CN108183191B - 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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- CN108183191B CN108183191B CN201810010167.4A CN201810010167A CN108183191B CN 108183191 B CN108183191 B CN 108183191B CN 201810010167 A CN201810010167 A CN 201810010167A CN 108183191 B CN108183191 B CN 108183191B
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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)
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- 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 m, again using the powder as coating material, it is mixed and made into coating slurry with binder, modifying agent and water, then PET nonwoven surface is coated in by infusion process, the composite diaphragm that lithium ion battery uses is made.This method goes out uniform macroporous structure in PET nonwoven fabric base reflector surface configuration using the unique pore property of porous dickite, improves the porosity of diaphragm；Composite diaphragm is improved to the wetability of electrolyte using dickite surface functional group and the good compatibility of electrolyte, and reduces the internal resistance of cell, to improve lithium ion battery charge and discharge cycles stability.The 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 field, it is related to a kind of high temperature resistant, is suitble to the dynamic of high current charge-discharge
Power type lithium ion battery separator and preparation method thereof.
Background technique:
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, bigger power and more electricity
Amount, therefore, to diaphragm, more stringent requirements are proposed.For example, power battery diaphragm should have heat resistance higher, gas permeability is more
Greatly, the features such as security performance is more preferable.Currently, 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 in power lithium-ion battery reluctantly.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 coat 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 membrane of Degussa company.Degussa company points out in patent US20050255769A1, with positive silicic acid
Ethyl ester or tetraisopropoxy titanium are silicon source or titanium source, generate SiO by sol-gel process2Or TiO2Gel, and with nanometer
Al2O3It is mixed and made into slurry, PET non-woven fabrics matrix surface is coated in, raising circulation 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, used PET non-woven fabrics as substrate, inorganic
Oxide is coating, and PVDF is coating, realizes membrane pore size size Control between several hundred nanometers, and has 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 mention
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 lower, liquid absorption amount is insufficient, limits further increasing for lithium ionic mobility, is unfavorable in battery
The reduction of resistance and battery high current charge-discharge, while the use of nanofiller 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 a kind of 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 active force is relatively weak between structural unit layer, lead to
The removing that can be realized dickite lamella after small organic molecule intercalation-removing is handled is crossed, specific oxidant (such as potassium chlorate)
Under effect, the removing of small organic molecule (such as urea) can result in the formation of dickite pore structure, that is, forming pore size is 0.1-1
μm perforation porous structure.If can will have using the dickite with porous structure as the coating material of PET non-woven fabrics
Hope utilize 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 functional group rich in aqueous electrolyte and
Organic electrolyte all has good adaptability, can be improved diaphragm to the wetability of different electrolytes, 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 increase 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 mentions
It is a kind of out to be coated in PET nonwoven fabric base body surface wheat flour using porous dickite as filler for the side of novel lithium ion battery diaphragm
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.
Summary of the invention:
The purpose of the present invention is to the too small, porosity in current application type lithium ion battery separator pore size compared with
Low, the problems such as liquid absorption amount is insufficient, using dickite as raw material, processing using urea, potassium chlorate to dickite obtains dickite
Porous structure feature, and using porous dickite as coating material, it is coated on PET non-woven fabrics matrix surface, preparation can be improved
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 separator, comprising the following steps:
A. the preparation of porous dickite
Dickite and a certain proportion of urea crush 5~20 minutes in pulverizer, make granularity 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 70 DEG C of baking ovens later 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. porous dickite/PET diaphragm preparation
After evenly mixing by porous dickite and binder, water, modifying agent 60-80:33-13:5:2 in mass ratio, 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
The dry PET nonwoven cloth diaphragm for just having obtained porous dickite coating in 40 DEG C of vacuum oven out.
Above-described dickite is the dickite for originating from the white county of Jilin governor, other siliceous miscellaneous phase contents are less than 5%, ground
Stone crystallization index Hinckley index value is opened greater than 1；The binder be LA132 (the aqueous electrode adhesive of LA type) or
LA132 and SBR (butadiene-styrene rubber) mixture；The modifying agent is silane coupling agent DL171.
