CN105280863A - Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery - Google Patents

Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery Download PDF

Info

Publication number
CN105280863A
CN105280863A CN201510656357.XA CN201510656357A CN105280863A CN 105280863 A CN105280863 A CN 105280863A CN 201510656357 A CN201510656357 A CN 201510656357A CN 105280863 A CN105280863 A CN 105280863A
Authority
CN
China
Prior art keywords
polyphenylene sulfide
basement membrane
preparation
particle
inorganic nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510656357.XA
Other languages
Chinese (zh)
Inventor
王罗新
陈萌
陈少华
吴静
殷先泽
王桦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Textile University
Original Assignee
Wuhan Textile University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Textile University filed Critical Wuhan Textile University
Priority to CN201510656357.XA priority Critical patent/CN105280863A/en
Publication of CN105280863A publication Critical patent/CN105280863A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403Manufacturing processes of separators, membranes or diaphragms
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409Separators, membranes or diaphragms characterised by the material
    • H01M50/431Inorganic material
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention relates to a preparation method of a polyphenylene sulfide ceramic composite membrane for a lithium ion battery. Aiming at the common security problem of lithium batteries in the existing ceramic composite membranes due to the insufficient temperature resistance of polyolefin basement membranes and easily melted and contracted basement membranes, the preparation method provided by the invention comprises a step of coating ceramic slurries prepared by inorganic nanoparticles and adhesives onto a surface of a polyphenylene sulfide basement membrane with a high melting point, and then the polyphenylene sulfide ceramic composite membrane can be prepared. Compared with a polyolefin ceramic composite membrane, the thermal stability of the polyphenylene sulfide ceramic composite membrane is obviously improved and the security of the lithium ion battery can be effectively improved. The preparation method of a modified polyphenylene sulfide non-woven fabric lithium ion battery membrane provided by the invention is simple in operation and low in cost; the prepared polyphenylene sulfide ceramic composite membrane for the lithium ion battery has outstanding thermal stability, excellent chemical resistance, and good mechanical strength, can be applied to power ion batteries or high capacity energy storage batteries, and has a good application prospect.

