CN106084271A - New method prepared by three layers of laminated film of nanoparticle/polyimides - Google Patents

New method prepared by three layers of laminated film of nanoparticle/polyimides Download PDF

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CN106084271A
CN106084271A CN201610549372.9A CN201610549372A CN106084271A CN 106084271 A CN106084271 A CN 106084271A CN 201610549372 A CN201610549372 A CN 201610549372A CN 106084271 A CN106084271 A CN 106084271A
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polyamic acid
nanoparticle
layers
microporous membrane
laminated film
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巩桂芬
王磊
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Harbin University of Science and Technology
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D04H3/009—Condensation or reaction polymers
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
    • C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors

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  • Chemical Kinetics & Catalysis (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract

New method prepared by three layers of laminated film of nanoparticle/polyimides.Use nanoparticle that Kapton is modified, the corona-resistance property of thin film can be made to significantly improve, but being continuously increased along with nanoparticle doped content, the mechanical property of Kapton declines the most therewith.The method of the present invention comprises the steps: the preparation of (1) biphenyl type polyamic acid；(2) method of electrostatic spinning prepares polyamic acid microporous membrane；(3) preparation of the equal benzene-type polyamic acid of nanoparticle doped；(4) at the polyamic acid of microporous membrane both sides coated nanoparticles doping；(5) three layers of laminated film of nanoparticle/polyamic acid are carried out hot imidization.The invention discloses new method prepared by three layers of laminated film of a kind of nanoparticle/polyimides.

