Method of manufacturing colorless transparent polyimide film having impregnated glass fabric and of flattening surface thereof

Patent metadata

Field	Value
Publication number	US-9469735-B2
Application number	US-201414768018-A
Country	US
Kind code	B2
Filing date	Feb 25, 2014
Priority date	Feb 27, 2013
Publication date	Oct 18, 2016
Grant date	Oct 18, 2016

Abstract

Disclosed is a method of manufacturing a colorless transparent polyimide film having impregnated glass fabric, wherein the surface of the polyimide film substrate having impregnated glass fabric is flattened by two flattening steps using a roll-to-roll process, thereby solving problems with an increase in surface roughness of the polyimide substrate when manufacturing the polyimide film having impregnated glass fabric in order to enhance thermal and mechanical properties of a film for use in flexible display substrates and in cover windows for flat panel displays and mobile phones. As the surface roughness of the polyimide film having impregnated glass fabric is flattened to the level of ones of nm from the level ranging of tens of nm to ones of μm, a thin film transistor process can be performed on the polyimide film substrate and the polyimide film is increased in optical transmittance and transparency and can thus be utilized as flexible display substrates and cover windows for flat panel displays and mobile phones.

First claim

What is claimed is:

1. A method of manufacturing a polyimide film having impregnated glass fabric, comprising:
(1) impregnating glass fabric with a polyamic acid solution, thus obtaining a polyamic acid film having impregnated glass fabric;
(2) flattening the polyamic acid film having impregnated glass fabric obtained in (1) (first flattening process) at a temperature between the Tg of the polyamic acid film and the imidization temperature of the polyamic acid;
(3) subjecting the polyamic acid film obtained in (2) to imidization, thus obtaining a polyimide film having impregnated glass fabric; and
(4) flattening the polyimide film having impregnated glass fabric obtained in (3) (second flattening process) at a temperature between the Tg of the polyimide film and the thermal decomposition temperature of the polyimide film;
wherein the flattening steps are performed by applying pressure using cylindrical rollers or flat plates having a surface roughness of 0.5 to 2 nm.

2. The method of claim 1 , wherein the polyamic acid solution in (1) is prepared by dissolving a dianhydride compound and a diamine compound in a solvent and then performing polymerization.

3. The method of claim 2 , wherein the dianhydride compound comprises any one or a mixture of two or more selected from the group consisting of 4,4′-oxydiphthalic anhydride (OPDA), pyromellitic dianhydride (PMDA), 3,3′,4,4′-diphenylsulfone tetracarboxylic dianhydride (DSDA), 3,3′,4,4′-benzophenone tetracarboxylic dianhydride (BTDA), 4-(2,5-dioxotetrahydrofuran-3-yl)-1,2,3,4-tetrahydronaphthalene-1,2-dicarboxylic anhydride (DTDA), 4,4′-bisphenol A dianhydride (BPADA), 4,4′-(hexafluoroisopropylidene)diphthalic anhydride (6FDA), bicycle[2.2.2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride (BCDA), 3,3′,4,4′-biphenyl tetracarboxylic dianhydride (BPDA), 5-(2,5-dioxotetrahydrofuryl)-3-methyl-3-cyclohexene-1,2-dicarboxylic anhydride (DOMDA), ethylene diamine tetraacetic dianhydride (EDTE), and 1,2,4,5-cyclohexanetetracarboxylic dianhydride (CHDA).

4. The method of claim 2 , wherein the diamine compound comprises any one or a mixture of two or more selected from the group consisting of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BAHFP), 1,3-bis(3-aminophenoxy)benzene (m-BAPB), 4,4′-bis(4-aminophenoxy)biphenyl (p-BAPB), 2,2-bis(3-aminophenyl)hexafluoropropane (BAPF), bis[4-(3-aminophenoxy)phenyl]sulfone (m-BAPS), 2,2-bis[4-(4-aminophenoxy)phenyl]sulfone (p-BAPS), bis(3-aminophenyl)sulfone (APS), m-xylylenediamine (m-XDA), p-xylylenediamine (p-XDA), 3,4′-oxydianiline (3,4-ODA), 2,2-bis(3-amino-4-methylphenyl)hexafluoropropane (BAMF), 4,4′-diaminooctafluorobiphenyl, 3,3′-dihydroxybenzidine, 2,2′-ethylenedianiline, 2,2′-bis(trifluoromethyl)benzidine (TFB), 2,2′,5,5′-tetrachlorobenzidine, bis(3-aminophenyl)methanone, 2,7-diaminofluorene, 2-chloro-p-phenylenediamine, 1,3-bis(3-aminopropyl)-tetramethyldisiloxane, 1,1-bis(4-aminophenyl)cyclohexane, 9,9-bis(4-aminophenyl)fluorene, 5-(trifluoromethyl)-1,3-phenylenediamine, 4,4′-methylenebis(2-methylcyclohexylamine), 4-fluoro-1,2-phenylenediamine, 4,4′-(1,3-phenylenediisopropylidene)bisaniline, 4-nitro-1,3-phenylenediamine, 4-chloro-1,3-phenylenediamine, 1,3,5-triazine-2,4,6-triamine (Melamine), 3,5-diaminobenzonitrile, 1,3-bis(aminomethyl)cyclohexane (m-CHDA), 1,4-bis(aminomethyl)cyclohexane (p-CHDA), 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane (6FBAPP), 2,2′-bis(trifluoromethyl)benzidine (MDB), 4,4′-oxydianiline (4,4′-ODA), 2,2-bis[4-(4-aminophenoxy)phenyl] propane (BAPP), 1,3-cyclohexanediamine, 1,4-cyclohexanediamine, and bis(4-aminophenyl) sulfide (4,4′-SDA).

5. The method of claim 4 , wherein the flattening steps are performed using cylindrical rollers.

6. The method of claim 4 , wherein the flattening steps are performed by positioning the polyamic acid film or the polyimide film between two flat plates and then applying pressure thereto.

7. The method of claim 1 , wherein imidization in (3) is performed by subjecting the polyamic acid film to a thermal process (thermal imidization) to give a polyimide film having impregnated glass fabric.

8. The method of claim 7 , wherein the polyamic acid film is subjected to thermal imidization in a temperature range of 100˜300° C.

9. The method of claim 1 , wherein imidization in (3) is performed by subjecting the polyamic acid film to a chemical process (chemical imidization) to give a polyimide film having impregnated glass fabric.

Assignees

• Korea Advanced Inst Sci & Tech

Inventors

• Yoon Choon Sup
• Oh Seung Hyun

Classifications

• C08J5/24 Primary

  Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs · CPC title

• C08J2379/08

  Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors · CPC title

• B32B5/02 Primary

  characterised by structural features of a {fibrous or filamentary} layer {(layer formed of metallic wires B32B15/02; layer formed of natural mineral fibres B32B19/02; layer formed of wood fibres B32B21/02)} · CPC title

• C08J5/00

  Manufacture of articles or shaped materials containing macromolecular substances (manufacture of semi-permeable membranes B01D67/00 - B01D71/00) · CPC title

• C08J5/18

  Manufacture of films or sheets · CPC title