Description

A kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film
Technical field
The present invention relates to a kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film, belong to new energy materials field.
Background technology
Lithium ion battery applications is extensive, becomes the focus of novel power supply investigative technique in recent years.In the structure of lithium battery, barrier film is one of interior layer assembly of key, in the material manufacturing battery, occupy very important status.At present, business-like lithium ion battery separator is based on microporous polyolefin film, its limitation is that barrier film is difficult to ensure high temperature integrity, namely severe heat shrinkage even melting destruction can be there is under the high temperature of barrier film more than 150 DEG C, the fail safe of lithium battery is reduced, and power, energy storage lithium ion battery require higher to the heat resistance of barrier film, conventional polyolefin barrier film is used to there is potential potential safety hazard.Take polyolefin porous membrane as basement membrane, adopt coating method to prepare polyolefin ceramic coating membrane, improve the heat resistance of barrier film and the fail safe of battery to a certain extent.
Chinese patent (publication number CN102651466A, CN102529247A, CN103682217A, CN104064710A) by carrying out preliminary treatment to polyolefin porous membrane or nonwoven substrate, then at membrane surface composite inorganic oxide ceramic coating, obtain the Ceramic Composite barrier film for lithium ion battery, thus the thermal endurance of raising barrier film, ionic conductivity and mechanical strength.But, polyolefin base membrane heat resistance is limited, being usually less than 150 DEG C, still there is the inadequate problem of polyolefin base membrane temperature tolerance in the organic/inorganic composite diaphragm based on polyolefin porous membrane or non-weaving cloth, and the battery damage that basement membrane fusing contraction causes and safety issue still exist.
Chinese patent mandate publication number CN102433745B, authorize publication date, 2013.5.29, denomination of invention is " power lithium battery diaphragm coating, power lithium battery diaphragm and preparation thereof ", this application scheme is manufactured paper with pulp with PET wet method or PET and natural fiber join the nonwoven fabrics copied for base material, masking liquid prepared by chlorination vinylidene and glycerol, clorox, DMF and SiC Nanometer Whiskers is coated on substrate surface, obtain lithium ion battery composite separation membrane, the method increase the pick up of barrier film, electric property, resistance to elevated temperatures.But the non-woven fabrics base material that this barrier film preparation method uses is comparatively thick due to fiber, can only prepare thicker composite diaphragm.
For the technical development of the security performance and high power battery that improve lithium ion battery further, with high temperature resistant, that corrosion-resistant material manufactures lithium ion battery separator technology is causing people concern.A kind of high-performance special fibrous raw material of polyphenylene sulfide, has the characteristics such as excellent chemical resistance, high temperature resistant and anti-adverse environment, fire-retardant, insulation, radiation proof, very applicablely prepares high-capacity lithium ion cell barrier film.
In existing polyphenylene sulfide lithium ion battery separator technology, China Patent Publication No. CN103205123A, publication date on July 17th, 2013, patent of invention name is called " a kind of production method of lithium battery polyphenylene sulfide diaphragm ", and this invention, by polyphenylene sulfide high-temperature digestion, obtains homogeneous phase solution, homogeneous phase solution casting machine is extruded and Quench, obtain polyphenylene sulfide porous film, battery diaphragm broken film temperature prepared by the method is high, good flame resistance.But this kind of procedure is comparatively loaded down with trivial details, and the organic solvent of use mostly is toxic solvent, not environmentally.China Patent Publication No. CN104795525A, publication date on July 22nd, 2015, patent of invention name is called " a kind of melt-blown polyphenylene sulfide nonwoven fabrics lithium battery diaphragm and preparation method thereof ", this invention adopts melt-blown polyphenylene sulfide nonwoven fabrics as base cloth, and hot rolling and thermal finalization process are carried out to base cloth, obtained polyphenylene sulfide lithium ion battery separator.This barrier film has the advantages such as fusing point is high, broken film temperature is high, good flame resistance, chemical resistance are good, dimensionally stable, absorbency are good.But polyphenylene sulfide meltblown nonwoven fabrics is applicable to prepare thicker lithium ion battery separator, preparing compared with there is membrane pore size excessive problem during thin membrane, easily causing the lithium battery assembled that the defects such as electric leakage occur.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the object of the present invention is to provide a kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film, slurry by inorganic nano-particle and bonding agent preparation is coated to dystectic polyphenylene sulfide membrane surface, obtain polyphenylene sulfide Ceramic Composite barrier film, effectively control the aperture of barrier film, improve the thermal stability of barrier film, the technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film.
Described preparation method refers to the surface-coated one deck ceramic size at polyphenylene sulfide basement membrane, obtained polyphenylene sulfide Ceramic Composite barrier film after dry, and its preparation method comprises the following steps:
1. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry.
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25 ~ 30%, binding agent mass concentration scope 2-18%.
Described inorganic nano-particle is one or more compositions mixed in any proportion in silicon dioxide or alundum (Al2O3) or titanium dioxide or zirconia or zinc oxide or magnesium oxide.
Described binding agent is the one in vinyl polysiloxane or Kynoar or Kynoar-hexafluoropropylene or polytetrafluoroethylene or poly-inclined fluorine diene-trichloroethylene.
Described solvent is the one of absolute ethyl alcohol or acetone or DMF.
2. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated to through 1. obtained ceramic coated slurry in the upper and lower surface that fusing point is 280 ~ 290 DEG C of polyphenylene sulfide basement membranes.
Wherein, described painting method is the one in rolling method or scraper for coating method or cast coating method or intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2 ~ 10um.
3. dry process
2. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 110 ~ 150 DEG C; Described drying mode can adopt directly dries or vacuumize or heated-air drying.
Described a kind of lithium ion battery polyphenylene sulfide Ceramic Composite membrane thicknesses is 14 ~ 80um, and porosity is porosity is 40 ~ 60%, and aperture is 0.1 ~ 0.4um.
Owing to have employed above technical scheme, the preparation method of a kind of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film of the present invention, has the following advantages:
The slurry of inorganic nano-particle and bonding agent preparation is coated to dystectic polyphenylene sulfide membrane surface by 1 the present invention, drying process forms the ceramic coating of one deck densification, effectively control aperture and the thickness of barrier film, owing to containing inorganic nano-particle in ceramic coating, not only increase the specific area of barrier film, also improve the thermal stability of barrier film and the being folded without breaking ability of tiny area, and the pick up to electrolyte.
