CN107698785A - A kind of polyimides based coextruded film and preparation method thereof - Google Patents
A kind of polyimides based coextruded film and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- 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
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- 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
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- C08K3/34—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention provides a kind of polyimides based coextruded film and preparation method, by the way that inorganic material material is incorporated into the reaction system of aromatic dianhydride monomer and aromatic diamine monomers, through low temperature polymerization, modified polyamide acid solution is obtained, most obtain polyimides based coextruded film through imidizate afterwards.The laminated film shows excellent heat-resisting quantity, low-expansion coefficient and mechanical performance, available for flexible display technologies field.
Description
Technical field
The present invention relates to flexible display technologies field, more particularly to a kind of polyimides based coextruded film and its preparation side
Method.
Background technology
Polyimides (polyimide, PI) is the high-molecular compound containing imide ring structure in molecular backbone, it
With performances such as excellent heat resistance, chemical resistance, electrical insulating property, mechanical performances, navigation space flight, electrically absolutely can be widely applied to
The fields such as edge, microelectronics.In recent years, polyimides starts to be used for field of flexible display.But in display technology field, as flexibility
The material of film substrate needs have relatively low thermal coefficient of expansion and higher thermal conductivity.And common Kapton is usual
It is low in the transmitance of visible region in brown or brown color, and thermal coefficient of expansion is higher, influences the stabilization of electronic component.
The content of the invention
In consideration of it, the present invention by the inorganic material material of specific proportioning be incorporated into the aromatic dianhydride monomer of specific structure with
In the reaction system of aromatic diamine monomers, through low temperature polymerization, modified polyamide acid solution is obtained, is most obtained afterwards through imidizate
Polyimides based coextruded film, the laminated film have relatively low thermal coefficient of expansion, and heat endurance also further improves, and machinery
Performance further optimizes, can be as the baseplate material of flexible display technologies.
In a first aspect, the invention provides a kind of preparation method of polyimides based coextruded film, comprise the following steps：
(1) inorganic nano material, dispersant, binding agent, solvent are mixed in proportion, stirred, obtain inorganic nano
Material paste, the inorganic nano material slurry include each component of following parts by weight：Nano inorganic material 4-8 parts, point
Powder 1-2 parts, binding agent 2-4 parts, organic solvent 80-200 parts；Wherein, the inorganic nano material include nano silicon,
One or more in nano-silicon nitride, nano aluminium oxide and nano titanium oxide；
(2) the aromatic dianhydride monomer as shown in following formula (I) and the aromatic diamine monomers shown in formula (II) are added to institute
State in inorganic nano material slurry, carry out polymerisation in a nitrogen atmosphere, obtain polymerization liquid；
H2N-Ar'—NH2(II),
Wherein, Ar is selected fromIn
One kind, Ar ' is selected from In one kind；
(3) in a nitrogen atmosphere, the polymerization liquid is toasted into film forming coated on base material；
(4) in a nitrogen atmosphere, film obtained by step (3) is subjected to imidization reaction at high temperature, then removes base
Material, obtain polyimides based coextruded film.
Wherein, in step (1), the particle diameter of the inorganic nano material is 20-50nm.
Wherein, in step (1), the dispersant is Sodium Polyacrylate, ammonium polyacrylate salt, ethyl acetate, butyl acetate
With the one or more in APES.
Wherein, in step (1), the binding agent is cumyl peroxide, hydroxypropyl methyl cellulose, nitrone derivative
One or more in thing, styrene-butadiene block copolymer and butadienyl triethoxysilane.
Wherein, in step (1), the organic solvent is aprotic polar solvent, selected from DMF
(DMF), one kind in DMAC N,N' dimethyl acetamide (DMAc), METHYLPYRROLIDONE (NMP), dimethyl sulfoxide (DMSO) (DMSO)
Or it is a variety of, but not limited to this.
Wherein, the gross weight of the aromatic dianhydride monomer and the aromatic diamine monomers is 90-150 parts.
Preferably, the gross weight of the aromatic dianhydride monomer and the aromatic diamine monomers and the inorganic nano material
Weight ratio be (12-35)：1.
