JP6754427B2 - 有機/無機複合素材の薄膜基板 - Google Patents
有機/無機複合素材の薄膜基板 Download PDFInfo
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- JP6754427B2 JP6754427B2 JP2018522936A JP2018522936A JP6754427B2 JP 6754427 B2 JP6754427 B2 JP 6754427B2 JP 2018522936 A JP2018522936 A JP 2018522936A JP 2018522936 A JP2018522936 A JP 2018522936A JP 6754427 B2 JP6754427 B2 JP 6754427B2
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- organic
- thin film
- composite material
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- inorganic composite
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- 239000000758 substrate Substances 0.000 title claims description 55
- 239000010409 thin film Substances 0.000 title claims description 46
- 229910003471 inorganic composite material Inorganic materials 0.000 title claims description 28
- 239000002245 particle Substances 0.000 claims description 60
- 239000010408 film Substances 0.000 claims description 55
- 239000002086 nanomaterial Substances 0.000 claims description 50
- 239000011247 coating layer Substances 0.000 claims description 40
- 239000010410 layer Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 28
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- -1 3- (trimethoxysilyl) propyl vinylcarbamate Chemical compound 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
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- 229920001187 thermosetting polymer Polymers 0.000 claims description 6
- 125000000524 functional group Chemical group 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
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- 150000004706 metal oxides Chemical class 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
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- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 239000003575 carbonaceous material Substances 0.000 claims description 4
- 150000002736 metal compounds Chemical class 0.000 claims description 4
- 239000002987 primer (paints) Substances 0.000 claims description 4
- 229910003437 indium oxide Inorganic materials 0.000 claims description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 3
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 claims description 2
- VXCWFNCPUBWGJG-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid zirconium Chemical compound [Zr].OC(=O)CCOC(=O)C=C.OC(=O)CCOC(=O)C=C.OC(=O)CCOC(=O)C=C.OC(=O)CCOC(=O)C=C VXCWFNCPUBWGJG-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- AWGVROXZUWZNIG-UHFFFAOYSA-N hafnium;3-prop-2-enoyloxypropanoic acid Chemical compound [Hf].OC(=O)CCOC(=O)C=C AWGVROXZUWZNIG-UHFFFAOYSA-N 0.000 claims description 2
