JP5449136B2 - フルオロポリマー被膜フィルム、それの形成方法、およびフルオロポリマー液体組成物 - Google Patents
フルオロポリマー被膜フィルム、それの形成方法、およびフルオロポリマー液体組成物 Download PDFInfo
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- JP5449136B2 JP5449136B2 JP2010506222A JP2010506222A JP5449136B2 JP 5449136 B2 JP5449136 B2 JP 5449136B2 JP 2010506222 A JP2010506222 A JP 2010506222A JP 2010506222 A JP2010506222 A JP 2010506222A JP 5449136 B2 JP5449136 B2 JP 5449136B2
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- fluoropolymer
- urethane
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- substrate film
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Description
本発明の一態様に従ってフルオロポリマー被膜フィルムに有用なフルオロポリマーは、フッ化ビニル(VF)のホモポリマーおよびコポリマーならびにフッ化ビニリデン(VF2)のホモポリマーおよびコポリマーから選択される。一実施形態では、フルオロポリマーは、フッ化ビニルのホモポリマーおよび少なくとも60モル%のフッ化ビニルを含むコポリマーならびにフッ化ビニリデンのホモポリマーおよび少なくとも60モル%のフッ化ビニリデンを含むコポリマーから選択される。より具体的な実施形態では、フルオロポリマーは、フッ化ビニルのホモポリマーおよび少なくとも80モル%のフッ化ビニルを含むコポリマーならびにフッ化ビニリデンのホモポリマーおよび少なくとも80モル%のフッ化ビニリデン含むコポリマーから選択される。フルオロポリマーと非フルオロポリマー、例えば、アクリルポリマーとのブレンド物もまた、本発明の幾つかの態様の実施に好適であるかもしれない。ホモポリマーポリフッ化ビニル(PVF)およびホモポリマーポリフッ化ビニリデン(PVDF)は、本発明の具体的な態様の実施に好適である。ホモポリマーポリフッ化ビニルおよびフッ化ビニルのコポリマーから選択されたフルオロポリマーが、本発明の実施に特に有効である。
本発明の一態様によるフルオロポリマー被膜フィルムに用いられる相溶性の架橋可能な接着性ポリマーは、カルボン酸、スルホン酸、アジリジン、アミン、イソシアネート、メラミン、エポキシ、ヒドロキシル、無水物およびそれらの組み合わせから選択された官能基を含む。一実施形態では、相溶性の架橋可能な接着性ポリマーは、(1)組成物中のフルオロポリマーと相溶性であるバックボーン組成と(2)基材フィルム表面上の補足的な官能基と反応することができるペンダント官能性とを有する。架橋可能な接着性ポリマーバックボーンとフルオロポリマーとの相溶性は変化するであろうが、相溶性の架橋可能な接着性ポリマーがフルオロポリマーコーティングを高分子基材フィルムに固定するために望ましい量でフルオロポリマー中へ導入できる程に十分なものである。しかしながら一般に、主としてフッ化ビニルおよびフッ化ビニリデンから誘導されたホモポリマーおよびコポリマーは、上記の官能基を有するアクリル、ウレタン、脂肪族ポリエステル、ポリエステルウレタン、ポリエーテル、エチレンビニルアルコールコポリマー、アミド、アクリルアミド、ウレアおよびポリカーボネート・バックボーンに有利に働く相溶性特性を示すであろう。