The utility model has the advantages that the present invention is coating raw material with the dickite with porous structure, PET non-woven fabrics is that basement membrane preparation is more
Hole dickite/PET diaphragm, the diaphragm prepare the hole forming machine of composite diaphragm with the Nano Ceramic Particles coating non-woven fabrics largely reported
System is different.The gap that the latter is formed after nonwoven surface is piled up using a large amount of nanoparticles is as the hole of diaphragm transmission lithium ion
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 then utilizes the macroporous structure (0.1-1 μm of aperture size) of porous dickite to pass as diaphragm
The channel of defeated lithium ion can effectively improve the conductivity of lithium ion, reduce resistance.Meanwhile utilizing dickite surface official abundant
It can roll into a ball, the stability of high temperature flowering structure, diaphragm can be significantly improved to the wetability, imbibition rate and heat of electrolyte after coating non-woven fabrics
Stability, to improve stable circulation performance of battery during high current charge-discharge.Porous dickite/PET diaphragm hole
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 diaphragm
(72%).
Detailed description of the invention
The stereoscan photograph of Fig. 1, porous dickite
Fig. 2, porous dickite/PET diaphragm LiMn is used2O4The 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 and a certain proportion of urea crush 5~20 minutes in pulverizer, make granularity 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 70 DEG C of baking ovens later 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. porous dickite/PET diaphragm preparation
After evenly mixing by porous dickite and binder, water, modifying agent 60-80:33-13:5:2 in mass ratio, 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
The dry PET nonwoven cloth diaphragm for just having obtained porous dickite coating in 40 DEG C of vacuum oven out.
Embodiment 1
A. dickite and a certain proportion of urea crush 10 minutes in pulverizer, make granularity 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 high fire in micro-wave oven and heats 17 minutes, is 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 is calcined 15 seconds, obtain porous dickite powder；
E. after evenly mixing by porous dickite and binder, water, modifying agent 80:13:5:2 in mass ratio, in refiner
Middle stirring obtains coating slurry for 1 hour；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, is then taken out dry in 40 DEG C of vacuum oven
Obtain the non-woven fabric compounded diaphragm 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 and a certain proportion of urea crush 15 minutes in pulverizer, make granularity 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 high fire in micro-wave oven and heats 15 minutes, is 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 is calcined 15 seconds, obtain porous dickite powder；
E. after evenly mixing by porous dickite and binder, water, modifying agent 70:23:5:2 in mass ratio, in refiner
Middle stirring obtains coating slurry for 2 hours；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, is then taken out dry in 40 DEG C of vacuum oven
Obtain the non-woven fabric compounded diaphragm 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 and a certain proportion of urea crush 5 minutes in pulverizer, make granularity 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 high fire in micro-wave oven and heats 20 minutes, is 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 is calcined 15 seconds, obtain porous dickite powder；
E. after evenly mixing by porous dickite and binder, water, modifying agent 60:33:5:2 in mass ratio, in refiner
Middle stirring obtains coating slurry for 1 hour；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, is then taken out dry in 40 DEG C of vacuum oven
Obtain the non-woven fabric compounded diaphragm 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 and a certain proportion of urea crush 20 minutes in pulverizer, make granularity 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 high fire in micro-wave oven and heats 10 minutes, is 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 is calcined 15 seconds, obtain porous dickite powder；
E. after evenly mixing by porous dickite and binder, water, modifying agent 75:18:5:2 in mass ratio, in refiner
Middle stirring obtains coating slurry for 2 hours；
F. PET non-woven fabrics is immersed in coating slurry 30 minutes, is then taken out dry in 40 DEG C of vacuum oven
Obtain the non-woven fabric compounded diaphragm 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
It is rapid:
A. dickite and a certain proportion of urea crush 5~20 minutes in pulverizer, make granularity 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 70 DEG C of baking ovens later 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, obtained
To porous dickite powder；
B. after evenly mixing by porous dickite and binder, water, modifying agent 60-80:33-13:5:2 in mass ratio, 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 oven in it is dry after obtain the PET nonwoven cloth diaphragm 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, and siliceous miscellaneous phase content is less than 5%, dickite
Crystallization index Hinckley index value is greater than 1；The binder is LA132 or LA132 and SBR mixture；The modifying agent
For silane coupling agent DL171.
3. a kind of porous dickite coats non-woven fabrics lithium ion battery separator, it is characterised in that: any according to claim 1-2
Method is made.
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| CN108183191B true CN108183191B (en) | 2019-09-03 |
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| CN108807799B (en) * | 2018-08-07 | 2020-04-28 | 吉林大学 | Expanded dickite modified lithium ion battery diaphragm and preparation method thereof |
| 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 |
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| CN103107301B (en) * | 2013-01-17 | 2015-04-08 | 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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