- 239000012788 optical film Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920006254 polymer film Polymers 0.000 claims description 2
- CXNQUHPJUJGOHC-UHFFFAOYSA-J prop-2-enoate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C CXNQUHPJUJGOHC-UHFFFAOYSA-J 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- OTYBJBJYBGWBHB-UHFFFAOYSA-N trimethylsilyl prop-2-enoate Chemical compound C[Si](C)(C)OC(=O)C=C OTYBJBJYBGWBHB-UHFFFAOYSA-N 0.000 claims description 2
- XKMZOFXGLBYJLS-UHFFFAOYSA-L zinc;prop-2-enoate Chemical compound [Zn+2].[O-]C(=O)C=C.[O-]C(=O)C=C XKMZOFXGLBYJLS-UHFFFAOYSA-L 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims 1
- 229920003023 plastic Polymers 0.000 claims 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 description 28
- 229910010272 inorganic material Inorganic materials 0.000 description 22
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 239000010954 inorganic particle Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000007740 vapor deposition Methods 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 6
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- 230000017525 heat dissipation Effects 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 150000002576 ketones Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 239000002390 adhesive tape Substances 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- 239000003054 catalyst Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 3
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- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 2
- BYCNMZYQCQZYLG-UHFFFAOYSA-N 2,2-dimethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1.C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 BYCNMZYQCQZYLG-UHFFFAOYSA-N 0.000 description 2
- FDSUVTROAWLVJA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)COCC(CO)(CO)CO FDSUVTROAWLVJA-UHFFFAOYSA-N 0.000 description 2
- NJWGQARXZDRHCD-UHFFFAOYSA-N 2-methylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC=C3C(=O)C2=C1 NJWGQARXZDRHCD-UHFFFAOYSA-N 0.000 description 2
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 2
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 2
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- QDVNNDYBCWZVTI-UHFFFAOYSA-N bis[4-(ethylamino)phenyl]methanone Chemical compound C1=CC(NCC)=CC=C1C(=O)C1=CC=C(NCC)C=C1 QDVNNDYBCWZVTI-UHFFFAOYSA-N 0.000 description 1
