JP6461860B2 - 透明導電性フィルムの製造方法 - Google Patents
透明導電性フィルムの製造方法 Download PDFInfo
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- JP6461860B2 JP6461860B2 JP2016107581A JP2016107581A JP6461860B2 JP 6461860 B2 JP6461860 B2 JP 6461860B2 JP 2016107581 A JP2016107581 A JP 2016107581A JP 2016107581 A JP2016107581 A JP 2016107581A JP 6461860 B2 JP6461860 B2 JP 6461860B2
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- film
- polyimide
- transparent conductive
- bis
- dianhydride
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- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 229920001721 polyimide Polymers 0.000 claims description 129
- 239000010408 film Substances 0.000 claims description 75
- 239000004642 Polyimide Substances 0.000 claims description 69
- 239000010410 layer Substances 0.000 claims description 51
- 239000010409 thin film Substances 0.000 claims description 30
- 229920005575 poly(amic acid) Polymers 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 13
- 230000004888 barrier function Effects 0.000 claims description 11
- 238000002834 transmittance Methods 0.000 claims description 10
- 230000009477 glass transition Effects 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 230000003746 surface roughness Effects 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 4
- 238000010030 laminating Methods 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- 239000011889 copper foil Substances 0.000 description 16
- -1 polyethylene terephthalate Polymers 0.000 description 15
- 150000004985 diamines Chemical class 0.000 description 12
- 150000008065 acid anhydrides Chemical class 0.000 description 10
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical group FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
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- 229910044991 metal oxide Inorganic materials 0.000 description 5
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 4
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 3
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- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 2
- QBSMHWVGUPQNJJ-UHFFFAOYSA-N 4-[4-(4-aminophenyl)phenyl]aniline Chemical group C1=CC(N)=CC=C1C1=CC=C(C=2C=CC(N)=CC=2)C=C1 QBSMHWVGUPQNJJ-UHFFFAOYSA-N 0.000 description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- UBGIFSWRDUBQIC-UHFFFAOYSA-N perylene-2,3,8,9-tetracarboxylic acid Chemical compound C1=CC2=C(C(O)=O)C(C(=O)O)=CC(C=3C4=C5C=C(C(C(O)=O)=C4C=CC=3)C(O)=O)=C2C5=C1 UBGIFSWRDUBQIC-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- VITYLMJSEZETGU-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5-decafluoro-n,n'-diphenylpentane-1,5-diamine Chemical compound C=1C=CC=CC=1NC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)NC1=CC=CC=C1 VITYLMJSEZETGU-UHFFFAOYSA-N 0.000 description 1
- JLTHXLWCVUJTFW-UHFFFAOYSA-N 1,1,2,2,3,3,4,4-octafluoro-n,n'-diphenylbutane-1,4-diamine Chemical compound C=1C=CC=CC=1NC(F)(F)C(F)(F)C(F)(F)C(F)(F)NC1=CC=CC=C1 JLTHXLWCVUJTFW-UHFFFAOYSA-N 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Description
