JP5782345B2 - 積層フィルムの製造方法 - Google Patents
積層フィルムの製造方法 Download PDFInfo
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- JP5782345B2 JP5782345B2 JP2011210900A JP2011210900A JP5782345B2 JP 5782345 B2 JP5782345 B2 JP 5782345B2 JP 2011210900 A JP2011210900 A JP 2011210900A JP 2011210900 A JP2011210900 A JP 2011210900A JP 5782345 B2 JP5782345 B2 JP 5782345B2
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
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- 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
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
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Description
前記第一積層フィルムは、前記第一積層フィルムの硬化層に、熱収縮性を有する第二透明樹脂フィルムを、粘着剤層を介して積層して第二積層フィルムを形成するために用いられるものであり、
前記硬化層の厚さは1μm未満であり、
前記硬化層の形成は、
活性エネルギー線硬化型化合物、光重合開始剤(但し、加熱減量試験における10%加熱減量温度が170℃以上である)および溶媒を含有する組成物溶液を、第一透明樹脂フィルムの片面または両面に、塗工して塗工層を形成する塗工工程(1)と、
前記塗工工程(1)の後に、前記塗工層に含まれる溶媒の乾燥を、得られる第一積層フィルムを150℃で1時間加熱した場合の熱収縮率が0.5%以下となるような温度条件下に制御して行なう熱処理工程(2)と、
前記熱処理工程(2)の後に、塗工層を硬化させる硬化工程(3)を含むことを特徴とする第一積層フィルムの製造方法、に関する。
当該第一積層フィルムの硬化層に、熱収縮性を有する第二透明樹脂フィルムを、粘着剤層を介して貼り合せる積層工程(4)をさらに含むことを特徴とする第二積層フィルムの製造方法、に関する。
(ハードコート層の形成)
ハードコート層の形成材料として、アクリル・ウレタン系樹脂(大日本インキ化学(株)製のユニディック17−806)100重量部に、光重合開始剤としての1−ヒドロキシ−シクロヘキシル−フェニルケトン(イルガキュア184,チバスペシャルティケミカルズ社製)5重量部を加えて、30重量%の濃度に希釈してなるトルエン溶液を調製した。
無機酸化物粒子と重合性不飽和基を含む有機化合物とを結合させてなるナノシリカ粒子を分散させた、活性エネルギー線硬化型化合物を含む硬化層形成材料(JSR(株)製、商品名「オプスターZ7540」,固形分:56重量%,溶媒:酢酸ブチル/メチルエチルケトン(MEK)=76/24(重量比))を準備した。前記硬化層形成材料は、活性エネルギー線硬化型化合物として、ジペンタエリスリトールおよびイソホロンジイソシアネート系ポリウレタン、表面を有機分子により修飾したシリカ微粒子(重量平均粒径100nm以下)を、前者:後者=2:3の重量比で含有する。この硬化層形成材料の活性エネルギー線硬化型化合物の固形分100重量部あたり、光重合開始剤として、2−メチル−1−(4−メチルチオフェニル)−2−モルフォリノプロパン−1−オン(イルガキュア907,チバスペシャルティケミカルズ社製,加熱減量試験における10%加熱減量温度:202℃)5重量部を混合した。この混合物に固形分濃度が10重量%、酢酸ブチル/メチルエチルケトン=2/1(重量比)になるように酢酸ブチルおよびメチルエチルケトンを加えて希釈し、硬化層形成材料を調製した。
第二透明樹脂フィルムである、厚さ25μmのポリエチレンテレフタレートフィルムの一方の面に、アルゴンガス80%と酸素ガス20%とからなる0.4Paの雰囲気中で、ポリエチレンテレフタレートフィルムの温度が100℃の条件下で、放電出力:6.35W/cm2、酸化インジウム97重量%、酸化スズ3重量%の焼結体材料を用いた反応性スパッタリング法により、厚さ22nmのITO膜を形成して、透明導電性フィルムを得た。上記ITO膜は、非晶質であった。
上記第一積層フィルムの硬化層に粘着剤層を形成し、当該粘着剤層に、透明導電性フィルムの透明導電性膜を形成していない側の面を貼り合せて、第二積層フィルムを作成した。前記粘着剤層は、厚さ20μm、弾性係数10N/cm2の透明なアクリル系の粘着剤層を形成した。粘着剤層組成物としては、アクリル酸ブチルとアクリル酸と酢酸ビニルとの重量比が100:2:5のアクリル系共重合体100重量部に、イソシアネート系架橋剤を1重量部配合してなるものを用いた。
実施例1の第一積層フィルムの作成(硬化層の形成)において、光重合開始剤として、2−ヒドロキシ−1−{4−[4−(2−ヒドロキシ−メチル−プロピオニル)ベンジル]フェニル}−2−メチループロパン−1−オン(イルガキュア127,チバスペシャルティケミカルズ社製,加熱減量試験における10%加熱減量温度:263℃)を用いたこと以外は、実施例1と同様にして、第二積層フィルムを得た。また、実施例1と同様に結晶化処理を施した。