Wherein, in step (2), the mol ratio of the aromatic dianhydride monomer and the aromatic diamines is 1:(0.95-
1.05).Preferably 1:1.
Wherein, in step (2), the temperature of the polymerisation is 30-60 DEG C.Preferably 45-60 DEG C.
Wherein, in step (2), the reaction time of the polymerisation is 2-10h.
Wherein, in step (3), it is 10-100 μm to be coated to the wet-film thickness formed on base material.Preferably 60-100 μm.
Wherein, in step (3), the temperature of the baking film forming is 120-150 DEG C, and the time of the baking is 6-60min.
Preferably, the time of the baking is 12-60min.
Polymerization liquid is first toasted film forming by the present invention before high temperature imidization reaction is carried out, and one will can gather
The organic solvent closed in reaction solution vapors away, and two, the polyamic acid contained in polymerization liquid can be subjected to part imidization,
Reduce the temperature and duration for subsequently entering every trade imidization reaction.
Preferably, in step (3), before by the polymerization liquid coated on base material, in addition to：To the polymerization
Reaction solution carries out vacuumizing and defoaming processing 12-24h.Vacuum defoamation processing is to carry out under agitation, and deaeration can be so as to
Smooth, bubble-free film surface is formed on base material in subsequently.
Wherein, in step (3), the base material includes glass, graphite, ceramics, but not limited to this.
Wherein, in step (4), the temperature of the imidization reaction is 400-450 DEG C, reaction time 6-60min.
Select to carry out imidization reaction at 300-400 DEG C in the present invention, one, the matter of film when reacting at such a temperature
Amount loss is less, and two, the resistance to elevated temperatures of laminated film can be further enhanced at such a temperature, be easy to preferably be applied to
Flexible film substrate manufacturing field.
Further, the heating rate of the imidization reaction is 5-20 DEG C/min.Preferably 5-12 DEG C/min.
Preferably, in step (4), the start temperature to be heated up in the imidization reaction is 130-160 DEG C.By step
(3) gained film is placed in the equipment (such as solidification case) of such initial temperature, is easy to proceed by heating by pre-set programs.
In the present invention, in step (2), contain polyamic acid in gained polymerization liquid, its structural formula is as follows：
N is the degree of polymerization, and n is 1-1000 natural number.Preferably, n 100-
1000 natural number.Such as can be 200,300,400,500,600,700,800 or 900 etc..
In the present invention, in step (4), after high temperature imidization reaction in gained polyimides based coextruded film, polyamides is sub-
Shown in the chemical structural formula of amine such as following formula (III)：
Wherein, Ar is selected from In one kind, Ar ' is selected from In one kind；N is the degree of polymerization, n
For 1-1000 natural numbers.
In the preparation method for the polyimides based coextruded film that first aspect present invention provides, based on inorganic nano material phase
Than polyimides, there is relatively low thermal coefficient of expansion, high bond energy, more excellent heat resistance.Inorganic nano material is added into
In the reaction monomers of polyimide material (aromatic dianhydride monomer and aromatic diamine monomers), through low temperature polymerization, baking film forming, height
Warm imidization reaction, obtain polyimides based coextruded film.Wherein, inorganic nano material is dispersed in the net of polyimides
In network structure, the heat conduction network structure of the inorganic nano material of IPN formula is formed, there is provided the transmission path of heat so that polyamides is sub-
The thermal coefficient of expansion of amine reduces, while further improves the heat endurance of laminated film, while can buffer internal stress, possesses excellent
Different mechanical performance.And matrix of the polyimides as laminated film, contribute to stabilization, be uniformly dispersed inorganic nano material,
The reaction monomers of its specific structure can also assign its preferable mechanical performance, in the poly- of the inorganic nano material and specific structure
Under the synergy of imide reaction monomer, so as to get polyimide/inorganic nano Material cladding film have relatively low heat concurrently
The coefficient of expansion, high thermal conductance, and higher heat endurance and mechanical performance, improve simple polyimide film in itself
Thermal coefficient of expansion it is higher the problem of.
The preparation side of polyimides based coextruded film provided by the invention is simple and easy to do, and extent of reaction degree of controllability is high, product
Purity is high, dissolvent residual is few, can industrialized production.
