JP6657588B2 - 積層体及びその製造方法 - Google Patents
積層体及びその製造方法 Download PDFInfo
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- JP6657588B2 JP6657588B2 JP2015085116A JP2015085116A JP6657588B2 JP 6657588 B2 JP6657588 B2 JP 6657588B2 JP 2015085116 A JP2015085116 A JP 2015085116A JP 2015085116 A JP2015085116 A JP 2015085116A JP 6657588 B2 JP6657588 B2 JP 6657588B2
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Description
本発明の実施形態に係る積層体は、有機高分子からなる基材上に、原子層堆積法により形成された機能層と、無機物質からなるオーバーコート層とをこの順に積層したものである。このオーバーコート層はスパッタ法、CVD法もしくは真空蒸着法にて形成された膜であり、遷移金属原子を含む無機膜で形成することにより、積層体の再表面を化学的に安定な物質で保護することができる。
原子層堆積法(ALD法)によって製造された原子層堆積膜(ALD膜)を備えた積層体は、薄膜無機EL、ディスプレイ、半導体メモリ(DRAM)など、ガラス基板やシリコン基板などの電子部品基板として商業生産が行われている。一方、本発明の対象となる積層体の基材は、有機高分子からなるためガラス基板やシリコン基板の様に前駆体が吸着する吸着サイトが十分に存在しない場合がある。
[積層体の構成]
図1は、本発明の実施形態に係る積層体の構成を示す断面図である。
図2は、図1に示す積層体1の製造工程の概略を示すフローチャートである。
次に、機能層3に用いられる無機膜について説明する。機能層3は原子層堆積法により形成されたALD膜である。ALD膜の前駆体材料として有機金属化合物が用いられる。ALD膜の前駆体材料としては、例えば、トリメチルアルミニウム(TMA)、四塩化チタン(TiCl4)、トリスジメチルアミノシラン(3DMAS)、ビスジエチルアミノシラン(BDEAS)を使用できる。他には、化学元素周期率表の第II族、第III族、第IV族、第V族元素、遷移金属元素およびランタノイド元素の少なくとも一つを含有した前駆体材料を用いることができる。これらの前駆体材料を、H2OやH2O2等の反応ガスを用いて酸化させる。もしくは、O2、N2、CO2やH2もしくはそれらの混合ガスに電圧を印加することによりプラズマを発生させ、前駆体を反応させることで前駆体材料に含有される金属の金属膜、酸化膜、窒化膜、酸窒化膜を形成し、ALD膜を得る。これらのALD膜の膜厚は、2nm以上であることが好ましく、5nm以上であることが特性を確保する上でより好ましい。ALD法の成膜繰返し回数は、10サイクル以上であることが好ましく、30サイクル以上であることが特性を確保する上でより好ましい。有機高分子の自由体積のサイズ、比率はそれぞれ有機高分子基材の種類によりさまざまであるため、ALD膜の膜厚及び成膜繰返し回数の下限値は特に限定されず、基材の材質に応じて適宜定めることができる。上記前駆体を用いて形成される機能層は例えば酸化膜の場合Al2O3、TiO2、SiO2やそれらの混合酸化膜、つまり、AlTixOy、TiAlxOyなど3元系の組成を有するものでも良い。
次に、機能層3上に形成するオーバーコート層の形成方法を説明する。オーバーコート層は無機膜からなり、PVD法、CVD法など無機膜を形成可能なあらゆる手段を用いて形成できる。CVD法の場合は使用できる有機金属化合物が限られること、蒸着法の場合は材料の融点にプロセス及び装置が大きく影響することを考慮すると、スパッタ法によりオーバーコート層を形成することが好ましい。オーバーコート層の膜組成は第III族、第IV族、第V族元素およびランタノイド元素の少なくとも一つ遷移金属元素を含む酸化膜、窒化膜、酸窒化膜である。例えば、オーバーコート層が酸化膜の場合、Ta2O5、V2O5、Nb2O5、HfOx、ZrOxやそれらの混合酸化膜であっても良い。
