JP6632115B2 - 接着性樹脂層及び接着性樹脂フィルム - Google Patents
接着性樹脂層及び接着性樹脂フィルム Download PDFInfo
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- JP6632115B2 JP6632115B2 JP2015142880A JP2015142880A JP6632115B2 JP 6632115 B2 JP6632115 B2 JP 6632115B2 JP 2015142880 A JP2015142880 A JP 2015142880A JP 2015142880 A JP2015142880 A JP 2015142880A JP 6632115 B2 JP6632115 B2 JP 6632115B2
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- adhesive resin
- resin layer
- acrylic
- adhesive
- temperature
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Description
また、本発明は、前記接着性樹脂層を介して、2枚の基材が積層されてなる積層体を形成するための接着性樹脂層を提供する。
また、本発明は、前記接着性樹脂層を介して、2枚の基材を積層し、得られた積層体を、2つの金型の間に挟持した状態で、前記積層体を加熱変形させ、前記接着性樹脂層が加熱硬化した後でも粘着力が10N/25mm以上であることを特徴とする接着性樹脂層を提供する。
また、本発明は、接着性樹脂層を介して、2枚の基材を積層し、得られた積層体を、2つの金型の間に挟持した状態で、前記接着性樹脂層を加熱硬化することを特徴とする積層体の製造方法を提供する。
式(1) 温度A<温度C<温度B<温度D
図1に、接着性樹脂フィルム10の一例の断面図を示す。接着性樹脂フィルム10は、2枚のセパレーター12,13と、これらの間に積層された接着性樹脂層11とを有する。接着性樹脂層11を構成する接着性樹脂組成物は、(A)アクリル系ポリマーと、(B)アクリル系モノマー又はアクリル系オリゴマーと、(C)熱重合開始剤とを含有する。接着性樹脂層11の両面11a,11bは、常温で粘着性を有する(粘着面となっている)。
第2の積層方法として、第2の基材22に接着性樹脂層11を積層し、その後オートクレーブ処理を実施し、接着性樹脂層11の上に、第1の基材21を積層した後、もしくは第1の基材21を積層させながら、2つの金型を用いて接着性樹脂層11を加熱硬化させる方法が挙げられる。
第3の積層方法として、第1の基材21、接着性樹脂層11、第2の基材22を同時に積層した後、もしくは積層すると同時に、2つの金型を用いて接着性樹脂層11を加熱硬化させる方法が挙げられる。
本発明の接着性樹脂層の製造に用いる接着剤原材料組成物は、有機溶剤に溶解している方が、より厚みの精度良く塗布することが可能となるため、有機溶剤を含むことが好ましい。接着剤原材料組成物から溶剤を乾燥することで、接着性樹脂層が得られる。つまり、接着剤原材料組成物の組成は、接着性樹脂層を構成する接着性樹脂組成物の組成に、溶剤を加えたものであってもよい。接着性樹脂層は、常温では(熱硬化前)、粘着剤層として機能することができる。
アミド基(−CONR2,Rは水素原子又はアルキル基等の置換基)を有するアクリル系モノマーとしては、アクリルアミド、メタクリルアミド等が挙げられる。
ニトリル基(−CN)を有するアクリル系モノマーとしては、アクリロニトリル、メタクリロニトリル等が挙げられる。
(D)架橋剤(硬化剤)による(A)アクリル系ポリマーの硬化は、被着体に貼合する前の接着性樹脂層を製造する段階で、エージングにより進行させてもよい。
本発明における接着性樹脂層(トランスファーテープ)は、接着剤原材料組成物をセパレーターフィルムに溶媒を含んだ状態で塗布し、乾燥し、さらにセパレーターフィルムにより保護されることで製造することができる。接着剤原材料組成物は、ダイやパイプドクターを用いて塗布することが好ましい。溶剤の乾燥においては、ドライヤー等で乾燥させることが好ましい。溶媒の乾燥時間に関しては、生産性を考慮すると、10分間以下であることが好ましく、2〜5分間であることがさらに好ましい。また、有機溶媒を十分に乾燥することが必要なため、有機溶媒の沸点以上の温度で乾燥させることが好ましく、熱重合開始剤の1分間半減期温度以下での乾燥をすることが好ましい。