Description

New method prepared by three layers of laminated film of nanoparticle/polyimides
Technical field:
The present invention relates to new method prepared by three layers of laminated film of a kind of nanoparticle/polyimides.
Background technology:
Kapton is one of polyimides commodity the earliest, and Kapton is best organic thin of current thermostability Film, can keep its physical property, life-time service temperature to reach more than 200 DEG C in a short time at 555 DEG C, be mainly used in the slot insulation of motor And the covering material of electric wire.And the electric property of Kapton, radiation resistance and fire resistance are the most very Prominent, in aerospace industry, electric industry and information industry, played very important effect.But polyimides by In itself being high molecular polymer, corona-resistance property is poor, limits it and adjusts in high-voltage generator, high-tension motor, pulsewidth The application in the fields such as the frequency conversion motor of system power supply.In recent years, hi-tech development makes rapid progress, and nanoparticle is with the table of its uniqueness Face effect causes the concern of numerous scientific research personnel.Research finds, uses nanoparticle to be modified Kapton, energy The corona-resistance property making thin film significantly improves, but being continuously increased along with nanoparticle doped content, the power of Kapton Learn performance to decline the most therewith, the most how to prevent under its mechanical property while improving Kapton corona-resistance property Fall, becomes the key of extension Kapton application.
Summary of the invention:
It is an object of the invention to provide new method prepared by three layers of laminated film of a kind of nanoparticle/polyimides.
Above-mentioned purpose is realized by following technical scheme:
New method prepared by three layers of laminated film of a kind of nanoparticle/polyimides, the method comprises the steps:
(1) preparation of biphenyl type polyamic acid；
(2) method of electrostatic spinning prepares polyamic acid microporous membrane；
(3) preparation of the equal benzene-type polyamic acid of nanoparticle doped；
(4) at the polyamic acid of microporous membrane both sides coated nanoparticles doping；
(5) three layers of laminated film of nanoparticle/polyamic acid are carried out hot imidization.
New method prepared by three layers of laminated film of described nanoparticle/polyimides, described biphenyl type polyamic acid Preparation, take the 4 of 2.80g, 4-diamino-diphenyl ether pours there-necked flask into, adds 29.6ml N,N-dimethylacetamide, is passed through Nitrogen is protected, and stirs 1 h under 10 DEG C of psychrolusias, by the 3 of 4.23g, and 3 ', 4,4 '-bibenzene tetracarboxylic dianhydride is the most progressively Joining in solution, feed time controls at 120min, continues stirring 24 hours, by transparent yellow after pole-climbing phenomenon to appear Thick polyamic acid liquid pour into small beaker seals standby.
New method prepared by three layers of laminated film of described nanoparticle/polyimides, prepared by described method of electrostatic spinning Polyamic acid microporous membrane, takes the biphenyl type polyamic acid liquid described in 10ml in the syringe pump of electrostatic spinning apparatus, and regulation is spun Filament voltage is 10kV, and injection speed is 0.3ml/h, and receiving range is 15cm, and spinning 5 h prepares the polyamic acid that thickness is 20 μm Microporous membrane.
New method prepared by three layers of laminated film of described nanoparticle/polyimides, described nanoparticle doped All the preparation of benzene-type polyamic acid, adds certain mass according to the different proportion of solid masses in polyamic acid in there-necked flask Nanoparticle granule, adds 34ml N,N-dimethylacetamide, is passed through nitrogen and protects, ultrasonic under 10 DEG C of psychrolusias Stirring 1 h, then take the 4 of 3g, 4-diamino-diphenyl ether pours there-necked flask into, after ultrasonic agitation 1h, by the Pyromellitic Acid of 3.28g Dianhydride is added step-wise in solution in batches, and feed time controls at 120min, then proceedes to stir 24 hours, by thick pale yellow The polyamic acid liquid of shape pour into small beaker seals standby.
New method prepared by three layers of laminated film of described nanoparticle/polyimides, described is coated with in microporous membrane both sides Cover the polyamic acid of nanoparticle doped, use self-control film-laying machine to carry out plastic film mulch, by microporous membrane in polyamic acid microporous membrane both sides Porosity calculate the concrete thickness of the spread glue in both sides；Utilize self-control film-laying machine one layer of 30 μm nanometer of paving on a glass Particle doping described equal benzene-type polyamic acid glue, then by utilize electrostatic spinning prepare described in microporous membrane be layered on this On solution, after described microporous membrane internal capillary is completely immersed in glue, recycling film-laying machine spreads one layer of 15 μm nanometer above Particle doping described equal benzene-type polyamic acid glue and place 0.5h, make polyamic acid glue be sufficiently submerged in microporous membrane, put Enter baking oven in case imidization.
New method prepared by three layers of laminated film of described nanoparticle/polyimides, described to nanoparticle/polyamides Three layers of laminated film of amino acid carry out hot imidization, use gradient heating, make polyamic acid generation dehydration closed-loop to prepare polyamides Imines thin film, the temperature and time of its imidization is as follows: 1) 80 DEG C of heat treatment 1h；2) 120 DEG C of heat treatment 1h；3) 150 DEG C Heat treatment 1h；4) 200 DEG C of heat treatment 1h；5) 250 DEG C of heat treatment 1h；6) 300 DEG C of heat treatment 1h.
Beneficial effects of the present invention:
