TWI558571B - Inorganic film and layered body - Google Patents
Inorganic film and layered body Download PDFInfo
- Publication number
- TWI558571B TWI558571B TW103122698A TW103122698A TWI558571B TW I558571 B TWI558571 B TW I558571B TW 103122698 A TW103122698 A TW 103122698A TW 103122698 A TW103122698 A TW 103122698A TW I558571 B TWI558571 B TW I558571B
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- Taiwan
- Prior art keywords
- refractive index
- film
- index gradient
- gradient film
- gas barrier
- Prior art date
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- 229920005989 resin Polymers 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 24
- 229910052725 zinc Inorganic materials 0.000 claims description 21
- 229910052718 tin Inorganic materials 0.000 claims description 19
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 229910010272 inorganic material Inorganic materials 0.000 claims description 9
- 239000011147 inorganic material Substances 0.000 claims description 9
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 239000010408 film Substances 0.000 description 243
- 239000007789 gas Substances 0.000 description 61
- 230000004888 barrier function Effects 0.000 description 58
- 239000010410 layer Substances 0.000 description 37
- 239000011701 zinc Substances 0.000 description 25
- 239000000463 material Substances 0.000 description 24
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- 238000002834 transmittance Methods 0.000 description 12
- 230000008859 change Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- -1 ethylene diester Chemical class 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
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- KYKLWYKWCAYAJY-UHFFFAOYSA-N oxotin;zinc Chemical compound [Zn].[Sn]=O KYKLWYKWCAYAJY-UHFFFAOYSA-N 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
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- 239000004814 polyurethane Substances 0.000 description 3
