CN109817867A - A kind of heat sensitive coatings material, thermal sensitivity diaphragm and the preparation method and application thereof - Google Patents
A kind of heat sensitive coatings material, thermal sensitivity diaphragm and the preparation method and application thereof Download PDFInfo
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- CN109817867A CN109817867A CN201811564103.5A CN201811564103A CN109817867A CN 109817867 A CN109817867 A CN 109817867A CN 201811564103 A CN201811564103 A CN 201811564103A CN 109817867 A CN109817867 A CN 109817867A
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- heat sensitive
- sensitive coatings
- thermal expansion
- diaphragm
- coatings 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
Abstract
The invention discloses a kind of heat sensitive coatings materials, thermal sensitivity diaphragm and the preparation method and application thereof.The heat sensitive coatings material, the component including following mass percent: polymeric binder 3% ~ 10%, inorganic, metal oxide 80% ~ 90%, dispersing agent 0.5% ~ 1% and thermal expansion polymer microballoon 5% ~ 15%.Heat sensitive coatings material provided by the invention includes polymeric binder, inorganic, metal oxide, dispersing agent and thermal expansion polymer microballoon.Battery security performance with higher during overcharging is made by thermal sensitivity diaphragm prepared by the heat sensitive coatings material, and there is preferable structural stability.
Description
Technical field
The present invention relates to battery diaphragm field, more particularly, to a kind of heat sensitive coatings material, thermal sensitivity diaphragm and its
Preparation method and application.
Background technique
With the development of electronic communication equipment, computer equipment and mobile communication equipment, to as these equipment power supplys
Lithium secondary battery demand it is growing day by day.The research and development tide of one lithium secondary battery is started in worldwide, this
Outside, lithium secondary battery serves not only as the power supply of mobile electronic device, can also be used as electric car, electric tool, satellite etc. and sets
Standby environmentally friendly power supply.
Lithium secondary battery includes lithium transition alkaline metal oxide anode, can the cathode of embedding lithium ionic insertion/deinsertion, positive electrode and negative electrode
Between diaphragm, as the electrolyte of lithium ion mobility carrier.The main function of diaphragm is to keep apart positive electrode and negative electrode, and incite somebody to action
Electrolyte is remained to guarantee high ionic conductivity.Currently, widely used diaphragm be MIcroporous polyolefin film, it is such every
Film closed pore temperature with higher and slower closed pore speed, so that ternary anode material for lithium-ion batteries system is in over-charging of battery
Safety when electric is unable to get guarantee.
In order to improve safety when ternary anode material for lithium-ion batteries system over-charging of battery, current line is generally logical in the industry
It crosses in membrane surface coated ceramic layer, improves overcharge safety by improving diaphragm temperature tolerance, but such method is in nickelic body
Applicability in system is poor, the diaphragm can not timely closed pore, lead to thermal runaway during over-charging of battery.The prior art
CN107492620A by base material film coat by the coating of polymeric binder, modified alkaline metal oxide and solvent come
The heat resistance and compatibility of diaphragm are improved, but the security performance during can not ensuring to overcharge completely.
Therefore, it is necessary to prepare a kind of diaphragm that overcharge safety can be high.
Summary of the invention
The present invention is to overcome the defect of the overcharge safety energy difference of diaphragm described in the above-mentioned prior art, provides a kind of thermal sensitivity
Coating material.The overcharge safety of the thermal sensitivity diaphragm as made from the heat sensitive coatings material can be high.
Another object of the present invention is to provide the preparation methods of above-mentioned heat sensitive coatings material.
Another object of the present invention is to provide application of the above-mentioned heat sensitive coatings material in battery diaphragm.
A further purpose of the present invention is to provide thermal sensitivity diaphragm made from above-mentioned heat sensitive coatings material.
A further purpose of the present invention is to provide the preparation method of above-mentioned thermal sensitivity diaphragm.
A further object of the present invention is to provide application of the above-mentioned thermal sensitivity diaphragm in lithium ion battery or capacitor.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of heat sensitive coatings material, the component including following mass percent: polymeric binder 3% ~ 10%, inorganic metal oxygen
Compound 80% ~ 90%, dispersing agent 0.5% ~ 1% and thermal expansion polymer microballoon 5% ~ 15%.