必要ならば、様々な色、不透明度および/または他の特性効果は、製造中に顔料およびフィラーをフルオロポリマーコーティング組成物分散系中へ組み込むことによって達成することができる。一実施形態では、顔料は、フルオロポリマー固形分を基準として約1〜約35重量%の量で使用される。使用できる典型的な顔料には、無機ケイ質顔料(例えば、シリカ顔料)などの透明な顔料、および通常の顔料の両方が含まれる。使用できる通常の顔料には、二酸化チタン、および酸化鉄などの金属酸化物;金属水酸化物;アルミニウムフレークなどの金属フレーク;クロム酸鉛などのクロム酸塩;硫化物;硫酸塩;炭酸塩;カーボンブラック;シリカ;タルク;陶土;フタロシアニンブルーおよびグリーン、有機レッド;有機えび茶色ならびに他の有機顔料および染料が含まれる。一実施形態では、顔料のタイプおよび量は、フィルム形成中に用いられるかもしれない高い処理温度での安定性のために選択されるだけでなく、フルオロポリマーコーティングの望ましい特性、例えば、耐候性にいかなる有意な悪影響も避けるように選択される。
フルオロポリマーコーティング組成物は、添加剤として1つ以上の光安定剤を含有してもよい。光安定剤添加剤には、ヒドロキシベンゾフェノンおよびヒドロキシベンゾトリアゾールなどの紫外線を吸収する化合物が含まれる。他の可能な光安定剤添加剤には、ヒンダードアミン光安定剤(HALS)および酸化防止剤が含まれる。必要ならば熱安定剤もまた使用することができる。
一実施形態では、フルオロポリマーコーティング組成物はバリア粒子を含む。具体的な実施形態では、粒子は小板形状の粒子である。かかる粒子は、水、溶剤および酸素などのガスが粒子それら自体を容易に通過することができないので、コーティングの塗布中に整列する傾向があり、水、溶剤およびガスの浸透を低下させる機械的バリアが生じたコーティング中に形成される。太陽電池モジュールで、例えば、バリア粒子は、フルオロポリマーの防湿性を実質的に増加させ、太陽電池に提供される保護を高める。幾つかの実施形態では、バリア粒子は、コーティング中にフルオロポリマー組成物の総乾燥重量を基準として約0.5〜約10重量%の量で存在する。
フルオロポリマー液体コーティング組成物は、フルオロポリマーの溶液の形態か分散系の形態かのいずれかでフルオロポリマーを含有してもよい。フルオロポリマーの典型的な溶液または分散系は、フィルム形成/乾燥工程中に泡立ち形成を避けるのに十分に高い沸点を有する溶剤を使用して調製される。分散形態のポリマーについては、フルオロポリマーの融合に役立つ溶剤が望ましい。これらの溶液または分散系中のポリマー濃度は、溶液の作業可能な粘度を達成するために調節され、特定のポリマー、組成物の他の成分、ならびに用いられるプロセス設備およびプロセス条件で変わるであろう。一実施形態では、溶液については、フルオロポリマーは、組成物の総重量を基準として約10重量%〜約25重量%の量で存在する。別の実施形態では、分散系については、フルオロポリマーは、液体組成物の総重量を基準として約25重量%〜約50重量%の量で存在する。
本発明に使用される高分子基材フィルムは、広範な数のポリマーから選択されてもよく、熱可塑性樹脂が、より高い加工温度に耐えるそれらの能力のために望ましい。高分子基材フィルムは、相溶性の架橋可能な接着性ポリマー、架橋剤、または両方と相互作用して基材フィルムへのフルオロポリマーコーティングの結合を促進する官能基をその表面上に含む。一実施形態では、高分子基材フィルムはポリエステル、ポリアミドまたはポリイミドである。具体的な実施形態では、高分子基材フィルム用のポリエステルは、ポリエチレンテレフタレート、ポリエチレンナフタレートおよびポリエチレンテレフタレート/ポリエチレンナフタレートの共押出物から選択される。