The present invention is by 4, and 4-diamino-diphenyl ether joins in N,N-dimethylacetamide, in N2 protection and 10 DEG C of psychrolusias Under the conditions of dissolve after, be dividedly in some parts 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride, obtain biphenyl type polyamic acid spinning liquid, and pass through High-voltage electrostatic spinning method prepares biphenyl type polyamic acid microporous membrane, and nanoparticle joins N, N-diformazan the most by a certain percentage In yl acetamide, under conditions of N2 protection and 10 DEG C of psychrolusias, ultrasonic agitation adds 4 after being uniformly dispersed, 4-diamino-diphenyl Ether, pyromellitic acid anhydride after it dissolves, obtain the equal benzene-type polyamic acid glue of nanoparticle doped, utilize film-laying machine to incite somebody to action It is layered on biphenyl polyimide microporous membrane both sides, after glue fully penetrates into microporous membrane, carries out heat by gradient heating sub- Amination treatment, obtains three layers of laminated film of polyimides.
The present invention relates to the preparation of biphenyl type polyamic acid microporous membrane, the equal benzene-type of microporous membrane both sides nanoparticle doped is gathered The hot imidization technique of the coating of amic acid and three layers of laminated film, introduces mechanical property in polypyromelliticimide matrix Biphenyl polyimide more preferable with hot property, is favorably improved mechanics and the thermal property of thin film, simultaneously as biphenyl type gathers Acid imide is to introduce with the form of nanofiber, hence with polypyromelliticimide glue and biphenyl polyimide fiber it Between the interaction at interface, the performances such as the polypyromelliticimide thin film mechanics of doped with nanometer particle are improved, it is achieved that The performances such as its mechanics are promoted while doped with nanometer particle improves Kapton corona-resistance property.
Detailed description of the invention:
Embodiment 1:
New method prepared by three layers of laminated film of a kind of nanoparticle/polyimides, the method comprises the steps:
(1) preparation of biphenyl type polyamic acid；
(2) method of electrostatic spinning prepares polyamic acid microporous membrane；
(3) preparation of the equal benzene-type polyamic acid of nanoparticle doped；
(4) at the polyamic acid of microporous membrane both sides coated nanoparticles doping；
(5) three layers of laminated film of nanoparticle/polyamic acid are carried out hot imidization.
Embodiment 2:
The new method prepared according to three layers of laminated film of the nanoparticle/polyimides described in embodiment 1, described biphenyl type gathers The preparation of amic acid, takes the 4 of 2.80g, and 4-diamino-diphenyl ether pours there-necked flask into, adds 29.6ml N, N-dimethylacetamide Amine, is passed through nitrogen and protects, and stirs 1 h under 10 DEG C of psychrolusias, by the 3 of 4.23g, and 3 ', 4,4 '-bibenzene tetracarboxylic dianhydride divides Criticizing and be added step-wise in solution, feed time controls at 120min, continues stirring 24 hours, by transparent after pole-climbing phenomenon to appear The polyamic acid liquid of yellow, viscous pour into small beaker seals standby.
Embodiment 3:
The new method prepared according to three layers of laminated film of the nanoparticle/polyimides described in embodiment 1 or 2, described electrostatic Spin processes prepares polyamic acid microporous membrane, takes the biphenyl type polyamic acid liquid described in 10ml in the syringe pump of electrostatic spinning apparatus In, regulation spinning voltage is 10kV, and injection speed is 0.3ml/h, and receiving range is 15cm, and it is 20 μm that spinning 5 h prepares thickness Polyamic acid microporous membrane.
Embodiment 4:
The new method prepared according to the three layers of laminated film of nanoparticle/polyimides described in embodiment 1 or 2 or 3, described receives The preparation of the equal benzene-type polyamic acid of rice corpuscles doping, adds in there-necked flask according to the different proportion of solid masses in polyamic acid Enter the nanoparticle granule of certain mass, add 34ml N,N-dimethylacetamide, be passed through nitrogen and protect, at 10 DEG C Ultrasonic agitation 1 h under psychrolusia, then take the 4 of 3g, 4-diamino-diphenyl ether pours there-necked flask into, after ultrasonic agitation 1h, by 3.28g Pyromellitic acid anhydride be added step-wise in solution in batches, feed time controls at 120min, then proceedes to stir 24 hours, The polyamic acid liquid of thick pale yellow shape is poured into small beaker seals standby.
Embodiment 5:
The new method prepared according to the three layers of laminated film of nanoparticle/polyimides described in embodiment 1 or 2 or 3 or 4, described Microporous membrane both sides coated nanoparticles doping polyamic acid, use self-control film-laying machine enter in polyamic acid microporous membrane both sides Row plastic film mulch, is calculated the concrete thickness of the spread glue in both sides by the porosity of microporous membrane；Utilize self-control plastic film mulch on a glass The described equal benzene-type polyamic acid glue of machine one layer of 30 μm nanoparticle doped of paving, the institute that then electrostatic spinning will be utilized to prepare The microporous membrane stated is layered on this solution, and after described microporous membrane internal capillary is completely immersed in glue, recycling film-laying machine is upper Face spreads the described equal benzene-type polyamic acid glue of one layer of 15 μm nanoparticle doped and places 0.5h, makes polyamic acid glue fill Sub-dip enters microporous membrane, puts into baking oven in case imidization.
Embodiment 6:
The new method prepared according to the three layers of laminated film of nanoparticle/polyimides described in embodiment 1 or 2 or 3 or 4 or 5, institute That states carries out hot imidization to three layers of laminated film of nanoparticle/polyamic acid, uses gradient heating, makes polyamic acid occur Dehydration closed-loop is to prepare Kapton, and the temperature and time of its imidization is as follows: 1) 80 DEG C of heat treatment 1h；2) 120 DEG C heat treatment 1h；3) 150 DEG C of heat treatment 1h；4) 200 DEG C of heat treatment 1h；5) 250 DEG C of heat treatment 1h；6) 300 DEG C of heat treatment 1h.

