JP6489448B2 - 導電フィルム - Google Patents
導電フィルム Download PDFInfo
- Publication number
- JP6489448B2 JP6489448B2 JP2016516994A JP2016516994A JP6489448B2 JP 6489448 B2 JP6489448 B2 JP 6489448B2 JP 2016516994 A JP2016516994 A JP 2016516994A JP 2016516994 A JP2016516994 A JP 2016516994A JP 6489448 B2 JP6489448 B2 JP 6489448B2
- Authority
- JP
- Japan
- Prior art keywords
- conductive film
- resin
- film according
- conductive
- stress relaxation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010408 film Substances 0.000 claims description 87
- 229920005989 resin Polymers 0.000 claims description 64
- 239000011347 resin Substances 0.000 claims description 64
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- 239000000463 material Substances 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 34
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- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 238000012360 testing method Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 20
- 239000011231 conductive filler Substances 0.000 claims description 16
- 229920001187 thermosetting polymer Polymers 0.000 claims description 13
- 239000004593 Epoxy Substances 0.000 claims description 11
- 238000004364 calculation method Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
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- 238000005259 measurement Methods 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
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- 238000002834 transmittance Methods 0.000 claims description 6
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- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 2
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- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 2
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
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- 125000002723 alicyclic group Chemical group 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- LUFPJJNWMYZRQE-UHFFFAOYSA-N benzylsulfanylmethylbenzene Chemical class C=1C=CC=CC=1CSCC1=CC=CC=C1 LUFPJJNWMYZRQE-UHFFFAOYSA-N 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
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- KMOUUZVZFBCRAM-UHFFFAOYSA-N 1,2,3,6-tetrahydrophthalic anhydride Chemical compound C1C=CCC2C(=O)OC(=O)C21 KMOUUZVZFBCRAM-UHFFFAOYSA-N 0.000 description 1
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- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 1
