JP6263122B2 - 特に電子的装置のカプセル化のための接着剤 - Google Patents
特に電子的装置のカプセル化のための接着剤 Download PDFInfo
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- JP6263122B2 JP6263122B2 JP2014536260A JP2014536260A JP6263122B2 JP 6263122 B2 JP6263122 B2 JP 6263122B2 JP 2014536260 A JP2014536260 A JP 2014536260A JP 2014536260 A JP2014536260 A JP 2014536260A JP 6263122 B2 JP6263122 B2 JP 6263122B2
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Landscapes
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Description
(a)少なくともコモノマー種としてのイソブチレンまたはブチレンと、仮想的ホモポリマーと見なして40℃超の軟化温度(softening temperature)を有する少なくとも1つのコモノマー種とを含む少なくとも1種のコポリマー、
(b)少なくとも部分的に水素化された接着樹脂の少なくとも1種、
(c)環状エーテルをベースとし、軟化温度が40℃未満、好ましくは20℃未満の反応性樹脂の少なくとも1種、
(d)カチオン硬化を開始するための光開始剤の少なくとも1種
を含む接着剤、好ましくは感圧接着剤に関する。
・ スルホニウム塩(例えばUS4,231,951A(特許文献14)、US4,256,828A(特許文献15)、US4,058,401A(特許文献16)、US4,138,255A(特許文献17)、およびUS2010/063221A1(特許文献18)を参照)、例えばトリフェニルスルホニウムヘキサフルオロアルセネート、
トリフェニルスルホニウムヘキサフルオロボレート、
トリフェニルスルホニウムテトラフルオロボレート、
トリフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
メチルジフェニルスルホニウムテトラフルオロボレート、
メチルジフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
ジメチルフェニルスルホニウムヘキサフルオロホスフェート、
トリフェニルスルホニウムヘキサフルオロホスフェート、
トリフェニルスルホニウムヘキサフルオロアンチモネート、
ジフェニルナフチルスルホニウムヘキサフルオロアルセネート、
トリトリルスルホニウムヘキサフルオロホスフェート、
アニシルジフェニルスルホニウムヘキサフルオロアンチモネート、
4−ブトキシフェニルジフェニルスルホニウムテトラフルオロボレート、
4−ブトキシフェニルジフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
4−クロロフェニルジフェニルスルホニウムヘキサフルオロアンチモネート、
トリス(4−フェノキシフェニル)スルホニウムヘキサフルオロホスフェート、
ジ(4−エトキシフェニル)メチルスルホニウムヘキサフルオロアルセネート、
4−アセチルフェニルジフェニルスルホニウムテトラフルオロボレート、
4−アセチルフェニルジフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
トリス(4−チオメトキシフェニル)スルホニウムヘキサフルオロホスフェート、
ジ(メトキシスルホニルフェニル)メチルスルホニウムヘキサフルオロアンチモネート、ジ(メトキシナフチル)メチルスルホニウムテトラフルオロボレート、
ジ(メトキシナフチル)メチルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
ジ(カルボメトキシフェニル)メチルスルホニウムヘキサフルオロホスフェート、
(4−オクチルオキシフェニル)ジフェニルスルホニウムテトラキス(3,5−ビス−トリフルオロメチルフェニル)ボレート、
トリス[4−(4−アセチルフェニル)チオフェニル]スルホニウムテトラキス(ペンタフルオロフェニル)ボレート、
トリス(ドデシルフェニル)スルホニウムテトラキス(3,5−ビス−トリフルオロメチルフェニル)ボレート、