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Description
ITOベースフィルム(ITO Base Film)は、スパッタリング工程を介して基材上にITOをバッファ層なしで直接蒸着する場合、ITO蒸着層と基材間の互いに異なる熱膨張率と屈折率によりITO蒸着層が剥離したり、蒸着されたフィルムの永久的な変形が発生したり、屈折率の不一致により視認性が低下したりする。
ガス遮断性バリアフィルムは、気体の透過度を下げるために、アルミニウムとハードコート層などを蒸着またはコーティングした後、これらを貼り合わせた構造のフィルムが主流をなしている。このような構造のフィルムは、蒸着、コーティング及び貼り合わせなどの複雑な工程が必要でありフィルムの単価を高める原因となるので、これらの工程を単純化することが可能なフィルムの組成及び製造方法の研究が急がれている。
このような強化ガラスは、圧縮強度、曲げ強度及び耐衝撃性は比較的強いものの、重く、外部からの衝撃及び熱衝撃による破損が発生しやすく、弾性変形率が非常に小さいガラスの特性上、フレキシブルディスプレイ(Flexible Display)には適用できないという問題がある。そこで、強化ガラスを代替することが可能な素材の研究が急がれている。
壊れないうえ、柔軟性に優れてフレキシブルディスプレイ(Flexible Display)にも適用可能なフィルムを提供し、
誘電率及び放熱性にも従来のガラスより優れるうえ、重さが軽くて軽量化も可能なフィルムを提供し、
膜厚が薄いながらも、指紋防止やUVカットなどの機能性を複合化してディスプレイの表面スクラッチを防止するためのフィルムを提供し、
ITOなどの酸化物層の蒸着により発生する内部応力の解消及び屈折率不一致の緩和のためのフィルムを提供し、
切断及び裁断作業が容易であり、ロール・ツー・ロール(Roll−to−Roll)の連続工程で製造が可能なフィルムを提供することを目的とする。
上部表面及び下部表面を含む基材と、
前記基材の前記上部表面及び前記下部表面の少なくとも一つにコーティングされ、ナノ素材粒子または表面処理されたナノ素材粒子からなる有機/無機層を形成するコーティング層と、
前記コーティングされたコーティング層の背面に備えられる接着層と、を含んでなる。
UV硬化型樹脂の官能基の例としては、図3及び図4に示すように、アクリル基、ウレタン基、ビニル基、アリル基などがあり、この中でも、アクリレートなどの不飽和二重結合を有するものが挙げられ、またはエポキシ基、シラノール基などの反応性置換基を有するも使用可能である。
このようなコーティング層の組成物が、多官能性アクリレートモノマーを含むと、コーティング層の組成物の無機粒子を有機媒体によく分散させて無機粒子の凝集を予防して沈殿を防止し、モノマー、オリゴマー、無機物が均一に混合されて光学特性及び表面硬度に優れたハードコート剤を提供する。
上記の群から選ばれた1種以上の化合物である光開始剤は、0.1〜5.0重量%、好ましくは0.5〜2重量%の含量で使用することができ、これにより、コーティング膜内の結合を最小化する効果をさらに期待することができる。
また、表面処理されたナノ素材粒子としては、表面処理されたAl2O3、ZnO、TiO2、SiO2を含む金属酸化物、金属化合物、グラフェン、CNTを含む炭素系物質及び金属素材のうちの少なくとも一つを挙げることができる。
金属ナノワイヤーを添加する場合、硬化後のフィルム内で伝導性ネットワークを形成してフィルムに導電性を与えるとともに、機械的にフレキシブルな特性を提供することができ、
ナノワイヤー形状の特徴により、粒子に比べて導電性フィルムの面抵抗を著しく下げることができるという効果があり、
金属酸化物系アルミナの添加の際に、アルミナが持つ優れた熱伝導性によりハードコートフィルムの熱伝導度が向上し、これらの粒子が補強材(Filler)として作用して表面硬度が向上し、
チタニア及びジルコニアを添加する場合には、これらの粒子が持つ高屈折特性により、高屈折層の厚さを減少できるという特徴があり、
シリカを添加する場合には、光学的に透明な特性を示すとともに硬度を向上させることができ、中空球シリカを使用するとき、これらの粒子の内部に生成された気孔により断熱効果及び低誘電率を与えることができる。
CNTを添加する場合には、表面抵抗が低くなって電気的特性が向上し、ガス遮断性が向上して水分と酸素に対するガス遮断性能を向上させることができ、
グラフェンを添加する場合には、フィルムを伸ばしたり曲げたりしても電気的性質が変わらないため、機械的にフレキシブルな特性及び優れた電気的特性を示すとともに、光学的特性にも優れるという利点があり、
ダイヤモンドを添加する場合には、ダイヤモンド(〜5ev)の広いバンドギャップが可視光線及び近赤外線の範囲で透明な特性を示し、フィルムの硬度を向上させることができる。
粒度が100nmを超えると、ハードコートフィルムの製造後にヘイズが上昇して光学的に透明でなくなり、鉛筆硬度改善の効果が低下する。無機素材粒子はゾル形態が最も好ましく、このような製品は、技術分野でよく知られている方法で製造することもでき、市販の様々な種類の溶媒に分散している適切なゾルを使用することもでき、ハードコート組成物に均一に分散できるゾルを選択して使用することもできる。
表面処理剤としては、3−(トリメトキシシリル)プロピルビニルカルバメート、3−(トリメトキシシリル)プロピルアクリレート、3−(トリメトキシシリル)プロピルメタクリレート、トリメチルシリルアクリレート、3−(2,3−エポキシプロポキシ)プロピルトリメトキシシラン、3−(2,3−エポキシプロピロキシ)プロピルトリエトキシシラン、アクリル酸亜鉛、アクリル酸ジルコニウム、ジルコニウムカルボキシエチルアクリレート、ハフニウムカルボキシエチルアクリレート、2−(ジメチルアミノ)エチルアクリレートなどよりなる群から選ばれる1種以上が挙げられるが、これに限定されるものではなく、前記化合物以外にも、公知の表面処理剤を使用することができる。