- WJMXTYZCTXTFJM-UHFFFAOYSA-N 1,1,1,2-tetraethoxydecane Chemical compound C(C)OC(C(OCC)(OCC)OCC)CCCCCCCC WJMXTYZCTXTFJM-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 125000005442 diisocyanate group Chemical group 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- FEIALZPTQXKFGA-UHFFFAOYSA-N C(C(=C)C)(=O)OCCCC(C(C)(C)C)CCCCCCC Chemical compound C(C(=C)C)(=O)OCCCC(C(C)(C)C)CCCCCCC FEIALZPTQXKFGA-UHFFFAOYSA-N 0.000 description 1
- KFKILXQFBVYKNF-UHFFFAOYSA-N CCC=COCCCC(C(C)(C)C)CCCCCCC Chemical compound CCC=COCCCC(C(C)(C)C)CCCCCCC KFKILXQFBVYKNF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- 229910007717 ZnSnO Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910002064 alloy oxide Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 1
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229920000831 ionic polymer Polymers 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
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- 229920001684 low density polyethylene Polymers 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N perisophthalic acid Natural products OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
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- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
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- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
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- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Classifications
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Description
本發明係關於一種具有較高之折射率且光學干涉得以抑制之無機膜及將該無機膜積層於樹脂等有機物而成之積層體。
於輕量且可自由地彎曲之可撓性裝置中，對於基材或元件本身係使用樹脂等有機物。對於使用包含樹脂等之可撓性基材作為基材之所謂可撓性裝置，要求除阻氣性及透明性以外亦兼具可撓性之阻氣膜作為密封構件。
專利文獻1中揭示有兼具阻氣性及可撓性之阻氣膜。於專利文獻1中，為了提高阻氣性而使用鋅錫氧化物。
[專利文獻1]日本專利特表2010-524732號公報
然而，專利文獻1中所揭示之鋅錫氧化物之折射率較高，於賦予至基材膜或增黏塗層等樹脂材料上之情形時，因與該等材料之折射率差而會產生光學干涉。因此，有光線透過率下降之問題。
本發明之目的在於提供一種於與樹脂等有機物積層時亦不降低光線透過率之無機膜及具有該無機膜之積層體。
本發明之無機膜具備：折射率梯度膜A，其包含無機材料，自一面朝向另一面，折射率自n1連續地變化至n2(n1<n2)且為功能性膜；及折射率梯度膜B，其包含無機材料，自一面朝向另一面，折射率自n3連續地變化至n4(n4<n3)且為功能性膜；於折射率梯度膜A之折射率為n2之側之面，以自上述折射率為n3之面側直接或間接地接觸之方式積層有折射率梯度膜B，n2與n3之差為0.1以下，並且上述無機材料為包含Si與Al中之至少一者、Zn、及Sn之複合氧化物。
於本發明之無機膜中，較佳為上述折射率梯度膜A與折射率梯度膜B中之至少一者包含含有Si、Zn及Sn之複合氧化物。
