JP6507309B2 - 複合材物品及その製造方法 - Google Patents
複合材物品及その製造方法 Download PDFInfo
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- JP6507309B2 JP6507309B2 JP2018507696A JP2018507696A JP6507309B2 JP 6507309 B2 JP6507309 B2 JP 6507309B2 JP 2018507696 A JP2018507696 A JP 2018507696A JP 2018507696 A JP2018507696 A JP 2018507696A JP 6507309 B2 JP6507309 B2 JP 6507309B2
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Description
本開示は、概して、無機バリア層を含む複合材物品及びその製造方法に関する。
耐透湿性のバリアフィルムを製造するためには、ポリマー及び酸化アルミニウム又は酸化ケイ素などの酸化物の層を可撓性ポリマーフィルム上に堆積する。こうしたバリアフィルムは、溶液コーティング、ロールコーティング、ディップコーティング、スプレーコーティング、スピンコーティングなどの液体コーティング技術;並びに化学蒸着(CVD)、プラズマ強化化学蒸着(PECVD)、スパッタリング及び液体及び/又は固体材料を熱蒸発させる真空プロセスなどのコーティング技術を含む、様々な製造方法によって調製することができる。そのようなバリアフィルム及びプロセスの例は、米国特許第5,440,446号(Shaw et al.);同第5,877,895号(Shaw et al.);同第6,010,751号(Shaw et al.);同第7,018,713号(Padiyath et al.);及び同第6,413,645号(Graff et al.)において見出すことができる。これらのバリアフィルムは、ガラス封止材料の可撓性代用品として、ディスプレイ、照明、及び太陽光市場において多くの用途を有する。
耐光性及び耐候性に関して優れた耐久性を有するバリアフィルム、及びそれを含む他の物品は引き続き必要とされている。特に、光分解及び光酸化に対して優れた耐性を有する可撓性の透明多層バリアフィルムが必要とされている。
基材と、
基材上に配置された下地ポリマー層であって、下記式で表される少なくとも1種のジ(メタ)アクリレート
(式中、
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基が一緒に、2〜7個の炭素原子を有するアルキレン基を形成していてもよい)を少なくとも60重量%含む重合性下地成分の重合反応生成物、を含む、下地ポリマー層と、
下地ポリマー層に結合された無機バリア層と、
基材とは反対側の無機バリア層上に配置された上部ポリマー層であって、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物、を含み、環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、上部ポリマー層と、
を含む、複合材物品を提供する。
基材上に下地ポリマー層を配置する工程であって、下地ポリマー層は、下記式で表される少なくとも1種のジ(メタ)アクリレート
(式中、
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基が一緒に、2〜7個の炭素原子を有するアルキレン基を形成していてもよい)を少なくとも60重量%含む重合性下地成分の重合反応生成物を含む、工程と、
無機バリア層を下地ポリマー層に結合する工程と、
下地ポリマー層とは反対側の無機バリア層上に上部ポリマー層を配置する工程であって、上部ポリマー層は、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物を含み、環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、工程と、
を順に含む、複合材物品の製造方法を提供する。
図1は、例示的な複合材物品100の概略断面図である。複合材物品100は、基材112;下地ポリマー層114;無機バリア層115;任意選択の接着改質層118;上部ポリマー層119、任意選択の感圧性接着剤層120及び任意選択のカバー層122、の順序で配置された層を含む。図1では、任意選択の接着改質層118は無機バリア層115と上部ポリマー層119との間に位置しているが、接着改質層は、任意のポリマー−ポリマー又はポリマー−酸化物境界面に配置できることが理解されるべきである。具体的には、接着改質層は、例えば、基材と下地ポリマー層との間、下地ポリマー層と無機バリア層との間、無機バリア層と上部ポリマー層との間、又は上部ポリマー層の上に配置してもよい。