Heat sensitive coatings material provided by the invention includes polymeric binder, inorganic, metal oxide, dispersing agent and heat
Expanded polymeric microspheres.Thermal expansion polymer microballoon has good electrolyte resistance and voltage endurance, improves heat sensitive coatings
The structural stability of material in use；There is good adhesive force by the coating material that thermal expansion polymer microballoon forms
And uniformity, there is temperature-sensitive sexual function.Compared with traditional coating material, the present invention is heated swollen using thermal expansion polymer microballoon
Swollen feature when so that battery temperature reaching the expansion temperature of thermal expansion polymer microballoon in coating material during overcharging, applies
Layer expansion rapidly, so that the internal resistance of cell increases rapidly, and then has the function that cut off electric current, to realize protection battery mistake
Fill the purpose of safety.
Preferably, the heat sensitive coatings material includes the component of following mass percent: polymeric binder 4%, inorganic
Metal oxide 85.5%, dispersing agent 0.5% and thermal expansion polymer microballoon 10%.
Preferably, the thermal expansion polymer microballoon is nucleocapsid structure.
Preferably, the shell is thermoplastic polymer, and core is protective gas.
Preferably, the expansion temperature of the thermal expansion polymer microballoon is 90 ~ 140 DEG C.
When temperature reaches the expansion temperature of thermoplastic polymer, thermal expansion polymer microballoon is acted on by internal gas pressure
Expansion rapidly increases 30 ~ 50 times in 10 s inner volumes.
Preferably, the thermoplastic polymer is thermal expansion type acrylic resin, thermal expansion type polyolefin resin, thermal expansion
One of type polyurethane resin is a variety of.
Using the thermoplasticity of the fluoropolymer resins such as acrylic resin, polyolefin resin, polyurethane resin, in certain temperature
Under, fluoropolymer resin is viscoelastic state by glassy transition.Nucleocapsid structure is made in thermoplastic polymer and protective gas, works as temperature
When degree reaches fluoropolymer resin and is changed into viscoelastic state, since when gases are heated, they expand, acted on by gas tension, outside fluoropolymer resin
Shell expands rapidly.
Preferably, the thermoplastic polymer is acrylic resin, hyperbranched poly allyl resin, hyperbranched polyethylene tree
One or more of rouge, ethylene-propylene copolymer, polyurethane resin.
It is highly preferred that the thermal expansion polymer microballoon is polyacrylic acid matrix microspheres, hyperbranched poly acrylic
One of thermal expansion microballoon, hyperbranched polyethylene matrix microspheres, ethylene-propylene copolymer matrix microspheres are several
Kind.Thermal expansion polymer microballoon can be by being prepared, can also be by being commercially available.
Preferably, the thermoplastic polymer does not dissolve in lithium battery electrolytes solvent.
Preferably, the lithium battery electrolytes solvent is ethylene carbonate, propene carbonate, dimethyl carbonate, carbonic acid two
Ethyl ester or methyl ethyl carbonate.
Preferably, the protective gas is one or more of carbon dioxide, nitrogen, argon gas, helium.
Preferably, the polymeric binder be polyacrylate, polyolefin modified polymer, epoxy resin, polyamide,
One or more of polyurethane.
Preferably, the dispersing agent is polyacrylate.
It is highly preferred that the polyacrylate is Sodium Polyacrylate or ammonium polyacrylate.
Preferably, the inorganic, metal oxide is aluminium oxide, silica, titanium oxide, zirconium oxide, zinc oxide, boehmite
One or more of.
The present invention protects the preparation method of above-mentioned heat sensitive coatings material simultaneously, and the preparation method includes the following steps:
After polymeric binder, inorganic, metal oxide and thermal expansion polymer microballoon are mixed dispersion, heat sensitive coatings material is obtained.
Preferably, specific step is as follows for the preparation method: dispersing agent is added to the water 30 ~ 60 min of moderate-speed mixer,
Then inorganic, metal oxide and thermal expansion polymer microballoon are added, 60 ~ 120 min of high-speed stirred is eventually adding polymer
Then binder, 30 ~ 60 min of moderate-speed mixer stir at low speed 30 ~ 60 min degasification, cross sieve later and obtain heat sensitive coatings material
Material.During the preparation process, water is generally deionized water.
It is highly preferred that specific step is as follows for the preparation method: dispersing agent being added to the water 30 min of stirring, then again
Inorganic, metal oxide is added and thermal expansion polymer microballoon, 60 min of high-speed stirred are eventually adding polymeric binder, middling speed
60 min are stirred, 30 min degasification are then stirred at low speed, sieve is crossed later and obtains heat sensitive coatings material.
Preferably, the dispersing agent is for dispersing inorganic, metal oxide.
Preferably, the low speed is 500 ~ 1000 r/min, and it is at a high speed 3000 r/min that middling speed, which is 1500 r/min,.