また、前記基材は、光学フィルム、高分子フィルム、シリコンウエハー、サファイアウエハー、PCB基板及び金属基板よりなる群から選ばれる1種以上を含む基材を使用することができる。また、基材の厚さは、10nm以上1mm以下であり、より好ましくは1μm以上500μm以下である。
さらに、前記表面処理されたナノ素材コーティング層をコーティングする段階の前に、前記基材の前記上部表面及び前記下部表面の少なくとも一つに接着剤を塗布する段階をさらに含むことができる。
また、図8及び図9に示すように、有機/無機層をサンドイッチ形式でオーバーコーティングすることも可能である。
前記コーティング層のナノ素材粒子または表面処理されたナノ素材粒子のサイズは、1nm以上200nm以下であることが好ましい。これは下記の実施例でより具体的に説明する。
100mlの無水エタノール(Anhydrous Ethanol)(C2H5OH)を250mlの三口フラスコに入れ、ここにAIP(Aluminum Isopropoixde、Al[OCH(CH3)2])を2.5g投入し、メカニカルスターラー(Mechanical Stirrer)を用いて400rpmにて室温で3時間攪拌させることにより、0.12M AIP溶液を製造する。メカニカルスターラー(Mechanical Stirrer)を用いて400rpmで攪拌されている0.12M AIP溶液に0.07〜0.21M NH4OH0.52mlを滴下し、4時間常温で反応させて合成する。合成された粉末を濾過洗浄した後、乾燥させて熱処理によって20〜60nm級のアルミナ粒子を製造した。
製造例1で製造された無機粒子を5時間フライス加工(milling)して無機粒子分散溶液を準備する。このとき、分散溶媒としてイソプロピルアルコール(Isopropyl Alcohol)などのアルコール有機溶媒を用いて、下記表2の如く分散溶液を製造した。
製造例2で製造された無機素材粒子分散液に表面処理剤を表3に示すように入れ、常温で3時間反応して製造した。BYK社製の分散剤を表面処理された無機素材粒子に対して10%添加して5時間ナノミルを用いて30%表面処理されたナノ素材分散液を下記表3の如く製造した。
分光光度計(日本、日本電色工業製、NDH700)を用いて、全光線透過率(Total Transmittance)及びヘイズ(Haze)を測定した。
2)反射率測定
分光色測計(CM−5)を用いて反射率を測定した。
3)鉛筆硬度
ASTM D3502測定法に従って鉛筆硬度試験機を用いて750gの荷重をかけ、鉛筆硬度を測定した。
実施例及び比較例で得られたナノ無機素材粒子結晶薄膜フィルムのコーティング層を表側にして、反対面を、両面テープを貼付した厚さ5mmのガラス板に貼付した。次いで、コート層を貫通して、基材フィルムに到達する100個の碁盤目状の切開線を、隙間間隔2mmのカッターガイドを用いて入れた。その後、粘着テープ(ニチバン社製、405番;幅24mm)を碁盤目状の切開面に貼付した。貼付の際に、界面に残った空気を消しゴムで押して完全に接着させた後、粘着テープを勢いよく垂直に引き離して、次の式から接着性を目視で求めた。また、1つの碁盤目内で部分的に剥離しているものも、剥離した個数に含ませた。
接着性(%)=(1−碁盤目の剥離した個数/100個)×100
接着性(%)が90〜100%である場合には◎とし、
接着性(%)が80〜89%である場合には○とし、
接着性(%)が0〜79%である場合には×とした。
コーティング層に対して、製造例3−1で製造した表面処理された無機素材粒子の固形分含量を50重量%、有機バインダーの固形分含量を50重量%(有機バインダーとしては、オリゴマー、6官能基モノマー及び4官能基モノマーを使用)、及び光開始剤である2,2−ジメトキシ−1,2−ジフェニルエタノン(2,2−dimethoxy−1,2−diphenyl ethanone)を1重量%含有して、30%表面処理されたナノ無機素材粒子結晶薄膜コーティング剤を下記表4のとおりに製造した。
PETフィルム上に前記コーティング剤を塗布して50℃で乾燥させた後、高圧水銀ランプ(0.5J/cm2)を用いて空気中でUV硬化させ、表面処理されたナノ無機素材粒子結晶薄膜を下記表4のとおりに製造した。
表3で製造した製造例3−2ないし3−14をそれぞれ使用した以外は実施例1と同様にして、下記表4のとおりに製造した。
製造例2で製造したナノ素材粒子分散液2−1ないし2−8をそれぞれ使用した以外は実施例1と同様にして、下記表4のとおりに製造した。
透明PIフィルムを使用した以外は実施例1ないし14と同様にして、下記表5のとおりに製造した。
透明PIフィルムを使用した以外は比較例1ないし8と同様にして、下記表5のとおりに製造した。
コーティング層に対して、製造例3−1で製造した表面処理された無機素材粒子の固形分含量を14重量%、有機バインダーの固形分含量を86重量%(有機バインダーとしては、オリゴマー、6官能基モノマー及び4官能基モノマーを使用)、及び光開始剤である2,2−ジメトキシ−1,2−ジフェニルエタノン(2,2−dimethoxy−1,2−diphenyl ethanone)を1重量%含有して、30%表面処理されたナノ無機素材粒子結晶薄膜コーティング剤を製造した。
透明PIフィルム上に前記コーティング剤を塗布して50℃で乾燥させた後、高圧水銀ランプ(0.5J/cm2)を用いて空気中でUV硬化させて、表面処理されたナノ無機素材粒子結晶薄膜を下記表6のとおりに製造した。