第1実施形態では、本開示は、
基材と、
基材上に配置された下地ポリマー層であって、下記式で表される少なくとも1種のジ(メタ)アクリレート
(式中、
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基が一緒に、2〜7個の炭素原子を有するアルキレン基を形成していてもよい)を少なくとも60重量%含む重合性下地成分の重合反応生成物、を含む、下地ポリマー層と、
下地ポリマー層に結合された無機バリア層と、
基材とは反対側の無機バリア層上に配置された上部ポリマー層であって、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物、を含み、環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、上部ポリマー層と、
を含む、複合材物品を提供する。
基材上に下地ポリマー層を配置する工程であって、下地ポリマー層は、下記式で表される少なくとも1種のジ(メタ)アクリレート
(式中、
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基が一緒に、2〜7個の炭素原子を有するアルキレン基を形成していてもよい)を少なくとも60重量%含む重合性下地成分の重合反応生成物を含む、工程と、
無機バリア層を下地ポリマー層に結合する工程と、
下地ポリマー層とは反対側の無機バリア層上に上部ポリマー層を配置する工程であって、上部ポリマー層は、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物を含み、環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、工程と、
を順に含む、複合材物品の製造方法を提供する。
積層構造体(LC)方法
実施例1〜2及び比較例A〜Kの複合材バリアフィルムを、0.05mm(0.002in)の厚さのエチレン−テトラフルオロエチレン(NORTON ETFEとしてSt.Gobain Performance Plastics(Wayne,New Jersey)から入手可能なETFE、エチレン−テトラフルオロエチレンフィルム)ポリマーシートに、0.05mm(0.002in)の厚さのUV吸収剤含有感圧性接着剤(PSA)(3M OPTICALLY CLEAR ADHESIVE 8172PCLとして3M Company(St.Paul)から入手可能)を使用して、積層した。PSAは、UV−B照射のほとんど全て及び波長が400nmに近づくにつれて部分的に透過させるがUV−A照射の大部分を遮断する。410nmを超える可視域の波長では、透過率は90%を超える。PSAはまずETFEフィルムに積層された。次に、1インチ(2.54cm)幅のテープ片(3M Polyester Tape 8403として3M Companyから入手可能)を、ウェブを横断する複合材バリアフィルムの切り口に沿って、複合材バリアフィルムの上部ポリマー層上に接着剤側を上にして置いた。次に、ETFE/PSA構造体を、上部アクリレートポリマーがPSAに隣接するように複合材バリアフィルムに積層した。このようにして、複合材バリアフィルムの上部ポリマー層がPSAに隣接する積層構造体を作製した。テープは、積層構造体の一方の端に沿ってETFE/PSA及び複合材バリアフィルムを離しておくのに役立った。これにより、その後のT形剥離試験でInstron引張試験機のグリップに固定することができるタブができた。
実施例1〜2及び比較例A〜Kについて上記で記載した通り、積層構造体(LC)を調製した。LCを6.5in(16.5cm)×9.5in(24.1cm)に切断した。2つのLCを次のように調製した。一方のLC(下部LC)は、比較例AのLC(下地ポリマー層を形成するためのアクリレートとしてのTCDD並びに上部ポリマー層を形成するための94wt%のTCDD及び6wt%のK90)と同じ組成及び構造であった。このLCは、SSMの下面を保護する目的で使用し、その後の耐候性評価は行わなかった。他方のLC(上部LC)は、評価を行う実施例又は比較例の複合材バリアフィルムを含んでいた。下部LCを、平らで清浄な作用面上に、ETFE側を下にして置いた。5.5in(14cm)×8.5in(21.6cm)、0.015in(0.38mm)の厚さの封止材フィルム(JURASOLとしてJuraFilms(Downer Grove,Illinois)から入手可能)を下部LCの上面中央に置いた。
