) mixture；The modifying agent is silane coupling agent DL171.
Advantageous effect：Using the dickite with porous structure as coating raw material, PET non-woven fabrics prepares more the present invention for basement membrane
Hole dickite/PET diaphragms, the diaphragm and the Nano Ceramic Particles coating non-woven fabrics largely reported prepare the hole forming machine of composite diaphragm
System is different.The latter transmits the hole of lithium ion by the use of the gap that a large amount of nano-particles are formed after nonwoven surface is piled up as diaphragm
Road, mostly in 20-80nm, pore size is smaller in aperture, when being unfavorable for power lithium-ion battery high current charge-discharge, a large amount of lithium ions
Quickly through resistance is larger.And the former is then passed using the macroporous structure (0.1-1 μm of aperture size) of porous dickite as diaphragm
The channel of defeated lithium ion can effectively improve the conductivity of lithium ion, reduce resistance.Meanwhile utilize the abundant official in dickite surface
It can roll into a ball, the stability of high temperature lower structure, wetability, imbibition rate and heat of the diaphragm to electrolyte can be significantly improved after coating non-woven fabrics
Stability, so as to improve stable circulation performance of the battery during high current charge-discharge.The hole of porous dickite/PET diaphragms
Gap rate is up to 68%, and imbibition rate reaches 198%, and ionic conductivity reaches 11.4mScm-1.LiMn is used for using the diaphragm2O4/
In graphite cell system, after 200 charge and discharge cycles, battery capacity conservation rate reaches 83%, hence it is evident that is better than commercial PE diaphragms
(72%).
Description of the drawings
The stereoscan photograph of Fig. 1, porous dickite
Fig. 2, the LiMn using porous dickite/PET diaphragms2O4The relationship of/graphite cell capacity retention ratio and cycle-index
(1C)
Specific embodiment：
The present invention is described in further detail in conjunction with the embodiments：
A. the preparation of porous dickite
Dickite crushes 5~20 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, urea
Quality is 10~25wt% of dickite quality, and mixture is placed in open glass container, is put into micro-wave oven high fire heating
It 10~20 minutes, is put into later in 70 DEG C of baking ovens and keeps the temperature 50 hours.Again by mixture and potassium chlorate mixed grinding 40 minutes, chloric acid
The dosage of potassium is the 4% of dickite quality.Finally the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and is calcined 15 seconds,
Obtain porous dickite powder.
B. the preparation of porous dickite/PET diaphragms
By porous dickite and binding agent, water, modifying agent 60-80 in mass ratio:33-13:5:After 2 uniformly mix, even
It is stirred in pulp grinder and has just obtained within 1-2 hours coating slurry, then PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken
Go out the dry PET nonwoven cloth diaphragms for just having obtained porous dickite coating in 40 DEG C of vacuum drying chamber.
Embodiment 1
A. dickite crushes 10 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, the matter of urea
Amount is the 10wt% of dickite quality；
B. mixture is placed in open glass container, is put into big fire in micro-wave oven and heats 17 minutes, be put into 70 DEG C later
50 hours are kept the temperature in baking oven；
C. by mixture and potassium chlorate mixed grinding 40 minutes, the dosage of potassium chlorate is the 4% of dickite quality；
D. the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and calcined 15 seconds, obtain porous dickite powder；
E. by porous dickite and binding agent, water, modifying agent in mass ratio 80:13:5:After 2 uniformly mix, in refiner
Middle stirring obtains coating slurry for 1 hour；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken out dry in 40 DEG C of vacuum drying chamber
Obtain the non-woven fabric compounded diaphragms of PET of porous dickite coating.
LiMn is used for using the diaphragm2O4In/graphite cell system, ionic conductivity 11.9mScm-1.It fills for 200 times
After discharge cycles, battery capacity conservation rate reaches 87%.
Embodiment 2
A. dickite crushes 15 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, the matter of urea
Amount is the 15wt% of dickite quality；
B. mixture is placed in open glass container, is put into big fire in micro-wave oven and heats 15 minutes, be put into 70 DEG C later
50 hours are kept the temperature in baking oven；
C. by mixture and potassium chlorate mixed grinding 40 minutes, the dosage of potassium chlorate is the 4% of dickite quality；
D. the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and calcined 15 seconds, obtain porous dickite powder；
E. by porous dickite and binding agent, water, modifying agent in mass ratio 70:23:5:After 2 uniformly mix, in refiner
Middle stirring obtains coating slurry for 2 hours；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken out dry in 40 DEG C of vacuum drying chamber
Obtain the non-woven fabric compounded diaphragms of PET of porous dickite coating.
LiMn is used for using the diaphragm2O4In/graphite cell system, ionic conductivity 12.2mScm-1.It fills for 200 times
After discharge cycles, battery capacity conservation rate reaches 88%.
Embodiment 3
A. dickite crushes 5 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, the matter of urea
Amount is the 20wt% of dickite quality；
B. mixture is placed in open glass container, is put into big fire in micro-wave oven and heats 20 minutes, be put into 70 DEG C later
50 hours are kept the temperature in baking oven；
C. by mixture and potassium chlorate mixed grinding 40 minutes, the dosage of potassium chlorate is the 4% of dickite quality；
D. the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and calcined 15 seconds, obtain porous dickite powder；
E. by porous dickite and binding agent, water, modifying agent in mass ratio 60:33:5:After 2 uniformly mix, in refiner
Middle stirring obtains coating slurry for 1 hour；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken out dry in 40 DEG C of vacuum drying chamber
Obtain the non-woven fabric compounded diaphragms of PET of porous dickite coating.