どの、化学物質暴露によって達成することができる。あるいはまた、表面は、反対面を冷却しながら一面または両面を直火に曝すことによって活性化することができる。表面活性化はまた、コロナ処理または大気窒素プラズマ処理などの高周波数スパーク放電にフィルムをかけることによって達成することもできる。さらに、表面活性化は、フィルムを形成するときに高分子基材中へ相溶性コモノマーを組み込むことによって達成することができる。当業者は、相溶性官能基を高分子基材フィルムの表面上に形成するために使用されてもよい多種多様な方法を理解するであろう。
本発明の一態様に従ってフルオロポリマー被膜フィルムを製造するためのフルオロポリマー組成物は、予め形成されたフィルムを形成する必要が全くなしに通常のケーティング方法によって好適な高分子基材フィルムに液体として直接塗布することができる。かかるコーティングの製造技法には、キャスティング、浸し塗り、吹き付け塗りおよび塗装の従来法が含まれる。フルオロポリマーコーティングが分散形態のフルオロポリマーを含有するとき、それは、スプレー、ロール、ナイフ、カーテン、グラビヤ塗布機などの、従来手段、または縞もしくは他の欠陥なしに一様なコーティングの塗布を可能にする任意の他の方法を用いて、基材フィルム上へ分散系をキャストすることによって典型的に塗布される。一実施形態では、キャストされた分散系の乾燥コーティング厚さは、約2.5μm(0.1ミル)〜約250μm(10ミル)、より具体的な実施形態では約13μm(0.5ミル)〜約130μm(5ミル)である。
フルオロポリマー被膜フィルムは、太陽電池モジュールに特に有用である。太陽電池モジュールのための典型的な構成は、透明張り材料としてガラスの厚い層を含む。ガラスは、架橋エチレン酢酸ビニルなどの耐湿性プラスチックシーリング配合物中に埋め込まれている結晶性シリコンウェーハおよびワイヤを含む太陽電池を保護する。あるいはまた、薄膜太陽電池は、封止材料で両面にまた覆いを付けられているキャリアシート上のCIGS(銅−インジウム−ガリウム−セレン化物)、CTS(カドミウム−テルル−スルフィド)、a−Si(非晶質シリコン)およびその他などの、様々な半導体材料から適用することができる。バックシートが封止材料に接着される。フルオロポリマー被膜フィルムは、かかるバックシートのために有用である。フルオロポリマーコーティングは、カルボン酸、スルホン酸、アジリジン、無水物、アミン、イソシアネート、メラミン、エポキシ、ヒドロキシル、およびそれらの組み合わせから選択された官能基を含有する相溶性の架橋可能な接着性ポリマーとブレンドされたフッ化ビニルのホモポリマーおよびコポリマーならびにフッ化ビニリデンのホモポリマーおよびコポリマーから選択されたフルオロポリマーを含む。高分子基材フィルムは、相溶性の架橋可能な接着性ポリマーと相互作用して基材フィルムへのフルオロポリマーコーティングの結合を促進する官能基をその表面上に含む。一実施形態では、高分子基材フィルムは、ポリエステル、より具体的な実施形態では、ポリエチレンテレフタレート、ポリエチレンナフタレートおよびポリエチレンテレフタレート/ポリエチレンナフタレート共押出物からなる群から選択されたポリエステルである。ポリエステルは、電気絶縁性および防湿性を提供し、バックシートの経済的な構成要素である。幾つかの実施形態では、高分子基材フィルムの両面は、フルオロポリマーで被膜され、フルオロポリマーのコーティングの2層間のポリエステルのサンドイッチを生み出す。フルオロポリマーフィルムは、優れた強度、耐候性、耐UV性、および防湿性をバックシートに与える。
180度剥離強度
剥離強度は、モデル4201 Instronを2インチ/分で使用し、ピーク値を記録し、3サンプルを平均して測定する(ASTM D1876−01 T−剥離試験(T−Peel Test))。サンプルが剥離開始工程中に手動により容易に剥離する場合には、0の値を記録した。