4−アセトアミドフェニルジフェニルスルホニウムテトラフルオロボレート、
4−アセトアミドフェニルジフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
ジメチルナフチルスルホニウムヘキサフルオロホスフェート、
トリフルオロメチルジフェニルスルホニウムテトラフルオロボレート、
トリフルオロメチルジフェニルスルホニウムテトラキス(ペンタフルオロベンジル)ボレート、
フェニルメチルベンジルスルホニウムヘキサフルオロホスフェート、
5−メチルチアントレニウムヘキサフルオロホスフェート、
10−フェニル−9,9−ジメチルチオキサンテニウムヘキサフルオロホスフェート、10−フェニル−9−オキソチオキサンテニウムテトラフルオロボレート、
10−フェニル−9−オキソチオキサンテニウムテトラキス(ペンタフルオロベンジル)ボレート、5−メチル−10−オキソチアントレニウムテトラフルオロボレート、
5−メチル−10−オキソチアントレニウムテトラキス(ペンタフルオロベンジル)ボレート、
および5−メチル−10,10−ジオキソチアントレニウムヘキサフルオロホスフェートであり、
・ ヨードニウム塩(例えばUS3,729,313A(特許文献19)、US3,741,769A(特許文献20)、US4,250,053A(特許文献21)、US4,394,403A(特許文献22)、およびUS2010/063221A1(特許文献18)を参照)、例えばジフェニルヨードニウムテトラフルオロボレート、
ジ(4−メチルフェニル)ヨードニウムテトラフルオロボレート、
フェニル−4−メチルフェニルヨードニウムテトラフルオロボレート、
ジ(4−クロルフェニル)ヨードニウムヘキサフルオロホスフェート、ジナフチルヨードニウムテトラフルオロボレート、
ジ(4−トリフルオロメチルフェニル)ヨードニウムテトラフルオロボレート、
ジフェニルヨードニウムヘキサフルオロホスフェート、
ジ(4−メチルフェニル)ヨードニウムヘキサフルオロホスフェート、
ジフェニルヨードニウムヘキサフルオロアルセネート、
ジ(4−フェノキシフェニル)ヨードニウムテトラフルオロボレート、
フェニル−2−チエニルヨードニウムヘキサフルオロホスフェート、
3,5−ジメチルピラゾリル−4−フェニルヨードニウムヘキサフルオロホスフェート、ジフェニルヨードニウムヘキサフルオロアンチモネート、
2,2’−ジフェニルヨードニウムテトラフルオロボレート、
ジ(2,4−ジクロルフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(4−ブロムフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(4−メトキシフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(3−カルボキシフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(3−メトキシカルボニルフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(3−メトキシスルホニルフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(4−アセトアミドフェニル)ヨードニウムヘキサフルオロホスフェート、
ジ(2−ベンゾチエニル)ヨードニウムヘキサフルオロホスフェート、
ジアリールヨードニウムトリストリフルオロメチルスルホニルメチド、例えばジフェニルヨードニウムヘキサフルオロアンチモネート、
ジアリールヨードニウムテトラキス(ペンタフルオロフェニル)ボレート、例えばジフェニルヨードニウムテトラキス(ペンタフルオロフェニル)ボレート、
(4−n−シロキシフェニル)フェニルヨードニウムヘキサフルオロアンチモネート、
[4−(2−ヒドロキシ−n−テトラシロキシ)フェニル]フェニルヨードニウムヘキサフルオロアンチモネート、
[4−(2−ヒドロキシ−n−テトラシロキシ)フェニル]フェニルヨードニウムトリフルオロスルホネート、
[4−(2−ヒドロキシ−n−テトラシロキシ)フェニル]フェニルヨードニウムヘキサフルオロホスフェート、
[4−(2−ヒドロキシ−n−テトラシロキシ)フェニル]フェニルヨードニウムテトラキス(ペンタフルオロフェニル)ボレート、
ビス(4−tert−ブチルフェニル)ヨードニウムヘキサフルオロアンチモネート、
ビス(4−tert−ブチルフェニル)ヨードニウムヘキサフルオロホスフェート、