- MODAACUAXYPNJH-UHFFFAOYSA-N 1-(methoxymethyl)-4-[4-(methoxymethyl)phenyl]benzene Chemical group C1=CC(COC)=CC=C1C1=CC=C(COC)C=C1 MODAACUAXYPNJH-UHFFFAOYSA-N 0.000 description 1
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
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Description
本実施形態で用いられる伸張−復元試験では、フィルム片(厚み:50μm、サンプル形状:ダンベル6号(測定部位幅:4mm、平行部分長さ:25mm))を用いて、ISO3384に準拠した引張−圧縮試験機(例えば、島津製作所製のオートグラフ(型式:AGS-X))を用いて、下記条件で伸張行程を行った後に復元行程を行い、下記算出方法によって応力緩和率R及び残留歪み率αを計算する。
試験片をつかみ具に取り付けたときに発生するたわみを除去するために、たわみ補正を0.05N以下の力で行う。
試験速度:25mm/min、0〜25%伸張まで
温度条件:23℃
伸張・保持条件:25%伸張で、保持時間5分
試験速度:0.1mm/min、引張力が0±0.05Nになるまで
温度条件:23℃
応力緩和率算出方法:伸張行程終了時の引張力の測定を行い、これを初期引張力FA0とする。その後、上述の伸張・保持条件で歪量を保持し5分後に引張力を測定する。これをFA(t5)とする。応力緩和率Rは下記式によって計算する。
20%≦R≦95%かつ
0%≦α≦3%
(熱硬化性樹脂)
・ポリロタキサン:(アドバンス・ソフトマテリアルズ社製「A1000」、PEGを軸分子、α−シクロデキストリンを環状分子とし、反応基としてOH基を有する)
・エポキシ樹脂(三菱化学製「JER1003」、メチル基が7〜8個、2官能、分子量1300)
・エポキシ樹脂(DIC製「EXA−4816」、分子量824、メチル基多数、2官能)
・エポキシ樹脂(新日鉄住友金属化学製「YP50」、分子量60000〜80000、メチル基多数、2官能)
・エチレンオキサイド付加型ヒドロキシフェニルフルオレン型エポキシ樹脂(大阪ガスケミカル製「EG−280」)
・プロピレンオキサイド付加型ビスフェノールA型エポキシ樹脂(ADEKA製「EP−4003S」)
(硬化剤)
・多官能フェノール系硬化剤(日本化薬(株)製「GPH−103」、ビフェニルアラルキル型フェノール)
・イミダゾール系硬化促進剤(四国化成製「2E4MZ」、2エチル4メチルイミダゾール)
・ポリイソシアネート(ポリイソシアネート、DIC製「DN950」)
・カチオン硬化剤(三新化学製「SI−150」、六フッ化アンチモンスルホニウム塩)
(樹脂基材比較例)
・PETフィルム(東洋紡社製「A4300」)
(カーボンナノチューブ(CNT)含有水溶液)
・SWCNT:IsoNonotubes−M(NanoIntegris社製、CNT直径1.7nm、長さ1μm)
・DWCNT:NANOCYL NC2100(Nanocyl社製、CNT直径3.5nm、長さ1〜10μm)
(銀ナノワイヤ)
・Agナノワイヤ含有溶液(Sigma―Aldrich製、直径60nm、長さ10μm)
下記表1に示す配合組成(質量部)で、固形分濃度が40質量%となるように、溶剤(メチルエチルケトン)に添加して、各成分を均一に混合し、樹脂基材1〜5用の樹脂組成物を調製した。
(実施例1〜2、4〜5、7〜8、10、比較例1〜2)
各CNTを秤量し、5wt%ドデシル硫酸ナトリウム水溶液に入れ、超音波で24時間分散させ濃度200ppmのCNT含有水溶液を得た。
AgナノワイヤをAg固形分濃度が0.5wt%となるように、水溶液で調整し、Agナノワイヤ含有水溶液を得た。
それぞれ表3に示す樹脂基材の一方の表面上にITO膜を20nm成膜した(製膜条件:マグネトロンスパッタ法,ITO焼結体をターゲットとし、Ar分圧0.5Pa、100W)。
本実施例で用いられる伸張−復元試験では、上記実施例および比較例のサンプルを用いて、下記条件で伸張行程を行った後に復元行程を行い、下記算出方法によって応力緩和率R及び残留歪み率αを計算した。
試験片をつかみ具に取り付けたときに発生するたわみを除去するために、たわみ補正を0.05N以下の力で行った。
試験速度:25mm/min、0〜25%伸張まで
温度条件:23℃
伸張・保持条件:25%伸張で、保持時間5分
試験速度:0.1mm/min、引張力が0±0.05Nになるまで
温度条件:23℃
応力緩和率算出方法:伸張行程終了時の引張力の測定を行い、これを初期引張力FA0とした。その後、上述の伸張・保持条件で歪量を保持し5分後に引張力を測定した。これをFA(t10)とする。応力緩和率Rは下記式によって計算した。
上記実施例および比較例のサンプルを用いて、ISO3384に準拠した引張−圧縮試験機で、下記条件で伸張行程を行い、伸張終了時の引張力の測定を行って、これを初期引張力FB0とした。その後、30分後に引張力FB(t30)を測定した。
試験片をつかみ具に取り付けたときに発生するたわみを除去するために、たわみ補正を行う。たわみ補正は、0.05N以下の力で行った。
試験速度:25mm/min、50%伸張まで
温度条件:23℃
伸張・保持条件:50%伸張で、保持時間30分
そして、FB(t30)/FB0の計算値を求めた。結果を表2および3に示す。
得られた各導電フィルムを、ISO3195に準拠した試験機で表面抵抗値を測定した。結果を表2および3に示す。
得られた各導電フィルムを、ISO2556に準拠した試験機で全光線透過率を測定した。結果を表2および3に示す。
