CN104640696A - 透明导电膜 - Google Patents
透明导电膜 Download PDFInfo
- Publication number
- CN104640696A CN104640696A CN201380032172.0A CN201380032172A CN104640696A CN 104640696 A CN104640696 A CN 104640696A CN 201380032172 A CN201380032172 A CN 201380032172A CN 104640696 A CN104640696 A CN 104640696A
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- Prior art keywords
- nesa coating
- coating
- polymer
- cellulose
- hydroxy
- Prior art date
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- 238000000576 coating method Methods 0.000 claims description 128
- 239000011248 coating agent Substances 0.000 claims description 123
- 229920000642 polymer Polymers 0.000 claims description 66
- 239000000758 substrate Substances 0.000 claims description 30
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- 229920001002 functional polymer Polymers 0.000 claims description 22
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- 239000000203 mixture Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
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- 229920002301 cellulose acetate Polymers 0.000 claims description 11
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- 230000003252 repetitive effect Effects 0.000 claims description 8
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- 150000002170 ethers Chemical class 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 abstract description 4
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- 239000010408 film Substances 0.000 description 35
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 4
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
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- 229940043265 methyl isobutyl ketone Drugs 0.000 description 4
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 4
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- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 3
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- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
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- 238000001125 extrusion Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- MJHNUUNSCNRGJE-UHFFFAOYSA-N trimethyl benzene-1,2,4-tricarboxylate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C(C(=O)OC)=C1 MJHNUUNSCNRGJE-UHFFFAOYSA-N 0.000 description 2
- RGCVYEOTYJCNOS-UHFFFAOYSA-N (4-cyano-2-methylphenyl)boronic acid Chemical compound CC1=CC(C#N)=CC=C1B(O)O RGCVYEOTYJCNOS-UHFFFAOYSA-N 0.000 description 1
- NEOGGGHDLGYATP-UHFFFAOYSA-N 1,6-dimethylimidazo[4,5-b]pyridin-2-amine Chemical compound CC1=CN=C2N=C(N)N(C)C2=C1 NEOGGGHDLGYATP-UHFFFAOYSA-N 0.000 description 1
- LZFNKJKBRGFWDU-UHFFFAOYSA-N 3,6-dioxabicyclo[6.3.1]dodeca-1(12),8,10-triene-2,7-dione Chemical compound O=C1OCCOC(=O)C2=CC=CC1=C2 LZFNKJKBRGFWDU-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
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- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 description 1
- FNJSWIPFHMKRAT-UHFFFAOYSA-N Monomethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(O)=O FNJSWIPFHMKRAT-UHFFFAOYSA-N 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- DRUKNYVQGHETPO-UHFFFAOYSA-N Nonanedioic acid dimethyl ester Natural products COC(=O)CCCCCCCC(=O)OC DRUKNYVQGHETPO-UHFFFAOYSA-N 0.000 description 1
- 229920000305 Nylon 6,10 Polymers 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 125000003262 carboxylic acid ester group Chemical group [H]C([H])([*:2])OC(=O)C([H])([H])[*:1] 0.000 description 1
- HKQOBOMRSSHSTC-UHFFFAOYSA-N cellulose acetate Chemical compound OC1C(O)C(O)C(CO)OC1OC1C(CO)OC(O)C(O)C1O.CC(=O)OCC1OC(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(COC(C)=O)O1.CCC(=O)OCC1OC(OC(=O)CC)C(OC(=O)CC)C(OC(=O)CC)C1OC1C(OC(=O)CC)C(OC(=O)CC)C(OC(=O)CC)C(COC(=O)CC)O1 HKQOBOMRSSHSTC-UHFFFAOYSA-N 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 238000004132 cross linking Methods 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- 229940014772 dimethyl sebacate Drugs 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- UHPJWJRERDJHOJ-UHFFFAOYSA-N ethene;naphthalene-1-carboxylic acid Chemical compound C=C.C1=CC=C2C(C(=O)O)=CC=CC2=C1 UHPJWJRERDJHOJ-UHFFFAOYSA-N 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 229940116333 ethyl lactate Drugs 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 125000001072 heteroaryl group Chemical group 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 210000004276 hyalin Anatomy 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
