TW202406983A - 聚醯亞胺前驅物組合物及使用彼所形成的光學多層結構體 - Google Patents
聚醯亞胺前驅物組合物及使用彼所形成的光學多層結構體 Download PDFInfo
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- TW202406983A TW202406983A TW112118688A TW112118688A TW202406983A TW 202406983 A TW202406983 A TW 202406983A TW 112118688 A TW112118688 A TW 112118688A TW 112118688 A TW112118688 A TW 112118688A TW 202406983 A TW202406983 A TW 202406983A
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- polyimide precursor
- precursor composition
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 128
- 239000000203 mixture Substances 0.000 title claims abstract description 127
- 239000004642 Polyimide Substances 0.000 title claims abstract description 109
- 239000002243 precursor Substances 0.000 title claims abstract description 90
- 230000003287 optical effect Effects 0.000 title claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 45
- -1 siloxane structure Chemical group 0.000 claims abstract description 25
- 239000010954 inorganic particle Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims description 57
- 150000004985 diamines Chemical class 0.000 claims description 31
- 125000003118 aryl group Chemical group 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 150000008065 acid anhydrides Chemical class 0.000 claims description 23
- 125000003700 epoxy group Chemical group 0.000 claims description 23
- 125000002947 alkylene group Chemical group 0.000 claims description 19
- 239000000975 dye Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 125000000962 organic group Chemical group 0.000 claims description 17
- 229910052736 halogen Inorganic materials 0.000 claims description 16
- 150000002367 halogens Chemical group 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 229910052731 fluorine Inorganic materials 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 239000010408 film Substances 0.000 claims description 9
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical compound FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000013039 cover film Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- MSTZGVRUOMBULC-UHFFFAOYSA-N 2-amino-4-[2-(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropan-2-yl]phenol Chemical compound C1=C(O)C(N)=CC(C(C=2C=C(N)C(O)=CC=2)(C(F)(F)F)C(F)(F)F)=C1 MSTZGVRUOMBULC-UHFFFAOYSA-N 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 239000005341 toughened glass Substances 0.000 claims description 6
- 239000001055 blue pigment Substances 0.000 claims description 5
- HHLMWQDRYZAENA-UHFFFAOYSA-N 4-[4-[2-[4-(4-aminophenoxy)phenyl]-1,1,1,3,3,3-hexafluoropropan-2-yl]phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC1=CC=C(C(C=2C=CC(OC=3C=CC(N)=CC=3)=CC=2)(C(F)(F)F)C(F)(F)F)C=C1 HHLMWQDRYZAENA-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001045 blue dye Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- BEKFRNOZJSYWKZ-UHFFFAOYSA-N 4-[2-(4-aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-yl]aniline Chemical compound C1=CC(N)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(N)C=C1 BEKFRNOZJSYWKZ-UHFFFAOYSA-N 0.000 claims description 2
- IWFSADBGACLBMH-UHFFFAOYSA-N 4-[4-[4-[4-amino-2-(trifluoromethyl)phenoxy]phenyl]phenoxy]-3-(trifluoromethyl)aniline Chemical group FC(F)(F)C1=CC(N)=CC=C1OC1=CC=C(C=2C=CC(OC=3C(=CC(N)=CC=3)C(F)(F)F)=CC=2)C=C1 IWFSADBGACLBMH-UHFFFAOYSA-N 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000005083 Zinc sulfide Substances 0.000 claims description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 125000002993 cycloalkylene group Chemical group 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- KDWQLICBSFIDRM-UHFFFAOYSA-N 1,1,1-trifluoropropane Chemical compound CCC(F)(F)F KDWQLICBSFIDRM-UHFFFAOYSA-N 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 9
- 239000010410 layer Substances 0.000 description 103
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- 239000003999 initiator Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 11