Second aspect, the invention provides a kind of polyimides based coextruded film, the polyimides based coextruded film bag
Polyimide matrix and the inorganic nano material being supported in the polyimide matrix are included, the polyimide matrix has three
Tie up network structure；Shown in the structural formula of the polyimide matrix such as following formula (III)：
Wherein, Ar is selected from In one kind, Ar ' is selected from In one kind；N is the degree of polymerization, n
For 1-1000 natural numbers.
Preferably, n is 100-1000 natural number.Such as can be 200,300,400,500,600,700,800 or 900
Deng.
Wherein, the inorganic nano material is wound/is entrenched in the polyimide matrix.
Wherein, the quality of the inorganic nano material accounts for the 2%-10% of the laminated film quality.Preferably 2.5%-
8%.
Wherein, dispersant and binding agent are also included in the laminated film.
Wherein, the thermal coefficient of expansion of the laminated film is 3-5.5ppm/K.
Wherein, the tensile modulus of elasticity of the laminated film is 9-20Gpa.
Wherein, the temperature range of the glass transition temperature (Tg) of the laminated film is at 180-240 DEG C.
Wherein, the heat decomposition temperature Td of the laminated film is 550-590 DEG C.Td be the laminated film in thermal decomposition,
Temperature during Mass lost the 1% of initial mass.
Wherein, the UV cut-off wavelength of the laminated film is 400nm；It is 75- in the light transmittance of visible region
80%.
The polyimides based coextruded film that second aspect of the present invention provides is using the method system described in first aspect present invention
, the polyimides based coextruded film had both shown excellent heat-resisting quantity, low-expansion coefficient and mechanical performance.Go back table simultaneously
Reveal more excellent flexibility and visible light transmissivity, can be as the baseplate material of flexible display technologies.
Advantages of the present invention will be illustrated partly in the following description, and a part is apparent according to specification
, or can be known by the implementation of the embodiment of the present invention.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Embodiment 1
A kind of preparation method of polyimides based coextruded film, including step：
1. takes 4 parts of nano silicon (particle diameter 30nm) in parts by weight, 1 part of dispersant (being specially ethyl acetate),
2 parts of binding agent (being specially hydroxypropyl methyl cellulose), 80 parts of organic solvent (being specially METHYLPYRROLIDONE), stirring
Uniformly, slurry is made；
2. is at room temperature, by pyromellitic acid anhydride and p-phenylenediamine in molar ratio 1:1 is weighed, gross weight 90
Part, it is added in the slurry prepared in step 1), in nitrogen atmosphere, carries out sufficient low temperature poly condensation 6h in 30 DEG C, obtain
To reaction paste；
3. in nitrogen atmosphere, reaction paste is evenly applied on clean smooth glass substrate, controls coating thickness
For 40 μm, 20min film forming is toasted at 120 DEG C；
4. is warming up to 450 DEG C with 5 DEG C/min heating rate in nitrogen atmosphere, by the film of step 3. from 150 DEG C,
60min is incubated at 450 DEG C, to carry out imidization reaction；Room temperature is cooled to, using laser lift-off technique by imidizate
The film obtained after reaction is peeled off from glass substrate, obtains polyimides based coextruded film.
Polyimides based coextruded film made from the present embodiment, including polyimide matrix and it is dispersed in the polyimides
Nano silicon in matrix, polyimide matrix and nano silicon form the network structure of IPN；The polyimides
The structural formula of matrix is：
The thermal coefficient of expansion of above-mentioned polyimides based coextruded film is 5ppm/K, tensile modulus of elasticity 9.5GPa, Tg's
Temperature range is 210 DEG C, 560 DEG C of heat decomposition temperature Td.The UV cut-off wavelength of the laminated film is 420nm,
Transmitance at 550nm is 86%, and it is 75% in the transmitance of whole visible region.