Claims (6)

1. the new method that prepared by three layers of laminated film of nanoparticle/polyimides, is characterized in that: the method includes walking as follows Rapid:
(1) preparation of biphenyl type polyamic acid；
(2) method of electrostatic spinning prepares polyamic acid microporous membrane；
(3) preparation of the equal benzene-type polyamic acid of nanoparticle doped；
(4) at the polyamic acid of microporous membrane both sides coated nanoparticles doping；
(5) three layers of laminated film of nanoparticle/polyamic acid are carried out hot imidization.
New method prepared by three layers of laminated film of nanoparticle/polyimides the most according to claim 1, is characterized in that: The preparation of described biphenyl type polyamic acid, takes the 4 of 2.80g, and 4-diamino-diphenyl ether pours there-necked flask into, adds 29.6ml N,N-dimethylacetamide, is passed through nitrogen and protects, and stirs 1 h under 10 DEG C of psychrolusias, by the 3 of 4.23g, and 3 ', 4,4 '-connection PMDA is added step-wise in solution in batches, and feed time controls at 120min, continues to stir after pole-climbing phenomenon to appear Mix 24 hours, the polyamic acid liquid of transparent yellow, viscous is poured into small beaker seals standby.
New method prepared by three layers of laminated film of nanoparticle/polyimides the most according to claim 1 and 2, its feature It is: described method of electrostatic spinning prepares polyamic acid microporous membrane to take the biphenyl type polyamic acid liquid described in 10ml in Static Spinning In the syringe pump of silk device, regulation spinning voltage is 10kV, and injection speed is 0.3ml/h, and receiving range is 15cm, spinning 5 h Prepared thickness is the polyamic acid microporous membrane of 20 μm.
4. the new method prepared according to the three layers of laminated film of nanoparticle/polyimides described in claim 1 or 2 or 3, it is special Levy and be: the preparation of the equal benzene-type polyamic acid of described nanoparticle doped, according in polyamic acid solid masses the most on year-on-year basis Example adds the nanoparticle granule of certain mass in there-necked flask, adds 34ml N,N-dimethylacetamide, is passed through nitrogen and enters Row protection, ultrasonic agitation 1 h under 10 DEG C of psychrolusias, then take the 4 of 3g, 4-diamino-diphenyl ether pours there-necked flask into, ultrasonic stirs After mixing 1h, being added step-wise in solution by the pyromellitic acid anhydride of 3.28g, feed time controls at 120min, then in batches Continue stirring 24 hours, the polyamic acid liquid of thick pale yellow shape is poured into small beaker seals standby.
5. the new method prepared according to the three layers of laminated film of nanoparticle/polyimides described in claim 1 or 2 or 3 or 4, It is characterized in that: the described polyamic acid in the doping of microporous membrane both sides coated nanoparticles, use self-control film-laying machine at polyamide Acid microporous membrane both sides carry out plastic film mulch, the porosity of microporous membrane calculate the concrete thickness of the spread glue in both sides；At glass plate The upper described equal benzene-type polyamic acid glue utilizing self-control film-laying machine one layer of 30 μm nanoparticle doped of paving, then will utilize quiet The described microporous membrane that Electrospun prepares is layered on this solution, after described microporous membrane internal capillary is completely immersed in glue, then Utilize film-laying machine spread the equal benzene-type polyamic acid glue described in one layer of 15 μm nanoparticle doped above and place 0.5h, make Polyamic acid glue is sufficiently submerged in microporous membrane, puts into baking oven in case imidization.
6. the new side prepared according to the three layers of laminated film of nanoparticle/polyimides described in claim 1 or 2 or 3 or 4 or 5 Method, is characterized in that: described carries out hot imidization to three layers of laminated film of nanoparticle/polyamic acid, uses gradient heating, Making polyamic acid generation dehydration closed-loop to prepare Kapton, the temperature and time of its imidization is as follows: 1) 80 DEG C Heat treatment 1h；2) 120 DEG C of heat treatment 1h；3) 150 DEG C of heat treatment 1h；4) 200 DEG C of heat treatment 1h；5) 250 DEG C of heat treatment 1h；6) 300 DEG C of heat treatment 1h.
CN201610549372.9A 2016-07-13 2016-07-13 New method prepared by three layers of laminated film of nanoparticle/polyimides Pending CN106084271A (en)