於本發明之無機膜中，較佳為於上述包含Si、Zn及Sn之複合氧化物中，Sn相對於Zn與Sn之總和之比Xs滿足70>Xs>0。
於本發明之無機膜中，較佳為上述折射率梯度膜A與折射率梯度膜B中之至少一者包含含有Al、Zn及Sn之複合氧化物。
於本發明之無機膜中，較佳為上述折射率梯度膜A包含含有Al、Zn及Sn之複合氧化物，上述折射率梯度膜B包含含有Si、Zn及Sn之複合氧化物。
本發明之積層體係於有機膜上構成依據本發明而構成之無機膜，且將有機膜之折射率設為n0時n0≦n1之積層體。
於本發明之積層體中，較佳為於上述無機膜上形成有樹脂層，且將樹脂層之折射率設為n5時，n4≧n5。
本發明之無機膜及積層體由於具有如上所示之構成，於折射率梯度膜A中，於膜厚方向上折射率自n1連續地增大至n2，進而，於折射率梯度膜B中，折射率自n3連續地減小至n4，且n2與n3之差為0.1以下，故而可抑制由折射率差引起之反射。因此，可防止光線透過率之下降。因此，即便使用可賦予各種功能之折射率較高之材料作為折射
率梯度膜A及折射率梯度膜B，亦可防止光線透過率之下降。因此，可兼具功能性與較高之光線透過率。
11‧‧‧基材
12‧‧‧平坦化層
13‧‧‧無機膜
13a‧‧‧折射率梯度膜
13b‧‧‧折射率梯度膜
14‧‧‧樹脂層
30‧‧‧基材膜
31‧‧‧卷對卷濺鍍裝置
32‧‧‧捲出捲取室
33‧‧‧捲出軸
34‧‧‧捲取軸
35‧‧‧導輥
36‧‧‧導輥
37‧‧‧筒輥
38‧‧‧真空泵
39‧‧‧真空泵
40‧‧‧成膜室
41‧‧‧靶
42‧‧‧靶
43‧‧‧雙極電源
44‧‧‧氬氣供給管線
45‧‧‧氧氣供給管線
圖1係表示具有本發明之一實施形態之無機膜之積層體的剖面圖。
圖2係表示圖1所示之積層體之各層之折射率的剖面圖。
圖3係表示用於形成本發明之無機膜之裝置之一例之構成的圖。
一面參照圖式一面對使用本發明之一實施形態之無機膜的積層體進行說明。如圖1所示，依序將包含有機物之平坦化層12、包含無機材料之折射率梯度膜13a、包含無機材料之折射率梯度膜13b、及樹脂層14於基材11上積層一體化而構成積層體。此處，作為折射率梯度膜A之折射率梯度膜13a及作為折射率梯度膜B之折射率梯度膜13b構成本實施形態之無機膜13。
如圖2所示，於折射率梯度膜13a中，作為與平坦化層12接觸之面之折射率的n1連續地單調遞增至作為與折射率梯度膜13b接觸之面之折射率的n2。於折射率梯度膜13b中，作為與折射率梯度膜13a接觸之面之折射率的n3連續地單調遞減至作為與樹脂層14接觸之面之折射率的n4。此處，各層之折射率為n1<n2，且n3>n4。進而，折射率n2與折射率n3於本實施形態中相等，設為n2=n3。
但是，n2與n3之折射率差只要為0.1以下即可。於該情形時，可減小折射率梯度膜13a與折射率梯度膜13b之界面之折射率之變化。藉此，可抑制由折射率差所引起之反射，可抑制光線透過率之下降。以下，該情況更具體地進行說明。
折射率梯度膜13a及折射率梯度膜13b係功能性膜。於本實施形態中，作為功能，表現出較高之阻氣性。此處，所謂阻氣性係指具有充
分地降低二氧化碳、氧氣、水蒸氣等氣體之透過的特性。
於本實施形態中，折射率梯度膜13a及折射率梯度膜13b具有上述折射率連續地變化之構造。而且，於折射率梯度膜13a與折射率梯度膜13b之界面，兩者之折射率雖然某程度較高，但折射率差較小而為0.1以下。因此，可抑制由折射率差所引起之反射。此外，於折射率相對較高之界面附近，可充分地表現出上述阻氣性。
另一方面，於與界面相反之側、即折射率梯度膜13a及折射率梯度膜13b之外側之面，折射率降低。因此，可確保充分之透光性。
如上所述，於將折射率越高則阻氣性等功能越提高之折射率梯度膜13a、13b如上所示進行積層而成之無機膜中，可有效地提高折射率較高之部分之阻氣性。而且，由於n2與n3之差為0.1以下，故而亦可抑制兩者之界面之光線透過率之下降。
作為構成如上所述折射率越高則阻氣性越提高之折射率梯度膜13a及折射率梯度膜13b的無機材料之組合，只要表現出此種功能，則無特別限定。例如可列舉：氧化矽與鋅錫氧化物、氧化矽與鋁鋅氧化物、氧化鋁與鋅錫氧化物等。
於本實施形態之積層體中，於基材11上依序積層有平坦化層12、折射率梯度膜13a、折射率梯度膜13b、及樹脂層14。因此，可消除各層間之折射率之急遽變化。因此，可防止由折射率差所引起之反射。藉由該抗反射效果，可提高積層體之光線透過率。
將折射率梯度膜13a及13b之每單位膜厚之折射率變化率分別設為折射率變化率A=(n3-n2)/t1[t1=梯度膜A之膜厚，單位：nm]及折射率變化率B=(n4-n5)/t2[t2=梯度膜B之膜厚，單位：nm]時，較理想為折射率變化率X滿足0≦X<0.01/nm，更理想為滿足0≦X<0.006/nm。此處，於作為每單位膜厚之折射率變化的折射率變化率X超過0.01/nm之情形時，會產生由急遽之折射率變化所引起之光學干