Embodiment 2
A kind of preparation method of polyimides based coextruded film, including step：
1. takes 6 parts of nano-silicon nitride (particle diameter 40nm) in parts by weight, 1.5 parts of dispersant (is specially alkyl phenol polyoxy
Vinethene), 3 parts of binding agent (being specially butadienyl triethoxysilane), 120 parts of organic solvent (specially N, N- dimethyl
Formamide), stir, slurry is made；
2. is at room temperature, by pyromellitic acid anhydride and m-phenylene diamine (MPD) in molar ratio 1:1 is weighed, gross weight 135
Part, it is added in the slurry prepared in step 1), in nitrogen atmosphere, fully carries out low temperature poly condensation 3h in 35 DEG C, obtain
Reaction paste；
3. in nitrogen atmosphere, reaction paste is evenly applied on clean smooth glass substrate, controls coating thickness
For 30 μm, 10min film forming is toasted at 130 DEG C；
4. is warming up to 420 with 8 DEG C/min heating rate in nitrogen atmosphere, by the very thin film of step 3. from 150 DEG C
DEG C, 30min is incubated at 450 DEG C, carries out imidization reaction；Room temperature is cooled to, using mechanical stripping technology by acid imide
Change the film obtained after reaction to peel off from glass substrate, obtain polyimides based coextruded film.
Polyimides based coextruded film made from the present embodiment, including polyimide matrix and it is dispersed in the polyimides
Nano silicon in matrix, polyimide matrix and nano silicon form the network structure of IPN, polyimide-based
The structural formula of body is：
The thermal coefficient of expansion of above-mentioned polyimides based coextruded film is 3.5ppm/K, tensile modulus of elasticity 12GPa, Tg's
Temperature range is 230 DEG C, and heat decomposition temperature Td is 580 DEG C；The UV cut-off wavelength of the laminated film is 430nm.Wherein,
Transmitance at 550nm is 88%, and the transmitance in whole visible region is 78%.
It should be noted that according to the above description the announcement of book and with illustrate, those skilled in the art in the invention also
Above-mentioned embodiment can be changed and changed.Therefore, the invention is not limited in disclosed and described above specific real
Mode is applied, some equivalent modifications and change to the present invention should also be as within the scope of the claims of the present invention.This
Outside, although having used some specific terms in this specification, these terms merely for convenience of description, not to the present invention
Form any restrictions.
Claims (10)
1. a kind of preparation method of polyimides based coextruded film, it is characterised in that comprise the following steps：
(1) inorganic nano material, dispersant, binding agent, solvent are mixed in proportion, stirred, obtain inorganic nano material
Slurry, the inorganic nano material slurry include each component of following parts by weight：Nano inorganic material 4-8 parts, dispersant
1-2 parts, binding agent 2-4 parts, organic solvent 80-200 parts；Wherein, the inorganic nano material includes nano silicon, nanometer
One or more in silicon nitride, nano aluminium oxide and nano titanium oxide；
(2) the aromatic dianhydride monomer as shown in following formula (I) and the aromatic diamine monomers shown in formula (II) are added to the nothing
In machine nano material slurry, polymerisation is carried out in a nitrogen atmosphere, obtains polymerization liquid；
H2N-Ar'-NH2(II),
Wherein, Ar is selected fromIn
One kind, Ar ' is selected from In one kind；
(3) in a nitrogen atmosphere, the polymerization liquid is toasted into film forming coated on base material；
(4) in a nitrogen atmosphere, film obtained by step (3) is subjected to imidization reaction at high temperature, removes base material, gathered
Imide laminated film.
2. preparation method as claimed in claim 1, it is characterised in that the aromatic dianhydride monomer and the aromatic diamines list
The gross weight of body is 90-150 parts.
3. preparation method as claimed in claim 2, it is characterised in that the aromatic dianhydride monomer and the aromatic diamines
Mol ratio is 1:(0.95-1.05).
4. preparation method as claimed in claim 1, it is characterised in that the particle diameter of the inorganic nano material is 20-50nm.
5. preparation method as claimed in claim 1, it is characterised in that the dispersant is Sodium Polyacrylate, ammonium polyacrylate
One or more in salt, ethyl acetate, butyl acetate and APES；The binding agent is peroxidating diisopropyl
Benzene, hydroxypropyl methyl cellulose, nitrone derivative, styrene-butadiene block copolymer and butadienyl triethoxysilane
In one or more；The organic solvent is selected from N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N- methyl -2- pyrroles
One or more in pyrrolidone and dimethyl sulfoxide (DMSO).