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- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- 238000006068 polycondensation reaction Methods 0.000 description 1
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- 229920000098 polyolefin Polymers 0.000 description 1
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- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000007767 slide coating Methods 0.000 description 1
- 238000007764 slot die coating Methods 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0274—Optical details, e.g. printed circuits comprising integral optical means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B23/00—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
- B32B23/04—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B23/042—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B23/00—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
- B32B23/04—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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Abstract
本发明公开并且要求保护透明导电膜,所述透明导电膜展现高透光率、低表面电阻率和优良的剥离粘着力。这类膜适用于电子应用中。
Description
概述
至少一个实施方案包括一种透明导电膜,所述透明导电膜包括:至少一个透明衬底;至少一个透明底漆层,其设置在至少一个透明衬底上,其中所述至少一个透明底漆层由至少一种透明底漆层涂料混合物形成,所述混合物包括至少一种羟基官能聚合物和至少一种可热固化单体;以及至少一种透明导电层,其设置在至少一个透明底漆层上,其中所述至少一个透明导电层由至少一种透明导电层涂料混合物形成,所述混合物包括至少一种第一纤维素酯聚合物和至少一种金属纳米线。
在至少一些实施方案中,至少一个透明衬底包括至少一种聚酯。
在至少一些实施方案中,至少一个透明衬底包括至少一种第一聚酯,所述第一聚酯包括至少约70wt%对苯二甲酸乙二醇酯重复单元。
在至少一些这类实施方案中,至少一种第一羟基官能聚合物包括纤维素酯聚合物、聚醚多元醇、聚酯多元醇或聚乙烯醇。
在至少一些上述实施方案中,至少一种第一羟基官能聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
在至少一些上述实施方案中,至少一种第一羟基官能聚合物包括乙酸丁酸纤维素聚合物。
在至少一些上述实施方案中,根据ASTM D817-96,至少一种第一羟基官能聚合物包括至少约1wt%,或至少约3wt%,或约4.8wt%的羟基含量。
在至少一些上述实施方案中,至少一种可热固化单体包括至少约三个醚基。
在至少一些上述实施方案中,至少一种可热固化单体包括至少一种三聚氰胺单体。
在至少一些上述实施方案中,至少一种可热固化单体包括六甲氧基甲基三聚氰胺。
在至少一些上述实施方案中,至少一种第一纤维素酯聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
在至少一些上述实施方案中,至少一种第一纤维素酯聚合物包括乙酸丁酸纤维素聚合物。