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 10
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- 239000007787 solid Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003431 cross linking reagent Substances 0.000 description 7
- 239000002270 dispersing agent Substances 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 125000002723 alicyclic group Chemical group 0.000 description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 229920005575 poly(amic acid) Polymers 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 6
- 238000001029 thermal curing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000000016 photochemical curing Methods 0.000 description 5
- 229920002647 polyamide Polymers 0.000 description 5
- 125000006586 (C3-C10) cycloalkylene group Chemical group 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- QCGKUFZYSPBMAY-UHFFFAOYSA-N methyl 7-oxabicyclo[4.1.0]heptane-4-carboxylate Chemical compound C1C(C(=O)OC)CCC2OC21 QCGKUFZYSPBMAY-UHFFFAOYSA-N 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 2
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- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 2
- LJGHYPLBDBRCRZ-UHFFFAOYSA-N 3-(3-aminophenyl)sulfonylaniline Chemical compound NC1=CC=CC(S(=O)(=O)C=2C=C(N)C=CC=2)=C1 LJGHYPLBDBRCRZ-UHFFFAOYSA-N 0.000 description 2
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- KMKWGXGSGPYISJ-UHFFFAOYSA-N 4-[4-[2-[4-(4-aminophenoxy)phenyl]propan-2-yl]phenoxy]aniline Chemical compound C=1C=C(OC=2C=CC(N)=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OC1=CC=C(N)C=C1 KMKWGXGSGPYISJ-UHFFFAOYSA-N 0.000 description 2
- NJWZAJNQKJUEKC-UHFFFAOYSA-N 4-[4-[2-[4-[(1,3-dioxo-2-benzofuran-4-yl)oxy]phenyl]propan-2-yl]phenoxy]-2-benzofuran-1,3-dione Chemical compound C=1C=C(OC=2C=3C(=O)OC(=O)C=3C=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OC1=CC=CC2=C1C(=O)OC2=O NJWZAJNQKJUEKC-UHFFFAOYSA-N 0.000 description 2
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- CQSISKINANYZED-UHFFFAOYSA-N 5-[4-[4-[(1,3-dioxo-2-benzofuran-5-yl)oxy]phenyl]sulfanylphenoxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC2=CC=C(C=C2)SC2=CC=C(C=C2)OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 CQSISKINANYZED-UHFFFAOYSA-N 0.000 description 2
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- 229910052794 bromium Inorganic materials 0.000 description 2
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- 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
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- 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
- C08G73/1057—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
- C08G73/106—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain containing silicon
-
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
本發明涉及一種聚醯亞胺前驅物組合物和光學多層結構體,所述聚醯亞胺前驅物組合物包含含有矽氧烷結構的聚醯亞胺前驅物以及無機顆粒,所述光學多層結構體包括形成在基板上的聚醯亞胺防飛散層結構,其係利用所述聚醯亞胺前驅物組合物所形成。根據一個實施方案的所述光學多層結構體的翹曲現象減少,從而使基板的彎曲最小化的同時顯著提高表面的硬度,因此具有優異的機械特性。
Description
本發明涉及一種聚醯亞胺前驅物組合物以及包括利用該聚醯亞胺前驅物組合物所形成的防飛散層(shatterproof layer)的光學多層結構體。
聚醯亞胺膜係用於顯示裝置的基板和覆蓋窗等的材料,且作為可替代強化玻璃的下一代材料備受關注。為了將膜應用於顯示裝置,必須改善固有的黃色指數特性並賦予無色透明的性能,而且為了可以應用於可折疊顯示裝置或可撓性顯示裝置,需要提高機械物理性能,因此對用於顯示裝置的聚醯亞胺膜的性能要求正在逐漸提升。
特別地,重要的是將根據使用者需要可彎曲或折疊的可撓性顯示裝置設計成可撓性結構,以在外部衝擊或者彎曲或折疊的過程中不易破碎。
一個實施態樣提供一種聚醯亞胺前驅物組合物,所述聚醯亞胺前驅物組合物可以形成可緩和熱膨脹-收縮行為的聚醯亞胺膜。
另一個實施態樣提供一種聚醯亞胺膜,所述聚醯亞胺膜由所述聚醯亞胺前驅物組合物所製備。
另一個實施態樣提供一種光學多層結構體,於所述光學多層結構體中,係在基板上形成有聚醯亞胺防飛散層,從而顯著改善翹曲(curl)現象,並且顯著提高表面硬度。
另一個實施態樣提供一種製備所述光學多層結構體的方法。
另一個實施態樣提供一種包括所述光學多層結構體的窗覆蓋膜(window cover film),以及包括所述窗覆蓋膜的可撓性顯示面板。
在一個一般的方案中,提供一種聚醯亞胺前驅物組合物,所述聚醯亞胺前驅物組合物包含:聚醯亞胺前驅物,其包含衍生自包含以下化學式1的結構的酸酐或二胺的單元;以及無機顆粒,
[化學式1]
在化學式1中,
R
1和R
2各自獨立地為未經取代或經一或多個鹵素取代的C
1-5烷基;
R
3和R
4各自獨立地為未經取代或經一或多個鹵素取代的C
6-10芳基;
L
1和L
2各自獨立地為C
1-10伸烷基;以及
x和y各自獨立地為1或更大的整數。
在另一個一般方案中,提供一種聚醯亞胺膜,所述聚醯亞胺膜由本實施方案的聚醯亞胺前驅物組合物形成。
在另一個一般方案中,提供一種光學多層結構體,所述光學多層結構體包括:基板;防飛散層,其係形成在所述基板上,並且包括由本實施方案的聚醯亞胺前驅物組合物所形成的聚醯亞胺膜;以及硬塗層,其係形成在所述防飛散層上。
