CN101311224B - Hybrid material composition, flexible transparent film comprising the same and photoelectric device - Google Patents
Hybrid material composition, flexible transparent film comprising the same and photoelectric device Download PDFInfo
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Abstract
The invention relates to a hybrid material composite with high transparency, high heat resistance and low thermal expansion coefficient, a flexible transparent film and photoconducting devices containing the composite. The composite comprises: a. silicon dioxide(SiO2) and b. polyamide, which is characterized in that the weight ratio of the silicon dioxide(SiO2) and the polyamide is between 1:9 and 9:1.
Description
Technical field
The present invention relates to a kind of hybrid material composition, the hybrid material composition of particularly a kind of high-transmittance, high heat-resisting, low thermal coefficient of expansion, and the film and the photoelectric device that utilize its gained.
Background technology
In recent years, along with the fast development of plane technique of display, in the improvement of indicating meter, also be focussed in particular on little, the lightweight demand of volume.In order to obtain slimming, lightweight, the method that present industry is adopted has two kinds: one is to use thinner glass, and two are to use plastic material to make substrate.Yet, if use the following glass of 0.5 millimeter thickness as substrate, the caused buckling phenomenon of the meeting own weight of Yi Fashengyin glass in manufacturing processed, and cause breaking.In addition, glass has fragile, not shock-resistant and congenital shortcoming such as thickness and weight is bigger.Therefore, this type of substrate will can't satisfy demands such as light weight, slimming and the deflection of new generation product application, folding use gradually.
Utilize plastic base (also being called flexibility (flexible) substrate) to form flat-panel screens; Except advantages such as the indicating meter than tradition use glass substrate has gentlier, but thinner, shock-resistant, difficult broken curved surface shows and can reel; And continuous mode also capable of using (roll-to-roll) is produced; So can significantly reduce production costs, therefore become the development trend of following indicating meter of new generation.Yet; There are many process conditions restrictions still need overcome at present; And plastic material character still need be improved; Just can make the comprehensive importing flat-panel screens of plastic base processing procedure and replace glass substrate, for example: 1. have high-clarity, high thermal stability, low thermal coefficient of expansion, and the exploitation of the plastic base material of high resistant manner simultaneously.2. the exploitation that has the nesa coating of deflection character.3. make the device process technique exploitation of thin film transistor (thin film transistor) on the plastic base.4. the relevant panel processing procedure of back segment and developing material and collocation etc.Wherein, the flexible flat indicating meter develops successful important key factor no more than the development progress of flexible transparent plastic baseplate material, its development trend with about the developing direction and the utilization of following whole flexible display panel.
Be applicable to the employed plastic base of flat-panel screens in order to provide, Japanese Patent JP2005-187768 has disclosed the method that inorganic materials is imported polyimide, with the further properties of materials (thermal stability, thermal expansivity) that improves.This method comprises utilizes organic solvent with aliphatics or the dissolving of half aliphatic polyimide, then adds the reaction of coupler and polyimide functional end-group, then adds silane oxide and water again and participates in reaction.Yet, owing to use silane oxide and water as reactant, at most can only blending small amounts of inorganic silica gel material (being at most 20%) in the matrix material that this patent disclosed, therefore make the effect of modification be restricted.
For increasing the blending ratio of inorganic materials, reach the purpose of modification, another prior art has disclosed mixes polyamic acid PAA (polyamic acid) with silicic acid oligomer (silicic acid oligomer).Though this method can be increased to 40% with the doping ratio of inorganics, yet the material of gained must pass through high temperature endless loop reaction so have yellow color, process substrate after its transparency obviously reduce.
Therefore, mutual solubility and the mixing proportion that how to improve polyimide and silicon-dioxide is the problem that the plane shows the process technique research to obtain high-clarity, high thermal stability, low thermal coefficient of expansion, and the plastic base of high resistant manner.