2 coating methods of the present invention adopt rolling methods or scraper for coating method or cast coating method or plate gravure coating method, by controlling the parameter of coating machine and the proportioning of composite filtering material, the coating thickness that can obtain the upper and lower surface of different polyphenylene sulfide basement membrane divides other polyphenylene sulfide Ceramic Composite barrier film, thus well control the percent thermal shrinkage of barrier film, pick up and ionic conductivity, height ratio capacity.
3 lithium ion battery polyphenylene sulfide Ceramic Composite barrier films of the present invention, at high temperature there are excellent intensity, rigidity and fatigue durability, especially can keep stable at 250 DEG C, the short circuit blast caused because of diaphragm retracts under can avoiding the condition of high temperature, improves the security performance of battery.
4 lithium ion battery polyphenylene sulfide Ceramic Composite barrier films of the present invention, simple to operate, cost is low, has excellent thermal stability, chemical resistance, anti-flammability, is expected to be applied to power lithium-ion battery and high-efficiency energy-storage lithium ion battery.
Embodiment
Below in conjunction with instantiation, the present invention is described in further detail.
The object of the present invention is to provide a kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film, by the slurry that inorganic nano-particle and bonding agent are prepared, be coated to polyphenylene sulfide membrane surface, obtain polyphenylene sulfide Ceramic Composite barrier film, effectively control the aperture of polyphenylene sulfide Ceramic Composite barrier film, improve polyphenylene sulfide Ceramic Composite barrier film thermal stability, obtain the polyphenylene sulfide Ceramic Composite barrier film with height ratio capacity.
A kind of preparation method of lithium ion battery polyphenylene sulfide Ceramic Composite barrier film:
Described preparation method refers to the surface-coated one deck ceramic size at polyphenylene sulfide basement membrane, obtained polyphenylene sulfide Ceramic Composite barrier film after dry, and its preparation method comprises the following steps:
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 280 ~ 290 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point.
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.5 ~ 3um, and polyphenylene sulfide basement membrane thickness is 10 ~ 60um, and porosity is 50 ~ 80%, and aperture is 0.8 ~ 3um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25 ~ 30%, binding agent mass concentration scope 2-18%.
Described inorganic nano-particle is one or more compositions mixed in any proportion in silicon dioxide or alundum (Al2O3) or titanium dioxide or zirconia or zinc oxide or magnesium oxide.
Described binding agent is the one in vinyl polysiloxane or Kynoar or Kynoar-hexafluoropropylene or polytetrafluoroethylene or poly-inclined fluorine diene-trichloroethylene.
Described solvent is the one of absolute ethyl alcohol or acetone or DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry.
Wherein, described painting method is the one in rolling method or scraper for coating method or cast coating method or intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2 ~ 10um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 110 ~ 150 DEG C; Described drying mode can adopt directly dries or vacuumize or heated-air drying.
Described a kind of lithium ion battery polyphenylene sulfide Ceramic Composite membrane thicknesses is 14 ~ 80um, and porosity is porosity is 40 ~ 60%, and aperture is 0.1 ~ 0.4um.
Specific embodiment
By above-mentioned preparation method.
embodiment 1
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 280 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.5um, and polyphenylene sulfide basement membrane thickness is 10um, and porosity is 50%, and aperture is 0.8um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25%, binding agent mass concentration scope 2%; Described inorganic nano-particle is silicon dioxide; Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 110 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 14um, and porosity is porosity is 40%, and aperture is 0.1um.
embodiment 2
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 280.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.6um, and polyphenylene sulfide basement membrane thickness is 12um, and porosity is 51%, and aperture is 0.9um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25.2%, binding agent mass concentration scope 2.5%; Described inorganic nano-particle is alundum (Al2O3); Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 112 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 17um, and porosity is porosity is 40.5%, and aperture is 0.11um.
embodiment 3
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 281 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.7um, and polyphenylene sulfide basement membrane thickness is 14um, and porosity is 52%, and aperture is 1.0um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25.4%, binding agent mass concentration scope 3%; Described inorganic nano-particle is titanium dioxide; Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 114 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 19um, and porosity is porosity is 41%, and aperture is 0.12um.
embodiment 4
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 281.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.8um, and polyphenylene sulfide basement membrane thickness is 16um, and porosity is 53%, and aperture is 1.1um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25.6%, binding agent mass concentration scope 3.5%; Described inorganic nano-particle is zirconia; Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 3um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 116 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 22um, and porosity is porosity is 41.5%, and aperture is 0.13um.
embodiment 5
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 282 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.9um, and polyphenylene sulfide basement membrane thickness is 18um, and porosity is 54%, and aperture is 1.2um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25.8%, binding agent mass concentration scope 4%; Described inorganic nano-particle is zinc oxide; Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 3.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 118 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 25um, and porosity is porosity is 42%, and aperture is 0.14um
embodiment 6
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 282.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 0.95um, and polyphenylene sulfide basement membrane thickness is 20um, and porosity is 55%, and aperture is 1.3um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26%, binding agent mass concentration scope 4.5%; Described inorganic nano-particle is magnesium oxide; Described binding agent is vinyl polysiloxane; Described solvent is absolute ethyl alcohol.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 4um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 120 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 28um, and porosity is porosity is 42.5%, and aperture is 0.15um
embodiment 7
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 283 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.0um, and polyphenylene sulfide basement membrane thickness is 22um, and porosity is 56%, and aperture is 1.4um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26.2%, binding agent mass concentration scope 5%; Described inorganic nano-particle is silicon dioxide; Described binding agent is Kynoar; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 4.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 122 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 31um, and porosity is porosity is 43%, and aperture is 0.16um