在另一個一般方案中,提供一種製備光學多層結構體的方法,所述方法包括以下步驟:將本實施方案的聚醯亞胺前驅物組合物塗布在基板上並進行乾燥以形成防飛散層;以及將用於形成硬塗層的組合物塗布在所述防飛散層上並進行固化以形成硬塗層。
在另一個一般方案中,提供一種窗覆蓋膜,所述窗覆蓋膜包括本實施方案的光學多層結構體。
在另一個一般方案中,提供一種可撓性顯示面板,所述可撓性顯示面板包括本實施方案的窗覆蓋膜。
本發明涉及一種聚醯亞胺前驅物組合物和光學多層結構體,所述聚醯亞胺前驅物組合物包含含有矽氧烷結構的聚醯亞胺前驅物以及無機顆粒,所述光學多層結構體包括形成在基板上的聚醯亞胺防飛散層結構,其係利用所述聚醯亞胺前驅物組合物所形成。根據一個實施態樣的所述光學多層結構體的翹曲現象減少,從而使基板的彎曲最小化的同時顯著提高表面的硬度,因此具有優異的機械特性。
本說明書中記載的實施態樣可以變形為各種其它形式,根據一個實施態樣的技術並不限定於以下說明的實施態樣。而且,在說明書全文中,除非另有特別相反的記載,否則「包含」或「包括」某構成要素是指還可以包含其它構成要素,而不是排除其它構成要素。
本說明書中使用的數值範圍包括下限值和上限值以及該範圍內的所有值、從定義的範圍的形式和跨度以邏輯推導出的增量、其中限定的所有值、以及以彼此不同形式限定的數值範圍之上限和下限的所有可能的組合。作為一個實例,當組成的含量限定在10至80%或20至50%時,應解釋為10至50%或50至80%的數值範圍也記載於本說明書中。除非本說明書中另有特別定義,否則由於實驗誤差或值的四捨五入而可能產生的數值範圍之外的值也包括在定義的數值範圍內。
以下,除非本說明書中另有特別定義,否則「約」可視為明確示出的值的30%、25%、20%、15%、10%或5%以內的值。
以下,除非本說明書中另有特別定義,否則「其組合」可以表示組成物的混合或共聚。
以下,除非本說明書中另有特別定義,否則「A及/或B」可以表示同時包含A和B的情況,也可以表示選擇A和B中的一種的情況。
以下,除非本說明書中另有特別定義,否則「聚合物」可以包括寡聚物(oligomer)和聚合物(polymer),並且可以包括均聚物和共聚物。所述共聚物可以是隨機共聚物(random copolymer)、嵌段共聚物(block copolymer)、接枝共聚物(graft copolymer)、交替共聚物(alternating copolymer)或梯度共聚物(gradient copolymer)或者包括它們全部。
以下,除非本說明書中另有特別定義,否則「聚醯胺酸」可以表示包含具有醯胺酸(amic acid)部分的結構單元的聚合物,「聚醯亞胺」可以表示包含具有醯亞胺部分的結構單元的聚合物。
以下,除非本說明書中另有特別定義,否則聚醯亞胺膜可以是包含聚醯亞胺的膜,具體而言,可以是藉由在二胺化合物溶液中將酸酐化合物進行溶液聚合以製備聚醯胺酸,然後進行醯亞胺化而獲得的高耐熱性膜。
以下,除非本說明書中另有特別定義,否則當描述層、膜、薄膜、區域、基板等部分在另一部分「上」或「上面」時,這不僅包括「直接」在另一部分「上」的情況,而且還包括在其中間存在其它元件的情況。
以下,除非本說明書中另有特別定義,否則「經取代的」是指化合物中的氫原子被取代基取代,例如,所述取代基可以選自氘、鹵素原子(F、Br、Cl或I)、羥基、硝基、氰基、胺基、疊氮基(azido group)、甲脒基(amidino group)、肼基、亞肼基(hydrazono group)、羰基、胺甲醯基、硫醇基、酯基、羧基或其鹽、磺酸基或其鹽、磷酸或其鹽、C
1-30烷基、C
2-30烯基、C
2-30炔基、C
6-30芳基、C
7-30芳基烷基、C
1-30烷氧基、C
1-20雜烷基、C
3-20雜芳基烷基、C
3-30環烷基、C
3-15環烯基、C
6-15環炔基、C
2-30雜環基及其組合。
超薄強化玻璃(ultrathin tempered glass,UTG)(超薄玻璃(ultrathin glass))是用於顯示器覆蓋窗的強化玻璃材料部件,已知為了UTG上的防飛散塗層而塗布聚醯亞胺膜的方法,但由於UTG和聚醯亞胺膜之間的熱膨脹係數(Thermal expansion coefficient)的差異,無法解決在乾燥步驟中膜發生翹曲的問題。另外,在現有的用於改善翹曲現象的材料中,藉由引入可撓性結構等來改善部分翹曲現象,但由於可撓的特性,存在表面的硬度顯著降低的問題。因此,一個實施方案提供一種聚醯亞胺前驅物及包含所述聚醯亞胺前驅物的組合物,其中,藉由在聚醯亞胺前驅物分子內引入應力鬆弛鏈段(Stress relaxation segment),在塗布在UTG上時可以使翹曲現象最小化的同時使表面硬度的降低最小化。
一個實施方案提供一種聚醯亞胺前驅物組合物,所述聚醯亞胺前驅物組合物係包含:聚醯亞胺前驅物以及無機顆粒,該聚醯亞胺前驅物係包含衍生自包含以下化學式1的結構的酸酐或二胺的單元:
[化學式1]
在化學式1中,
R
1和R
2可以各自獨立地為未經取代或經一或多個鹵素取代的C
1-5烷基;
R
3和R
4可以各自獨立地為未經取代或經一或多個鹵素取代的C
6-10芳基;
L
1和L
2可以各自獨立地為C
1-10伸烷基;以及
x和y可以各自獨立地為1或更大的整數。
在一個實施態樣中,所述R
1和R
2可以各自獨立地為未經取代或經一或多個鹵素取代的C
1-3烷基、未經取代或經一或多個鹵素取代的C
1-2烷基、或者未經取代或經一或多個鹵素取代的甲基。此外,所述R
3和R
4可以各自獨立地為未經取代或經一或多個鹵素取代的C
4-8芳基、未經取代或經一或多個鹵素取代的C
6-8芳基、或者未經取代或經一或多個鹵素取代的苯基。此外,所述L
1和L
2可以各自獨立地為C
1-5伸烷基、C
2-5伸烷基、或伸丙基。所述經一或多個鹵素取代的烷基或芳基可以是經一或多個選自I、Br、Cl及/或F的鹵素取代。
在一個實施態樣中,所述x和y可以各自獨立地為1至50、1至30或1至20,但並不必須限定於此。此外,例如,將x和y之和設為100時,x可以為1至99,y可以為99至1,或者x可以為10至90,y可以為90至10。
在一個實施態樣中,包含化學式1的結構的酸酐及/或二胺可以是包含以下化學式3的二甲基矽氧烷-二苯基矽氧烷(dimethylsiloxane-diphenylsiloxane,DMS-DPS)結構的酸酐及/或二胺:
[化學式3]
。
在一個實施態樣中,所述聚醯亞胺前驅物可以包含衍生自包含由化學式1表示的結構的二胺的單元,並且包含化學式1的結構的二胺的一個實例是具有以下結構的信越化學(Shin-etsu)公司的X-22-1660B-3:
。
其中,a和b可以各自獨立地為1或更大的整數,或者可以為1至50、1至30或1至20,但並不必須限定於此。此外,例如,將a和b之和設為100時,a可以為1至99,b可以為99至1,或者a可以為10至90,b可以為90至10。
根據一個實施態樣的聚醯亞胺前驅物組合物包含衍生自包含化學式1的結構的酸酐及/或二胺的單元,因此將其塗布在超薄強化玻璃上時,可以使不同層之間的熱特性差異導致的翹曲現象最小化。
在一個實施態樣中,所述聚醯亞胺前驅物組合物可以包含分配係數(distribution coefficient)為負數的溶劑及/或分配係數為正數的溶劑。作為分配係數為負數的溶劑的實例,可以列舉丙二醇甲醚(glycol methyl ether,PGME)、二甲基甲醯胺(dimethyl formamide,DMF)、二甲基乙醯胺(dimethyl acetamide,DMAc)、N,N-二甲基丙醯胺(N,N-dimethylpropanamide,DMPA)、N-乙基吡咯烷酮(N-ethylprrolidone,NEP)、或甲基吡咯烷酮(methylpyrrolidone,NMP)。此外,作為分配係數為正數的溶劑的實例,可以列舉環己酮(cyclohexanone,CHN)、N,N-二乙基丙醯胺(N,N-diethylpropaneamide,DEPA)、N,N-二乙基乙醯胺(N,N-diethylacetamide,DEAc)、或N,N-二乙基甲醯胺(N,N-diethylformamide,DEF)。
雖然不受特定理論的約束,但在一個實施態樣中,所述聚醯亞胺前驅物組合物中使用包含分配係數為負數的溶劑和分配係數為正數的溶劑的混合溶劑,從而可以有效地改善翹曲現象。或者,在一個實施態樣中,藉由同時使用分配係數為負數的溶劑和分配係數為正數的溶劑,顯著提高組合物(溶液)的均勻性,從而可以改善白濁現象(cloudiness)和相分離現象,因此可以製備無色透明的聚醯亞胺膜。此外,藉由同時使用所述分配係數為負數的溶劑和分配係數為正數的溶劑,而將聚醯亞胺膜塗布在基板上時,可以使不同層之間的熱特性差異導致的翹曲現象最小化。然而,根據聚醯亞胺前驅物的單體,可以使用不同的溶劑,因此並不必須限定於特定的溶劑或溶劑的組合。