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Cited By (4)

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CN106939518A (en) * 2017-04-14 2017-07-11 哈尔滨理工大学 The preparation method of three layers of laminated film of polyimides with electro-magnetic screen function
CN107630294A (en) * 2017-10-27 2018-01-26 长沙新材料产业研究院有限公司 A kind of polyimide nanofiber membrane
CN109021565A (en) * 2018-06-24 2018-12-18 北京化工大学 A kind of method that in-situ hydrolysis method prepares the polyimide material of resistance to elemental oxygen
CN111732747A (en) * 2020-07-03 2020-10-02 浙江中科玖源新材料有限公司 Polyimide film with good insulating and bonding properties and preparation method thereof

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CN102189724A (en) * 2010-03-11 2011-09-21 东丽纤维研究所（中国）有限公司 Ultralow dielectric constant film with sandwich structure and preparation method thereof
CN102490426A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Corona resistance polyimide thin film and preparation method thereof
CN102490423A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Conductive polyimide film and preparation method thereof

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CN102189724A (en) * 2010-03-11 2011-09-21 东丽纤维研究所（中国）有限公司 Ultralow dielectric constant film with sandwich structure and preparation method thereof
CN101834015A (en) * 2010-03-31 2010-09-15 鞍山华辉光电子材料科技有限公司 Flexible transparent conducting film for polyimide substrate and preparation method thereof
CN102490426A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Corona resistance polyimide thin film and preparation method thereof
CN102490423A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Conductive polyimide film and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106939518A (en) * 2017-04-14 2017-07-11 哈尔滨理工大学 The preparation method of three layers of laminated film of polyimides with electro-magnetic screen function
CN107630294A (en) * 2017-10-27 2018-01-26 长沙新材料产业研究院有限公司 A kind of polyimide nanofiber membrane
CN107630294B (en) * 2017-10-27 2020-08-07 长沙新材料产业研究院有限公司 Polyimide nanofiber membrane
CN109021565A (en) * 2018-06-24 2018-12-18 北京化工大学 A kind of method that in-situ hydrolysis method prepares the polyimide material of resistance to elemental oxygen
CN109021565B (en) * 2018-06-24 2020-06-19 北京化工大学 Method for preparing atomic oxygen resistant polyimide material by in-situ hydrolysis method
CN111732747A (en) * 2020-07-03 2020-10-02 浙江中科玖源新材料有限公司 Polyimide film with good insulating and bonding properties and preparation method thereof

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Application publication date: 20161109