本発明においてのプレス時間に関しては生産性の観点から短時間、例えば5分間以内で反応が終わることが好ましい。また、プレス温度・時間に関しては、積層体の強度が十分になるように設定することができる。
アクリル系ポリマーを含むポリマー溶液として、SKダイン(登録商標)2094(綜研化学株式会社)、架橋剤としてE−AX(綜研化学株式会社)を用い、アクリル系ポリマー100重量部に対して、架橋剤0.2重量部の割合で配合した。得られた混合物に、反応性を持つ流動性樹脂成分として、アクリル系モノマーの4−ヒドロキシブチルアクリレート(大阪有機化学工業株式会社;4HBA)40重量部と、熱重合開始剤として、t−ブチルペルオキシ−2−エチルヘキサノエート(日油株式会社製;製品名:パーブチル(登録商標)O)0.08重量部とを加えて、接着剤原材料組成物を調製した。接着剤原材料組成物は、溶媒として、酢酸エチル(沸点77℃)を含み、コーティングするための塗料として、粘度等の性状が改善されている。
その接着剤原材料組成物を、セパレーター(藤森工業株式会社製;製品名:125E−0010DG2.5AS、厚み125μm)の上面に、アプリケーターを用いて、乾燥後における接着剤樹脂層(粘着剤層)の厚みが50μmとなるように塗布した後、乾燥工程において90℃、2分間の条件で溶剤を乾燥させて接着性樹脂層が積層された積層体を作製した。
次に、得られた積層体の接着性樹脂層の上面に、セパレーター(藤森工業株式会社製;製品名;38E−0010BDAS、厚み38μm)を貼合して、実施例1の接着性樹脂フィルムを作製した。
その後、1週間のエージングを行うことで、アクリル系ポリマーと架橋剤(エポキシ系)の反応を終了させて、架橋されたアクリル系ポリマーと、反応性を持つ流動性樹脂成分と、熱重合開始剤との3種類が存在する接着性樹脂層を形成した。
次に、評価方法及びその結果について、説明する。
昇温速度10℃/分の示差走査熱量測定(DSC)により、接着性樹脂層の発熱開始温度及びピーク温度を測定した。ピーク温度は、発熱ピーク(発熱量が最大となるピーク)の温度の測定値である。発熱開始温度は、ピーク温度が最低となる発熱ピークがベースラインから立ち上がる時の温度の測定値である。測定範囲は、少なくとも20℃〜210℃であり、その範囲で発熱ピークが確認されない場合、接着性樹脂層が熱重合開始剤を含まないときは「なし」、接着性樹脂層が熱重合開始剤を含むときは「観察できず」とした。
基材として、15cm×15cmに裁断した厚み100μmの平坦なポリエチレンテレフタレート(PET)フィルムを2枚用意した。これらの厚みは同じであっても異なっても構わないが、この評価方法では同じ厚みにした。接着性樹脂フィルムから片側のセパレーターを剥離して1枚目のPETフィルムに貼合し、さらに反対側のセパレーターを剥離して2枚目のPETフィルムを貼合し、接着性樹脂層を介して2枚のPETフィルムで挟んだ積層フィルムを作製した。ここまでを積層工程とする。
多次元形状を形成できるようにした金型を使用し、上下の金型の間に積層フィルムを設置し、金型の温度を設定温度まで上昇した。その設定温度(実施例9は150℃、実施例1〜8、12〜19は200℃、実施例10は250℃、実施例11は300℃)を熱プレス温度とし、熱プレス温度に達する前の状態をプレヒーティングとする。熱プレス温度まで熱が上がった時点で上下の金型をプレスし、積層フィルムを変形させた。上下の金型が合わさっている時間をプレス時間とし、本評価方法では2分間に設定した。2分経過後金型を開き、積層フィルムを取り出した。
◎:積層フィルムに気泡、欠陥が目視にて観察されず外観が良好であった。
○:積層フィルムに気泡、もしくは欠陥がわずかに目視にて観察されたが実害のないレベルの外観であった。
△:積層フィルムに気泡、もしくは欠陥がわずかに目視にて観察されたが許容範囲内であった。
×:積層フィルムに気泡、もしくは欠陥が目視にて観察され、外観が許容範囲外であった。
◎:積層フィルムにキワの浮きが確認できない。
○:積層フィルムにごくわずかにキワの浮きが確認できる。
△:積層フィルムにキワの浮きが確認できるが許容範囲内である。
×:積層フィルムにキワの浮きが確認でき、許容範囲外である。
◎:接着強度が30N/25mm以上
○:接着強度が20N/25mm以上、30N/25mm未満
△:接着強度が10N/25mm以上、20N/25mm未満
×:接着強度が10N/25mm未満
◎:積層フィルムに気泡が確認できない。
○:積層フィルムにごくわずかに気泡が確認できる。
△:積層フィルムに気泡が確認できるが許容範囲内である。
×:積層フィルムに気泡が確認でき、許容範囲外である。