在一個實施態樣中,當聚醯亞胺前驅物組合物中包含的溶劑是分配係數為負數的溶劑和分配係數為正數的溶劑的混合溶劑時,所述分配係數為負數的溶劑和分配係數為正數的溶劑的質量比可以為5:5至9.5:0.5。或者,所述質量比可以為5:5至9:1、6:4至9:1、6.5:3.5至9:1、7:3至9:1或7.5:2.5至8.5:1.5,但並不必須限定於此。
在一個實施態樣中,所述聚醯亞胺前驅物組合物中所包含的溶劑的分子內可以包含至少一個羥基(-OH),具體可以包含一個以上、二個以上、三個以上、或一個至三個羥基(-OH)。或者,所述溶劑可以是包含醚基(-O-)和氧代基(oxo group)(=O)中的任一種以上的溶劑。
在一個實施態樣中,相對於聚醯亞胺前驅物的總重量,衍生自包含化學式1的結構的酸酐及/或二胺的單元的含量可以為20重量%以上、25重量%以上、30重量%以上、40重量%以上、20至70重量%、20至60重量%、25至60重量%、30至55重量%或20至50重量%,但並不必須限定於此。
在一個實施態樣中,相對於聚醯亞胺前驅物中所包含的衍生自二胺的單元的總重量,衍生自包含化學式1的結構的酸酐及/或二胺的單元的含量可以為30重量%以上。或者,含量例如可以為40重量%以上、50重量%以上、60重量%以上、40至90重量%、40至80重量%或40至60重量%,但並不必須限定於此。
在一個實施態樣中,相對於聚醯亞胺前驅物中所包含的單體中的二胺的總莫耳數,衍生自包含化學式1的結構的酸酐及/或二胺的單元的含量可以為50至99莫耳%、60至99莫耳%、70至99莫耳%、75至99莫耳%、70至95莫耳%、80至95莫耳%、90至95莫耳%、或約93莫耳%,但並不必須限定於此。
在一個實施態樣中,包含化學式1的結構的酸酐及/或二胺的分子量可以為3000公克/莫耳以上、3500公克/莫耳以上、4000公克/莫耳以上、3000至5500公克/莫耳、3500至5000公克/莫耳或4000至5500公克/莫耳,但並不必須限定於此。
在一個實施態樣中,所述聚醯亞胺前驅物可以進一步包含衍生自由以下化學式2表示的二胺的單元:
[化學式2]
在化學式2中,
R
11和R
21各自獨立地為氫或C
1-20一價有機基團;
L
11是-SO
2-、-O-或-C(=O)O-,或者是包含前述鍵的任一或多者的C
1-20二價有機基團;以及
化學式2不包含氟原子鍵。
在一個實施態樣中,R
11和R
21可以各自獨立地選自C
1-15一價有機基團、C
1-10一價有機基團、C
1-8一價有機基團、C
1-5一價有機基團、或C
1-3一價有機基團,例如,所述有機基團可以選自烷基、烯基、炔基、環烷基、雜環烷基、芳基、雜芳基、氧代基(=O)、酯、醯胺、或其組合,但並不必須限於此。
在一個實施態樣中,L
11可以是包含-SO
2-、-O-和-C(=O)O-中的任一種以上的C
1-18二價有機基團、C
1-15二價有機基團、C
1-10二價有機基團、或C
1-6二價有機基團,或者是-SO
2-、-O-和-C(=O)O-中的任一種以上與選自C
1-10伸烷基、C
5-18伸環烷基及C
6-18伸芳基中的任一種以上的組合,但並不必須限於此。此外,L
11例如可以為-SO
2-、-O-、-C(=O)O-、
、
、
、
、
或
。此外,L
11可以被羥基、硫醇基、硝基、氰基、C
1-10烷基、C
6-20芳基或C
5-20環烷基取代。但是,L
11不包含氟原子鍵。
在一個實施態樣中,由化學式2的結構表示的二胺例如可以為1,3-雙(4-胺基苯氧基)苯(1,3-bis(4-aminophenoxy)benzene,TPER)、4,4'-二胺基二苯醚(4,4'-oxydianiline,ODA)、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷(2,2-bis[4-(4-aminophenoxy)phenyl]propane,BAPP)、4,4'-二胺基二苯碸(4,4'-diaminodiphenyl sulfone,4,4'-DDS)、3,3'-二胺基二苯碸(3,3'-diaminodiphenyl sulfone,3,3'-DDS)、1,3-雙(3-胺基苯氧基)苯(1,3-bis(3-aminophenoxy)benzene,133APB)、或1,4-雙(4-胺基苯氧基)苯(1,4-bis(4-aminophenoxy)benzene,144APB)。在一個實施態樣中,所述聚醯亞胺前驅物包含一個以上或二個以上的由化學式2的結構表示的二胺,但不限於此。
根據一個實施態樣的聚醯亞胺前驅物包含衍生自包含化學式1的結構的酸酐及/或二胺的單元,同時進一步包含衍生自不含氟原子的化學式2表示的二胺的單元,由此製備的聚醯亞胺膜可以是無色透明,同時在玻璃基板之間產生的殘餘應力低,並且可以具有高黏合性和機械物理性能,而且可以保持約100至180℃的適當的玻璃轉化溫度。
在一個實施態樣中,所述聚醯亞胺前驅物可以進一步包含衍生自氟系二胺的單元。所述氟系二胺是指包含氟原子的二胺。作為所述氟系二胺的實例,可以列舉2,2'-雙(三氟甲基)聯苯胺(2,2'-bis(trifluoromethyl)benzidine,TFMB)、2,2-雙[4-(4-胺基苯氧基)苯基]六氟丙烷(2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane,HFBAPP)、2,2-雙(4-胺基苯基)六氟丙烷(2,2-bis(4-aminophenyl)hexafluoropropane,BAHF)、2,2'-雙(三氟甲基)-4,4'-二胺基二苯醚(2,2'-bis(trifluoromethyl)-4,4'-diaminodiphenylether)、4,4'-雙(4-胺基-2-三氟甲基苯氧基)聯苯(4,4'-bis(4-amino-2-trifluoromethylphenoxy)biphenyl)、或1,4-雙(4-胺基-2-三氟甲基苯氧基)苯(1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene)等。
此外,所述聚醯亞胺前驅物還可以進一步包含衍生自本發明技術領域中所一般使用的二胺的單元。例如,所述衍生自二胺的單元可以包含衍生自芳香族二胺的單元,所述芳香族二胺可以是包含至少一個芳環的二胺,所述芳環可以是單環,或者二個以上的芳環稠合的稠環,或者二個以上的芳環藉由單鍵、經取代或未經取代的C
1-5伸烷基、O或C(=O)所連接的非稠環。例如,可以進一步包含衍生自2,2-雙(3-胺基-4-羥基苯基)-六氟丙烷(2,2-bis(3-amino-4-hydroxyphenyl)-hexafluoropropane,6FAP)、對苯二胺(p-phenylenediamine,pPDA)、間苯二胺(m-phenylenediamine,mPDA)、對亞甲基二苯胺(p-methylenedianiline,pMDA)、或間亞甲基二苯胺(m-methylenedianiline,mMDA)的單元。
在一個實施態樣中,所述聚醯亞胺前驅物組合物可以包含衍生自一般在本領域中所使用的酸酐的單元。例如,所述酸酐可以包括包含芳環的酸酐、包含脂環的酸酐、四羧酸二酐或其組合。在一個實施態樣中,所述酸酐可以為選自以下群組的一或多個酸酐:乙二醇雙(4-偏苯三酸酐)(ethylene glycol bis(4-trimellitate anhydride),TMEG-100)、4,4'-氧二鄰苯二甲酐(4,4'-oxydiphthalic anhydride,ODPA)、2,2-雙[4-(2,3-二羧基苯氧基)苯基]丙烷二酐(2,2-bis[4-(2,3-dicarboxyphenoxy)phenyl]propane dianhydride)、4,4'-(3,4-二羧基苯氧基)二苯硫醚二酐(4,4'-(3,4-dicarboxyphenoxy)diphenylsulfide dianhydride)、焦蜜石酸二酐(pyromellitic dianhydride,PMDA)、3,3',4,4'-聯苯四羧酸二酐(3,3',4,4'-biphenyltetracarboxylic dianhydride,BPDA)、1,2,3,4-環丁烷四羧酸二酐(1,2,3,4-cyclobutanetetracarboxylic dianhydride,CBDA)、3,3',4,4'-二苯甲酮四羧酸二酐(3,3',4,4'-benzophenonetetracarboxylic dianhydride,BTDA)、4,4'-(4,4'-亞異丙基二苯氧基)雙(鄰苯二甲酐)(4,4'-(4,4'-isopropylidenediphenoxy) bis(phthalic anhydride),BPADA)、3,3',4,4'-二苯基碸四羧酸二酐(3,3',4,4'-diphenylsulfone tetracarboxylic dianhydride,DSDA)、2,2-雙(3,4-二羧基苯基)六氟丙烷二酐(2,2-bis-(3,4-dicarboxylphenyl) hexafluoropropane dianhydride,6FDA)、對伸苯基雙(偏苯三酸酐)(p-phenylenebis(trimellitate anhydride),TMHQ)、2,2-雙(4-羥基苯基)丙烷二苯甲酸酯-3,3',4,4'-四羧酸二酐(2,2-bis(4-hydroxyphenyl) propanedibenzoate-3,3',4,4'-tetracarboxylicdianhydride,ESDA)、萘四羧酸二酐(naphthalenetetracarboxylic dianhydride,NTDA)及其衍生物。