Summary of the invention
The object of the present invention is to provide the hybrid material composition of a kind of high-transmittance, high heat-resisting, low thermal coefficient of expansion, can be used to further form the flexible transparent film that is applicable to optoelectronic equipment (for example: display unit or solar cell).
For reaching above-mentioned purpose, high-transmittance of the present invention, high hybrid material composition heat-resisting, low thermal coefficient of expansion can comprise a. silicon-dioxide (SiO
2) and the b. polyimide, it is characterized in that this silicon-dioxide (SiO
2) and the weight ratio of polyimide between 1: 9 to 9: 1, preferred weight ratio is between 2: 8 to 9: 1.It can comprise following fabrication steps: with silicon-dioxide (SiO
2) be dissolved in the organic solvent and uniform mixing, wherein this silicon-dioxide (SiO with polyimide
2) and the weight ratio of polyimide system between 2: 8 to 9: 1; And, add silicone surfactant and participate in reaction with polar functional group.
In addition, one embodiment of the present invention provides flexible transparent film, and this film can comprise a. silicon-dioxide (SiO
2) and the b. polyimide, it is characterized in that this silicon-dioxide (SiO
2) and the weight ratio of polyimide between 1: 9 to 9: 1.It can comprise following fabrication steps: with silicon-dioxide (SiO
2) be dissolved in the organic solvent and uniform mixing obtains solution this silicon-dioxide (SiO wherein with polyimide
2) and the weight ratio of polyimide between 2: 8 to 9: 1; In above-mentioned solution, add silicone surfactant, obtain coating composition with polar functional group; And, utilize this coating composition to form rete, and this rete is heat-treated.Wherein this heat treated temperature is between 100～300 degree.
Below through several embodiment and comparing embodiment and conjunction with figs., illustrating further method of the present invention, characteristic and advantage, but be not to be used for limiting scope of the present invention, scope of the present invention should be as the criterion with appended claims.
Description of drawings
Fig. 1 shows the analytical results of the thermogravimetric analysis of the embodiment of the invention 5 and comparing embodiment 1 gained substrate.
Fig. 2-4 shows that the silica/polyimides of the embodiment of the invention 5 gained blendes together film (numbering: SiO2/BB64) the surface scan formula electron microscope spectrogram under different enlargement ratios.
Embodiment
The present invention provides the silica/polyimides hybrid material composition; It has high-transmittance, high heat-resisting, low thermal coefficient of expansion; The upper and lower plate that can be applicable to bendable flat-panel screens supports, and said composition is mainly formed according to the different ratios hybrid reaction by silicon-dioxide and polyimide.
Silicon-dioxide is except having high transparent, high heat-stable characteristic; Also has the ultra low heat expansion coefficient; And polyimide has high transparent, high heat-resisting and good flexibility, forms so the present invention mainly utilizes silicon-dioxide to mix according to different ratios with polyimide to have that height is transparent, height is heat-resisting and silica/polyimides low thermal coefficient of expansion blendes together the compsn of thin-film material.In addition, the present invention utilizes this silicon-dioxide of organic solution dissolving in advance, forming the silicon-dioxide of microstructure, and further mixes with polyimide, and the addition of silicon-dioxide is improved, and obtains characteristics such as high transparent, high heat-resisting and low thermal coefficient of expansion.
A series of preferred embodiments are described according to the present invention comprises the film that silica/polyimides blendes together material, and its penetration coefficient can be higher than 90%, glass transition temp can be higher than 350 degree, thermal expansivity can be less than 30ppm/ ℃.
The preparation of this silica/polyimides matrix material is following: with silicon-dioxide (SiO
2) be dissolved in the organic solvent, wherein be dissolved in the silicon-dioxide (SiO in this organic solvent
2) solid content less than 40%.Then, add polyimide solution, wherein the weight ratio of this silicon-dioxide and polyimide is between 2: 8 to 9: 1.Behind the uniform mixing, add silicone surfactant again and participate in reaction with polar functional group.