embodiment 8
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 283.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.1um, and polyphenylene sulfide basement membrane thickness is 24um, and porosity is 57%, and aperture is 1.5um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26.4%, binding agent mass concentration scope 5.5%; Described inorganic nano-particle is alundum (Al2O3); Described binding agent is Kynoar; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is rolling method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 124 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 34um, and porosity is porosity is 43.5%, and aperture is 0.17um
embodiment 9
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 284 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.2um, and polyphenylene sulfide basement membrane thickness is 26um, and porosity is 58%, and aperture is 1.6um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26.6%, binding agent mass concentration scope 6%; Described inorganic nano-particle is titanium dioxide; Described binding agent is Kynoar; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 5.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 126 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 37um, and porosity is porosity is 44%, and aperture is 0.18um
embodiment 10
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 284.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.2um, and polyphenylene sulfide basement membrane thickness is 26um, and porosity is 58%, and aperture is 1.6um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26.6%, binding agent mass concentration scope 6.5%; Described inorganic nano-particle is zirconia; Described binding agent is Kynoar; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 6um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 128 DEG C; Described drying mode can adopt direct oven dry.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 38um, and porosity is porosity is 44.5%, and aperture is 0.19um
embodiment 11
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 285 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.3um, and polyphenylene sulfide basement membrane thickness is 28um, and porosity is 59%, and aperture is 1.7um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 26.8%, binding agent mass concentration scope 7%; Described inorganic nano-particle is zinc oxide; Described binding agent is Kynoar; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 6.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 130 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 41um, and porosity is porosity is 45%, and aperture is 0.20um
embodiment 12
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 285.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.4um, and polyphenylene sulfide basement membrane thickness is 30um, and porosity is 60%, and aperture is 1.8um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 27%, binding agent mass concentration scope 7.5%; Described inorganic nano-particle is magnesium oxide; Described binding agent is Kynoar; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 7.0um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 132 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 44um, and porosity is porosity is 45.5%, and aperture is 0.21um
embodiment 13
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 286 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.5um, and polyphenylene sulfide basement membrane thickness is 32um, and porosity is 61%, and aperture is 1.9um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 27.2%, binding agent mass concentration scope 8%; Described inorganic nano-particle is silicon dioxide; Described binding agent is Kynoar-hexafluoropropylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 7.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 134 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 47um, and porosity is porosity is 46%, and aperture is 0.22um
embodiment 14
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 286.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.6um, and polyphenylene sulfide basement membrane thickness is 34um, and porosity is 62%, and aperture is 2.0um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 27.4%, binding agent mass concentration scope 8.5%; Described inorganic nano-particle is alundum (Al2O3); Described binding agent is Kynoar-hexafluoropropylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.0um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 136 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 50um, and porosity is porosity is 46.5%, and aperture is 0.23um
embodiment 15
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 287 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.7um, and polyphenylene sulfide basement membrane thickness is 36um, and porosity is 63%, and aperture is 2.1um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 27.6%, binding agent mass concentration scope 9%; Described inorganic nano-particle is titanium dioxide; Described binding agent is Kynoar-hexafluoropropylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.1um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 137 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 52.2um, and porosity is porosity is 47%, and aperture is 0.24um
embodiment 16
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 287.5 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.8um, and polyphenylene sulfide basement membrane thickness is 38um, and porosity is 64%, and aperture is 2.15um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 27.8%, binding agent mass concentration scope 9.5%; Described inorganic nano-particle is zirconia; Described binding agent is Kynoar-hexafluoropropylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is scraper for coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.2um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 138 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 54.4um, and porosity is porosity is 47.5%, and aperture is 0.25um
embodiment 17
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 288 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.9um, and polyphenylene sulfide basement membrane thickness is 40um, and porosity is 65%, and aperture is 2.2um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 28%, binding agent mass concentration scope 10%; Described inorganic nano-particle is zinc oxide; Described binding agent is Kynoar-hexafluoropropylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.3um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 139 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 56.6um, and porosity is porosity is 48%, and aperture is 0.26um
embodiment 18
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 288.2 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 1.95um, and polyphenylene sulfide basement membrane thickness is 42um, and porosity is 66%, and aperture is 2.25um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 28.2%, binding agent mass concentration scope 10.5%; Described inorganic nano-particle is magnesium oxide; Described binding agent is Kynoar-hexafluoropropylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.4um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 140 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 58.8um, and porosity is porosity is 48.5%, and aperture is 0.27um
embodiment 19
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 288.4 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.0um, and polyphenylene sulfide basement membrane thickness is 44um, and porosity is 67%, and aperture is 2.3um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 28.4%, binding agent mass concentration scope 11%; Described inorganic nano-particle is silicon dioxide; Described binding agent is polytetrafluoroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.5um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 141 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 61um, and porosity is porosity is 49%, and aperture is 0.28um