実施例では、いずれも積層体に気泡などの外観上の不具合は確認できなかった。これは、接着性樹脂組成物中に、(A)アクリル系ポリマー以外に、流動性の高い成分として(B)アクリル系モノマー又はアクリル系オリゴマーが接着性樹脂組成物中に含まれているためと考えられる。
比較例2では、反応性を持つ流動性樹脂成分が接着性樹脂組成物中に含まれているが、開始剤が光重合開始剤であるため、熱プレス中には硬化反応が進まず、また一部の低分子成分が気化し、金型から圧力が解放される時に温度による揮発及び密着性低下によって剥離してしまったと考えられる。この例の場合は熱プレス中に何らかの方法で紫外線照射を行い、硬化反応を進めることができればこの課題は解決されるが、不透明な金型内に紫外線を照射するのは困難である。
比較例4では、1分間半減期温度が低い過酸化物を開始剤として用いたことにより、発熱開始温度が低すぎて熱プレス中に硬化反応が進まず、比較例2と同様の理由で剥離してしまったと考えられる。
比較例8では、1分間半減期が高い過酸化物を開始剤として用いたことにより、DSCによる測定において210℃以下でピークを観察することができず、熱プレス時の温度では重合反応が開始せず、比較例2と同様の理由で剥離してしまったと考えられる。
比較例6では、反応性を持つ流動性樹脂成分に対する熱重合開始剤の量が多すぎるためDSCによる測定値における発熱開始温度、ピーク温度が低く、熱プレス前から重合反応が進行し、反応してもポリマーの分子量が大きくならず、密着性が向上しないため発泡してしまうと考えられる。
比較例1〜3、7の熱プレス前でのDSCでは、発熱ピークが確認されなかった。熱による反応は確認できないため、熱硬化反応が進んでいないと判断できる。
比較例5の熱プレス前でのDSCでは、熱重合開始剤の発熱が確認されるだけで、反応性を持つ流動性樹脂成分が無いため重合反応は進行しない。
比較例4、8の熱プレス前でのDSCでは、発熱ピークは確認されたが、発熱開始温度及びピーク温度が高いため、上記の熱プレス条件では、熱硬化反応が進まなかったと判断できる。
実施例15〜18において接着性樹脂自体の熱分析をDSCで行った。この結果から、熱重合開始剤の種類にもよるが、100℃以上で急激に反応がスタートすることが確認された。このことから、接着剤原材料組成物及び接着性樹脂組成物に使用できる有機溶剤の沸点は100℃以下が好ましく、より好ましくは80℃以下であることが分かる。
Claims (5)
- アクリル系の接着性樹脂組成物からなる単層の接着性樹脂層であって、
前記接着性樹脂組成物が、少なくとも(A)アクリル系ポリマーと、(B)アクリル系モノマー又はアクリル系オリゴマーと、(C)熱重合開始剤とを含有し、
前記接着性樹脂組成物が、前記(A)アクリル系ポリマー100重量部に対して、前記(B)アクリル系モノマー又はアクリル系オリゴマーを20〜50重量部含有し、且つ、前記(B)アクリル系モノマー又はアクリル系オリゴマーの少なくとも一部として、水酸基を含有するアクリル系モノマーを15重量部以上又は硬化性ウレタンアクリレートを20重量部以上含有し、
前記(C)熱重合開始剤が、n−ブチル4,4−ビス(t−ブチルペルオキシ)バレレート、1,1,3,3−テトラメチルブチルペルオキシ−2−エチルヘキサノエート、t−ブチルペルオキシ−2−エチルヘキサノエート、1,1−ビス(t−ヘキシルペルオキシ)シクロヘキサン、t−ヘキシルペルオキシベンゾエートのいずれかを有効成分とする熱重合開始剤であり、
前記接着性樹脂層が、常温で両面に粘着性を有し、昇温速度10℃/分の示差走査熱量測定(DSC)において、80℃以上で発熱が確認され始め、120℃〜210℃の間にピークが少なくとも1つ確認されることを特徴とする接着性樹脂層。 - 前記接着性樹脂組成物が、前記(A)〜(C)以外の成分として、(D)架橋剤を含有し、
前記接着性樹脂層において、前記(A)アクリル系ポリマーが、前記(D)架橋剤により架橋されていることを特徴とする請求項1に記載の接着性樹脂層。 - 請求項1又は2に記載の接着性樹脂層が、2枚のセパレーターの間に積層されてなることを特徴とする接着性樹脂フィルム。
- 請求項1又は2に記載の接着性樹脂層を介して、2枚の基材が積層されてなる積層体を形成するための接着性樹脂層。
- 請求項1又は2に記載の接着性樹脂層を介して、2枚の基材を積層し、得られた積層体を、2つの金型の間に挟持した状態で、前記積層体を加熱変形させ、前記接着性樹脂層が加熱硬化した後でも粘着力が10N/25mm以上であることを特徴とする接着性樹脂層。
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