在至少一些上述实施方案中,至少一种金属纳米线包括至少一种银纳米线。
在至少一些上述实施方案中,透明导电膜展现小于约100欧姆/平方的四点表面电阻率。
在至少一些上述实施方案中,根据ASTM D3359-92A,透明导电膜展现为5的剥离粘着力值。
这些实施方案和其它变化和修改可以从随后的描述、示例性实施方案、实施例和权利要求书中更好地理解。提供的任何实施方案只是通过说明性实施例的方式给出。本身实现的其它合乎需要的目的和优点可被本领域技术人员想到或变得明显。
描述
在本文件中提及的所有出版物、专利和专利文件均以全文引用的方式并入,恰如以引用的方式单独地并入一般。
2012年6月26日提交的名称为透明导电膜(TRANSPARENTCONDUCTIVE FILM)的美国临时申请号61/664,268在此以全文引用的方式并入。
特征在于包括银纳米线和纤维素酯聚合物的导电层的透明导电膜(TCF)公开于2012年5月3日提交的美国专利申请公布2012/0107600(包括纤维素酯的透明导电膜(TRANSPARENTCONDUCTIVE FILMS COMPRISING CELLULOSE ESTERS))中,所述申请在此以全文引用的方式并入。这类TCF可展现高透光率和低表面电阻率。但是,开发保留这些性质,同时还展现优良的剥离粘着力的TCF已成为一种挑战。
透明导电膜
透明并且导电的膜已在近年来广泛用于触摸面板显示器、液晶显示器、电致发光、有机发光二极管装置、光伏太阳能电池中。基于氧化铟锡(ITO)的透明导电膜直到最近由于它的高导电性、透明性和相对高的稳定性已成为针对大多数应用选择的透明导体。但是,以氧化铟锡为基础的透明导电膜具有局限性,由于铟的成本高、需要复杂的并且昂贵的真空沉积设备和处理,和它固有的脆性和开裂倾向,尤其当氧化铟锡沉积在柔性衬底上时。
测量透明导电膜(TCF)的性质的两个重要参数为总透光率(%T)和膜表面导电性。较高透光率允许显示器应用的清晰的图像品质,照明和太阳能转换应用的较高效率。较低电阻率对于可使功率消耗最小化的大多数透明导电膜应用来说是最合乎需要的。
透明衬底
一些实施方案提供一种TCF,其包括至少一个透明衬底。衬底可为刚性或柔性的。
合适的刚性衬底包括例如玻璃、聚碳酸酯、丙烯酸树脂等。
当TCF的不同层的涂料混合物涂布到柔性衬底上时,衬底优选地为柔性、透明聚合物膜,所述膜具有任何所需厚度并且由一种或多种聚合物材料构成。衬底需要展现在导电层的涂布和干燥期间的尺寸稳定性并且展现具有对上覆层的合适粘着性质。制造这类衬底的有用聚合物材料包括聚酯(如聚对苯二甲酸乙二醇酯和聚萘二甲酸乙二醇酯)、乙酸纤维素和其它纤维素酯、聚乙烯醇缩乙醛、聚烯烃、聚碳酸酯和聚苯乙烯。优选的衬底由具有良好热稳定性的聚合物组成,如聚酯和聚碳酸酯。还可将支撑材料处理或退火以减小收缩并且促进尺寸稳定性。还可使用透明多层衬底。
在至少一些实施方案中,提供包括透明衬底的透明导电膜,所述透明衬底包括至少一种聚酯。至少一种聚酯可例如包括至少约70wt%对苯二甲酸乙二醇酯重复单元。或所述聚酯可包括至少约75wt%,或至少约80wt%,或至少约85wt%,或至少约90wt%或至少约95wt%对苯二甲酸乙二醇酯重复单元。
这类聚酯可例如通过包括酸或酯部分的一种或多种单体与包括醇部分的一种或多种单体的缩聚制得。包括酸或酯部分的单体的非限制实例包括例如芳族酸或酯、脂族酸或酯和非芳族环状酸或酯。包括酸或酯部分的示例性单体包括例如对苯二甲酸、对苯二甲酸二甲酯、间苯二甲酸、间苯二甲酸二甲酯、邻苯二甲酸、邻苯二甲酸甲酯、偏苯三酸、偏苯三酸三甲酯、萘二甲酸、萘二甲酸二甲酯、己二酸、己二酸二甲酯、壬二酸、壬二酸二甲酯、癸二酸、癸二酸二甲酯等。包括醇部分的示例性单体包括例如乙二醇、丙二醇、丁二醇、己二醇、新戊二醇、二乙二醇、环己烷二甲醇等。
这类聚酯可例如包括重复单元,所述重复单元包括来自包括酸或酯部分的单体的第一残基,所述第一残基通过酯键结合到来自包括醇部分的单体的第二残基。示例性重复单元为例如对苯二甲酸乙二醇酯、间苯二甲酸乙二醇酯、萘二甲酸乙二醇酯、对苯二甲酸二乙二醇酯、间苯二甲酸二乙二醇酯、萘二甲酸二乙二醇酯、对苯二甲酸环己二醇酯、间苯二甲酸环己二醇酯、萘二甲酸环己二醇酯等。这类聚酯可包括一种以上类型的重复基团并且可有时称为共聚酯。
透明底漆层
一些实施方案提供包括设置在至少一个透明衬底上的至少一个透明底漆层的TCF,其中至少一个透明底漆层由至少一种透明底漆层涂料混合物形成,所述混合物包括至少一种羟基官能聚合物和至少一种可热固化单体。这类底漆层可在一些情况下称为载体层、中间层、粘着力促进剂层、夹层等。这类底漆层用以促进至少一个透明导电层对至少一个透明衬底的粘着力。
羟基官能聚合物为包括羟基的聚合物,所述羟基能够与可热固化单体上例如像醚基的反应性基团反应以形成共价键。羟基官能聚合物的实例包括例如纤维素酯聚合物、聚醚多元醇、聚酯多元醇、聚乙烯醇等。
纤维素酯聚合物包括乙酸纤维素酯,例如像乙酸纤维素、三乙酸纤维素、丙酸纤维素、乙酸丙酸纤维素、乙酸丁酸纤维素(CAB)等。