ビス(4−tert−ブチルフェニル)ヨードニウムトリフルオロスルホネート、
ビス(4−tert−ブチルフェニル)ヨードニウムテトラフルオロボレート、ビス(ドデシルフェニル)ヨードニウムヘキサフルオロアンチモネート、
ビス(ドデシルフェニル)ヨードニウムテトラフルオロボレート、
ビス(ドデシルフェニル)ヨードニウムヘキサフルオロホスフェート、
ビス(ドデシルフェニル)ヨードニウムトリフルオロメチルスルホネート、
ジ(ドデシルフェニル)ヨードニウムヘキサフルオロアンチモネート、ジ(ドデシルフェニル)ヨードニウムトリフレート、
ジフェニルヨードニウムビスルフェート、4,4’−ジクロロジフェニルヨードニウムビスルフェート、
4,4’−ジブロモジフェニルヨードニウムビスルフェート、
3,3’−ジニトロジフェニルヨードニウムビスルフェート、4,4’−ジメチルジフェニルヨードニウムビスルフェート、
4,4’−ビス−スクシンイミドジフェニルヨードニウムビスルフェート、3−ニトロジフェニルヨードニウムビスルフェート、
4,4’−ジメトキシジフェニルヨードニウムビスルフェート、
ビス−(ドデシルフェニル)ヨードニウムテトラキス(ペンタフルオロフェニル)ボレート、
(4−オクチルオキシフェニル)フェニルヨードニウムテトラキス(3,5−ビス−トリフルオロメチルフェニル)ボレート、
および(トリルクミル)ヨードニウムテトラキス(ペンタフルオロフェニル)ボレートであり、ならびに
・ フェロセニウム塩(例えばEP542716B1(特許文献23)を参照)、例えばη5(2,4−シクロペンタジエン−1−イル)−[(1,2,3,4,5,6,9)−(1−メチルエチル)ベンゼン]鉄である。
・可塑剤、例えば可塑化オイル、もしくは例えば低分子ポリブテンなどの低分子液体ポリマー
・一次酸化防止剤、例えば立体障害フェノール
・二次酸化防止剤、例えばホスファイトもしくはチオエーテル
・プロセス安定化剤、例えばC−ラジカルスカベンジャー
・光保護剤、例えばUV吸収剤もしくは立体障害アミン
・加工助剤
・湿潤添加剤
・付着促進剤
・末端ブロック強化樹脂、ならびに/または
・場合によっては、好ましくはエラストマー性質のさらなるポリマー;これに対応して利用可能なエラストマーに含まれるのは、なかでも純粋な炭化水素をベースとするエラストマー、例えば天然のもしくは合成されたポリイソプレンもしくはポリブタジエンのような不飽和ポリジエン、化学的に実質的に飽和状態のエラストマー、例えば飽和エチレンプロピレンコポリマー、α−オレフィンコポリマー、ポリイソブチレン、ブチルゴム、エチレンプロピレンゴム、および化学的に官能化された炭化水素、例えばハロゲン含有の、アクリレート含有の、アリル含有の、もしくはビニルエーテル含有のポリオレフィンである。
・水蒸気および酸素の低い体積浸透性、これは、WVTRの値(Mocon)が10g/m2d未満で、OTRの値(Mocon)が1000cm3/m2・d・bar未満であることから明らかである。
・水蒸気および酸素の低い界面浸透性、これは、WVTRの値(Ca試験)が1g/m2d未満であることから明らかであり、目標土台上への接着剤の優れた表面流動をもたらす。
・任意選択であるが好ましくは、透過率が好ましくは90%超の高い透明性
・任意選択であるが好ましくは、5.0%未満、好ましくは2.5%未満のヘイズ
・例えばロール・ツー・ロール・プロセスにおける秀でたラミネート挙動、これは、ガラス上での未架橋の系の接着力が1.5N/cm超、好ましくは2.5N/cm超、およびガラス上での架橋された系の動的せん断強度が25N/cm2超、好ましくは50N/cm2超、非常に好ましくは100N/cm2超であることから明らかである。
接着力
接着力の決定は以下のように実施した。すなわち、規定の被接着下地としてガラスプレート(フロートガラス)を用いた。貼付可能な平面要素には、比較的容易に剥離するライナーの側に、36μmのPETフィルムを貼り合わせた。試験すべき貼付可能な平面要素を幅20mmおよび長さ約25cmに裁断し、把持区間を設け、その直後に4kgのスチールローラを用いて10m/minの送りで、それぞれ選択された被接着下地に5回押しつけた。その後すぐ、このようにして貼り付けた平面要素を、引張試験機(Zwick社)を用いて180°の角度で、室温および300mm/minで被接着下地から剥ぎ取り、このために必要な力を測定した。測定値(単位はN/cm)は、3回の個別の測定からの平均値として示した。試験は、未架橋のサンプルで行われた。