The present invention protects application of the above-mentioned heat sensitive coatings material in battery diaphragm simultaneously.
The present invention also protects a kind of thermal sensitivity diaphragm, and the thermal sensitivity diaphragm includes basement membrane and above-mentioned heat sensitive coatings material
Material.
Preferably, the basement membrane is polymer microporous film.
Preferably, the polymer in the polymer microporous film is low density polyethylene (LDPE), high density polyethylene (HDPE), low-density line
Property polyethylene, ultra-high molecular weight polyethylene, polypropylene, polyethylene terephthalate, polybutylene terephthalate, polyamides
One or more of amine, polyimides, polyurethane.
The present invention also protects the preparation method of above-mentioned thermal sensitivity diaphragm, and the preparation method includes the following steps: will be above-mentioned
Heat sensitive coatings material is coated on basement membrane, obtains thermal sensitivity diaphragm.
Preferably, the thermal sensitivity diaphragm includes basement membrane and heat sensitive coatings.
Preferably, the heat sensitive coatings with a thickness of 1 ~ 4 μm.
Preferably, the thermal sensitivity diaphragm with a thickness of 7 ~ 40 μm.It is highly preferred that the thermal sensitivity diaphragm with a thickness of
25 μm。
Preferably, the porosity of the basement membrane is 30% ~ 70%.It is highly preferred that the porosity of the basement membrane is 50%.
Preferably, the mode of the coating is one or more of intaglio plate coating, spraying, dip-coating.It is highly preferred that described
The mode of coating is intaglio plate coating.
Preferably, the temperature of the intaglio plate coating is 40 ~ 60 DEG C.
Preferably, the speed of the intaglio plate coating is 10 ~ 40m/min.It is highly preferred that the speed of the intaglio plate coating is 20
m/min。
The present invention also protects application of the above-mentioned thermal sensitivity diaphragm in lithium ion battery or capacitor.
Compared with prior art, the beneficial effects of the present invention are:
Heat sensitive coatings material provided by the invention includes polymeric binder, inorganic, metal oxide, dispersing agent and thermal expansion
Polymer microballoon.The thermal sensitivity diaphragm as made from the heat sensitive coatings material makes battery peace with higher during overcharging
Full performance, and there is preferable structural stability.
Detailed description of the invention
Fig. 1 is that diaphragm produced by the present invention overcharges curve at 1C 6.5V.
Specific embodiment
The invention will be further described With reference to embodiment, but embodiments of the present invention are not limited to
This.Raw material in embodiment can be by being commercially available；Unless stated otherwise, the present invention uses reagent, method and apparatus for
The art conventional reagent, method and apparatus.
Thermal expansion polymer microballoon is nucleocapsid structure；Shell is acrylic resin, hyperbranched poly allyl resin, hyperbranched poly
The thermoplastic polymers such as vinyl, ethylene-propylene copolymer, polyurethane resin；Core is carbon dioxide, nitrogen, argon gas, helium.
Thermal expansion polymer microballoon can be by being prepared, can also be by being commercially available.In embodiment, used
Thermal expansion polymer microballoon buys the product that other company's productions also can be used in Akzo Nobel N.V..
Embodiment 1
A kind of heat sensitive coatings material, the component including following mass percent: polyacrylate binder 4%, aluminium oxide
85.5%, Sodium Polyacrylate 0.5% and polyacrylic acid matrix microspheres 10%.
A kind of thermal sensitivity diaphragm and preparation method thereof, includes the following steps:
(1) slurry preparation: the Sodium Polyacrylate of 0.5 mass parts is added in the deionized water of 65.5 mass parts, in 1500 r/
30 min are stirred under min, and the aluminium oxide of 85.5 mass parts and the polyacrylic acid matrix microspheres of 10 mass parts is then added,
60 min are stirred at 3000 r/min of high speed, are eventually adding the polyacrylate binder of 4 mass parts, 1500 r/min of middling speed
60 min of lower stirring, then 500 r/min of low speed stirs 30 min degasification, crosses sieve later and obtains heat sensitive coatings material.
(2) it is coated with: heat sensitive coatings material is coated in 12 μm of polyethylene micropore film sides using plate gravure coating method,
Obtain 4 μm of heat sensitive coatings.In coating process, temperature control is 40 ~ 60 DEG C, and coating speed is 20 m/min, is wound
To thermal sensitivity diaphragm.
Embodiment 2
A kind of heat sensitive coatings material, the component including following mass percent: polyacrylate binder 4%, aluminium oxide
85.5%, Sodium Polyacrylate 0.5% and hyperbranched poly polypropylene matrix microspheres 10%.