6. preparation method as claimed in claim 1, it is characterised in that in step (2), the temperature of the polymerisation is 30-
60 DEG C, the reaction time of the polymerisation is 2-10h.
7. preparation method as claimed in claim 1, it is characterised in that the temperature of the baking film forming is 120-150 DEG C, described
The time of baking is 6-60min.
8. preparation method as claimed in claim 1, it is characterised in that in step (4), the temperature of the imidization reaction is
400-450 DEG C, reaction time 6-60min.
9. a kind of polyimides based coextruded film, the polyimides based coextruded film includes polyimide matrix and is supported on institute
The inorganic nano material in polyimide matrix is stated, the polyimide matrix has three-dimensional net structure；The polyimides
Shown in the structural formula of matrix such as following formula (III)：
Wherein, Ar is selected from In one kind,
Ar ' is selected from In
One kind；N is the degree of polymerization, and n is 1-1000 natural numbers.
10. polyimides based coextruded film as claimed in claim 9, it is characterised in that the quality of the inorganic nano material
Account for the 2%-10% of the laminated film quality.
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| CN108342082A (en) * | 2018-02-27 | 2018-07-31 | 深圳市华星光电半导体显示技术有限公司 | A kind of preparation method of the flexible material with sealer |
| CN108822092A (en) * | 2018-08-31 | 2018-11-16 | 吉林大学 | A kind of polyimides and preparation method thereof of dianhydride monomer of the structure containing pyrazine and preparation method thereof and a kind of structure containing pyrazine |
| CN108898073A (en) * | 2018-06-12 | 2018-11-27 | 武汉天马微电子有限公司 | Display panel and preparation method thereof and display device |
| CN108986665A (en) * | 2018-07-24 | 2018-12-11 | 武汉华星光电半导体显示技术有限公司 | Fexible film production method, fexible film, display panel and electronic equipment |
| CN109082119A (en) * | 2018-07-02 | 2018-12-25 | 东营欣邦电子科技有限公司 | A kind of cellulose modified polyimides corona-resistant film and preparation method thereof |
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| CN112920603A (en) * | 2021-01-28 | 2021-06-08 | 苏州泰仑电子材料有限公司 | High-temperature-resistant scratch-resistant high-transparency PI film |
| US11059204B2 (en) | 2018-02-27 | 2021-07-13 | Shenzhen China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Method for manufacturing flexible material having surface protecting layer |
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| CN108342082A (en) * | 2018-02-27 | 2018-07-31 | 深圳市华星光电半导体显示技术有限公司 | A kind of preparation method of the flexible material with sealer |
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| CN109082119A (en) * | 2018-07-02 | 2018-12-25 | 东营欣邦电子科技有限公司 | A kind of cellulose modified polyimides corona-resistant film and preparation method thereof |
| CN108986665A (en) * | 2018-07-24 | 2018-12-11 | 武汉华星光电半导体显示技术有限公司 | Fexible film production method, fexible film, display panel and electronic equipment |
| CN108822092A (en) * | 2018-08-31 | 2018-11-16 | 吉林大学 | A kind of polyimides and preparation method thereof of dianhydride monomer of the structure containing pyrazine and preparation method thereof and a kind of structure containing pyrazine |
| CN108822092B (en) * | 2018-08-31 | 2020-05-08 | 吉林大学 | Dianhydride monomer containing pyrazine structure and preparation method thereof, polyimide containing pyrazine structure and preparation method thereof |
| CN112920603A (en) * | 2021-01-28 | 2021-06-08 | 苏州泰仑电子材料有限公司 | High-temperature-resistant scratch-resistant high-transparency PI film |
| CN116278282A (en) * | 2023-04-06 | 2023-06-23 | 临沂千源包装印刷有限公司 | Preparation method of heat-resistant polyethylene-nylon composite film |
| CN116278282B (en) * | 2023-04-06 | 2023-08-08 | 临沂千源包装印刷有限公司 | Preparation method of heat-resistant polyethylene-nylon composite film |
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Application publication date: 20180216 |