例如,所述酸酐可以為由以下化學式4或化學式5表示的化合物:
[化學式4]
在化學式4中,X
1可以各自獨立地為C
3-10脂環或C
4-10芳環,Y
1可以是包含單鍵、經取代或未經取代的C
1-20脂肪族鏈、經取代或未經取代的C
3-10脂環及/或者經取代或未經取代的C
4-10芳環的連接基團(linker)。具體地,Y
1可以包含C
1-20伸烷基、C
1-10伸烷基、C
1-5伸烷基、C
3-10伸環烷基、C
4-10伸芳基、藉由C
1-20伸烷基連接的二個以上的C
3-10伸環烷基、或藉由C
1-20伸烷基連接的二個以上的C
4-10伸芳基。
[化學式5]
在化學式5中,X
2可以各自獨立地為C
3-10脂環或C
4-10芳環,Y
2可以是包含單鍵、經取代或未經取代的C
1-20脂肪族鏈、經取代或未經取代的C
3-10脂環及/或者經取代或未經取代的C
4-10芳環的連接基團。具體地,Y
2可以包含C
1-20伸烷基、C
1-10伸烷基、C
1-5伸烷基、C
3-10伸環烷基、C
4-10伸芳基、藉由C
1-20伸烷基連接的二個以上的C
3-10伸環烷基、或藉由C
1-20伸烷基連接的二個以上的C
4-10伸芳基。
具體地,所述酸酐可以為由以下化學式表示的化合物群組中的任一種以上:
、
、
、
。
在一個實施態樣中,以聚醯亞胺前驅物的單體的總莫耳數為基準,所述酸酐的含量可以為約30至70莫耳%、40至60莫耳%、45至55莫耳%、或約50莫耳%。或者,相對於聚醯亞胺前驅物的總重量,所述酸酐的含量可以為20至70重量%、20至60重量%、30至60重量%、20至50重量%、30至50重量%、或約40重量%,但並不必須限定於此。
根據一個實施態樣的無機顆粒可以為無機奈米顆粒,平均直徑例如可以為5至50奈米,或者例如可以為5至30奈米或5至20奈米,但並不必須限定於此。
所述平均直徑例如可以藉由用光學顯微鏡觀察顆粒來測量,或者可以利用掃描式電子顯微鏡(scanning electron microscope,SEM)、穿透式電子顯微鏡(transmission electron microscope,TEM)、掃描探針顯微鏡(scanning probe microscope,SPM)、掃描穿隧式顯微鏡(scanning tunneling microscope,STM)、原子力顯微鏡(atomic force microscope,AFM)進行測量,或者可以利用粒徑分析儀進行測量。例如,可以利用雷射粒徑分析儀對包含無機顆粒的組合物照射雷射,並從繞射和顆粒尺寸的相關關係推導得到顆粒的尺寸。例如,可以為D50、D10或D90值。或者,例如可以為面積(area)平均(Ma)值、數平均(Mn)值或體積平均(Mv)值。
在一個實施態樣中,所述無機顆粒例如可以包含二氧化矽、氧化鋯、氧化鈦、氧化鋅、硫化鋅、氧化鉻、鈦酸鋇或其組合。所述無機奈米顆粒可以以分散在有機溶劑中的形式與所述聚醯亞胺樹脂混合,並且可以是為了提高分散性而進行了表面處理的物質。例如,根據一個實施態樣的無機顆粒的表面可以被C
1-5烷氧基取代,具體地,例如可以被甲氧基或乙氧基取代。另外,所述表面處理可以不受限制地使用習知的表面處理方法來進行,因此不受特別限定。
在一個實施態樣中,所述無機顆粒可以化學鍵結到由化學式1表示的化合物的取代基。此外,根據一個實施態樣的聚醯亞胺前驅物組合物包含上述無機顆粒,因此可以顯著且優異地改善傳統的防飛散層的表面硬度降低的現象。因此,由於根據一個實施態樣的聚醯亞胺前驅物組合物所形成的防飛散層包含由化學式1表示的單元,從而提高可撓性而緩和熱膨脹-收縮行為,因此可以使基板的彎曲現象最小化,並且同時包含無機顆粒,從而可以顯著改善表面硬度。
在一個實施態樣中,相對於聚醯亞胺前驅物組合物的總重量,所述無機顆粒的含量可以為1至30重量%、2至25重量%、5至20重量%、或1至25重量%,但並不必須限定於上述範圍。
在一個實施態樣中,以聚醯亞胺前驅物組合物的總重量為基準,聚醯亞胺前驅物組合物的固形物含量可以為40重量%以下、10至40重量%、35重量%以下、30重量%以下、或20至40重量%。其中,固形物可以為聚醯胺酸及/或聚醯亞胺。
在一個實施態樣中,所述聚醯亞胺前驅物及/或聚醯亞胺的分子量可以為500至200,000公克/莫耳或10,000至100,000公克/莫耳,但並不必須限定於此。
在一個實施態樣中,所述聚醯亞胺前驅物組合物可以進一步包含藍色系顏料和染料中的任一種以上。
所述藍色系顏料或染料的最大吸收波長只要是包括黃色系波長範圍的範圍,則不受特別限制,但波長範圍例如可以為520至680奈米、520至650奈米、550至650奈米或550至620奈米。藉由使用具有上述範圍的最大吸收波長的顏料或染料,可以有效地抵消由根據一個實施態樣的聚醯亞胺前驅物組合物所製備的聚醯亞胺膜的藍色或紫色波長的光吸收現象,並且可以更有效地改善黃色指數。而且,根據在聚醯亞胺前驅物組合物的製備中所使用的單體的種類和組成,或者根據聚醯亞胺膜的光學物理性能,適當地選擇無機顏料的最大吸收波長範圍,從而可以使膜的黃色指數、折射率、厚度方向的相位差等光學物理性能更優異。
所述顏料可以不受特別限制地使用藍色系顏料或具有520至680奈米的最大吸收波長的習知的顏料,例如可以是包含天然礦物或者選自以下之一或多個金屬的無機顏料:鋅、鈦、鉛、鐵、銅、鉻、鈷、鉬、錳及鋁中、或其金屬氧化物。所述顏料可以與分散劑一起包含在顏料分散液中而使用。
所述無機顏料的平均粒徑可以為30至100奈米。或者,所述平均粒徑並不必須限於此,但例如可以為50至100奈米或70至100奈米。所述無機顏料的平均粒徑例如可以在分散液中測量或者在聚醯亞胺膜中測量。此外,例如,所述顏料在分散之前的固體相的平均粒徑例如可以為10至70奈米,例如可以為30至70奈米,或者可以為50至70奈米。
對於所述顏料,為了提高分散性,可以使用超聲波等方法,並且也可以使用分散劑。所述分散劑只要可以防止顏料之間的聚集並可以提高顏料的分散性和分散穩定性,則不受特別限制,但例如可以為具有官能基團的分散劑,該官能基團對吸附在顏料的官能基團和對分散介質(所述有機溶劑)具有高親和性,並且可以藉由調節所述二種官能基團的平衡來確定分散劑。根據作為待分散對象的顏料表面狀態,可以使用各種種類的所述分散劑。例如,根據一個實施態樣的顏料分散劑可以具有酸性官能基團,在這種情況下,酸性官能基團可以吸附在顏料上。所述酸性官能基團例如可以為羧酸(carboxylic acid)。
所述染料可以不受特別限制地使用藍色系染料或具有520至680奈米的最大吸收波長的習知的染料,例如可以列舉酸性染料、直接染料、媒染染料等。或者,可以列舉在色彩索引(英國染色家學會(The society of Dyers and Colourists)出版)中分類為具有除顏料以外的顏色的化合物,或者染色指南(染色紗)中記載的習知的染料。或者,作為化學結構,可以列舉偶氮系染料、花青系染料(cyanine-based dye)、三苯甲烷系染料、酞青系染料(phthalocyanine-based dye)、蒽醌系染料、萘醌系染料、醌亞胺系染料、次甲基系染料(methine-based dye)、次甲基偶氮系染料、方酸菁系染料(squarylium-based dye)、吖啶系染料、苯乙烯系染料、香豆素系染料、喹啉系染料、硝基系染料及靛藍系染料等。
在一個實施態樣中,以聚醯亞胺前驅物組合物中所包含的聚醯胺酸及/或聚醯亞胺的固形物為基準,所述顏料的含量可以為10至1500 ppm,或者例如可以為100至1500 ppm或500至1500 ppm。其中,所述聚醯胺酸及/或聚醯亞胺固形物可以是指聚醯胺酸及/或聚醯亞胺。
在一個實施態樣中,以聚醯亞胺前驅物組合物中所包含的聚醯胺酸及/或聚醯亞胺的固形物為基準,所述染料的含量可以為10至500 ppm,或者例如可以為10至300 ppm、10至200 ppm、50至200 ppm、或80至200 ppm。其中,所述聚醯胺酸及/或聚醯亞胺固形物可以是指聚醯胺酸及/或聚醯亞胺。
在一個實施態樣中,所述聚醯亞胺前驅物組合物可以進一步包含本發明技術領域中所一般使用的添加劑,例如可以進一步包含阻燃劑、增黏劑、抗氧化劑、抗紫外線劑或增塑劑。
一個實施方案提供一種由上述聚醯亞胺前驅物組合物形成的聚醯亞胺膜。
此外,一個實施方案提供一種光學多層結構體,所述光學多層結構體包括:基板;防飛散層,其形成在所述基板上,並且包括由聚醯亞胺前驅物組合物形成的聚醯亞胺膜,所述聚醯亞胺前驅物組合物包含聚醯亞胺前驅物和無機顆粒,所述聚醯亞胺前驅物包含衍生自包含以下化學式1的結構的酸酐及/或二胺的單元;以及硬塗層,其形成在所述防飛散層上:
[化學式1]