According to the present invention, this organic solvent can be DMAC N,N (DMAC), N (DMF), DMSO 99.8MIN. (DMSO), gamma-butyrolactone (γ-butyrolactone).This silicone surfactant with polar functional group can be aminosiloxane (aminosiloxane), isocyanic acid siloxanes (isocynate siloxane).This polyimide has suc as formula the structure shown in (I):
Wherein, n is greater than 1; G is one or more polycyclic naphthenic base, heterocyclic radical, the naphthenic base with one or more unsaturated link(age)s and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Optionally can be replaced by halogen, alkyl, sulfane base, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base; Wherein alkyl, sulfane base, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain the 1-12 carbon atom, and it is a straight or branched; And; A is polycyclic naphthenic base, heterocyclic radical, the naphthenic base with one or more unsaturated link(age)s and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Optionally can be replaced by halogen, alkyl, sulfane base, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base, wherein alkyl, sulfane base, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain the 1-12 carbon atom, and it is a straight or branched.
In addition, according to one preferred embodiment of the present invention, the described G of its Chinese style (I) can be
Polyimide of the present invention typical polycondensation capable of using (polycondensation) comes synthetic; Its compound method has two kinds; First method divides two stages to carry out; At first diamines (diamine) and dicarboxylic anhydride (dianhydride) monomer are reacted in polar solvent; Form precursor (precursor) polyamic acid of polyimide, and then carry out inferior amidation (imidization) reaction, make its dehydration endless loop transform into polyimide with pyroprocess (300～400 ℃) or chemical method.Second method is that diamines and dicarboxylic anhydride monomer are reacted in phenol solvent (meta-cresol (m-cresol), chlorophenol (Cl-phenol)), is warming up to the reflux temperature reaction, forms polyimide.
Following spy enumerates embodiment 1～8, in order to explanation the present invention, so that make the present invention can be more clear:
The preparation of polyimide
Embodiment 1: polyimide B1317-BAPPm's (BB) is synthetic
At room temperature; Use three-necked bottle and pass to nitrogen,
dissolves in the meta-cresol (m-cresol) of 32.94g with 0.0147 mole BAPPm pentanoic.Treat again 0.015 mole B1317 dicarboxylic anhydride
to be added after the BAPPm pentanoic dissolves fully; After B1317 dissolves fully; Continue stirring 1 hour, and form the polyamic acid solution of sticky shape.Then, be heated to 220 ℃, continue 3 hours, in this reaction process, with de-watering apparatus water is got rid of simultaneously.Reaction solution is splashed in the methyl alcohol, make the polyimide deposition, and in vacuum drying oven, dried 12 hours, obtain polyimide B1317-BAPPm (BB).
Reaction formula is as follows:
The preparation of silica/polyimides composite membrane
Embodiment 2:
At room temperature, 3g silicon-dioxide is dissolved among the DMAc with solid content 20%, then 7g B1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%, and both are put into the 20g sample bottle.Then; Add the 0.3g aminosiloxane in sample bottle; After at room temperature stirring 30 minutes, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour; And take off from glass, the silica/polyimides that just can obtain thickness and be 537 μ m blendes together film (SiO2/BB37).At last, measure this silica/polyimides blend together film (numbering: coefficient of expansion SiO2/BB37) and penetration coefficient, the result sees also table 1.
Embodiment 3:
At room temperature, 4g silicon-dioxide is dissolved among the DMAc with solid content 20%, then 6g B1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%, and both are put into the 20g sample bottle.Then; Add the 0.2g aminosiloxane in sample bottle; After at room temperature stirring 30 minutes, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour; And take off from glass, the silica/polyimides that just can obtain thickness and be 55 μ m blendes together film (SiO2/BB46).At last, measure this silica/polyimides blend together film (numbering: coefficient of expansion SiO2/BB46) and penetration coefficient, the result sees also table 1.