embodiment 20
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 288.6 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.1um, and polyphenylene sulfide basement membrane thickness is 46um, and porosity is 68%, and aperture is 2.35um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 28.6%, binding agent mass concentration scope 11.5%; Described inorganic nano-particle is alundum (Al2O3); Described binding agent is polytetrafluoroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.6um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 142 DEG C; Described drying mode can adopt vacuumize.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 63.2um, and porosity is porosity is 49.5%, and aperture is 0.29um
embodiment 21
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 288.8 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.2um, and polyphenylene sulfide basement membrane thickness is 48um, and porosity is 69%, and aperture is 2.4um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 28.8%, binding agent mass concentration scope 12%; Described inorganic nano-particle is titanium dioxide; Described binding agent is polytetrafluoroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.7um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 143 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 65.4um, and porosity is porosity is 50%, and aperture is 0.30um
embodiment 22
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.3um, and polyphenylene sulfide basement membrane thickness is 50um, and porosity is 70%, and aperture is 2.45um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29%, binding agent mass concentration scope 12.5%; Described inorganic nano-particle is zirconia; Described binding agent is polytetrafluoroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.8um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 144 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 67.6um, and porosity is porosity is 51%, and aperture is 0.31um
embodiment 23
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.2 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.4um, and polyphenylene sulfide basement membrane thickness is 52um, and porosity is 71%, and aperture is 2.5um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.2%, binding agent mass concentration scope 13%; Described inorganic nano-particle is zinc oxide; Described binding agent is polytetrafluoroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 8.9um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 145 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 69.8um, and porosity is porosity is 52%, and aperture is 0.32um
embodiment 24
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.3 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.45um, and polyphenylene sulfide basement membrane thickness is 53um, and porosity is 72%, and aperture is 2.55um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.4%, binding agent mass concentration scope 13.5%; Described inorganic nano-particle is magnesium oxide; Described binding agent is polytetrafluoroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is cast coating method, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.0um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 146 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 71um, and porosity is porosity is 53%, and aperture is 0.33um
embodiment 25
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.4 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.5um, and polyphenylene sulfide basement membrane thickness is 54um, and porosity is 73%, and aperture is 2.6um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.6%, binding agent mass concentration scope 14%; Described inorganic nano-particle is silicon dioxide; Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.1um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 147 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 72.2um, and porosity is porosity is 54%, and aperture is 0.34um
embodiment 26
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.6 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.6um, and polyphenylene sulfide basement membrane thickness is 55um, and porosity is 74%, and aperture is 2.65um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.8%, binding agent mass concentration scope 14.5%; Described inorganic nano-particle is alundum (Al2O3); Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.2um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 147.5 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 73.4um, and porosity is porosity is 55%, and aperture is 0.35um
embodiment 27
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.7 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.7um, and polyphenylene sulfide basement membrane thickness is 56um, and porosity is 75%, and aperture is 2.7um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.85%, binding agent mass concentration scope 15%; Described inorganic nano-particle is titanium dioxide; Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is DMF.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.4um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 148 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 74.8um, and porosity is porosity is 56%, and aperture is 0.36um
embodiment 28
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289.8 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.8um, and polyphenylene sulfide basement membrane thickness is 57um, and porosity is 76%, and aperture is 2.8um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.9%, binding agent mass concentration scope 16%; Described inorganic nano-particle is zirconia; Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.6um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 148.5 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 76.2um, and porosity is porosity is 57%, and aperture is 0.37um
embodiment 29
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 289 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 2.9um, and polyphenylene sulfide basement membrane thickness is 58um, and porosity is 78%, and aperture is 2.9um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 29.95%, binding agent mass concentration scope 17%; Described inorganic nano-particle is zinc oxide; Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 9.8um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 149 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 77.6um, and porosity is porosity is 58%, and aperture is 0.38um
embodiment 30
1. polyphenylene sulfide basement membrane preparation
By melt-blown polyphenylene sulfide superfine fiber through lapping, hot pressing, stretching expanding, it is 290 DEG C of polyphenylene sulfide basement membranes that thermal finalization process obtains fusing point;
Wherein, the diameter of described polyphenylene sulfide meltblown superfine fibre is 3.0um, and polyphenylene sulfide basement membrane thickness is 60um, and porosity is 80%, and aperture is 3.0um.
2. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 30%, binding agent mass concentration scope 18%; Described inorganic nano-particle is magnesium oxide; Described binding agent is poly-inclined fluorine diene-trichloroethylene; Described solvent is acetone.
3. the coating processing of polyphenylene sulfide basement membrane
Coating machine is adopted evenly to be coated in the upper and lower surface of 1. obtained polyphenylene sulfide basement membrane by through 2. obtained ceramic coated slurry;
Wherein, described painting method is intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 10um.
4. dry process
3. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 150 DEG C; Described drying mode can adopt heated-air drying.
Polyphenylene sulfide Ceramic Composite membrane thicknesses is 80um, and porosity is porosity is 60%, and aperture is 0.40um.