得られた各導電フィルムを、長さ6cm、幅5mmの寸法で切り出し、フィルム延伸機につかみ具間距離が4cmとなるようにセットした。そして、フィルムの伸張前と伸張率25%の伸張時、さらにつかみ具を戻しフィルムが元の位置へ復元したところで、それぞれ抵抗計(日置電機社製RM3548)を用いて端子間距離が3cmとなる位置で抵抗値を測定した。伸縮前の抵抗値からの抵抗増加量を100分率で示した結果を表2および3に示す。
比較例1〜3では、従来の熱可塑フィルムで、導電フィルム用の可とう性基材として実績のあるPETフィルム(A4300)を樹脂基材とし、本発明の実施例として使われる導電材料のCNTおよびAgナノワイヤを用いてそれぞれ導電フィルムを作成し、実施例との比較を行った。
Claims (13)
- 弾性変形可能な樹脂基材上に、繊維状導電フィラーによる網目構造を有する導電層を形成した導電フィルムであって、
前記樹脂基材が、(A)ポリロタキサン、(B)エポキシ樹脂と、(C)硬化剤とを含む樹脂組成物、又は、(D)炭素数が2〜3のアルキレンオキサイド変性された変性基を有し且つその変性基がエポキシ1mol分子中に4mol以上含まれること、2mol以上のエポキシ基を有すること、及びエポキシ当量が450eq/mol以上であることを特徴とするエポキシ樹脂と、(E)硬化剤とを含む樹脂組成物で構成されていること、並びに、
以下の伸張−復元試験により測定される応力緩和率Rおよび残留歪みαが、以下の式を満たすことを特徴とする、導電フィルム。
20%≦R≦95%かつ
0%≦α≦3%
〔伸張−復元試験〕
フィルム片(厚み:50μm、サンプル形状:ダンベル6号(測定部位幅:4mm、平行部分長さ:25mm))を用いて、ISO3384に準拠した引張−圧縮試験機で、下記条件で伸張行程を行った後に復元行程を行い、下記算出方法によって応力緩和率R及び残留歪み率αを計算する。
伸張行程条件:
試験片をつかみ具に取り付けたときに発生するたわみを除去するために、たわみ
補正を0.05N以下の力で行う。
試験速度:25mm/min、0〜25%伸張まで
温度条件:23℃
伸張・保持条件:25%伸張で、保持時間5分
復元行程条件:
試験速度:0.1mm/min、引張力が0±0.05Nになるまで
温度条件:23℃
応力緩和率算出方法:伸張行程終了時の引張力の測定を行い、これを初期引張力FA0とする。その後、上述の伸張・保持条件で歪量を保持し5分後に引張力を測定する。これをFA(t5)とする。応力緩和率Rは下記式によって計算する。
- 前記樹脂基材が少なくとも熱硬化性樹脂を含有する、請求項1記載の導電フィルム。
- 前記熱硬化性樹脂がエポキシ樹脂である、請求項2記載の導電フィルム。
- 前記繊維状導電フィラーが、カーボンナノチューブ、カーボンナノバッド、金属ナノワイヤ、又は、それらの組合せのうち少なくとも一つ含有する、請求項1〜3のいずれかに記載の導電フィルム。
- 前記繊維状導電フィラーの繊維長さが1μm以上であり、かつ、長さ/直径のアスペク
ト比が50以上である、請求項1〜4のいずれかに記載の導電フィルム。 - 前記導電層の厚みが1μm以下である、請求項1〜5のいずれかに記載の導電フィルム。
- 前記導電層の一部もしくは全体が、弾性変形可能な前記樹脂基材に埋め込まれている、請求項1〜6のいずれかに記載の導電フィルム。
- 前記樹脂基材の表面が、Raで50nm以上5μm以下の微細凹凸構造を有している、請求項1〜7のいずれかに記載の導電フィルム。
- 全光線透過率が70%以上である、請求項1〜8のいずれかに記載の導電フィルム。
- 請求項1〜9のいずれかに記載の導電フィルムの導電層を、部分的に除去することによりパターニングしている、導電フィルム。
- 請求項1〜10に記載の導電フィルムを用いるディスプレイ。
- 請求項1〜10に記載の導電フィルムを用いるタッチセンサ。
- 請求項1〜10に記載の導電フィルムを用いる太陽電池。
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JP2017537467A (ja) * | 2014-11-27 | 2017-12-14 | パナソニックIpマネジメント株式会社 | シート状伸縮性構造体及びそれに用いられる伸縮性樹脂シート用樹脂組成物、伸縮性樹脂シート |
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US9839119B2 (en) | 2017-12-05 |
CN105579499B (zh) | 2018-11-13 |
CN109370245B (zh) | 2021-10-26 |
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US20160266668A1 (en) | 2016-09-15 |
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WO2015052853A1 (en) | 2015-04-16 |
US9468092B2 (en) | 2016-10-11 |
JP6380942B2 (ja) | 2018-08-29 |
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US20160264813A1 (en) | 2016-09-15 |
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US20180263113A1 (en) | 2018-09-13 |
JP6681598B2 (ja) | 2020-04-15 |
CN105579499A (zh) | 2016-05-11 |
CN109370245A (zh) | 2019-02-22 |
JP2018172697A (ja) | 2018-11-08 |
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