涉，而變得無法獲得充分之透過率提高效果。
於將上述積層體之膜厚設為t之情形時，作為膜厚t之值之範圍，並無特別限定，為了獲得充分之阻氣性，較佳為30nm≦t≦3000nm，更佳為50nm≦t≦1000nm。
作為構成阻氣積層體之基材11之材料，並無特別限定，例如可列舉：聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、聚丙烯酸丁酯等丙烯酸系樹脂，聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、間苯二甲酸共聚物等聚酯系樹脂，聚乙烯系樹脂、聚丙烯系樹脂等聚烯烴系樹脂等。再者，合成樹脂可僅使用1種，亦可併用2種以上。
作為構成包含有機層之平坦化層12的材料，只要為可獲得表面之平滑性者，則無特別限定，例如可藉由如下方法而獲得：製作包含具有自由基聚合性基之烷氧基矽烷、不具有自由基聚合性基之烷氧基矽烷及水之組合物，塗佈該組合物後，對所塗佈之上述組合物照射活性能量線。
平坦化層之厚度較佳為0.01~100μm，更佳為0.1~50μm，尤佳為1~10μm。於厚度未達0.01μm之情形時，有不具有充分之阻氣性之虞。又，關於厚度超過100μm之平坦化層，有剛性過度增高而使阻氣性膜之操作性降低之虞。
折射率梯度膜13a係1)具有於膜厚方向上折射率連續地單調遞增之折射率梯度構造，2)於與平坦化層12之界面，平坦化層12之折射率n0及與平坦化層12接觸之面之折射率n1滿足n0≦n1之條件，3)如上所述折射率n2與折射率n3之差為0.1以下即可。
作為構成折射率梯度膜13a之材料，只要包含Si與Al中之至少一者、Zn、及Sn，則無特別限定。除該等材料以外，例如亦可包含：In、Ti、Mg、Zr、Ni、Ta、W、Cu或包含該等之2種以上的合金之氧化物或氮氧化物。就提昇高溫時之阻氣性之觀點而言，較佳為折射率
梯度膜13a包含含有Al、Zn及Sn之複合氧化物。
作為n1之值，為了減小其與有機物之n0之折射率差，較佳為1.7以下，尤佳為1.6以下。又，作為n2之值，並無特別限定，於為了獲得阻氣性而選擇材料之情形時，較佳為大於1.7之值，更佳為1.8以上。
折射率梯度膜13b係1)具有於膜厚方向上折射率連續地單調遞減之折射率梯度構造，2)於與樹脂層14之界面，與樹脂層14之折射率n5之面接觸之面之折射率n4滿足n4≧n5之條件，3)如上所述折射率n2與折射率n3之差為0.1以下即可。
作為構成折射率梯度膜13b之材料，只要包含Si與Al中之至少一者、Zn、及Sn，則無特別限定。除該等材料以外，例如亦可包含：In、Ti、Mg、Zr、Ni、Ta、W、Cu或包含該等之2種以上的合金之氧化物或氮氧化物。就提昇高溫時之阻氣性之觀點而言，較佳為折射率梯度膜13b包含含有Al、Zn及Sn之複合氧化物。
作為n4之值，為了減小其與作為有機物之樹脂層14之折射率n5之折射率差，較佳為1.7以下，尤佳為1.6以下。
再者，折射率梯度膜13a及折射率梯度膜13b可由相同材料構成，亦可由不同材料構成。又，亦可於折射率梯度膜13a與折射率梯度膜13b之間，形成折射率與n2或n3相等之功能性膜。即，折射率梯度膜13a與折射率梯度膜13b亦可經由功能性膜等而間接地積層。
於上述無機膜中，於折射率梯度膜13a之折射率為n2之側之面，可使折射率梯度膜13b自折射率為n3之面側如上所述間接地積層，又，亦可如上所示以直接接觸之方式積層。
作為樹脂層14，並無特別限定，只要包含有機物即可。作為樹脂層之功能，例如可列舉：平坦化、應力緩和、密接性提高、與其他構件之層壓。例如可列舉：乙烯-不飽和羧酸-丙烯酸酯共聚物、乙烯-
不飽和羧酸-甲基丙烯酸酯共聚物、熱塑性彈性體、低密度聚乙烯、乙烯-乙酸乙烯酯共聚物、聚偏二氯乙烯、離子聚合物、氯乙烯-乙酸乙烯酯共聚物、乙烯-乙烯醇共聚物、硝化纖維素、乙酸纖維素、聚矽氧、作為二異氰酸酯與聚醚多元醇之縮合物的聚醚-聚胺基甲酸酯、作為二異氰酸酯與聚酯多元醇之縮合物的聚酯-聚胺基甲酸酯等聚胺基甲酸酯系樹脂等。再者，層壓材料可僅使用1種，亦可併用2種以上。
其次，對折射率梯度膜13a及折射率梯度膜13b之形成方法進行說明。作為形成折射率梯度膜13a及折射率梯度膜13b之方法，並無特別限定，例如可列舉：濺鍍法、蒸鍍法、離子鍍著法等物理氣相沈積法(PVD，Physical Vapor Deposition)、或化學氣相沈積法(CVD，Chemical Vapor Deposition)等。於該等成膜方法中，只要以折射率連續地變化之方式改變成膜條件即可。藉此，可形成具有折射率梯度構造之折射率梯度膜13a及折射率梯度膜13b。折射率梯度膜13a及折射率梯度膜13b之形成方法可為相同方法，亦可使用不同方法。