Claims (2)

1. the lithium ion battery preparation method of polyphenylene sulfide Ceramic Composite barrier film, comprise the preparation of polyphenylene sulfide basement membrane, it is characterized in that: described preparation method refers to the surface-coated one deck ceramic size at polyphenylene sulfide basement membrane, obtained polyphenylene sulfide Ceramic Composite barrier film after dry, its preparation method comprises the following steps:
1. ceramic coated slurry preparation
Inorganic nano-particle and bonding agent are dissolved in solvent, stir, obtained ceramic coated slurry;
Wherein, in described ceramic coated slurry, inorganic nano-particle mass concentration scope 25 ~ 30%, binding agent mass concentration scope 2-18%;
Described inorganic nano-particle is one or more compositions mixed in any proportion in silicon dioxide or alundum (Al2O3) or titanium dioxide or zirconia or zinc oxide or magnesium oxide;
Described binding agent is the one in vinyl polysiloxane or Kynoar or Kynoar-hexafluoropropylene or polytetrafluoroethylene or poly-inclined fluorine diene-trichloroethylene;
Described solvent is the one of absolute ethyl alcohol or acetone or DMF;
2. the coating processing of polyphenylene sulfide basement membrane
Adopt coating machine evenly will be coated in the upper and lower surface that fusing point is 280 ~ 290 DEG C of polyphenylene sulfide basement membranes through 1. obtained ceramic coated slurry;
Wherein, described painting method is the one in rolling method or scraper for coating method or cast coating method or intaglio plate coating, and the coating thickness of the upper and lower surface of polyphenylene sulfide basement membrane is respectively 2 ~ 10um;
3. dry process
2. the polyphenylene sulfide basement membrane after applying through step is placed in drying box drying under the condition of 110 ~ 150 DEG C; Described drying mode can adopt directly dries or vacuumize or heated-air drying.
2. a kind of lithium ion battery polyphenylene sulfide Ceramic Composite membrane thicknesses according to claim 1 is 14 ~ 80um, and porosity is 40 ~ 60%, and aperture is 0.1 ~ 0.4um.
CN201510656357.XA 2015-10-12 2015-10-12 Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery Pending CN105280863A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510656357.XA CN105280863A (en) 2015-10-12 2015-10-12 Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510656357.XA CN105280863A (en) 2015-10-12 2015-10-12 Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery

Publications (1)

Publication Number Publication Date
CN105280863A true CN105280863A (en) 2016-01-27

Family

ID=55149507

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510656357.XA Pending CN105280863A (en) 2015-10-12 2015-10-12 Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery

Country Status (1)

Country Link
CN (1) CN105280863A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108886123A (en) * 2016-02-17 2018-11-23 达拉米克有限责任公司 Improved partition, lead-acid battery and associated method and system
CN110528314A (en) * 2019-06-19 2019-12-03 武汉纺织大学 A kind of composite sheet and its preparation method and application of the polyphenylene sulfide superfine fiber containing melt-blown
CN112310557A (en) * 2020-11-03 2021-02-02 天津工业大学 Preparation method of polyphenylene sulfide-based diaphragm based on viscous flow modification technology
CN112358637A (en) * 2020-11-03 2021-02-12 浙江新和成特种材料有限公司 Polyphenylene sulfide film suitable for ultrathin coating and preparation method and application thereof
CN113862821A (en) * 2021-09-24 2021-12-31 天津工业大学 Polyphenylene sulfide fiber fabric type alkaline water electrolysis diaphragm and preparation method thereof
CN114583383A (en) * 2022-03-07 2022-06-03 潍坊科技学院 Heat-resistant flame-retardant composite diaphragm and preparation method and application thereof
CN114744368A (en) * 2022-06-13 2022-07-12 四川新能源汽车创新中心有限公司 Lithium battery diaphragm with compact structure and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101317284A (en) * 2005-11-28 2008-12-03 株式会社Lg化学 Organic/inorganic composite porous membrane and electrochemical device using the same
CN103238249A (en) * 2010-11-30 2013-08-07 株式会社Lg化学 Lithium secondary battery
CN104247090A (en) * 2012-01-19 2014-12-24 索尼公司 Separator, non-aqueous electrolyte battery, battery pack, electronic device, electric vehicle, electricity storage device, and power system
CN104584267A (en) * 2013-02-12 2015-04-29 三星Total株式会社 Organic/inorganic composite coating porous separator and secondary battery element using same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101317284A (en) * 2005-11-28 2008-12-03 株式会社Lg化学 Organic/inorganic composite porous membrane and electrochemical device using the same
CN103238249A (en) * 2010-11-30 2013-08-07 株式会社Lg化学 Lithium secondary battery
CN104247090A (en) * 2012-01-19 2014-12-24 索尼公司 Separator, non-aqueous electrolyte battery, battery pack, electronic device, electric vehicle, electricity storage device, and power system
CN104584267A (en) * 2013-02-12 2015-04-29 三星Total株式会社 Organic/inorganic composite coating porous separator and secondary battery element using same