高分子基材の少なくとも片面にALD法によってAl2O3膜(ALD膜)を成膜した。このとき、前駆体ガスとして、トリメチルアルミニウム(TMA)を使用した。また、前駆体ガスと同時に、プロセスガスとしてO2とN2を、パージガスとしてO2とN2を、反応ガス兼プラズマ放電ガスとしてO2を、それぞれ成膜室へ供給した。その際の処理圧力は10〜50Paとした。さらに、プラズマガス励起用電源として、13.56MHzの電源を用いた。そして、ICP(Inductively Coupled Plasma:誘導結合プラズマ)モードでプラズマ放電を実施した。
ALD膜を形成した上記積層中間体をスパッタ装置の成膜室内のステージに載置した。成膜室内の圧力を5.0×10−4Pa以下とした後、Arを流量30sccmで、O2を流量10sccmで成膜室内に導入し、排気側のオリフィスを調整することにより、成膜室内の圧力を2.5×10−1Paに維持した。次に、ステージとターゲット間に直流電圧を印加し、反応性スパッタリングによりオーバーコート層を形成した。スパッタリングターゲットとしてTaターゲットを用い、定電力300wattで成膜した。そのときの電圧が610V、電流が0.51Aで、ステージの回転速度が6rpm、ターゲット−ステージ間距離は200mmであった。
得られた積層フィルムの機能は、耐久性試験前後の水蒸気透過率(WVTR)を指標として評価した。水蒸気透過率測定方法及び耐久性試験方法は以下の通りである。
水蒸気透過率測定装置として、モダンコントロール社のMOCON Aquatran(登録商標)もしくはMOCON Prematran(登録商標)を用いて、40℃/90%RHの雰囲気でサンプルの水蒸気透過率を測定した。ここで、水蒸気透過率が0.02〔g/m2/day〕以下の積層体はAquatranを用いて測定を実施した。
耐久性試験は、加速寿命試験装置として使われているPCT(Pressure Cooker Test)装置(ESPEC社製)を用い、105℃/100%RHの環境下にサンプルを96時間投入した後、約24時間常温で放置した。常温放置後のサンプルの水蒸気透過率を、上記の水蒸気透過度測定方法により測定して、耐久性試験後の水蒸気透過率を求めた。
実施例1では、高分子基材として、ポリイミド(PI)からなる基材を使用した。PI基材上に機能層として膜厚10nmのAl2O3のALD膜を形成した。ALD膜上に、Ta2O5膜をスパッタ法により30秒間成膜し、膜厚5nmのオーバーコート層を形成して、実施例1の機能性フィルムを得た。得られた機能性フィルムについて耐久性試験前後の水蒸気透過率(WVTR)を測定したところ、耐久性試験前で0.01〔g/m2/day〕、耐久性試験後で1.03〔g/m2/day〕であった。
実施例2では、スパッタ法によるTa2O5膜の成膜時間を1分間として、膜厚10nmのオーバーコート層を形成したことを除いて、実施例1と同じ条件で機能性フィルムを作製した。得られた機能性フィルムについて耐久性試験前後の水蒸気透過率(WVTR)を測定したところ、耐久性試験前で0.003〔g/m2/day〕、耐久性試験後で0.5〔g/m2/day〕であった。
実施例3では、スパッタ法によるTa2O5膜の成膜時間を2分間として、膜厚20nmのオーバーコート層を形成したことを除いて、実施例1と同じ条件で機能性フィルムを作製した。得られた機能性フィルムについて耐久性試験前後の水蒸気透過率(WVTR)を測定したところ、耐久性試験前で0.0006〔g/m2/day〕、耐久性試験後で0.1〔g/m2/day〕であった。
実施例4では、高分子基材として、ポリエチレンテレフタレート(PET)からなる基材を使用した。PET基材上に機能層としてAl2O3のALD膜を形成した。ALD膜上に、Ta2O5膜をスパッタ法により2分間成膜し、膜厚20nmのオーバーコート層を形成して、実施例4の機能性フィルムを得た。得られた機能性フィルムについて耐久性試験前の水蒸気透過率(WVTR)を測定したところ、0.0005〔g/m2/day〕であった。