再者，於上述實施形態中，折射率梯度膜13a及折射率梯度膜13b係發揮出阻氣性之功能膜，但本發明之功能膜之功能並不限定於阻氣性。即，可使用折射率較高且表現出各種功能之功能性膜。作為此種功能，例如可列舉透明導電膜等。導電性較高之折射率梯度膜例如可藉由使用InSnO、AlZnO等作為材料而構成。
於本發明中，如上所述於折射率梯度膜A及折射率梯度膜B中，以折射率自外側朝向兩者之界面增高之方式使折射率梯度，兩者之界面之折射率差較小而為0.1以下，因而於外側表面，可藉由較低之折射率而確保充分之透光性。又，於兩者之界面附近，由於n2與n3之差、即折射率差較小，並且折射率n2、n3本身較高，故而可表現出良好之功能，並且抑制光線透過率之下降。
作為本發明之一應用例，可列舉SiZnSnO阻氣膜。作為折射率梯度膜A及折射率梯度膜B，以折射率自外側朝向兩者之界面增高之方式使折射率梯度，使SiZnSnO膜中之Si含量以朝向兩者之界面連續地減少之方式變化而形成SiZnSnO膜。
於SiZnSnO阻氣膜中，為了獲得較高之阻氣性、彎曲性，較佳為Sn相對於Zn與Sn之總和的重量比Xs滿足70>Xs>0，更佳為滿足50≧Xs>0，進而較佳為滿足30>Xs≧5，最佳為滿足10≧Xs≧5。
作為本發明之另一應用例，可列舉AlZnSnO阻氣膜。作為折射率梯度膜A及折射率梯度膜B，以折射率自外側朝向兩者之界面增高之方式使折射率梯度，使AlZnSnO膜中之Al含量以朝向兩者之界面連續地減少之方式變化而形成AlZnSnO膜。
又，於AlZnSnO阻氣膜中，為了獲得較高之阻氣性、彎曲性，較佳為Sn相對於Zn與Sn之總和的重量比Xs滿足50≧Xs>0，更佳為滿足50>Xs>0，進而較佳為滿足30≧Xs>0，最佳為滿足30≧Xs≧10。
於本發明中，亦可使用AlZnSnO阻氣膜作為折射率梯度膜A，使用SiZnSnO阻氣膜作為折射率梯度膜B。於該情形時，係以折射率自外側朝向兩者之界面增高之方式使折射率梯度，使SiZnSnO膜中之Si含量或AlZnSnO膜中之Al含量以朝向兩者之界面連續地減少之方式變化而形成。但於本發明中，亦可使用SiZnSnO阻氣膜作為折射率梯度膜A，使用AlZnSnO阻氣膜作為折射率梯度膜B。
繼而，說明本發明之實施例，但本發明並不限定於下述實施例。
(實施例1)
製作障壁膜作為積層體。障壁膜之基材係使用PET(polyethylene terephthalate，聚對苯二甲酸乙二酯)膜(Toray公司製造，商品名：
「Lumirror 50T60」)。
≪平坦化層之形成≫
其次，向包含3-甲基丙烯醯氧基丙基三甲基矽烷80重量份、四乙氧基矽烷53重量份、四丁醇鈦30重量份及水4.9重量份之組合物中，添加2-甲基-1-[4-(甲硫基)苯基]-2-嗎啉基丙烷-1-酮(Ciba Specialty Chemicals公司製造，商品名：「Irgacure 907」)0.1重量份，使用9W之紫外線燈照射紫外線15分鐘而進行預聚合。藉由利用凹版塗佈機將該組合物塗佈於上述基材之一面，並使用電子束照射裝置(ESI公司製造，製品名：「EC300/165/800」)，於加速電壓175kV、照射線量150kGy之條件下對所塗佈之組合物照射電子束，進行3-甲基丙烯醯氧基丙基三甲基矽烷之自由基聚合而形成自由基聚合物，其後藉由將於一面具有照射過電子束之組合物的聚對苯二甲酸乙二酯膜於45℃、相對濕度65%RH之環境下放置1小時，促進水解及脫水縮合反應，而形成使上述自由基聚合物之主鏈間進行交聯的四乙氧基矽烷之脫水縮合物，從而獲得平坦化層(厚度8μm)。
≪無機膜之形成方法≫
使用圖3所示之卷對卷濺鍍裝置31形成阻氣層。本裝置包含捲出捲取室32與成膜室40。捲出捲取室32具備捲出軸33、捲取軸34、導輥35及36、及筒輥37，利用真空泵38進行排氣而成為減壓狀態。於捲出軸33上安裝成為基材之坯膜，自坯膜所捲出之基材膜30係經由導輥35、筒輥37及導輥36而捲取於捲取軸34上。又，成膜室40具備靶41及42，且連接於雙極電源43。利用該雙極電源43，可向靶41與靶42交替地供給脈衝電源。進而，成膜室40連接有氬氣供給管線44與氧氣供給管線45，可向成膜室40內供給氬氣及氧氣。成膜室40亦連接有真空泵39，可對成膜室內進行減壓。藉由對成膜室40進行減壓後，以特定流量供給氬氣及氧氣，進而向靶41、靶42供給電力，可於該靶與筒輥37
間之空間形成電漿。藉由該電漿而使構成靶41及靶42之材料自該靶表面射出。而且，所射出之材料堆積於通過筒輥37面上之基材表面，而形成薄膜。雙極電源43可任意地控制供給至靶41與靶42之脈衝頻率。藉由控制脈衝頻率，可控制自靶41表面射出且堆積於基材上之材料之量與自靶42表面射出且堆積於基材膜30上之材料之量的比。於選擇不同材料作為靶41與靶42之情形時，藉由控制脈衝頻率，可控制堆積於基材膜30上之合金氧化物之組成。
≪折射率梯度膜A之形成≫