酸素(OTR)および水蒸気(WVTR)に関する浸透性の決定は、DIN53380の第3部またはASTM F−1249に基づいて行われる。このために感圧接着剤を50μmの層厚で、透過性の膜の上に置く。酸素透過性は23℃および相対湿度50%で、測定機Mocon OX−Tran2/21を用いて測定する。水蒸気透過性は37.5℃および相対湿度90%で決定する。
電子構成物の耐用期間を決定するための尺度としてカルシウム試験を採用した。カルシウム試験を図4に示している。これについては真空中で、20×20mm2の大きさの薄いカルシウム層23をガラスプレート21上に堆積させ、その後、窒素雰囲気下で貯蔵する。カルシウム層23の厚さは約100nmである。カルシウム層23をカプセル化するために、試験すべき接着剤22および支持体材料としての柔軟な薄いガラス板24(35μm、Schott社)を備えた接着テープ(26×26mm2)を使用する。薄いガラス板は安定化のため、光学的に高透明性のアクリレート感圧接着剤の50μm厚の転写式接着テープ25により、100μm厚のPETフィルム26でラミネートしていた。接着剤22がすべての側ではみ出した3mmの縁(A−A)を設けてカルシウム面23を覆うように、接着剤22をガラスプレート21上に適用する。非透過性のガラス支持体24により、感圧接着剤を通るかまたは界面に沿った浸透だけが確定される。
接着樹脂軟化温度は、環球法として知られておりASTM E28に基づいて標準化されている該当する方法論に基づいて実施される。
コポリマー、硬質ブロックおよび軟質ブロック、ならびに未硬化の反応性樹脂の軟化温度は、DIN53765:1994−03に基づき、示差走査熱量測定(DSC)による熱量測定によって決定する。加熱曲線は、加熱速度10K/minで延びている。サンプルは、穴の開いた蓋を備えたAl製るつぼ内で、窒素雰囲気中で測定する。第2の加熱曲線を評価する。非晶質の物質の場合はガラス転移温度が生じ、(半)結晶性の物質の場合は溶融温度が生じる。ガラス転移は、サーモグラムにおける段として認識可能である。ガラス転移温度はこの段の中心点として評価する。溶融温度は、サーモグラムにおけるピークとして認識可能である。実熱量が最大になる温度を溶融温度として記録する。
接着剤の透過性をVISスペクトルにより決定した。VISスペクトルの撮影は、Kontron社のUVIKON923で実施した。測定されるスペクトルの波長領域は、1nmの解像度で、800nm〜400nmの間の全波長を含んでいる。参照としてエンプティチャネル測定(Leerkanalmessung)をこの波長領域全体にわたり実施した。結果を提示するために、上記領域内での透過性測定の平均値が求められた。界面反射損失の補整は行わない。
ヘイズ値は、透過される光のうち、光を通された試料により前方へ大きな角度で散乱される割合を表す。つまりヘイズ値は、クリアな見通しを妨害する表面または構造物内での材料欠陥を定量化する。
モル質量とも言う平均分子量MW(重量平均)の決定は、ゲル浸透クロマトグラフィ(GPC)によって行う。溶離液として、トリフルオロ酢酸0.1体積%を含むTHFを用いる。測定は25℃で行う。プレカラムとして、PSS−SDV、5μm、103Å、ID8.0mm×50mmを使用する。分離にはカラムPSS−SDV、5μm、103Å、105Å、および106Åを、それぞれID8.0mm×300mmで用いる。試料濃度は4g/lであり、貫流量は1分当たり1.0mlである。PS標準に対して測定する。
転写式接着テープを2枚のガラスプレート(フロートガラス)の間に貼り付け、UV光で硬化させる。24時間の貯蔵後、この複合体を、23℃および相対湿度50%で、両方のガラスプレートを180°の角度で互いから引き離すように、引張試験機において50mm/minで分離し、最大力をN/cm2で確定する。これに関しては一辺の長さが25mmの正方形の試験サンプルを試験する。
例1
例2
例3
例4
例5
例6
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例8
例9
例10
Claims (23)
- (a)少なくともコモノマー種としてのイソブチレンと、仮想的ホモポリマーと見なして40℃超の軟化温度を有する少なくとも1つのコモノマー種とを含む少なくとも1種のコポリマー、
ここで、当該1種または複数のコポリマーが、軟化温度が−20℃未満の第1のポリマーブロック(「軟質ブロック」)の少なくとも1種と、軟化温度が+40℃超の第2のポリマーブロック(「硬質ブロック」)の少なくとも1種とを有するブロックコポリマー、星型コポリマー、および/またはグラフトコポリマーであり、