このように、これまでに検討されてきた透明導電性フィルムのポリイミドフィルムは透明性、耐熱性、線膨張係数(寸法安定性)のバランスを充足するものがなかった。
なお、これらのポリイミドフィルムの特性値について、ポリイミドフィルムが複数のポリイミド層から形成される場合には、全てのポリイミド層を含んだフィルム全体で示すものである。
PMDA:ピロメリット酸二無水物
DMAc:N,N-ジメチルアセトアミド
6FDA:2,2'-ビス(3,4-ジカルボキシフェニル)ヘキサフルオロプロパン二無水物
BPDA:3,3',4,4'-ビフェニルテトラカルボン酸二無水物
3mm×15mmのサイズのポリイミドフィルムを、熱機械分析(TMA)装置にて5.0gの荷重を加えながら一定の昇温速度(20℃/min)で30℃から260℃の温度範囲で引張り試験を行い、温度に対するポリイミドフィルムの伸び量から熱膨張係数(ppm/K)を測定した。
ポリイミドフィルム(50mm×50mm)をU4000形分光光度計にて、440nmから780nmにおける光透過率の平均値を求めた。
ガラス転移温度は、粘弾性アナライザ(レオメトリックサイエンスエフィー株式会社製RSA−II)を使って、10mm幅のサンプルを用いて、1Hzの振動を与えながら、室温から400℃まで10℃/分の速度で昇温した際の、損失正接(Tanδ)の極大から求めた。
東京インスツルメント社製の分光ポラリメーター「Poxi-spectra」を用いて、ポリイミドフィルムの面内方向のリタデーションを求めた。
ポリイミドフィルムの空気面(フィルム作成時に金属箔に触れていない面)の表面粗さRaについて、ブルカー社製の原子間力顕微鏡(AFM)「Multi Mode8」を用いて表面観察をタッピングモードで行った。10μm角の視野観察を4回行い、それらの平均値を求めた。表面粗さ(Ra)は、算術平均粗さ(JIS B0601-1991)を表す。
銅箔とポリイミドフィルムとの積層体の状態で25cm×25cmのサイズに切り出し、銅箔側にエッチングレジスト層を設けて、これを一辺が30cmの正方形の四辺に10cm間隔で直径1mmの点が16箇所配置するパターンに形成した。エッチングレジスト開孔部の露出部分をエッチングし、16箇所の銅箔残存点を有するCHE測定用ポリイミドフィルムを得た。このフィルムを120℃で2時間乾燥した後、23℃/30%RH・50%RH・70%RHの恒温恒湿機で各湿度において24時間静置し、二次元測長機により測定した各湿度での銅箔点間の寸法変化から湿度膨張係数(ppm/%RH)を求めた。
得られたフィルムの上に100nmの酸化インジウム・スズ(ITO,In:Sn=9:1)を積層して透明導電性薄膜(導電層)を形成し、透明導電性フィルムを得た。大きさ10cm四方の透明導電性フィルムの凸面を下にして平面に置いた場合の浮いた四隅を目視にて観察し、フラットな場合は◎、わずかにカールが発生した場合○とした。
JIS K7194に準拠し、4端子法で表面抵抗率を測定し、比抵抗を算出した。
(ポリイミドA)
窒素気流下で、200mlのセパラブルフラスコの中で攪拌しながらTFMB25.2gを溶剤DMAcに溶解させた。次いで、この溶液にPMDA14.5gと6FDA5.2gを加えた。その後、溶液を室温で5時間攪拌を続けて重合反応を行い、一昼夜保持した。粘稠なポリアミド酸溶液が得られ、高重合度のポリアミド酸Aが生成されていることが確認された。
(ポリイミドB)
窒素気流下で、200mlのセパラブルフラスコの中に攪拌しながら、ジアミンとしてTFMB25.7g、酸無水物としてPMDA15.7g及び6FDA3.6gをそれぞれ仕込み、その後、溶液を室温で5時間攪拌を続けて重合反応を行い、一昼夜保持した。粘稠なポリアミド酸溶液が得られ、高重合度のポリアミド酸Bが生成されていることが確認された。
(ポリイミドC)
窒素気流下で、200mlのセパラブルフラスコの中で攪拌しながらTFMB26.3gを溶剤DMAcに溶解させた。次いで、この溶液にPMDA16.9gと6FDA1.8gを加えた。その後、溶液を室温で5時間攪拌を続けて重合反応を行い、一昼夜保持した。粘稠なポリアミド酸溶液が得られ、高重合度のポリアミド酸Cが生成されていることが確認された。
(ポリイミドD)
ジアミンとしてTFMB23.4gを、また、酸無水物としてPMDA10.3g及び6FDA11.3gをそれぞれ使用した他は、ポリイミドAと同様に実施し、フィルム状のポリイミドDを得た。
(ポリイミドE)
ジアミンとしてTFMB23.0gを、また、酸無水物としてPMDA9.3g及び6FDA12.7gをそれぞれ使用した他は、ポリイミドAと同様に実施し、フィルム状のポリイミドEを得た。
(ポリイミドF)
ジアミンとしてTFMB23.5gを、また、酸無水物としてBPDA21.5gを使用した他は、ポリイミドAと同様に実施し、フィルム状のポリイミドFを得た。
窒素気流下で、200mlのセパラブルフラスコの中で攪拌しながらTFMB18.9gを溶剤DMAcに溶解させた。次いで、この溶液に6FDA26.1gを加えた。その後、溶液を室温で5時間攪拌を続けて重合反応を行い、一昼夜保持した。粘稠なポリアミド酸溶液Gが得られ、高重合度のポリアミド酸が生成されていることが確認された。
市販の100μmのPETフィルム上に、ポリイミドフィルムに行なったと同様に酸化インジウム・スズを積層して、透明導電性フィルムを得た。
Claims (7)
- ポリイミドフィルム上に気相堆積法によって透明導電性薄膜を積層して透明導電性フィルムを製造する方法であって、基材上にポリアミド酸の樹脂溶液を塗布し、熱処理して前記ポリアミド酸をイミド化することにより、前記基材上に440nmから780nmの波長領域での透過率が80%以上であり、かつ線膨張係数(CTE)が15ppm/K以下、面内方向のリタデーションが10nm以下であるポリイミドフィルムを形成した後、該ポリイミドフィルムの温度を250℃以上にして比抵抗が1mΩ・cm以下の透明導電性薄膜からなる導電層を形成し、該基材は、前記熱処理終了後にポリイミドフィルムから除去されることを特徴とする透明導電性フィルムの製造方法。
- 前記ポリイミドフィルムの少なくとも片面にガスバリア層を形成した後、ガスバリア層上に導電層を形成することを特徴とする請求項1に記載の透明導電性フィルムの製造方法。
- ポリイミドフィルムのガラス転移温度が300℃以上であることを特徴とする請求項1又は2に記載の透明導電性フィルムの製造方法。
- ポリイミドフィルムにおける導電層が積層される面の表面粗さRaが5nm以下であることを特徴とする請求項1〜3のいずれかに記載の透明導電性フィルムの製造方法。
- 導電層を形成する透明導電性薄膜がITOからなることを特徴とする請求項1〜4のいずれかに記載の透明導電性フィルムの製造方法。
- 前記一般式(1)で表される構造単位aと前記一般式(2)で表される構造単位bとの
存在比率(モル%)がa:b=85:15〜95:5の範囲であることを特徴とする請求
項6に記載の透明導電性フィルムの製造方法。
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