將單面形成有平坦化層之基材膜設置於捲出軸33，進而安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=70：30wt%)靶作為靶42。利用真空泵38及真空泵39對卷對卷濺鍍裝置31進行排氣，將其減壓至3.0×10-4Pa。其後，一面將基材膜自捲出軸33以通過導輥35、筒輥37、導輥36之路徑向捲取軸34之方向搬送，一面於成膜室40內於以下所示之條件下於平坦化層上形成SiZnSnO薄膜，而獲得折射率梯度膜A。
(成膜條件A)
基材搬送速度：0.1m/min，張力100N，筒輥冷卻溫度：10℃
氬氣流量：80sccm，氧氣流量：80sccm
電源輸出：5kW，電力脈衝比：靶41：靶42=3：1
≪折射率梯度膜B之形成≫
其次，一面將形成有折射率梯度膜A且捲取於捲取軸34之基材膜自捲取軸34向捲出軸33之方向搬送，一面於成膜條件A所示之條件下於折射率梯度膜A之表面形成SiZnSnO膜，而獲得折射率梯度膜B。
≪樹脂層之形成≫
於折射率梯度膜B之表面貼附黏著材料(積水化學工業公司製造，商品名：「Double Tack Tape」，產品編號：5405A，厚度50μm)，獲得樹脂層。
≪耐候性樹脂基材之貼合≫
貼附黏著材料後，與ETFE(四氟乙烯與乙烯之共聚物)膜(旭硝子公司製造，商品名：「Aflex」，厚度100μm)貼合而製作阻氣膜1。
(實施例2)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，將基材膜搬送條件設為0.075m/min，除此以外，以與實施例1相同之方式製作阻氣膜2。
(實施例3)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，將基材膜搬送條件設為0.2m/min，除此以外，以與實施例1相同之方式製作阻氣膜3。
(實施例4)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=90：10wt%)靶作為靶42，除此以外，以與實施例1相同之方式製作阻氣膜4。
(實施例5)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=95：5wt%)靶作為靶42，除此以外，以與實施例1相同之方式製作阻氣膜5。
(實施例6)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=30：70wt%)靶作為靶42，除此以外，以與實施例1相同之方式製作阻氣膜6。
(實施例7)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Al作為靶41，安裝ZnSn合金(Zn：Sn=70：30wt%)靶作為靶42，將基材膜
搬送條件設為0.05m/min，除此以外，以與實施例1相同之方式製作阻氣膜7。
(實施例8)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Al作為靶41，安裝ZnSn合金(Zn：Sn=90：10wt%)靶作為靶42，將基材膜搬送條件設為0.05m/min，除此以外，以與實施例1相同之方式製作阻氣膜8。
(實施例9)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Al作為靶41，安裝ZnSn合金(Zn：Sn=50：50wt%)靶作為靶42，將基材膜搬送條件設為0.05m/min，除此以外，以與實施例1相同之方式製作阻氣膜9。
(實施例10)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，將基材膜搬送條件設為0.15m/min，除此以外，以與實施例1相同之方式製作阻氣膜10。
(實施例11)
於折射率梯度膜A及折射率梯度膜B之成膜條件A下，安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=50：50wt%)靶作為靶42，除此以外，以與實施例1相同之方式製作阻氣膜11。
(實施例12)
於折射率梯度膜A之成膜條件A下，安裝Al作為靶41，安裝ZnSn合金(Zn：Sn=90：10wt%)靶作為靶42，將基材膜搬送條件設為0.05m/min，進而於折射率梯度膜B之成膜條件A下，安裝Si作為靶41，安裝ZnSn合金(Zn：Sn=90：10wt%)靶作為靶42，將基材膜搬送條件設為0.15m/min，除此以外，以與實施例1相同之方式製作阻氣膜12。
(比較例1)
安裝ZnSn合金(Zn：Sn=70：30wt%)作為靶41及靶42。於成膜條件B所示之條件下於平坦化層上形成ZnSnO膜作為阻氣層，而製作阻氣膜13。
(成膜條件B)
基材搬送速度：0.1m/min，張力100N，筒輥冷卻溫度：10℃
氬氣流量：80sccm，氧氣流量：80sccm
電源輸出：5kW，電力脈衝比：靶：靶=1：1