LiMn is used for using the diaphragm2O4In/graphite cell system, ionic conductivity 11.4mScm-1.It fills for 200 times
After discharge cycles, battery capacity conservation rate reaches 84%.
Embodiment 4
A. dickite crushes 20 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, the matter of urea
Amount is the 25wt% of dickite quality；
B. mixture is placed in open glass container, is put into big fire in micro-wave oven and heats 10 minutes, be put into 70 DEG C later
50 hours are kept the temperature in baking oven；
C. by mixture and potassium chlorate mixed grinding 40 minutes, the dosage of potassium chlorate is the 4% of dickite quality；
D. the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and calcined 15 seconds, obtain porous dickite powder；
E. by porous dickite and binding agent, water, modifying agent in mass ratio 75:18:5:After 2 uniformly mix, in refiner
Middle stirring obtains coating slurry for 2 hours；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken out dry in 40 DEG C of vacuum drying chamber
Obtain the non-woven fabric compounded diaphragms of PET of porous dickite coating.
LiMn is used for using the diaphragm2O4In/graphite cell system, ionic conductivity 11.6mScm-1.It fills for 200 times
After discharge cycles, battery capacity conservation rate reaches 85%.
Claims (3)
1. a kind of preparation method of porous dickite coating non-woven fabrics lithium ion battery separator, which is characterized in that including following step
Suddenly：
A. dickite crushes 5~20 minutes with a certain proportion of urea in pulverizer, and granularity is made to be less than 270 mesh, the matter of urea
Amount is 10~25wt% of dickite quality, and mixture is placed in open glass container, is put into micro-wave oven high fire heating 10
It~20 minutes, is put into later in 70 DEG C of baking ovens and keeps the temperature 50 hours；Again by mixture and potassium chlorate mixed grinding 40 minutes, potassium chlorate
Dosage be the 4% of dickite quality；Finally the mixture for mixing potassium chlorate is put into 550 DEG C of electric furnace and is calcined 15 seconds, is obtained
To porous dickite powder；
B. by porous dickite and binding agent, water, modifying agent 60-80 in mass ratio:33-13:5:After 2 uniformly mix, it is being homogenized
It is stirred in machine and obtains within 1-2 hours coating slurry, then PET non-woven fabrics is immersed in coating slurry 30 minutes, then taken out 40
DEG C vacuum drying chamber in it is dry after obtain the PET nonwoven cloth diaphragms of porous dickite coating.
2. a kind of preparation method of porous dickite coating non-woven fabrics lithium ion battery separator described in accordance with the claim 1,
It is characterized in that, the dickite is the dickite for originating from the white county of Jilin governor, other siliceous dephasign contents are less than 5%, and ground is opened
Stone crystallization index Hinckley index values are more than 1；The binding agent is LA132 (the aqueous electrode adhesive of LA types) or LA132
With SBR (butadiene-styrene rubber) mixture；The modifying agent is silane coupling agent DL171.
3. a kind of porous dickite coating non-woven fabrics lithium ion battery separator, it is characterised in that：It is any according to claim 1-2
Method is made.
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| Application Number | Priority Date | Filing Date | Title |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810010167.4A CN108183191B (en) | 2018-01-05 | 2018-01-05 | A kind of porous dickite coating non-woven fabrics lithium ion battery separator and preparation method thereof |
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| CN108183191B CN108183191B (en) | 2019-09-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807799A (en) * | 2018-08-07 | 2018-11-13 | 吉林大学 | A kind of lithium ion battery separator and preparation method thereof of puffing dickite modification |
| CN109004157A (en) * | 2018-08-07 | 2018-12-14 | 吉林大学 | A kind of galapectite coating non-woven fabrics lithium ion battery separator and preparation method thereof |
| CN111180637A (en) * | 2020-01-07 | 2020-05-19 | 四川东为氢源科技有限公司 | Sodium ion battery diaphragm and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107301A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院金属研究所 | Novel lithium ion battery diaphragm with inorganic coating and preparation method thereof |
| CN105712364A (en) * | 2016-01-20 | 2016-06-29 | 吉林大学 | Method for expanding aluminosilicate mineral layered structure |
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2018
- 2018-01-05 CN CN201810010167.4A patent/CN108183191B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107301A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院金属研究所 | Novel lithium ion battery diaphragm with inorganic coating and preparation method thereof |
| CN105712364A (en) * | 2016-01-20 | 2016-06-29 | 吉林大学 | Method for expanding aluminosilicate mineral layered structure |
Non-Patent Citations (1)
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| J.NUNES-PEREIRA ET AL.: "Microporous membranes of NaY zeolite/poly(vinylidene fluoride–trifluoroethylene) for Li-ion battery separators", 《JOURNAL OF ELECTROANALYTICAL CHEMISTRY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807799A (en) * | 2018-08-07 | 2018-11-13 | 吉林大学 | A kind of lithium ion battery separator and preparation method thereof of puffing dickite modification |
| CN109004157A (en) * | 2018-08-07 | 2018-12-14 | 吉林大学 | A kind of galapectite coating non-woven fabrics lithium ion battery separator and preparation method thereof |
| CN108807799B (en) * | 2018-08-07 | 2020-04-28 | 吉林大学 | Expanded dickite modified lithium ion battery diaphragm and preparation method thereof |
| CN111180637A (en) * | 2020-01-07 | 2020-05-19 | 四川东为氢源科技有限公司 | Sodium ion battery diaphragm and preparation method and application thereof |
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| CN108183191B (en) | 2019-09-03 |
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