LCを約7cm×14cmの矩形試験片にレザーカットし、サンプルを保持し、またLCの裏側又はPET側から入ってくる光も遮断する金属固定具にセットした。黒色の陽極酸化アルミニウムも、LCサンプルの裏側と固定具との間に置いた。光は、LCの前側又は上側、すなわち、ETFE側を通って入った。セットしたLCサンプルを、200、400、600、及び場合によっては1000時間(hr)、以下の通り劣化させた。空気を充填した環境チャンバを、65℃及び15%の相対湿度に保った。放射線は、ASTM D7869昼光フィルターを通してキセノンアークランプにより照射した。放射照度は、340nmで昼光フィルター後の分光放射照度が1.3(W/m2)/nmとなるように制御した。ランプがついているとき、チャンバ内の黒色プレートは約90℃の温度であった。
85℃及び85%の相対湿度という条件に設定した、空気を充填した環境チャンバ(型番SE−1000−3、Thermotron Industries(Holland,Michigan))内で、暗所で、SSMを500及び1000時間劣化させた。
未劣化の及び光劣化したLCを、0.5in(1.27cm)幅のストリップにレザーカットした。ASTM D1876−08T形剥離試験法に従って、ストリップを剥離試験した。剥離試験機(Testworks 4ソフトウェアと共に「INSIGHT 2 SL」という商品名でMTS(Eden Prairie,Minnesota)から市販されている)によって、10in/min(25.4cm/min)の剥離速度で、ストリップを剥離した。複合材バリアフィルムを作製するために使用したウェブベースの蒸気コーティングプロセスでは、ストリップをウェブ方向又は機械進行方向に剥離した(比較例A、複合材バリアフィルムを製造するための一般的手順Aを参照)。個々のストリップの剥離強度は、約1.3〜15.1cmまで広げた時の剥離強度の平均として得た。報告した平均剥離強度の値は、4つのストリップの4つの剥離強度の平均である。
未劣化の又は高温高湿劣化させたSSMを、PTFEコーティングアルミニウム箔(及びエッジテープ)から上部LCを切り離すことによって分解した。次に、これらの上部LCを1.0インチ(2.54cm)幅のストリップにレザーカットし、ASTM D1876−08 T形剥離試験法に従って剥離試験した。剥離試験機(TESTWORKS 4ソフトウェアと共にINSIGHT 2 SLとしてMTS(Eden Prairie,Minnesota)から入手可能)によって、10in/min(25.4cm/min)の剥離速度で、ストリップを剥離した。複合材バリアフィルムを作製するために使用したウェブベースの蒸気コーティングプロセスでは、ストリップをウェブ方向又は機械進行方向に剥離した(比較例A、複合材バリアフィルムを製造するための一般的手順Aを参照)。個々のストリップの剥離強度は、約1.3〜15.1cmまで広げた時の剥離強度の平均として得た。報告した平均剥離強度の値は、4つのストリップの4つの剥離強度の平均である。
ASTM F−1249に従って、50℃及び100%の相対湿度(RH)で、MOCON,Inc.(Minneapolis,Minnesota)製のMOCON PERMATRAN−W Model 700 WVTR試験システムを用いて、複合材バリアフィルムの水蒸気透過速度を測定した。この機器の検出下限は0.005(g/m2)/日であった。
ASTM D−3985に従って、23℃及び0%の相対湿度(RH)で、MOCON,Inc.(Minneapolis,Minnesota)製のOX−TRAN透過率試験モデル702を用いて、複合材バリアフィルムの酸素透過速度を測定した。この機器の検出下限は、0.010(cc/m2)/日又は0.010(立方センチメートル/m2)/日であった。
複合材バリアフィルムの平均分光透過率Tvisを、入射角0°でUV−Vis分光計を用いて、400nm〜700nmの光透過率%を平均することによって、測定した。
下記の複合材バリアフィルムを製造するための一般的手順Aを行って、比較例Aの複合材バリアフィルムを製造した。下地及び上部ポリマー層になるアクリレートの選択並びにそれぞれが超音波噴霧器を通過する流速は、比較例Aに固有のものであった。
比較例Aのモノマー及び条件もまた参考までに記載している表2に明記されているように、アクリレートの選択及びそれらの超音波噴霧器を通過する各流速を変えて、比較例Aで記載されている複合材バリアフィルムを製造するための一般的手順Aを繰り返すことによって、実施例1〜2及び比較例B〜Kの複合材バリアフィルムを製造した。