Embodiment 4:
At room temperature, 5g silicon-dioxide is dissolved among the DMAc with solid content 20%, then 5gB1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%, and both are put into the 20g sample bottle.Then; Add the 0.2g aminosiloxane in sample bottle; After at room temperature stirring 30 minutes, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour; And take off from glass, the silica/polyimides that just can obtain thickness and be 52 μ m blendes together film (SiO2/BB55).At last, measure this silica/polyimides blend together film (numbering: coefficient of expansion SiO2/BB55) and penetration coefficient, the result sees also table 1.
Embodiment 5:
At room temperature, 6g silicon-dioxide is dissolved among the DMAc with solid content 20%, then 4gB1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%, and both are put into the 20g sample bottle.Then; Add the 0.2g aminosiloxane in sample bottle; After at room temperature stirring 30 minutes, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour; And take off from glass, the silica/polyimides that just can obtain thickness and be 53 μ m blendes together film (SiO2/BB64).At last, measure this silica/polyimides blend together film (numbering: coefficient of expansion SiO2/BB64) and penetration coefficient, the result sees also table 1.
Embodiment 6:
At room temperature, 7g silicon-dioxide is dissolved among the DMAc with solid content 20%, then 3gB1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%, and both are put into the 20g sample bottle.Then; Add the 0.12g aminosiloxane in sample bottle; After at room temperature stirring 30 minutes, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour; And take off from glass, the silica/polyimides that just can obtain thickness and be 51 μ m blendes together film (SiO2/BB73).At last, measure this silica/polyimides blend together film (numbering: coefficient of expansion SiO2/BB73) and penetration coefficient, the result sees also table 1.
Comparing embodiment 1:
At room temperature, 10g B1317-BAPPm (BB) is dissolved among the DMAc with solid content 20%.Then, it is coated on glass with the scraper mode, and put into baking oven and under 80 ℃ and 150 ℃, respectively toasted 1 hour, and take off, just can obtain the Kapton that thickness is 57 μ m from glass.At last, measure the thermal expansivity and the penetration coefficient of this Kapton, the result sees also table 1.
Table 1
As shown in table 1, along with the increase of dioxide-containing silica, the thermal expansivity of this film significantly reduces, and especially when the weight ratio of silicon-dioxide and polyimide reaches 7: 3 (when dioxide-containing silica accounts for 70%), thermal expansivity more can be lower than 30ppm/ ℃.In addition, even dioxide-containing silica reaches 70%, this film still has high penetration coefficient.
Thermotolerance, strength test and surface analysis
The silica/polyimides of embodiment 5 gained is blended together film, and (numbering: SiO2/BB64) the pure Kapton with comparing embodiment 1 gained carries out thermogravimetric analysis (Thermal Gravimetric Analysis), and its result asks for an interview Fig. 1.Learn that by knowing among the figure dioxide-containing silica accounts for 60% film, its heat-resisting character is obviously improved many than pure polyimide substrate.In addition, please with reference to Fig. 2-4, the silica/polyimides that they are respectively embodiment 5 gained blendes together film (numbering: SiO2/BB64) the surface scan formula electron microscope spectrogram under different enlargement ratios.
Then; The silica/polyimides of embodiment 5 gained is blended together film, and (numbering: SiO2/BB64) the pure Kapton with comparing embodiment 1 gained carries out strength analysis; Measure its Young's modulus (Young ' s modulus (Gpa)), maximum stress (stress), and maximum tension (strain), its result is as shown in table 2.
Table 2
As shown in table 2, the silica/polyimides of embodiment 5 gained blendes together film (numbering: SiO2/BB64) have higher physical strength, be suitable as the employed supporting substrate of flat-panel screens and replace the conventional glass substrate.
Though the present invention discloses as above with preferred embodiment, so it is not in order to limit the present invention.Those skilled in the art under any the present invention are not breaking away from the spirit and scope of the present invention, and Ying Kezuo changes arbitrarily and retouching, and therefore, protection scope of the present invention should be as the criterion with appended claims institute restricted portion.