A kind of thermal sensitivity diaphragm and preparation method thereof:
The present embodiment the difference from embodiment 1 is that, thermal expansion polymer microballoon is hyperbranched poly in (1) the step of the present embodiment
Polypropylene matrix microspheres；
Other raw material dosages and operating procedure are same as Example 1.
Embodiment 3
A kind of heat sensitive coatings material, the component including following mass percent: polyacrylate binder 4%, aluminium oxide
85.5%, Sodium Polyacrylate 0.5% and hyperbranched polyethylene matrix microspheres 10%.
A kind of thermal sensitivity diaphragm and preparation method thereof:
The present embodiment the difference from embodiment 1 is that, thermal expansion polymer microballoon is hyperbranched poly in (1) the step of the present embodiment
Vinyl thermal expansion microballoon；
Other raw material dosages and operating procedure are same as Example 1.
Embodiment 4
A kind of heat sensitive coatings material, the component including following mass percent: polyacrylate binder 4%, aluminium oxide
85.5%, Sodium Polyacrylate 0.5% and ethylene-propylene copolymer matrix microspheres 10%.
A kind of thermal sensitivity diaphragm and preparation method thereof:
The present embodiment the difference from embodiment 1 is that, thermal expansion polymer microballoon is Propylene polymerization in (1) the step of the present embodiment
Object matrix microspheres；
Other raw material dosages and operating procedure are same as Example 1.
Embodiment 5
A kind of heat sensitive coatings material, the component including following mass percent: polyolefin modified polymeric binder 4%, oxidation
Silicon 80%, ammonium polyacrylate 1% and polyacrylic acid matrix microspheres 15%.
A kind of thermal sensitivity diaphragm and preparation method thereof:
The present embodiment the difference from embodiment 1 is that, the polyolefin modified poly- of 4 mass parts is added the step of the present embodiment in (1)
Close object binder, the silica of 80 mass parts, the polyacrylic acid matrix microspheres of 15 mass parts, 1 mass parts polypropylene
Sour ammonium；
Other raw material dosages and operating procedure are same as Example 1.
Embodiment 6
A kind of heat sensitive coatings material, the component including following mass percent: epoxy adhesive 4.5%, titanium oxide 90%,
Sodium Polyacrylate 0.5% and polyacrylic acid matrix microspheres 5%.
A kind of thermal sensitivity diaphragm and preparation method thereof:
The present embodiment the difference from embodiment 1 is that, epoxy resin that 4.5 mass parts are added the step of the present embodiment in (1) is viscous
Tie agent, the titanium oxide of 90 mass parts, the polyacrylic acid matrix microspheres of 5 mass parts, 0.5 mass parts Sodium Polyacrylate；
Other raw material dosages and operating procedure are same as Example 1.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, thermal expansion polymer microballoon, and oxygen is not added in (1) the step of comparative example 1
Change aluminium is 95.5 mass parts；
Other raw material dosages and operating procedure are same as Example 1.
The test of diaphragm overcharge safety
Thermal sensitivity diaphragm made from embodiment 1 ~ 6 and comparative example 1 is subjected to overcharge safety verifying, using Soft Roll model
505076,2500 mAh of design capacity, anode use NCM523 ternary material, and cathode uses artificial graphite, respectively test implementation
The diaphragm sample 1C 6.5V overcharge safety of example 1 ~ 4 and comparative example 1.Test results are shown in figure 1, and S1 ~ S4 difference is marked in figure
Indicate that thermal sensitivity diaphragm made from embodiment 1 ~ 4, DS1 are diaphragm made from comparative example 1.
Table 1 is the test data of internal resistance made from embodiment 1 ~ 6 and comparative example 1 and microspheres variation.From table 1
Test result it is found that battery temperature reaches 120 DEG C of expansion temperature of thermoplastic polymer in coating material during overcharge
When, thermal expansion polymer microballoon is acted on expansion rapidly by internal gas pressure, in the partial size of 10 s thermal expansion polymer microballoons
3 ~ 4 times are increased, volume increases 30 ~ 50 times.So that increasing 4.5 ~ 10 times in 10 s of the internal resistance of cell, and then reaches and cut
The effect of stream is powered off, realizes the purpose of protection over-charging of battery safety.