如ASTM D817-96试验方法所测定,羟基官能聚合物可由它们的羟基含量(表示为重量百分比)表征。尤其有用的羟基官能聚合物包括至少约1wt%,或至少约3wt%,或约4.8wt%的羟基含量。示例性羟基官能聚合物为可获自田纳西州金斯堡的Eastman Chemical公司的CAB 533-0.4乙酸丁酸纤维素聚合物,所述聚合物具有以典型平均批量计4.8wt%的羟基含量。
可热固化单体为已知的。这些单体可例如包括具有一个或多个醚基,如一个、两个、三个或更多个醚基的单体。这类醚基可例如包括一个或多个甲氧基、乙氧基或其它基团。这类醚基可与例如像羟基的其它官能基反应,或它们可与其它醚基反应。这类反应可导致聚合或交联。具有芳族或杂芳族环的可热固化单体,例如像官能化的三聚氰胺单体,可提供与如聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯的这类衬底的改进涂层相容性。六甲氧基甲基三聚氰胺为示例性可热固化单体。
透明底漆层涂料混合物还可包括热引发剂以促进聚合和交联反应。示例性引发剂为对甲苯磺酸。
透明底漆层涂料混合物可一般包括有机溶剂。这些有机溶剂可出于如控制溶液粘度、改进润湿性和衬底涂布等的目的来使用。有机溶剂的实例包括酮、酯和醇,例如像甲基乙基酮、乙酸丁酯、乙醇等。
透明底漆层可通过使用各种涂布程序将透明底漆层涂料混合物涂布到透明衬底上来形成,所述涂布程序如绕线棒涂布(wire woundrod coating)、浸渍涂布、气刀涂布、幕帘式涂布(curtain coating)、滑动涂布(slide coating)、固模涂布(solid-die coating)、辊涂、凹版式涂布或挤压涂布。这类涂料混合物可例如具有6wt%与20wt%之间的固体和在室温下介于5cp与30cp之间的粘度。
这类涂层可在涂敷之后干燥,以提供具有例如100nm与500nm之间的厚度的涂层。例如,在280°F(138℃)烘箱中的两分钟干燥说明于实施例中。
透明导电层
一些实施方案提供包括设置在至少一个透明底漆层上的至少一个透明导电层的TCF,其中至少一个透明导电层由至少一种透明导电层涂料混合物形成,所述混合物包括至少一种第一纤维素酯聚合物和至少一种金属纳米线。
合适的透明导电层涂料混合物公开于2012年5月3日公布的美国专利申请公布2012/0107600(包括纤维素酯的透明导电膜(TRANSPARENT CONDUCTIVE FILMS COMPRISING CELLULOSE ESTERS))中,所述申请在此以全文引用的方式并入。
对于透明导电膜的实际制造过程而言,在单一涂层溶液中具有如银纳米线和聚合物粘合剂的两种导电组分为合乎需要的并且是重要的。聚合物粘合剂溶液起双重作用,作为分散剂以促进银纳米线的分散和作为增粘剂以稳定银纳米线涂层分散液,以使得银纳米线的沉降不会在涂布过程期间的任何时刻发生。这简化了涂布过程,并且允许一次涂布,并且避免首先涂布裸银纳米线以形成脆弱并且易碎的膜,随后顶涂(over-coat)聚合物以形成透明导电膜的方法。
为了使透明导电膜适用于各种装置应用中,还重要的是,透明导电膜的粘合剂为光学透明的和柔性的;还具有高机械强度、硬度和良好的热和光稳定性。还合乎需要的是,透明导电膜的聚合物粘合剂含有具有N、O、S或具有孤对电子的其它元素的官能基以提供良好的配位键合,用于在银纳米线和聚合物溶液的分散和涂布期间稳定化银纳米线。
因此,使用具有如羟基和羧酸酯基的高氧含量的聚合物粘合剂为有利的。这些聚合物对银纳米线表面具有强亲和力,并且促进涂层溶液中银纳米线的分散和稳定。大多数富氧聚合物还具有在通常用以制备有机溶剂涂布薄膜的极性有机溶剂中具有良好溶解性的额外益处。
在用于制备基于银纳米线的透明导电膜并且从如2-丁酮(甲基乙基酮,MEK)、甲基异丁基酮、丙酮、甲醇、乙醇、2-丙醇、乙酸乙酯或其混合物的有机溶剂涂布时,如乙酸丁酸纤维素(CAB)、乙酸纤维素(CA)或乙酸丙酸纤维素(CAP)的纤维素酯聚合物优于其它富氧聚合物粘合剂。它们的使用产生涂布膜的透光率和导电性大大提高的透明导电膜。此外,这些纤维素酯聚合物具有至少100℃的玻璃化转变温度,可形成具有高机械强度和硬度的透明并且柔性的膜,并且具有高热和光稳定性。与此相反,采用聚氯酯或聚乙烯醇缩丁醛聚合物粘合剂的类似制备的透明导电膜示出较不合乎需要的透明性和导电性。
纤维素酯聚合物的存在量占干燥透明导电膜的约40wt%至约90wt%。优选地,纤维素酯聚合物的存在量占干燥膜的约60wt%至约85wt%。
在一些构造中,最多50wt%的纤维素酯混合物可由一种或多种其它聚合物替代。这些聚合物应与纤维素聚合物相容。相容意味聚合物当干燥时形成透明的单相混合物。其它一种或多种聚合物可提供进一步益处,如提高对支撑物的粘着力以及提高硬度和防刮性。如上所述,所有聚合物的总wt%为干燥透明导电膜的约50wt%至约90wt%。优选地,所有聚合物的总重量占干燥膜的约70wt%至约85wt%。聚酯和聚丙烯酸聚合物为有用的其它聚合物的实例。