其中,包含聚醯亞胺前驅物(包含衍生自包含化學式1的結構的酸酐及/或二胺的單元)和無機顆粒的聚醯亞胺前驅物組合物可以參照與前述實施態樣的聚醯亞胺前驅物組合物相關的內容。
在一個實施態樣中,顯示器的顯示元件可以位於基板的任一面或光學多層結構體的最下層。
在一個實施態樣中,所述基板可以為超薄強化玻璃(UTG)基板。或者,基板可以由以下樹脂製備:聚酯系樹脂,例如聚對苯二甲酸乙二酯、聚鄰苯二甲酸乙二酯、聚對苯二甲酸丁二酯等;纖維素系樹脂,例如二乙醯纖維素(diacetyl cellulose)、三乙醯纖維素等;聚碳酸酯系樹脂;丙烯酸系樹脂,例如聚(甲基)丙烯酸甲酯、聚(甲基)丙烯酸乙酯等;苯乙烯系樹脂,例如聚苯乙烯丙烯腈-苯乙烯共聚物等;聚烯烴系樹脂,例如具有聚乙烯、聚丙烯、環系或降冰片烯(norbornene)結構的聚烯烴基樹脂、乙烯丙烯共聚物等;聚醯亞胺系樹脂;聚醯胺系樹脂;聚醚碸系樹脂;碸系樹脂等,該等樹脂可以單獨使用或混合使用二種以上。
在一個實施態樣中,所述基板的厚度不受特別限制,但例如可以為1至50微米、5至50微米、10至50微米、10至40微米、20至50微米、20至40微米、或25至35微米。
在一個實施態樣中,所述防飛散層可以形成在基板的一面上。根據一個實施態樣的光學多層結構體包含由所述聚醯亞胺前驅物組合物形成的聚醯亞胺,從而可以增強耐飛散特性,同時藉由與硬塗層和基板的相互作用,可以使基板的彎曲現象和表面硬度降低的現象最小化。
在一個實施態樣中,所述防飛散層可以形成在基板的正面上或形成為與基板的正面接觸的形式。此外,本說明書中使用的術語「正面」可以是指在多層結構體的層疊結構中更靠近使用者的方向的面。相反,「後面」可以是指在多層結構體的層疊結構中遠離使用者的方向的面。在根據一個實施態樣的層疊結構中,顯示器的顯示元件可以位於最後面。
在一個實施態樣中,所述防飛散層的厚度不受特別限制,但例如可以為1至100微米、1至80微米、1至50微米、1至30微米、5至20微米或5至15微米,但並不必須限定於此。
在一個實施態樣中,所述硬塗層可以形成在防飛散層的一面上,因此可以保護多層結構體免受外部的物理損傷和化學損傷。
在一個實施態樣中,所述硬塗層可以藉由將用於形成硬塗層的組合物進行固化來形成,例如可以是將用於形成硬塗層的組合物進行光固化後再進行熱固化的複合硬塗層。
在一個實施態樣中,所述硬塗層可以藉由包含具有環氧基的烷氧基矽烷(alkoxysilane)的縮合物而形成,例如,所述具有環氧基的烷氧基矽烷的縮合物可以是包含環氧基的矽氧烷(siloxane)系樹脂,但並不必須限定於此。當所述具有環氧基的烷氧基矽烷的縮合物固化時,可以具有優異的硬度和彎曲特性。
所述環氧基可以是選自環狀環氧基、脂肪族環氧基和芳香族環氧基中的任一種以上,所述矽氧烷樹脂可以是指矽原子和氧原子形成共價鍵的聚合物化合物。
在一個實施態樣中,所述具有環氧基的烷氧基矽烷的縮合物可以是具有環氧基的倍半矽氧烷(silsesquioxane)樹脂,具體地,倍半矽氧烷樹脂的矽原子可以直接被環氧基取代,或者取代所述矽原子的取代基可以被環氧基取代,更具體地,所述具有環氧基的烷氧基矽烷的縮合物可以是被2-(3,4-環氧環己基)乙基取代的倍半矽氧烷樹脂,但並不必須限定於此。
在一個實施態樣中,所述具有環氧基的烷氧基矽烷的縮合物的重量平均分子量可以為1000至20,000公克/莫耳、1000至18,000公克/莫耳、或2000至15,000公克/莫耳。當重量平均分子量在上述範圍時,可以進一步提高所述用於形成硬塗層的組合物的流動性、塗布性、固化反應性等。
在一個實施態樣中,所述具有環氧基的矽氧烷系化合物可以包含衍生自以下化學式6所表示的烷氧基矽烷化合物的重複單元:
[化學式6]
R
61 nSi(OR
62)
4-n在化學式6中,R
61可以是經碳原子數為3至6的環氧環烷基或環氧乙烷基(oxiranyl group)所取代的直鏈或支鏈的碳原子數為1至6的烷基,所述烷基可以包含醚基,R
62可以是直鏈或支鏈的碳原子數為1至7的烷基,n可以為1至3的整數。
由化學式6表示的烷氧基矽烷化合物可以列舉例如2-(3,4-環氧環己基)乙基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三乙氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷(3-glycidoxypropyltrimethoxysilane)等,且可以單獨使用或混合使用二種以上,但並不必須限定於此。
在一個實施態樣中,相對於用於形成硬塗層的組合物的總重量,所述具有環氧基的烷氧基矽烷的縮合物的含量可以為20至70重量%或20至50重量%,但並不必須限定於此。
在一個實施態樣中,用於形成硬塗層的組合物可以具有優異的流動性和塗布性,並且在用於形成硬塗層的組合物的固化時可以實現均勻的固化,因此可以有效地防止過度固化導致的裂紋等物理缺陷,並且可以表現出優異的硬度。
在一個實施態樣中,所述硬塗層的厚度可以為1至100微米、1至80微米、1至50微米、1至30微米、1至20微米、或3至15微米,但並不必須限定於此。
在一個實施態樣中,所述光學多層結構體可以進一步包括黏附增強層、防靜電層、耐指紋層、防刮擦層(anti-scratch layer)、低折射層、低反射層、疏水層、防反射層及/或衝擊吸收層(shock absorption layer)等。
在根據一個實施態樣的光學多層結構體中,藉由在基板上層疊單層的從根據一個實施態樣的用於形成聚醯亞胺防飛散層的組合物(或聚醯亞胺前驅物組合物)所形成的防飛散層,並且在防飛散層上形成硬塗層,從而可以具有優異的表面硬度。根據一個實施態樣的光學多層結構體的表面硬度可以為0.5H以上。或者,例如可以為1H以上、5H以下、4H以下、3H以下、0.5H至5H、1H至4H、或1H至3H。所述表面硬度可以是光學多層結構體的最外層的表面硬度,或者可以是構成光學多層結構體的防飛散層及/或硬塗層的表面硬度。在一個實施態樣中,所述表面硬度可以藉由利用鉛筆硬度試驗機(pencil hardness tester)並利用秤砣施加750公克的荷重來測量,具體地,可以將鉛筆和試樣的角度設為約45˚,並以20毫米/分鐘的速度測量10毫米。此時,可以對每個試樣測量3次,將其平均值作為表面硬度值。此外,如果試樣的劃痕為2個以上,則判定為不良,表面硬度值可以表示發生不良之前的硬度值。
在基板上層疊單層的從根據一個實施態樣的用於形成聚醯亞胺防飛散層的組合物(或聚醯亞胺前驅物組合物)所形成的防飛散層,並且在防飛散層上形成硬塗層,藉此可以顯著改善基板的彎曲現象。在一個實施態樣中,在藉由利用尺測量所述多層結構體或塗布有防飛散層的基板(例如,超薄玻璃基板)的二端部分距離地面的高度來計算翹曲量的情況(或者分別測量二端的值並計算其平均值的情況)下,該值可以為3.0毫米以下、2.0毫米以下、0.1至5.0毫米、0.1至4.0毫米、0.1至3.0毫米、0.1至2.0毫米、或0.5至1.5毫米,但並不必須限於此。
一個實施方案提供一種製備光學多層結構體的方法。
具體地,所述製備方法包括以下步驟:將包含聚醯亞胺前驅物組合物的用於形成防飛散層的組合物塗布在基板上並進行乾燥以形成防飛散層,所述聚醯亞胺前驅物組合物包含聚醯亞胺前驅物和無機顆粒,所述聚醯亞胺前驅物包含衍生自包含化學式1的結構的酸酐或二胺的單元;以及將用於形成硬塗層的組合物塗布在所述防飛散層上並進行固化以形成硬塗層。
其中,所述聚醯亞胺前驅物組合物可以使用與前述實施態樣的聚醯亞胺前驅物組合物相同的組合物。
在一個實施態樣中,所述防飛散層可以藉由塗布用於形成防飛散層的組合物後進行乾燥來形成,所述乾燥例如可以包括二次乾燥步驟。例如,可以包括如下步驟:在約30至60℃、40至60℃或45至55℃的溫度下進行第一次乾燥約30至120秒、30至90秒或50至80秒,然後在約150至300℃、180至280℃、200至280℃或200至250℃的溫度下進行第二次乾燥約1至30分鐘、1至20分鐘、5至20分鐘或5至15分鐘。
在一個實施態樣中,所述硬塗層可以藉由進一步包含具有多官能環氧基的交聯劑而形成。其中,所述交聯劑可以包含具有脂環式環氧基的化合物,例如,所述交聯劑可以包含鍵結有二個3,4-環氧環己基的化合物,但並不必須限定於此。所述交聯劑可以具有與所述具有環氧基的烷氧基矽烷的縮合物相似的結構和性質,在這種情況下,可以促進所述具有環氧基的烷氧基矽烷的縮合物的交聯。
在一個實施態樣中,所述硬塗層可以藉由進一步包含熱引發劑及/或光引發劑而形成。
在一個實施態樣中,在所述硬塗層中使用熱引發劑的情況下,可以縮短固化半衰期,並且在低溫條件下也可以快速進行熱固化,從而可以防止在高溫條件下長期熱處理時發生的損傷和變形。對用於形成硬塗層的組合物施加熱時,所述熱引發劑可以促進所述環氧矽氧烷樹脂或交聯劑的交聯反應。作為所述熱引發劑,可以使用陽離子型熱引發劑,但並不必須限定於此。
此外,在形成硬塗層時,藉由聯合使用利用所述熱引發劑的熱固化和利用所述光引發劑的光固化,可以提高硬塗層的固化度、硬度、可撓性等。例如,可以將所述用於形成硬塗層的組合物塗布在基板等上,藉由照射紫外線(光固化),使至少一部分固化,然後進一步施加熱(熱固化),從而實質上完全固化。