Fig. 1 is that diaphragm produced by the present invention overcharges curve at 1C 6.5V, it is seen then that thermal sensitivity made from embodiment 1 ~ 4
Diaphragm can be tested by overcharge safety.Equally, thermal sensitivity diaphragm made from embodiment 5 ~ 6 can also be surveyed by overcharge safety
Examination.However, situation on fire occurs during overcharging in comparative example 1, thermal runaway occurs for battery mainly due to battery mistake at this time
It is relatively small to fill process internal resistance, overcharge process polarization it is smaller, cause its side reaction phase duration longer, to make battery
Accumulated inside more heat transfer leads to thermal runaway.
Internal resistance made from 1 embodiment 1 ~ 6 of table and comparative example 1 and microspheres variation
It follows that thermal sensitivity diaphragm provided by the invention utilizes the characteristics of thermal expansion polymer microballoon expanded by heating, so that mistake
When battery temperature reaches the expansion temperature of thermal expansion polymer microballoon in coating material during filling, heat sensitive coatings are swollen rapidly
It is swollen, so that the internal resistance of cell increases rapidly, and then has the function that cut off electric current, to realize protection over-charging of battery safety
Purpose.The overcharge safety of thermal sensitivity diaphragm produced by the present invention can be high, and chemical stability is good.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of heat sensitive coatings material, which is characterized in that the component including following mass percent: polymeric binder 3% ~
10%, inorganic, metal oxide 80% ~ 90%, dispersing agent 0.5% ~ 1% and thermal expansion polymer microballoon 5% ~ 15%.
2. heat sensitive coatings material according to claim 1, which is characterized in that the component including following mass percent:
Polymeric binder 4%, inorganic, metal oxide 85.5%, dispersing agent 0.5% and thermal expansion polymer microballoon 10%.
3. heat sensitive coatings material according to claim 1 or 2, which is characterized in that the thermal expansion polymer microballoon is
Nucleocapsid structure；The shell is thermoplastic polymer, and core is protective gas.
4. heat sensitive coatings material according to claim 3, which is characterized in that the thermoplastic polymer is acrylic acid tree
One or more of rouge, hyperbranched poly allyl resin, hyperbranched polyethylene resin, ethylene-propylene copolymer, polyurethane resin.
5. heat sensitive coatings material according to claim 3, which is characterized in that the dispersing agent is polyacrylate.
6. heat sensitive coatings material according to claim 1, which is characterized in that the inorganic, metal oxide is oxidation
One or more of aluminium, silica, titanium oxide, zirconium oxide, zinc oxide, boehmite.
7. the preparation method of the described in any item heat sensitive coatings materials of claim 1 ~ 6, which is characterized in that including walking as follows
It is rapid: after polymeric binder, inorganic, metal oxide, dispersing agent and thermal expansion polymer microballoon are mixed dispersion, to obtain temperature-sensitive
Property coating material.
8. application of the described in any item heat sensitive coatings materials of claim 1 ~ 6 in battery diaphragm.
9. a kind of thermal sensitivity diaphragm, which is characterized in that including basement membrane and the described in any item heat sensitive coatings materials of claim 1 ~ 6
Material.
10. application of the thermal sensitivity diaphragm as claimed in claim 9 in lithium ion battery or capacitor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811564103.5A CN109817867A (en) | 2018-12-20 | 2018-12-20 | A kind of heat sensitive coatings material, thermal sensitivity diaphragm and the preparation method and application thereof |
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| CN201811564103.5A CN109817867A (en) | 2018-12-20 | 2018-12-20 | A kind of heat sensitive coatings material, thermal sensitivity diaphragm and the preparation method and application thereof |
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Cited By (3)
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| CN112599926A (en) * | 2019-09-17 | 2021-04-02 | 上海恩捷新材料科技有限公司 | Self-partition functional battery diaphragm, lithium ion battery and preparation method of self-partition functional battery diaphragm |
| CN113436787A (en) * | 2021-06-30 | 2021-09-24 | 江苏科麦特科技发展有限公司 | Heat-sensitive conductive film and preparation method and application thereof |
| CN115548583A (en) * | 2022-11-24 | 2022-12-30 | 合肥长阳新能源科技有限公司 | High-safety lithium ion battery composite diaphragm and application thereof |
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Effective date of registration: 20200220 Address after: 519000 New Green Science Park, Mount Everest Avenue, Jing'an Town, Doumen District, Zhuhai, Guangdong Applicant after: ZHUHAI PENGHUI ENERGY Co.,Ltd. Address before: 511483 Guangdong city of Guangzhou province Panyu District Shawan Town Nishimura Liang Road No. 912 Applicant before: GUANGZHOU GREAT POWER ENERGY & TECHNOLOGY Co.,Ltd. |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190528 |