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108886123A (en) * 2016-02-17 2018-11-23 达拉米克有限责任公司 Improved partition, lead-acid battery and associated method and system
CN110528314A (en) * 2019-06-19 2019-12-03 武汉纺织大学 A kind of composite sheet and its preparation method and application of the polyphenylene sulfide superfine fiber containing melt-blown
CN110528314B (en) * 2019-06-19 2022-07-01 武汉纺织大学 Composite sheet containing melt-blown polyphenylene sulfide superfine fibers and preparation method and application thereof
CN112358637B (en) * 2020-11-03 2022-06-21 浙江新和成特种材料有限公司 Polyphenylene sulfide film suitable for ultrathin coating and preparation method and application thereof
CN112358637A (en) * 2020-11-03 2021-02-12 浙江新和成特种材料有限公司 Polyphenylene sulfide film suitable for ultrathin coating and preparation method and application thereof
CN112310557A (en) * 2020-11-03 2021-02-02 天津工业大学 Preparation method of polyphenylene sulfide-based diaphragm based on viscous flow modification technology
CN112310557B (en) * 2020-11-03 2022-12-23 天津工业大学 Preparation method of polyphenylene sulfide-based diaphragm based on viscous flow modification technology
CN113862821A (en) * 2021-09-24 2021-12-31 天津工业大学 Polyphenylene sulfide fiber fabric type alkaline water electrolysis diaphragm and preparation method thereof
CN113862821B (en) * 2021-09-24 2022-08-05 天津工业大学 Polyphenylene sulfide fiber fabric type alkaline water electrolysis diaphragm and preparation method thereof
CN114583383A (en) * 2022-03-07 2022-06-03 潍坊科技学院 Heat-resistant flame-retardant composite diaphragm and preparation method and application thereof
CN114583383B (en) * 2022-03-07 2023-10-31 潍坊科技学院 Heat-resistant flame-retardant composite diaphragm and preparation method and application thereof
CN114744368A (en) * 2022-06-13 2022-07-12 四川新能源汽车创新中心有限公司 Lithium battery diaphragm with compact structure and preparation method thereof
CN114744368B (en) * 2022-06-13 2022-08-30 四川新能源汽车创新中心有限公司 Lithium battery diaphragm with compact structure and preparation method thereof

Similar Documents

Publication Publication Date Title
CN105280863A (en) Preparation method of polyphenylene sulfide ceramic composite membrane for lithium ion battery
CN104835931B (en) Nonwoven fabric lithium ion battery composite diaphragm and preparation method thereof
CN103078077B (en) Lithium ion battery diaphragm with special structure and preparation method thereof
CN103928649A (en) Novel modified non-woven fabric lithium-ion battery diaphragm and preparation method thereof
CN104766938B (en) A kind of compound lithium ion battery separator and preparation method thereof
CN102931370B (en) Nanofiber composite nano-fiber membrane and preparation method thereof
CN103100264A (en) Battery and capacitor diaphragm filter material formed by wet nonwoven fabrics and preparation method of filter material
CN206505967U (en) A kind of barrier film and lithium ion battery for lithium ion battery
CN103474602B (en) A kind of lithium ion battery pore-creating ceramics barrier film and preparation method thereof
CN110148699A (en) A kind of preparation process of the high-performance coating diaphragm of surface coating organic layer
CN105789536B (en) A kind of melt-blown polyphenylene sulfide non-woven fabrics/aramid nano-fiber composite diaphragm preparation
CN108807804B (en) Battery separator and method for producing same
CN108039439B (en) Composite diaphragm and preparation method thereof
KR20190140681A (en) Separator for electrochemical device, comprising a patterned adhesive layer and a method of manufacturing the separator
CN102522514A (en) High-temperature resistant micropore thin film material and application thereof
CN109509855A (en) A kind of aramid fiber ceramic diaphragm and its preparation method and application
KR20140139127A (en) A dye-sensitized solar cell including a composite substrate
CN110429227A (en) A kind of preparation method of fibrous type lithium ion battery separator
CN101728504B (en) Lithium ion battery diaphragm flexible substrate by wet papermaking and manufacturing method thereof
CN113258211A (en) High-liquid-storage-rate coated diaphragm and preparation method and application thereof
CN105702900A (en) Preparation for para-aramid nanofiber lithium ion battery diaphragm based on pyrolysis-caused-holes
CN105098125A (en) Alumina particle-filled composite multi-arc hole membrane material and preparation method and application thereof
TW201351757A (en) Structure of an electrochemical separation membrane and manufacturing method for fabricating the same
CN110112365A (en) Battery pole piece and preparation method thereof, battery core and battery
CN106981607A (en) A kind of lithium ion battery separator and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160127

RJ01 Rejection of invention patent application after publication