所述用於形成硬塗層的組合物可以藉由所述光固化而被半固化或部分固化,所述半固化或部分固化的用於形成硬塗層的組合物可以藉由所述熱固化而實質上完全被固化。例如,當僅藉由光固化對所述用於形成硬塗層的組合物進行固化時,固化時間可能會變得過長或者有部分固化可能無法完全進行。然而,當在所述光固化之後進行所述熱固化時,未藉由光固化被固化的部分可以藉由熱固化實質上完全被固化,並且可以減少固化時間。
此外,一般而言,隨著固化時間的增加(例如,曝光時間的增加),向已固化至適當的程度的部分提供過多的能量,從而可能會發生過度固化。當發生所述過度固化時,硬塗層可能失去可撓性或發生翹曲和裂紋等機械缺陷。然而,當聯合使用所述光固化和所述熱固化時,所述用於形成硬塗層的組合物可以在短時間內實質上完全固化,並且可以在保持硬塗層的可撓性的同時進一步提高硬度。
以上,對所述用於形成硬塗層的組合物進行光固化並進一步進行熱固化的方法進行了說明,但光固化和熱固化的順序並不特別受限於此。即,在一些實施態樣中,可以先進行所述熱固化後再進行所述光固化。
在一個實施態樣中,相對於100重量份的所述具有環氧基的烷氧基矽烷的縮合物,所述熱引發劑的含量可以為0.1至20重量份或1至20重量份,但並不必須限定於此。此外,例如,相對於總共100重量份的用於形成硬塗層的組合物,所述熱引發劑的含量可以為0.01至15重量份、0.1至15重量份或0.3至10重量份,但並不必須限定於此。
在一個實施態樣中,所述光引發劑可以包含光陽離子引發劑。所述光陽離子引發劑可以引發所述環氧矽氧烷樹脂和環氧系單體的聚合。作為所述光陽離子引發劑,可以使用碘鎓鹽、鎓鹽及/或有機金屬鹽等,例如可以使用二芳基碘鎓鹽、三芳基鋶鹽、芳基重氮鹽、鐵-芳烴錯合物(iron-arene composite)等,且可以單獨使用或混合使用二種以上,但並不必須限定於此。
所述光引發劑的含量不受特別限定,例如,相對於100重量份的所述具有環氧基的烷氧基矽烷的縮合物,所述光引發劑的含量可以為0.1至15重量份或1至15重量份,但並不必須限定於此。
此外,例如,相對於總共100重量份的用於形成硬塗層的組合物,所述光引發劑的含量可以為0.01至10重量份、0.1至10重量份、或0.3至5重量份,但並不必須限定於此。
在一個實施態樣中,所述用於形成硬塗層的組合物可以進一步包含溶劑。所述溶劑不受特別限定,並且可以使用本領域中習知的溶劑。
作為所述溶劑的非限制性的實例,可以列舉醇系溶劑(甲醇、乙醇、異丙醇、丁醇、甲基賽珞蘇(methyl cellosolve)、乙基賽珞蘇等)、酮系溶劑(甲基乙基酮、甲基丁基酮、甲基異丁基酮、二乙基酮、二丙基酮、環己酮等)、己烷系溶劑(己烷、庚烷、辛烷等)、苯系溶劑(苯、甲苯、二甲苯等)等。該等可以單獨使用或混合使用二種以上。
在一個實施態樣中,所述用於形成硬塗層的組合物可以進一步包含無機填充劑。所述無機填充劑可以進一步提高硬塗層的硬度。
所述無機填充劑不受特別限定,例如,可以使用金屬氧化物,例如二氧化矽、氧化鋁、氧化鈦等;氫氧化物,例如氫氧化鋁、氫氧化鎂、氫氧化鉀等;金屬顆粒,例如金、銀、銅、鎳、其合金等;導電顆粒,例如碳、碳奈米管、富勒烯(fullerene)等;玻璃;陶瓷等,或者考量到與用於形成硬塗層的組合物的其它成分的相容性,可以使用二氧化矽,並且該等可以單獨使用或混合使用二種以上,但並不必須限定於此。
在一個實施態樣中,所述用於形成硬塗層的組合物可以進一步包含潤滑劑。所述潤滑劑可以進一步改善收卷效率(winding efficiency)、抗黏連性(blocking resistance)、耐磨性、耐刮擦性等。
所述潤滑劑的種類不受特別限定,例如,可以使用蠟類,例如聚乙烯蠟、石蠟、合成蠟、或褐煤蠟(montan wax)等;合成樹脂類,例如矽系樹脂、氟系樹脂等等,該等可以單獨使用或者混合使用二種以上,但並不必須限定於此。
此外,所述用於形成硬塗層的組合物可以進一步包含例如抗氧化劑、紫外線(UV)吸收劑、光穩定劑、熱聚合抑制劑、調平劑(leveling agent)、表面活性劑、潤滑劑、防污劑等添加劑。
在一個實施態樣中,所述塗布可以藉由模具塗布機、氣刀、反向輥、噴霧、刮刀、鑄造(casting)、凹版和旋塗等來進行,但並不必須限定於此。
一個實施方案提供一種包括根據一個實施態樣的光學多層結構體的窗覆蓋膜,以及包括所述窗覆蓋膜的可撓性顯示面板或可撓性顯示裝置。
根據一個實施態樣的多層結構體中,不僅使翹曲現象最小化,而且表面硬度高,因此可以有效地應用於窗覆蓋膜及/或可撓性顯示面板。
所述窗覆蓋膜可以用作可撓性顯示裝置的最外面的窗基板。可撓性顯示裝置可以是一般的液晶顯示裝置、電致發光顯示裝置、電漿顯示裝置、場發射顯示裝置等各種圖像顯示裝置。
以下,對實施例和實驗例進行具體例示和說明。但是,下述實施例和實驗例僅用於例示一部分,本說明書中記載的技術並不限定於此。
< 實施例 1> 1-1. 用於形成防飛散層的組合物的製備
在氮氣氣流流動的攪拌器中填充230公克的溶劑,所述溶劑是將丙二醇甲醚(PGME)和環己酮(CHN)以8:2的質量比混合的溶劑。在將反應器的溫度保持在25℃的狀態下,加入29.0公克的2,2'-雙(三氟甲基)聯苯胺(TFMB)和29.6公克的二甲基矽氧烷-二苯基矽氧烷(DMS-DPS)寡聚物二胺化合物(信越化學公司,X-22-1660B-3,分子量為4400公克/莫耳)並進行溶解。向其中添加40.0公克的乙二醇雙(4-偏苯三酸酐)(TMEG-100),在50℃下攪拌溶解8小時並在常溫下攪拌溶解24小時,從而製備聚醯胺酸樹脂。此時,使各單體的莫耳比為(TFMB+X-22-1660B-3):TMEG-100=0.99:1.0。然後,相對於組合物的總重量,添加5重量%的二氧化矽奈米顆粒(直徑:15奈米),其中所述二氧化矽奈米顆粒以30重量%分散在N,N-二甲基丙醯胺(DMPA)中,然後攪拌3小時,從而製備固形物含量為23重量%的用於形成聚醯亞胺-防飛散層的組合物。
1-2. 用於形成硬塗層的組合物的製備
將2-(3,4-環氧環己基)乙基三甲氧基矽烷(2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane,ECTMS,TCI公司)和水以24.64公克:2.70公克(0.1莫耳:0.15莫耳)的比例混合,從而製備混合物,然後加入到250毫升的二口(2-neck)燒瓶中。在所述混合物中加入0.1毫升的四甲基氫氧化銨(tetramethylammoniumhydroxide,TMAH,奧德里奇(Aldrich)公司)催化劑和100毫升的四氫呋喃(tetrahydrofuran,THF,奧德里奇公司),並在25℃下攪拌36小時。之後,進行層分離,並用二氯甲烷(methylene chloride,奧德里奇公司)萃取產物層,用MgSO
4去除萃取物的水分,並將溶劑進行真空乾燥,從而獲得環氧矽氧烷系樹脂。
將30公克的上述製備的環氧矽氧烷系樹脂、10公克的作為交聯劑的(3',4'-環氧環己基)甲基3,4-環氧環己烷羧酸酯((3',4'-epoxycyclohexyl)methyl 3,4-epoxycyclohexanecarboxylate)、5公克的雙[(3,4-環氧環己基)甲基]己二酸酯(bis[(3,4-epoxycyclohexyl)methyl] adipate)、0.5公克的作為光引發劑的(4-甲基苯基)[4-(2-甲基丙基)苯基]碘鎓六氟磷酸鹽((4-methylphenyl)[4-(2-methylpropyl)phenyl]iodoniumhexafluorophosphate)和54.5公克的甲基乙基酮(methyl ethyl ketone)進行混合,從而製備用於形成硬塗層的組合物。
1-3. 光學多層結構體的製備
利用#30邁耶棒(Mayer bar),將上述製備的用於形成防飛散層的組合物塗布在玻璃基板(UTG,30微米)的正面上,並在50℃下乾燥1分鐘,然後在230℃下乾燥10分鐘,從而形成厚度為10微米的聚醯亞胺防飛散層。
接著,利用#10邁耶棒,將上述製備的用於形成硬塗層的組合物塗布在上述形成的防飛散層上,並在60℃下乾燥5分鐘後照射1焦耳/平方公分(J/cm
2)的紫外線,然後在120℃下固化15分鐘,形成厚度為10微米的硬塗層,從而製備UTG光學多層結構體。
< 實施例 2 和實施例 3>
除了在製備用於形成防飛散層的組合物的過程中分別添加組合物的總重量的10重量%和20重量%的二氧化矽奈米顆粒之外,藉由與所述實施例1相同的方法製備UTG光學多層結構體。
< 比較例 1>
除了在製備用於形成防飛散層的組合物的過程中未添加二氧化矽奈米顆粒之外,藉由與所述實施例1相同的方法製備UTG光學多層結構體。
< 實施例 4> 4-1. 用於形成防飛散層的組合物的製備
在氮氣氣流流動的攪拌器中填充188公克的DMPA,然後在將反應器的溫度保持在常溫的狀態下,在相同的溫度下添加0.0058莫耳的DMS-DPS寡聚物二胺化合物(信越化學公司,X-22-1660B-3,分子量為4340公克/莫耳)和0.0502莫耳的1,3-雙(4-胺基苯氧基)苯(TPER)並進行溶解。在相同的溫度下,向其中添加0.0561莫耳的TMEG-100,並在60℃下攪拌4小時後在常溫下攪拌24小時,從而製備聚醯胺酸樹脂。然後,相對於組合物的總重量,添加5重量%的二氧化矽奈米顆粒(直徑:15奈米),其中所述二氧化矽奈米顆粒以30重量%分散在DMPA中,然後攪拌3小時,從而製備固形物含量為23重量%的用於形成聚醯亞胺-防飛散層的組合物。