かつ、
軟質ブロックが非極性に形成されており、かつイソブチレンをホモポリマーブロックまたはコポリマーブロックとして含んでおり、
硬質ブロックが、スチレンおよび/またはスチレン誘導体から形成されており、
(b)少なくとも部分的に水素化された接着樹脂の少なくとも1種、
ここで、1種または複数の接着樹脂が、少なくとも70%の水素化度を有し、かつ、45〜71℃のDACP値および72〜82℃のMMAP値を有し、
(c)環状エーテルをベースとし、少なくとも1つのエポキシド基を担持し、軟化温度が40℃未満の反応性樹脂の少なくとも1種、
(d)カチオン硬化を開始するための光開始剤の少なくとも1種
を含む、浸透物に対する電子的装置のカプセル化のための接着剤。 - 1種または複数のコポリマーが、モル質量MWが300,000g/mol以下の統計コポリマー、交互コポリマー、ブロックコポリマー、星型コポリマー、および/またはグラフトコポリマーであることを特徴とする請求項1に記載の接着剤。
- 1種または複数のコポリマーが、モル質量MWが200,000g/mol以下の統計コポリマー、交互コポリマー、ブロックコポリマー、星型コポリマー、および/またはグラフトコポリマーであることを特徴とする請求項1に記載の接着剤。
- 軟質ブロックが非極性に形成されており、かつイソブチレンをホモポリマーブロックまたはコポリマーブロックとして含んでおり、イソブチレンがそれ自体と、または、非極性コモノマーと共重合されていることを特徴とする請求項1〜3のいずれか一つに記載の接着剤。
- 前記反応性樹脂の軟化温度が20℃未満である、請求項1〜4のいずれか一つに記載の接着剤。
- 少なくとも1種のブロックコポリマーが、2つの末端にある硬質ブロックおよび1つの真ん中にある軟質ブロックから形成されるトリブロックコポリマーであることを特徴とする請求項1〜5のいずれか一つに記載の接着剤。
- 1種または複数の接着樹脂が、少なくとも95%の水素化度を有することを特徴とする請求項1〜6のいずれか一つに記載の接着剤。
- 接着剤が、少なくとも1種の脂肪族または環状脂肪族の反応性樹脂を含むことを特徴とする請求項1〜7のいずれか一つに記載の接着剤。
- 接着剤が、350nm未満でUV光を吸収してカチオン硬化を可能にし、スルホニウム、ヨードニウム、およびメタロセンをベースとする系である光開始剤を含むことを特徴とする請求項1〜8のいずれか一つに記載の接着剤。
- 接着剤が、250nm超〜350nm未満でUV光を吸収する光開始剤を含むことを特徴とする請求項1〜9のいずれか一つに記載の接着剤。
- 感圧接着剤が、可塑剤、一次酸化防止剤、二次酸化防止剤、プロセス安定化剤、光保護剤、加工助剤、末端ブロック強化樹脂、ポリマーから成る群から選択された1種または複数の添加剤を含むことを特徴とする請求項1〜10のいずれか一つに記載の接着剤。
- 感圧接着剤が、ナノスケールの充填剤、透明な充填剤、ならびに/またはゲッターおよび/もしくはスカベンジャー充填剤から選択される1種または複数の充填剤を含むことを特徴とする請求項1〜11のいずれか一つに記載の接着剤。
- 接着剤が、スペクトルの可視光(約400nm〜800nmの波長領域)内で透明であることを特徴とする請求項1〜12のいずれか一つに記載の接着剤。
- 接着剤のヘイズが、5.0%未満を示すことを特徴とする請求項1〜13のいずれか一つに記載の接着剤。
- 接着剤のヘイズが、2.5%未満を示すことを特徴とする請求項1〜14のいずれか一つに記載の接着剤。
- 請求項1〜15のいずれか一つに記載の接着剤の少なくとも1つの層および支持体を含む接着テープにおいて、
支持体が、WVTR<0.1g/(m2d)およびOTR<0.1cm3/(m2d bar)の浸透バリアを有することを特徴とする接着テープ。 - 支持体が、コーティングされたプラスチックフィルムであることを特徴とする請求項16に記載の接着テープ。
- 支持体が、最大1mmの層厚の柔軟な薄いガラスの層を有しており、前記支持体が、最大1mmの層厚の薄いガラスの層から成り、前記薄いガラスがホウケイ酸ガラスまたはアルカリを含有しないアルミノホウケイ酸ガラスであることを特徴とする請求項16に記載の接着テープ。
- 薄いガラスが、テープ状の幾何形状で存在することを特徴とする請求項18に記載の接着テープ。