例如像银或铜纳米线的金属纳米线为对导电膜和使用所述导电膜制备的物品赋予导电性的基本组分。透明导电膜的导电性主要受以下控制:a)单个纳米线的导电性,b)端子之间纳米线的数目,和c)纳米线之间的连通性。低于某一纳米线浓度(也称为渗透阈值),端子之间的导电性为零,因为由于纳米线间隔太远,无法提供连续的电流通路。高于这个浓度,存在至少一个可用的电流通路。在提供更多电流通路时,层的总电阻将减小。但是,在提供更多电流通路时,透射穿过导电膜的光的百分比由于纳米线的光吸收和散射而减小。同样,在导电膜中金属纳米线的量增大时,透明膜的雾度由于金属纳米线的光散射而增大。类似效应将发生在使用导电膜制备的透明物品中。
在一个实施方案中,金属纳米线具有约20至约3300的长宽比(长度/宽度)。在另一实施方案中,金属纳米线具有约500至1000的长宽比(长度/宽度)。具有约5μm至约100μm(微米)的长度和约30nm至约200nm的宽度的金属纳米线为可用的。具有约50nm至约120nm的宽度和约15μm至约100μm的长度的金属纳米线也适用于透明导电网状膜的构造。
金属纳米线可由本领域已知的方法制备。具体地说,银纳米线可通过在多元醇(例如乙二醇或丙二醇)和聚(乙烯吡咯烷酮)的存在下的银盐(例如硝酸银)的溶液相还原来合成。均匀大小的银纳米线的大规模生产可根据例如Ducamp-Sanguesa,C.等,J.of Solid State Chemistry,(1992),100,272-280;Sun,Y.等,Chem.Mater.(2002),14,4736-4745;以及Sun,Y.等,Nanoletters,(2003),3(7),955-960中所述的方法制备。
透明导电层涂料混合物可一般包括有机溶剂。这些有机溶剂可出于如控制溶液粘度、改进润湿性和衬底涂布等的目的来使用。有机溶剂的实例包括甲苯、2-丁酮(甲基乙基酮,MEK)、甲基异丁基酮、丙酮、甲醇、乙醇、2-丙醇、乙酸乙酯、乙酸丙酯、乳酸乙酯或四氢呋喃,或其混合物。甲基乙基酮为尤其有用的涂层溶剂。
透明导电层可通过使用各种涂布程序将透明导电层涂料混合物涂布到透明底漆层上来形成,所述涂布程序如绕线棒涂布、浸渍涂布、气刀涂布、幕帘式涂布、滑动涂布、槽模涂布(slot-die coating)、辊涂、凹版式涂布或挤压涂布。表面活性剂和其它涂层助剂可并入涂层制剂中。这类涂料混合物可例如具有6wt%与20wt%之间的固体和在室温下介于5cp与30cp之间的粘度。
这类涂层可在涂敷之后干燥,以提供具有例如100nm与500nm之间的厚度的涂层。例如,在280°F(138℃)烘箱中的两分钟干燥说明于实施例中。
透明导电膜性质
在涂布并且干燥之后,透明导电膜应具有小于1,000欧姆/平方,或小于500欧姆/平方,或小于100欧姆/平方的表面电阻率,如使用可获自俄亥俄州托莱多的Electronic Design to Market公司的R-CHEK型号RC2175表面电阻率仪表所测量。
在涂布并且干燥之后,透明导电膜应具有尽可能高的%透射率。至少70%的透射率为有用的。至少80%和至少90%的透射率甚至更有用。
在涂布并且干燥之后,当根据ASTM D3359-92A评估时,透明导电膜应展现如“5”评分的特殊拉脱粘着力性质。这个程序描述于实施例1中。
示例性实施方案
在此以全文引用的方式并入的2012年6月26日提交的标题为透明导电膜(TRANSPARENT CONDUCTIVE FILM)的美国临时申请号61/664,268公开以下17个非限制示例性实施方案:
A.一种透明导电膜,其包括:
至少一个透明衬底;
至少一个透明底漆层,其设置在所述至少一个透明衬底上,所述至少一个透明底漆层由至少一种透明底漆层涂料混合物形成,所述混合物包括至少一种羟基官能聚合物和至少一种可热固化单体;以及
至少一个透明导电层,其设置在所述至少一个透明底漆层上,所述至少一个透明导电层由至少一种透明导电层涂料混合物形成,所述混合物包括至少一种第一纤维素酯聚合物和至少一种金属纳米线。
B.根据实施方案A所述的透明导电膜,其中所述至少一个透明衬底包括至少一种聚酯。
C.根据实施方案A至B中任一项所述的透明导电膜,其中所述至少一个透明衬底包括至少一种第一聚酯,所述聚酯包括至少约70wt%对苯二甲酸乙二醇酯重复单元。
D.根据实施方案A至B中任一项所述的透明导电膜,其中所述至少一种第一羟基官能聚合物包括纤维素酯聚合物、聚醚多元醇、聚酯多元醇或聚乙烯醇。
E.根据实施方案A至D中任一项所述的透明导电膜,其中所述至少一种第一羟基官能聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
F.根据实施方案A至E中任一项所述的透明导电膜,其中所述至少一种第一羟基官能聚合物包括乙酸丁酸纤维素聚合物。
G.根据实施方案A至F中任一项所述的透明导电膜,其中根据ASTM D817-96,所述至少一种第一羟基官能聚合物包括至少约1wt%的羟基含量。