(阻氣性)
為了對所獲得之阻氣膜之阻氣性進行評估，利用差壓式透濕度測定裝置(GTR Tech公司製造，產品編號：GTR-300XASC)於40℃、90%之條件下測定水蒸氣透過率。
(透明性)
關於阻氣膜之透明性之評估，利用霧度計(東洋精機製作所公司製造，商品名：「HAZE GUARD 2」)，基於JIS K7361而測定全光線透過率。
(彎曲性)
阻氣膜之彎曲性係基於JIS C5016所示之耐彎曲性試驗而進行。將所獲得之阻氣膜以彎曲半徑成為5mm之方式固定於耐彎曲性試驗裝置之固定板與可動板上，行程設為120mm，反覆彎曲次數設為10000次而進行試驗，根據試驗後之水蒸氣透過率進行評估。
(折射率)
阻氣膜之各層之折射率係利用反射分光膜厚計(大塚電子公司製造，FE-3000)進行測定。
(Sn比率之測定)
對試樣表面蒸鍍碳後，利用FIB(focused ion beam，聚焦離子束)
製作薄膜切片，利用穿透型電子顯微鏡FE-TEM(Field Emission-Transmission Electron Microscopy，場發射穿透式電子顯微鏡)(日本電子公司製造：JEM-2010FEF)並藉由EDS(Energy Dispersive X-ray Spectroscopy，能量分散X射線譜)射線分析而進行測定。
(評估結果)
將阻氣性、透明性、彎曲性評估結果示於表1及表2。
[阻氣性評估基準]
水蒸氣透過率：WVTR(g/m2/day)
WVTR<1.0×10-3 A
1.0×10-3≦WVTR<5.0×10-3 B
5.0×10-3≦WVTR<1.0×10-2 C
WVTR≧1.0×10-2 D
[彎曲性評估基準]
耐彎曲性試驗後之水蒸氣透過率：B-WVTR(g/m2/day)
B-WVTR<1.0×10-3 A
1.0×10-3≦B-WVTR<5.0×10-3 B
5.0×10-3≦B-WVTR<1.0×10-2 C
B-WVTR≧1.0×10-2 D
根據實施例，由於為具有折射率梯度構造之無機膜，故而可獲得與比較例(單層膜)相比透明性更高之阻氣膜。進而，藉由將Sn相對於SiZnSnO膜中所含之Zn與Sn之總和的比率：Xs(wt%)設為70>Xs>0，可獲得阻氣性較高之阻氣膜。
12‧‧‧平坦化層
13a‧‧‧折射率梯度膜
13b‧‧‧折射率梯度膜
14‧‧‧樹脂層
Claims (7)
- 一種無機膜，其具備：折射率梯度膜A，其包含無機材料，自一面朝向另一面，折射率自n1連續地變化至n2(n1<n2)且為功能性膜；及折射率梯度膜B，其包含無機材料，自一面朝向另一面，折射率自n3連續地變化至n4(n4<n3)且為功能性膜；於折射率梯度膜A之折射率為n2之側之面，以自上述折射率為n3之面側直接或間接地接觸之方式積層有折射率梯度膜B，n2與n3之差為0.1以下；並且上述無機材料為包含Si與Al中之至少一者、Zn、及Sn之複合氧化物。
- 如請求項1之無機膜，其中上述折射率梯度膜A與折射率梯度膜B中之至少一者包含含有Si、Zn及Sn之複合氧化物。
- 如請求項2之無機膜，其中於上述包含Si、Zn及Sn之複合氧化物中，Sn相對於Zn與Sn之總和之比Xs滿足70>Xs>0。
- 如請求項1之無機膜，其中上述折射率梯度膜A與折射率梯度膜B中之至少一者包含含有Al、Zn及Sn之複合氧化物。
- 如請求項1之無機膜，其中上述折射率梯度膜A包含含有Al、Zn及Sn之複合氧化物，上述折射率梯度膜B包含含有Si、Zn及Sn之複合氧化物。
- 一種積層體，其係於有機膜上形成有如請求項1至5中任一項之無機膜，且將有機膜之折射率設為n0時，n0≦n1。
- 如請求項6之積層體，其中於上述無機膜上形成有樹脂層，且將樹脂層之折射率設為n5時，n4≧n5。
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| JP2010137447A (ja) * | 2008-12-12 | 2010-06-24 | Toyobo Co Ltd | 透明導電性積層フィルム |
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| US4440822A (en) * | 1977-04-04 | 1984-04-03 | Gordon Roy G | Non-iridescent glass structures |
| US5168003A (en) * | 1991-06-24 | 1992-12-01 | Ford Motor Company | Step gradient anti-iridescent coatings |
| JPH0741337A (ja) * | 1993-07-30 | 1995-02-10 | Glaverbel Sa | 光彩防止透明体 |