- (光)電子的装置のカプセル化のための請求項1〜19のいずれか一つに記載の接着剤または接着剤を用いて形成された片面または両面で接着性の接着テープの使用。
- 感圧接着剤および/または電子的装置のカプセル化すべき領域が、感圧接着剤の適用の前、最中、および/または後に加熱されることを特徴とする請求項20に記載の使用。
- 感圧接着剤が、電子的装置への適用後に、部分的または最終的に架橋されることを特徴とする請求項20または21に記載の使用。
- 電子構造物と感圧接着剤とを備えており、
電子構造物が少なくとも部分的には感圧接着剤によりカプセル化されている電子的装置において、
感圧接着剤が請求項1〜22のいずれか一つに基づいて形成されていることを特徴とする電子的装置。
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WO2011017298A1 (en) * | 2009-08-04 | 2011-02-10 | 3M Innovative Properties Company | Non-halogentaed polyisobutylene -thermoplastic elastomer blend pressure sensitive adhesives |
-
2012
- 2012-02-16 DE DE102012202377A patent/DE102012202377A1/de not_active Withdrawn
- 2012-10-19 PL PL12775254T patent/PL2768919T3/pl unknown
- 2012-10-19 EP EP12775254.1A patent/EP2768919B1/de active Active
- 2012-10-19 WO PCT/EP2012/070779 patent/WO2013057265A1/de active Application Filing
- 2012-10-19 US US14/351,800 patent/US20140315016A1/en not_active Abandoned
- 2012-10-19 CN CN201280063692.3A patent/CN104011161B/zh active Active
- 2012-10-19 KR KR1020147013553A patent/KR101959973B1/ko active IP Right Grant
- 2012-10-19 JP JP2014536260A patent/JP6263122B2/ja active Active
- 2012-10-19 MX MX2014004595A patent/MX2014004595A/es active IP Right Grant
- 2012-10-19 BR BR112014009386A patent/BR112014009386A2/pt not_active Application Discontinuation
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Also Published As
Publication number | Publication date |
---|---|
KR101959973B1 (ko) | 2019-03-19 |
CN104011161B (zh) | 2016-08-31 |
CN104011161A (zh) | 2014-08-27 |
JP2014534309A (ja) | 2014-12-18 |
MX2014004595A (es) | 2014-05-27 |
BR112014009386A2 (pt) | 2017-04-18 |
WO2013057265A1 (de) | 2013-04-25 |
TWI572689B (zh) | 2017-03-01 |
TW201345996A (zh) | 2013-11-16 |
KR20140090636A (ko) | 2014-07-17 |
DE102012202377A1 (de) | 2013-04-25 |
EP2768919B1 (de) | 2015-08-05 |
PL2768919T3 (pl) | 2016-01-29 |
EP2768919A1 (de) | 2014-08-27 |
US20140315016A1 (en) | 2014-10-23 |
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