H.根据实施方案A至G中任一项所述的透明导电膜,其中根据ASTM D817-96,所述至少一种第一羟基官能聚合物包括至少约3wt%的羟基含量。
J.根据实施方案A至H中任一项所述的透明导电膜,其中根据ASTM D817-96,所述至少一种第一羟基官能聚合物包括约4.8wt%的羟基含量。
K.根据实施方案A至J中任一项所述的透明导电膜,其中所述至少一种可热固化单体包括至少约三个醚基。
L.根据实施方案A至K中任一项所述的透明导电膜,其中所述至少一种可热固化单体包括至少一种三聚氰胺单体。
M.根据实施方案A至L中任一项所述的透明导电膜,其中所述至少一种可热固化单体包括六甲氧基甲基三聚氰胺。
N.根据实施方案A至M中任一项所述的透明导电膜,其中所述至少一种第一纤维素酯聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
P.根据实施方案A至N中任一项所述的透明导电膜,其中所述至少一种第一纤维素酯聚合物包括乙酸丁酸纤维素聚合物。
Q.根据实施方案A至P中任一项所述的透明导电膜,其中所述至少一种金属纳米线包括至少一种银纳米线。
R.根据实施方案A至Q中任一项所述的透明导电膜,其展现小于约100欧姆/平方的四点表面电阻率。
S.根据实施方案A至R中任一项所述的透明导电膜,根据ASTMD3359-92A,其展现为5的剥离粘着力值。
实施例
实施例1(比较)
银层涂料混合物通过共混54重量份的银纳米线的1.85wt%异丙醇分散液、3重量份的乙酸丁酸纤维素聚合物(CAB 381-20,EastmanChemical)、33重量份的乙酸丙酯和10重量份的乙酸乙酯来制备。混合物具有3wt%与8wt%之间的固体和在室温下介于30cp与150cp之间的粘度。
然后制备涂布样品。将几毫升银层涂料混合物涂敷到铬凹版印刷板的顶部边缘,所述铬凹版印刷板刻印有200-500线网(line screen)。将5至7mil聚对苯二甲酸乙二醇酯(PET)缠绕到基于乙烯丙烯二烯单体(EPDM)的橡胶压印辊上,所述橡胶压印辊然后从顶部边缘滚向印刷板的底部边缘,将墨水从凹版凹部转移到PET膜。然后将涂布膜置于280°F(138℃)烘箱中两分钟。干燥银层厚度在100nm与500nm之间。
涂布膜的表面电阻率在涂布膜已从烘箱冷却之后评估。膜的涂布侧的四点表面电阻率使用R-CHEK装置测量。样品展现48欧姆/平方的表面电阻率。
涂布膜的剥离粘着力然后根据ASTM D3359-92A评估。每一膜的涂布侧用刀片划线并且用无绒棉垫轻轻移除碎屑。然后将粘着胶带(明尼苏达州圣保罗的3M公司的#610半透明压敏胶带)施加到交叉阴影区域,并且用橡胶辊使其平滑直到胶带与涂布膜之间无气泡。然后将胶带快速剥离。对涂布膜的外观给出0至5级的分数:5=划线切口的边缘完全光滑;4=涂层的薄片在划线的一些交叉点处脱离,小于约5%的试验区域受影响;3=涂层的薄片沿一些边缘并且在划线的一些交叉点处脱离,约5%至15%的试验区域受影响;2=涂层的薄片沿划线的一些边缘并且在正方形的部分上脱离,约15%至35%的试验区域受影响;1=涂层沿划线的边缘以大带状物的形式脱离,大于约35%的试验区域受影响;0=涂层完全移除。达到5分的膜给予“通过”的评分,同时达到小于5分的膜给予“失败”的评分。这种样品的外观被评为“失败”。
实施例2(比较)
底漆层涂料混合物通过共混12重量份的支链饱和热塑性聚酯聚合物(2200,Bostik)和88重量份的甲基乙基酮来制备。混合物具有6wt%与20wt%之间的固体和在室温下介于5cp与30cp之间的粘度。
银层涂料混合物通过共混54重量份的银纳米线的1.85wt%异丙醇分散液、3重量份的乙酸丁酸纤维素聚合物(CAB 381-20,EastmanChemical)、33重量份的乙酸丙酯和10重量份的乙酸乙酯来制备。混合物具有3wt%与8wt%之间的固体和在室温下介于30cp与150cp之间的粘度。
然后制备涂布样品。将底漆层涂料混合物使用凹版台式打样机(gravure benchtop proofer)涂敷到5至7mil PET膜。然后将涂布膜置于280°F(138℃)烘箱中两分钟。干燥底漆层厚度在100nm与500nm之间。
然后将银层涂料混合物使用实施例1的方法涂敷到涂布PET膜的底漆层。干燥银层厚度在100nm与500nm之间。
涂布膜的表面电阻率在涂布膜已从烘箱冷却之后评估。膜的涂布侧的四点表面电阻率使用R-CHEK装置测量。样品展现无穷大的表面电阻率。
涂布膜的剥离粘着力然后根据实施例1的方法评估。这种样品的外观被评为“通过”。
实施例3(发明)
底漆层涂料混合物通过共混6重量份的乙酸丁酸纤维素聚合物(CAB 553-0.4,Eastman Chemical)、6重量份的六甲氧基甲基三聚氰胺(303,Cytec)、77.4重量份的甲基乙基酮、10重量份的丁醇和0.6重量份对-甲苯磺酸来制备。混合物具有6wt%与20wt%之间的固体和在室温下介于5cp与30cp之间的粘度。