| DE10200760A1 (de) | 2002-01-10 | 2003-07-24 | Clariant Gmbh | Nanokompositmaterial zur Herstellung von Brechzahlgradientenfolien |
| JP5045148B2 (ja) | 2006-04-27 | 2012-10-10 | セイコーエプソン株式会社 | プラスチック偏光レンズ |
| CN101432638A (zh) | 2006-04-27 | 2009-05-13 | 精工爱普生株式会社 | 塑料偏振透镜 |
| DE102007019994A1 (de) | 2007-04-27 | 2008-10-30 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Transparente Barrierefolie und Verfahren zum Herstellen derselben |
| CN101493533B (zh) * | 2009-02-11 | 2011-03-30 | 广东东邦科技有限公司 | 一种反射型防眩性偏光片、其专用涂层及其制备方法 |
| CN101866956B (zh) | 2009-04-16 | 2013-02-06 | 北京北方微电子基地设备工艺研究中心有限责任公司 | 一种减反射膜及其制备方法 |
| JP5779863B2 (ja) | 2009-11-30 | 2015-09-16 | 大日本印刷株式会社 | 光学フィルムの製造方法、光学フィルム、偏光板及びディスプレイ |
-
2014
- 2014-06-27 US US14/653,774 patent/US9844926B2/en active Active
- 2014-06-27 CN CN201480003177.5A patent/CN104812570B/zh active Active
- 2014-06-27 WO PCT/JP2014/067187 patent/WO2015002089A1/ja not_active Ceased
- 2014-06-27 JP JP2014538950A patent/JP5667732B1/ja active Active
- 2014-06-27 KR KR1020177004468A patent/KR20170021900A/ko not_active Withdrawn
- 2014-06-27 KR KR1020157016576A patent/KR101775252B1/ko active Active
- 2014-07-01 TW TW103122698A patent/TWI558571B/zh active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05193995A (ja) * | 1991-06-24 | 1993-08-03 | Ford Motor Co | 傾斜屈折率を有する虹色防止被覆透明嵌込み窓ガラス物品 |
| US20080310019A1 (en) * | 2007-06-14 | 2008-12-18 | Yoon-Sung Um | Refractive index decrement film, polarizing member having the same and display device having the same |
| JP2010137447A (ja) * | 2008-12-12 | 2010-06-24 | Toyobo Co Ltd | 透明導電性積層フィルム |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2015002089A1 (ja) | 2017-02-23 |
| US9844926B2 (en) | 2017-12-19 |
| KR20170021900A (ko) | 2017-02-28 |
| JP5667732B1 (ja) | 2015-02-12 |
| TW201518113A (zh) | 2015-05-16 |
| WO2015002089A1 (ja) | 2015-01-08 |
| KR101775252B1 (ko) | 2017-09-05 |
| KR20160028995A (ko) | 2016-03-14 |
| CN104812570B (zh) | 2017-03-15 |
| US20150321455A1 (en) | 2015-11-12 |
| CN104812570A (zh) | 2015-07-29 |
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