表3で製造した製造例3−2ないし3−14をそれぞれ使用した以外は実施例29と同様にして、下記表6のとおりに製造した。
製造例2で製造したナノ素材粒子分散液2−1ないし2−8をそれぞれ使用した以外は実施例29と同様にして、下記表6のとおりに製造した。
実施例1ないし42は、比較例1ないし24に比べてコーティング膜の厚さを薄く構成することができ、光透過率を向上させることができ、ヘイズ及び反射率の減少に効果的な特徴を示す。また、鉛筆硬度及び接着性に優れるうえ、熱伝導率が向上する効果を奏することができる。
20 コーティング層
21 有機/無機層1
21’ 有機/無機層2
21” 有機/無機層3
22 有機層
23 表面処理された無機層または無機層
30 接着層
40 接着層または粘着及びUVカット層
Claims (17)
- 上部表面及び下部表面を含む基材と、
前記基材の上部表面、下部表面またはこれらの両方にコーティングされ、表面処理剤で表面処理されたナノ素材粒子からなる有機/無機層を形成するコーティング層と、
前記コーティングされたコーティング層の背面に備えられる接着層と、を含んでなり、
前記コーティング層の組成物は、多官能性アクリレートモノマー及びオリゴマーを含む硬化型樹脂をさらに含み、
前記多官能性アクリレートモノマー及びオリゴマーの混合重量比は、6官能基50.0〜70.0重量%、3または4官能基15.0〜30.0重量%、アクリレートオリゴマー15.0〜30.0重量%であり、
前記多官能性アクリレートモノマー、オリゴマー及び前記ナノ素材粒子中の前記ナノ素材粒子の含有量は14〜50重量%であることを特徴とする、有機/無機複合素材の薄膜基板。 - 前記ナノ素材粒子は、Al2O3、ZnO、TiO2及びSiO2の少なくとも一つを含む金属酸化物、金属化合物、グラフェン及びCNTの少なくとも一つを含む炭素系物質、並びに金属素材からなる群より選ばれる少なくとも一つを含むことを特徴とする、請求項1に記載の有機/無機複合素材の薄膜基板。
- 前記ナノ素材粒子は、表面処理されたAl2O3、ZnO、TiO2及びSiO2の少なくとも一つを含む金属酸化物、金属化合物、グラフェン及びCNTの少なくとも一つを含む炭素系物質、並びに金属素材からなる群より選ばれる少なくとも一つを含んでなり、
前記基材と表面処理されたナノ素材コーティング層との間にはプライマーコーティング層がさらに備えられ、
前記プライマーコーティング層は、熱硬化性アクリル系樹脂、熱硬化性エポキシ樹脂、熱硬化性ウレタン樹脂及びUV硬化性樹脂からなる群より選ばれる少なくとも一つを含んでなり、
また、前記基材は、光学フィルム、高分子フィルム、シリコンウエハー、サファイアウエハー、PCB基板及び金属基板よりなる群から選ばれる1種以上を含んでなることを特徴とする、請求項1に記載の有機/無機複合素材の薄膜基板。 - 前記ナノ素材粒子は、アルミナ、チタニア、ジルコニア、シリカ、酸化インジウム、酸化スズ及び酸化亜鉛のうちのいずれか一つまたは2つ以上の混合物からなることを特徴とする、請求項2に記載の有機/無機複合素材の薄膜基板。
- 前記表面処理されたナノ素材粒子に含まれる表面処理剤は、3−(トリメトキシシリル)プロピルビニルカルバメート、3−(トリメトキシシリル)プロピルアクリレート、3−(トリメトキシシリル)プロピルメタクリレート、トリメチルシリルアクリレート、3−(2,3−エポキシプロポキシ)プロピルトリメトキシシラン、3−(2,3−エポキシプロピロキシ)プロピルトリエトキシシラン、アクリル酸亜鉛、アクリル酸ジルコニウム、ジルコニウムカルボキシエチルアクリレート、ハフニウムカルボキシエチルアクリレート、及び2−(ジメチルアミノ)エチルアクリレートよりなる群から選ばれる1種以上からなることを特徴とする、請求項3に記載の有機/無機複合素材の薄膜基板。
- 前記コーティング層は、前記基材の上部表面、下部表面またはこれらの両方に少なくとも1回積層されてコーティングされることを特徴とする、請求項1に記載の有機/無機複合素材の薄膜基板。
- 前記コーティング層は、硬化後の膜厚が1nm以上300μm以下であることを特徴とする、請求項1に記載の有機/無機複合素材の薄膜基板。
- 前記コーティング層のナノ素材粒子または表面処理されたナノ素材粒子のサイズは、1nm以上200nm以下であることを特徴とする、請求項1に記載の有機/無機複合素材の薄膜基板。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含むプリント回路基板。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含むガラス基板。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含むディスプレイ用フィルム。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含む保護フィルム。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含む電子製品。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含むプラスチック基板。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含む電子パッケージモジュール。
- 請求項1ないし請求項8のいずれか1項に記載の有機/無機複合素材の薄膜基板を含む自動車製品。
- 請求項1ないし請求項8のいずれか一項に記載の有機/無機複合素材の薄膜基板を含むディスプレイ用素子。
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