実施例1の第一積層フィルムの作成(硬化層の形成)において、光重合開始剤として、1−ヒドロキシ−シクロヘキシル−フェニルケトン(イルガキュア184,チバスペシャルティケミカルズ社製,加熱減量試験における10%加熱減量温度:154℃)を用いたこと以外は、実施例1と同様にして、第二積層フィルムを得た。また、実施例1と同様に結晶化処理を施した。
実施例1の第一積層フィルムの作成(硬化層の形成)において、光重合開始剤として、1−ヒドロキシ−シクロヘキシル−フェニルケトン(イルガキュア184,チバスペシャルティケミカルズ社製,加熱減量試験における10%加熱減量温度:154℃)を用いたこと、塗工層の乾燥温度を80℃に変えたこと、紫外線照射後に150℃で1分間の加熱処理をさらに行なったこと以外は、実施例1と同様にして、第二積層フィルムを得た。また、実施例1と同様に結晶化処理を施した。
試料(光重合開始剤)は水などの揮発性不純物を取り除くために、試験前に100℃で5分間の前処理を施した。その後、試料(光重合開始剤)約10mgを熱重量分析装置(セイコーインスツルメンツ(株)製,Tg/DTA6200)で窒素気流中における昇温速度5℃/分にて加熱処理して、下記式から算出される加熱減量M(%)が10%になる温度を測定した。昇温170℃での加熱減量Mは、170℃時点の試料の重量を測定し、下記式から170℃における加熱減量M(%)を算出した。
加熱処理前の試料の重量(M0)、加熱処理後の試料の重量(M1)。
M(%)={(M0−M1)/M0}×100
ハードコート層を有する第一積層フィルムを、10cm四方に切り出し、初期状態の寸法(初期寸法)と、150℃で1時間加熱処理した後の寸法(加熱後寸法)を測定し、これらの測定値から、下記式により、MD方向とTD方向の熱収縮率を算出した。
熱収縮率(%)={(初期寸法―加熱後寸法)/初期寸法}×100
スチールウールに250g/25mmφの荷重をかけ、硬化層表面を10cmの長さで10往復した後、硬化層表面の状態を目視により観察し下記基準で評価した。
○:全面に薄い傷が確認できる。
×:全面に著しい傷が確認できる。
結晶化処理が施された第二積層フィルムを10cm四方に切り出し、カールが凸になっている面が下側になるように水平面上に置き、角の4点のうちで最も水平面から長い点の距離(mm)を測定した。ITOの形成面を上にした凹になる場合をプラス、ハードコート層の形成面を上にして凹になる場合をマイナスとして標記する。
10 第一透明樹脂フィルム
11 硬化層
12 機能層(ハードコート層)
2 第二積層フィルム
20 第二透明樹脂フィルム
21 アンダーコート層
22 透明導電性膜
3 粘着剤層
Claims (7)
- 熱収縮性を有する第一透明樹脂フィルムの片面または両面に硬化層を形成する第一積層フィルムの製造方法を製造した後、当該第一積層フィルムの硬化層に、熱収縮性を有する第二透明樹脂フィルムを、粘着剤層を介して貼り合せる積層工程(4)を含む第二積層フィルムの製造方法であって、
前記第一積層フィルムにおける前記硬化層の厚さは1μm未満であり、
前記硬化層の形成は、
活性エネルギー線硬化型化合物、光重合開始剤(但し、加熱減量試験における10%加熱減量温度が170℃以上である)および溶媒を含有する組成物溶液を、第一透明樹脂フィルムの片面または両面に、塗工して塗工層を形成する塗工工程(1)と、
前記塗工工程(1)の後に、前記塗工層に含まれる溶媒の乾燥を、得られる第一積層フィルムを150℃で1時間加熱した場合の熱収縮率が0.5%以下となるような温度条件下に制御して行なう熱処理工程(2)と、
前記熱処理工程(2)の後に、塗工層を硬化させる硬化工程(3)を含み、
前記第二透明樹脂フィルムは、前記硬化層に貼り合せない他方の片面に、直接またはアンダーコート層を介して、透明導電性膜を有することを特徴とする第二積層フィルムの製造方法。 - 前記光重合開始剤が、2−ヒドロキシ−1−{4−[4−(2−ヒドロキシ−メチル−プロピオニル)ベンジル]フェニル}−2−メチループロパン−1−オン、および/または2−メチル−1−(4−メチルチオフェニル)−2−モルフォリノプロパン−1−オンであることを特徴とする請求項1記載の第二積層フィルムの製造方法。
- 前記光重合開始剤の使用量が、活性エネルギー線硬化型化合物100重量部に対して、0.1重量部以上であることを特徴とする請求項1または2記載の第二積層フィルムの製造方法。
- 熱処理工程(2)の温度が、125〜165℃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第二積層フィルムの製造方法。
- 第一積層フィルムの一方の片面の最外層に硬化層、他の片面の最外層に機能層を有することを特徴とする請求項1〜4のいずれかに記載の第二積層フィルムの製造方法。
- 機能層がハードコート層であることを特徴とする請求項5記載の第二積層フィルムの製造方法。
- 前記透明導電性膜が、金属酸化物により形成された非晶質透明導電性薄膜であり、積層工程(4)の後に、前記非晶質透明導電性薄膜を加熱により結晶質化する結晶化工程(5)をさらに含むことを特徴とする請求項1〜6のいずれかに記載の第二積層フィルムの製造方法。
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JP2012091163A (ja) | 2012-05-17 |
CN103140298B (zh) | 2014-06-18 |
CN103140298A (zh) | 2013-06-05 |
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