Claims (22)
- 基材と、
前記基材上に配置された下地ポリマー層であって、下記式で表される少なくとも1種のジ(メタ)アクリレート
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基は一緒に、2〜7個の炭素原子を有するアルキレン基を形成する)を少なくとも60重量%含む重合性下地成分の重合反応生成物、を含む、下地ポリマー層と、
前記下地ポリマー層に結合された無機バリア層と、
前記基材とは反対側の前記無機バリア層上に配置された上部ポリマー層であって、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物、を含み、前記環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、上部ポリマー層と、
を含む、複合材物品。 - R2はメチルである、請求項1に記載の複合材物品。
- R1はHである、請求項1又は2に記載の複合材物品。
- 前記13〜24個の炭素原子を有する脂環式(メタ)アクリレートは、トリシクロデカンジメタノールジアクリレートを含む、請求項1〜3のいずれか一項に記載の複合材物品。
- 前記基材は、可撓性透明ポリマーフィルムを含む、請求項1〜4のいずれか一項に記載の複合材物品。
- 前記無機バリア層は、酸化ケイ素、酸化アルミニウム、及び酸化ケイ素アルミニウムのうちの少なくとも1つを含む、請求項1〜5のいずれか一項に記載の複合材物品。
- 前記上部ポリマー層と前記基材との間に配置された接着改質層を更に含む、請求項1〜6のいずれか一項に記載の複合材物品。
- 前記接着改質層は、接着促進層を含む、請求項7に記載の複合材物品。
- 前記上部ポリマー層上に配置された接着剤層を更に含む、請求項1〜8のいずれか一項に記載の複合材物品。
- 前記基材とは反対側の最外層に配置されたカバー層を更に含む、請求項1〜9のいずれか一項に記載の複合材物品。
- 前記基材は、ポリマーフィルム、電子ディスプレイ、電子光源、薄膜トランジスタ、及び光起電力デバイスのうちの少なくとも1つを含む、請求項1〜10のいずれか一項に記載の複合材物品。
- 基材上に下地ポリマー層を配置する工程であって、前記下地ポリマー層は、下記式で表される少なくとも1種のジ(メタ)アクリレート
各R1は独立して、H又はメチルであり、
各R2は独立して、1〜4個の炭素原子を有するアルキル基を表すか、又は2つのR2基は一緒に、2〜7個の炭素原子を有するアルキレン基を形成する)を少なくとも60重量%含む重合性下地成分の重合反応生成物を含む、工程と、
無機バリア層を前記下地ポリマー層に結合する工程と、
前記下地ポリマー層とは反対側の前記無機バリア層上に上部ポリマー層を配置する工程であって、前記上部ポリマー層は、13〜24個の炭素原子を有する脂環式(メタ)アクリレートを少なくとも60重量%含む重合性上部成分の重合反応生成物を含み、前記環構造は、置換基を除いて、C、N、O、及びSから選択される6〜14個の原子で構成されている、工程と、
を順に含む、複合材物品の製造方法。 - 前記下地ポリマー層は、前記重合性下地成分の蒸着を含むプロセスによって形成される、請求項12に記載の方法。
- 前記上部ポリマー層は、前記重合性上部成分の蒸着を含むプロセスによって形成される、請求項12又は13に記載の方法。
- 前記無機バリア層は、前記下地ポリマー層が前記基材上に配置される間に、前記下地ポリマー層上にスパッタ蒸着される、請求項12〜14のいずれか一項に記載の方法。
- 前記上部ポリマー層と前記基材との間に接着改質層を配置する工程を更に含む、請求項12〜15のいずれか一項に記載の方法。
- 前記接着改質層は、接着促進層を含む、請求項16に記載の方法。
- 前記上部ポリマー層上に接着剤層を配置する工程を更に含む、請求項12〜17のいずれか一項に記載の方法。
- 前記基材とは反対側の前記接着剤層上にカバー層を配置する工程を更に含む、請求項18に記載の方法。
- 前記基材は、ポリマーフィルム、電子ディスプレイ、電子光源、薄膜トランジスタ、及び光起電力デバイスのうちの少なくとも1つを含む、請求項12〜19のいずれか一項に記載の方法。
- 前記重合性下地成分は、ネオペンチルグリコールジ(メタ)アクリレートを含む、請求項12〜20のいずれか一項に記載の方法。
- 前記重合性上部成分は、トリシクロデカンジメタノールジアクリレートを含む、請求項12〜21のいずれか一項に記載の方法。
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