Claims (12)
1. hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion, its by
A. silicon-dioxide (SiO
2);
B. polyimide;
C. silicone surfactant; And
D. organic solvent
Form,
Wherein, utilize this silicon-dioxide of this organic solvent dissolution (SiO in advance
2), and this silicon-dioxide (SiO
2Solid content in this organic solvent is less than 40%;
And, this silicon-dioxide (SiO in this hybrid material composition
2) and the weight ratio of polyimide between 1: 9 to 9: 1.
2. the hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion as claimed in claim 1, wherein this silicon-dioxide (SiO
2) and the weight ratio of polyimide between 2: 8 to 9: 1.
3. the hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion as claimed in claim 1, wherein this silicone surfactant has polar functional group.
4. the hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion as claimed in claim 3, wherein this silicone surfactant with polar functional group is an aminosiloxane.
5. the hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion as claimed in claim 1, wherein this polyimide has suc as formula the structure shown in (I):
Formula (I)
Wherein, n is greater than 1;
G is more than one polycyclic naphthenic base, heterocyclic radical, the naphthenic base with an above unsaturated link(age) and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Can be replaced by halogen, alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base; Wherein alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain 1-12 carbon atom, and it is a straight or branched; And
A is polycyclic naphthenic base, heterocyclic radical, the naphthenic base with an above unsaturated link(age) and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Can be replaced by halogen, alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base; Wherein alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain 1-12 carbon atom, and it is a straight or branched.
6. flexible transparent film; This film is to use the following hybrid material composition that is used to make the flexible transparent film of high-transmittance, high heat-resisting, low thermal coefficient of expansion to process, and the hybrid material composition of the said flexible transparent film that is used to make high-transmittance, high heat-resisting, low thermal coefficient of expansion is by a. silicon-dioxide (SiO
2); B. polyimide; C. silicone surfactant and d. organic solvent are formed, and wherein, utilize this silicon-dioxide of this organic solvent dissolution (SiO in advance
2), and this silicon-dioxide (SiO
2) solid content in this organic solvent is less than 40%, and this silicon-dioxide (SiO in this hybrid material composition
2) and the weight ratio of polyimide between 1: 9 to 9: 1.
7. flexible transparent film as claimed in claim 6, wherein this silicon-dioxide (SiO
2) and the weight ratio of polyimide between 2: 8 to 9: 1.
8. flexible transparent film as claimed in claim 6, wherein this silicone surfactant has polar functional group.
9. flexible transparent film as claimed in claim 6, wherein this silicone surfactant with polar functional group is an aminosiloxane.
10. flexible transparent film as claimed in claim 6, wherein this polyimide has suc as formula the structure shown in (I):
Formula (I)
Wherein, n is greater than 1;
G is more than one polycyclic naphthenic base, heterocyclic radical, the naphthenic base with an above unsaturated link(age) and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Can be replaced by halogen, alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base; Wherein alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain the 1-12 carbon atom, and it is a straight or branched; And
A is polycyclic naphthenic base, heterocyclic radical, the naphthenic base with an above unsaturated link(age) and heterocyclic radical, aryl, heteroaryl, aliphatic group, ring grease dialkylene, aralkyl or heteroaralkyl; And each ring has 3 to 8 annular atomses; And the hydrogen on each annular atoms; Can be replaced by halogen, alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base; Wherein alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base or alkynyloxy group contain 1-12 carbon atom, and it is a straight or branched.
11. flexible transparent film as claimed in claim 10, wherein the hydrogen on each annular atoms of A can be replaced by halogen, alkyl, alkoxyl group, alkane thiazolinyl, alkane alkynyl, alkene oxygen base, alkynyloxy group or aromatic base.
12. a photoelectric device comprises each described flexible transparent film in the claim 6～11.
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| CN113462157B (en) * | 2021-07-21 | 2023-09-26 | 马鞍山东毅新材料科技有限公司 | High-temperature-resistant polyimide display panel film and production process thereof |
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