比較例1では、PI基材上に機能層として、膜厚10nmのAl2O3のALD膜を形成した。オーバーコート層であるTa2O5膜は形成しなかった。得られたフィルムについて耐久性試験前後での水蒸気透過率を測定したところ、耐久性試験前で0.04〔g/m2/day〕、耐久性試験後で1.21〔g/m2/day〕であった。
比較例2では、PI基材上に機能層を形成せずに、膜厚5nmのTa2O5膜を形成した。得られたフィルムについて耐久性試験前の水蒸気透過率を測定したところ、1.02〔g/m2/day〕であり、PI基材のみの水蒸気透過率1.09〔g/m2/day〕とほぼ同じ値であった。
比較例3では、PI基材上に機能層を形成せずに、膜厚10nmのTa2O5膜を形成した。得られたフィルムについて耐久性試験前後の水蒸気透過率を測定したところ、耐久性試験前で0.59〔g/m2/day〕であり、耐久性試験後で0.91〔g/m2/day〕であった。
比較例4では、PI基材上に機能層を形成せずに、膜厚20nmのTa2O5膜を形成した。得られたフィルムについて耐久性試験前後の水蒸気透過率を測定したところ、耐久性試験前で0.49〔g/m2/day〕であり、耐久性試験後で0.76〔g/m2/day〕であった。
比較例5では、高分子基材としてポリプロピレン(PP)からなる基材を使用した。PP基材上に機能層としてAl2O3のALD膜を形成した。ALD膜上に、Ta2O5膜をスパッタ法により2分間成膜し、膜厚20nmのオーバーコート層を形成して、比較例5に係るフィルムを得た。得られたフィルムについて耐久性試験前の水蒸気透過率(WVTR)を測定したところ、0.30〔g/m2/day〕であった。
また、実施例3及び4と比較例5との対比から分かるように、機能層の前駆体が吸着できないポリプロピレンを基材として使用した場合、機能層上にオーバーコート層を形成しても水蒸気透過率を十分に低下させることができなかった。したがって、ALD膜を積層する基材表面に前駆体が吸着可能な官能基(吸着サイト)が存在することの重要性が確認された。
以上述べたように、本発明の積層体によれば、有機高分子基材上に、原子層堆積膜を機能層として形成した後に、物理成膜法もしくは化学気相蒸着法にてオーバーコート層(OC層)を形成している。これにより、機能層のみと比較し、大幅に水蒸気透過率が低くなり、且つ耐久性試験後の水蒸気透過率の基材同等までの劣化を抑制することができる。
2 基材
3 機能層(ALD膜)
4 オーバーコート層(OC層)
10 巻出し室
11 巻出し部
20 第1の成膜室
21、21’ 前駆体領域
22、22’ パージ領域
23 反応領域
30 第2の成膜室
31 メインロール
32 原料供給部
33 膜組成物
Claims (1)
- 酸素原子または窒素原子を含む官能基を有する有機高分子を含有する基材と、
前記基材の表面の少なくとも一部に形成され、前記基材の表面に存在する前記官能基に結合した酸化アルミニウムの原子層堆積膜よりなる、厚みが2nm以上の機能層と、
前記機能層上にスパッタ法、CVD法、真空蒸着法のいずれかの方法により形成され、五酸化タンタルよりなる、厚みが5nm以上20nm以下のオーバーコート層とを備え、
前記基材が、ポリイミドからなり、
105℃/100%RHの環境下に96時間投入後、約24時間常温で放置する耐久性試験前に、40℃/90%RHの雰囲気で測定した水蒸気透過率が0.01g/m2/day以下であり、前記耐久性試験後に40℃/90%RHの雰囲気で測定した水蒸気透過率が1.03g/m2/day以下である、積層体。
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PCT/JP2016/002037 WO2016166986A1 (ja) | 2015-04-17 | 2016-04-15 | 積層体及びその製造方法 |
EP16779780.2A EP3284591A4 (en) | 2015-04-17 | 2016-04-15 | LAMINATE AND METHOD FOR THE MANUFACTURE THEREOF |
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