银层涂料混合物通过共混54重量份的银纳米线的1.85wt%异丙醇分散液、3重量份的乙酸丁酸纤维素聚合物(CAB 381-20,EastmanChemical)、33重量份的乙酸丙酯和10重量份的乙酸乙酯来制备。混合物具有3wt%与8wt%之间的固体和在室温下介于30cp与150cp之间的粘度。
然后制备涂布样品。将底漆层涂料混合物使用凹版台式打样机(gravure benchtop proofer)涂敷到5至7mil PET膜。然后将涂布膜置于280°F(138℃)烘箱中两分钟。干燥底漆层厚度在100nm与500nm之间。
然后将银层涂料混合物使用实施例1的方法涂敷到涂布PET膜的底漆层。干燥银层厚度在100nm与500nm之间。
涂布膜的表面电阻率在涂布膜已从烘箱冷却之后评估。膜的涂布侧的四点表面电阻率使用R-CHEK装置测量。样品展现48欧姆/平方的表面电阻率。
涂布膜的剥离粘着力然后根据实施例1的方法评估。这种样品的外观被评为“通过”。
已参考具体实施方案详细描述了本发明,但应理解的是变化和修改可以在本发明的精神和范围内实现。目前公开的实施方案因此在所有方面被认为是说明性的而不是限制性的。本发明的范围由随附权利要求书指示,并且在其等效物含义和范围内产生的所有改变旨在包括于其中。
Claims (10)
1.一种透明导电膜,其包括:
至少一个透明衬底;
至少一个透明底漆层,其设置在所述至少一个透明衬底上,所述至少一个透明底漆层由至少一种透明底漆层涂料混合物形成,所述混合物包括至少一种羟基官能聚合物和至少一种可热固化单体;以及
至少一个透明导电层,其设置在所述至少一个透明底漆层上,所述至少一个透明导电层由至少一种透明导电层涂料混合物形成,所述混合物包括至少一种第一纤维素酯聚合物和至少一种金属纳米线。
2.根据权利要求1所述的透明导电膜,其中所述至少一个透明衬底包括至少一种聚酯,所述聚酯包括至少约70wt%对苯二甲酸乙二醇酯重复单元。
3.根据权利要求1所述的透明导电膜,其中所述至少一种第一羟基官能聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
4.根据权利要求1所述的透明导电膜,其中根据ASTMD817-96,至少一种第一羟基官能聚合物包括至少约3wt%的羟基含量。
5.根据权利要求1所述的透明导电膜,其中根据ASTMD817-96,所述至少一种第一羟基官能聚合物包括约4.8wt%的羟基含量。
6.根据权利要求1所述的透明导电膜,其中所述至少一种可热固化单体包括至少约三个醚基。
7.根据权利要求1所述的透明导电膜,其中所述至少一种可热固化单体包括至少一种三聚氰胺单体。
8.根据权利要求1所述的透明导电膜,其中所述至少一种可热固化单体包括六甲氧基甲基三聚氰胺。
9.根据权利要求1所述的透明导电膜,其中所述至少一种第一纤维素酯聚合物包括乙酸纤维素聚合物、乙酸丁酸纤维素聚合物或乙酸丙酸纤维素聚合物。
10.根据权利要求1所述的透明导电膜,其中所述至少一种金属纳米线包括至少一种银纳米线。
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US13/905,380 US20130341071A1 (en) | 2012-06-26 | 2013-05-30 | Transparent conductive film |
PCT/US2013/046490 WO2014004194A2 (en) | 2012-06-26 | 2013-06-19 | Transport conductive film |
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EP (1) | EP2864116A2 (zh) |
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CN109937458A (zh) * | 2016-11-28 | 2019-06-25 | 昭和电工株式会社 | 导电性膜和导电性膜的制造方法 |
CN110720129A (zh) * | 2017-08-02 | 2020-01-21 | 昭和电工株式会社 | 导电膜的制造方法、导电膜和金属纳米线墨 |
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TW201415496A (zh) | 2014-04-16 |
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US20130341071A1 (en) | 2013-12-26 |
WO2014004194A8 (en) | 2015-01-08 |
EP2864116A2 (en) | 2015-04-29 |
KR20150052811A (ko) | 2015-05-14 |
WO2014004194A2 (en) | 2014-01-03 |
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