4-2. 用於形成硬塗層的組合物的製備
將ECTMS和水以24.64公克:2.70公克(0.1莫耳:0.15莫耳)的比例混合,從而製備混合物,然後加入到250毫升的二口燒瓶中。在所述混合物中添加0.1毫升的TMAH催化劑和100毫升的THF,並在25℃下攪拌36小時。之後,進行層分離,並用二氯甲烷萃取產物層,用MgSO
4去除萃取物的水分,並將溶劑進行真空乾燥,從而獲得環氧矽氧烷系樹脂。
將30公克的上述製備的環氧矽氧烷系樹脂、10公克的作為交聯劑的(3',4'-環氧環己基)甲基3,4-環氧環己烷羧酸酯、5公克的雙[(3,4-環氧環己基)甲基]己二酸酯、0.5公克的作為光引發劑的(4-甲基苯基)[4-(2-甲基丙基)苯基]碘鎓六氟磷酸鹽和54.5公克的甲基乙基酮進行混合,從而製備用於形成硬塗層的組合物。
4-3. 光學多層結構體的製備
利用#30邁耶棒,將上述製備的用於形成防飛散層的組合物塗布在玻璃基板(UTG,30微米)的正面上,並在50℃下乾燥1分鐘,然後在230℃下乾燥10分鐘,從而形成厚度為10微米的聚醯亞胺基防飛散層。
接著,利用#10邁耶棒,將上述製備的用於形成硬塗層的組合物塗布在上述形成的防飛散層上,並在60℃下乾燥5分鐘後照射1焦耳/平方公分的紫外線,然後在120℃下固化15分鐘,形成厚度為5微米的硬塗層,從而製備UTG光學多層結構體。
< 實施例 5 和實施例 6>
除了在製備用於形成防飛散層的組合物的過程中分別添加組合物的總重量的10重量%和20重量%的二氧化矽奈米顆粒之外,藉由與所述實施例4相同的方法製備UTG光學多層結構體。
< 比較例 2>
除了在製備用於形成防飛散層的組合物的過程中未添加二氧化矽奈米顆粒之外,藉由與所述實施例4相同的方法製備UTG光學多層結構體。
< 實驗例 >
利用所述實施例和比較例中製備的UTG光學多層結構體,按照如下方法測量基板的彎曲特性和表面硬度,並將其結果示於下表1中。
1. 基板的彎曲(翹曲)的測量
利用尺測量所述實施例和比較例中製備的UTG光學多層結構體的二端部分從地面開始發生翹曲的程度,翹曲量(毫米)計算為在二端測量的值的平均值。
當所述平均值為3.0毫米以下時,評價為O,當所述平均值超過3.00毫米時,評價為X。
2. 表面硬度的測量
利用鉛筆硬度試驗機(Ocean Science(海洋科學)公司,COAD.607),利用秤砣施加750公克的荷重並測量鉛筆硬度。鉛筆(三菱公司)和試樣的角度設為45˚,並以20毫米/分鐘的速度測量10毫米。每個試樣測量3次,如果劃痕為2個以上,則判定為不良,將發生不良之前的硬度作為表面硬度。
[表1]
無機顆粒的含量(重量%) | 翹曲量(毫米) | 表面硬度 | ||
實施例1 | 5 | 0.5 | O | 1H |
實施例2 | 10 | 0.7 | O | 3H |
實施例3 | 20 | 1.5 | O | 3H |
實施例4 | 5 | 0.5 | O | 1H |
實施例5 | 10 | 0.7 | O | 3H |
實施例6 | 20 | 1.5 | O | 3H |
比較例1 | 0 | 0.5 | O | HB |
比較例2 | 0 | 0.5 | O | HB |
藉由所述表1可以確認,在包含作為無機顆粒的二氧化矽顆粒的實施例1至實施例6的UTG光學多層結構體中,翹曲量為3.0毫米以下,具有最小化的翹曲現象,而且與不包含無機顆粒的比較例相比,顯著改善了表面硬度降低的現象。
以上,藉由較佳的實施例和實驗例對一個實施態樣進行了詳細說明,但一個實施態樣的範圍並不限定於特定實施例,應根據申請專利範圍進行解釋。
10:顯示器的顯示元件
20:基板
30:防飛散層
40:硬塗層
100:光學多層結構體
圖1是示出根據一個實施方案的光學多層結構體的結構的示意圖。
100:光學多層結構體
10:顯示器的顯示器件
20:基板
30:防飛散層
40:硬塗層
Claims (19)
- 一種聚醯亞胺前驅物組合物,其係包含聚醯亞胺前驅物以及無機顆粒,該聚醯亞胺前驅物係包含衍生自包含以下化學式1的結構的酸酐或二胺的單元: [化學式1] 在化學式1中, R 1和R 2各自獨立地為未經取代或經一或多個鹵素取代的C 1-5烷基; R 3和R 4各自獨立地為未經取代或經一或多個鹵素取代的C 6-10芳基; L 1和L 2各自獨立地為C 1-10伸烷基;以及 x和y各自獨立地為1或更大的整數。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,該聚醯亞胺前驅物進一步包含衍生自以下化學式2所表示的二胺的單元: [化學式2] 在化學式2中, R 11和R 21各自獨立地為氫或C 1-20一價有機基團; L 11是-SO 2-、-O-或-C(=O)O-,或者是包含前述鍵的任一或多者的C 1-20二價有機基團;以及 化學式2不包含氟原子鍵。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,該聚醯亞胺前驅物進一步包含衍生自氟系二胺的單元。
- 如請求項3所述的聚醯亞胺前驅物組合物,其中,該氟系二胺包含選自以下群組中的一或多者:2,2'-雙(三氟甲基)聯苯胺(2,2’-bis(trifluoromethyl)benzidine,TFMB)、2,2-雙[4-(4-胺基苯氧基)苯基]六氟丙烷(2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane,HFBAPP)、2,2-雙(4-胺基苯基)六氟丙烷(2,2-bis(4-aminophenyl)hexafluoropropane,BAHF)、2,2'-雙(三氟甲基)-4,4'-二胺基二苯醚、4,4'-雙(4-胺基-2-三氟甲基苯氧基)聯苯及1,4-雙(4-胺基-2-三氟甲基苯氧基)苯。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,R 1和R 2各自獨立地為未經取代或經一或多個鹵素取代的C 1-3烷基; R 3和R 4各自獨立地為未經取代或經一或多個鹵素取代的C 6-8芳基;以及 L 1和L 2各自獨立地為C 1-5伸烷基。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,化學式1的結構為以下化學式3的結構: [化學式3] 在化學式3中, L 1和L 2各自獨立地為C 1-10伸烷基;以及 x和y各自獨立地為1或更大的整數。
- 如請求項2所述的聚醯亞胺前驅物組合物,其中,R 11和R 21各自獨立地為氫或C 1-10一價有機基團;以及 L 11是-SO 2-、-O-或-C(=O)O-,或者是包含前述鍵的任一或多者的C 1-15二價有機基團。
- 如請求項2所述的聚醯亞胺前驅物組合物,其中,L 11是-SO 2-、-O-或-C(=O)O-,或者是前述鍵的任一或多者與選自以下群組中的任一或多者的組合:C 1-10伸烷基、C 5-18伸環烷基及C 6-18伸芳基。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,該無機顆粒包含二氧化矽、氧化鋯、氧化鈦、氧化鋅、硫化鋅、氧化鉻、鈦酸鋇或其組合。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,相對於聚醯亞胺前驅物組合物的總重量,該無機顆粒的含量為1至30重量%。
- 如請求項1所述的聚醯亞胺前驅物組合物,其中,該聚醯亞胺前驅物組合物進一步包含藍色系顏料及染料的一或多者。
- 如請求項11所述的聚醯亞胺前驅物組合物,其中,該藍色系顏料及染料的最大吸收波長為520至680奈米。
- 一種聚醯亞胺膜,其係由請求項1至12中任一項所述的聚醯亞胺前驅物組合物所形成。
- 一種光學多層結構體,其包含: 基板; 防飛散層(shatterproof layer),其係形成在該基板上,並且包括請求項13所述的聚醯亞胺膜;以及 硬塗層,其係形成於該防飛散層上。
- 如請求項14所述的光學多層結構體,其中,該基板是超薄強化玻璃(ultrathin tempered glass)(超薄玻璃(ultrathin glass,UTG))基板。
- 如請求項14所述的光學多層結構體,其中,該硬塗層包含具有環氧基的矽氧烷系化合物。
- 一種製備光學多層結構體的方法,包含以下步驟: 將請求項1至12中任一項所述的聚醯亞胺前驅物組合物塗布在基板上並進行乾燥以形成防飛散層;以及 將用於形成硬塗層的組合物塗布在該防飛散層上並進行固化以形成硬塗層。
- 一種窗覆蓋膜(window cover film),其包含請求項14所述的光學多層結構體。
- 一種可撓性顯示面板,其包含請求項18所述的窗覆蓋膜。
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