湿潤キャビネットから取り出した後、サンプルをカミソリナイフおよび直線エッジで切り込み線を入れて1/4インチ幅のストリップを生成する。1インチ突出部を取っ手として使用し、このタブを、フィルムが破壊するかまたは剥離が生じるかのいずれかまで、ゆっくりした等張力で、おおよそ180度の角度で引っ張る。EVA/ガラス界面かEVA/フルオロポリマーコーティング界面かのいずれかでのフィルム破壊および剥離は、合格結果と考えられる。フルオロポリマーコーティングとPET基材との間の剥離は、不合格と考えられる。
湿潤キャビネットから取り出した後、サンプルを、ステンレススチール型板の支援下に、カミソリナイフで切り込み線を入れて、フィルムを貫いてガラス表面まで、約3/32インチ(2.4mm)離れた、11の平行な切れ目を作る。この手順を、第1切れ目に直角に繰り返して100の正方形の格子を生成する。透明なテープ(3M Brand No.467 PSAテープ)のストリップ、0.75×2.16インチ(1.9×5.5cm)を、テープが刻印線に平行の方向に向いた状態で、刻印区域の一面に強く押し付ける。テープを次に90°角度で素速く、しかしぐいと引っ張ることなく引き離す。フルオロポリマーコーティングとPET基材との間のいかなる破損も不合格と考えられる。
実施例1
実施例1は、未改質高分子基材フィルムへのフルオロポリマーコーティングの接着を実証する。ヘキサメチレンジイソシアネートのイソシアヌレート三量体(Desmodur(登録商標)N−3300、Bayer MaterialScience)を使用してPVFベースのフルオロポリマーコーティングへ架橋された様々なポリエステルジオールおよびトリオール(Desmophen(登録商標)、Bayer MaterialScience)は、未改質PETへの接着性を示す。表1に示すポリエステルは代表的なものである。
1.表1に示すポリエステルのそれぞれを、プロピレンカーボネート中の42%固形分PVF分散系(プロピレンカーボネート中のポリエステルの50%固形分溶液を使用する100部PVF当たり30部ポリエステル)、ポリエステルヒドロキシル含有率に対して当量のDesmodur(登録商標)N−3300(ポリイソシアネート架橋剤)および100部PVF当たり0.02部ジブチルスズジラウレートと組み合わせた。
実施例2は、未改質高分子基材フィルム上のフルオロポリマーコーティングの接着強度への相溶性の架橋接着性ポリマー組成物の影響を実証する。幾つかの相溶性の架橋接着性ポリマーは、他のものより良好に機能し、はるかにより低い濃度で接着を促進することができる。表3は、100部PVF当たり10〜30部ポリエステルに変えたDesmophen(登録商標)F−2060BおよびS−101P−55ポリエステルについての結果を示す。表4は、100部PVF当たり1〜10部ポリエステルのDesmophen(登録商標)F−2060Bについての結果を示す。サンプル10〜25はそれぞれ、より重いPETウェブ、5ミルMylar(登録商標)A(DuPont Teijin Films)を使用して作製した。
実施例3は、未改質高分子基材フィルム上のフルオロポリマーコーティングの接着強度への架橋剤組成の影響を実証する。表5は、使用したDesmodur(登録商標)N−3300架橋剤の量の関数としての様々なポリエステルについての接着結果を示す。
実施例4は、未改質高分子基材フィルム上のフルオロポリマーコーティングの接着強度への架橋剤組成の影響を実証する。加えて、本実施例は、高分子基材フィルム上のフルオロポリマーコーティングの接着強度への顔料の影響を実証する。表6は、HMDIイソシアヌレート三量体(Desmodur(登録商標)N−3300)かHMDIビウレット三量体(Desmodur(登録商標)N−75)かのいずれかで架橋されたポリエステルDesmophen(登録商標)F−2060Bについての接着結果の比較を示す。結果は、Desmodur(登録商標)N−75が同様にうまくこのシステムで接着を促進するのに有効であることを示す。サンプル46〜55は、3ミルMelinex(登録商標)442ウェブについて上の実施例1に記載された手順を用いたが、加えて100部PVF当たり45部の白色顔料を含有した。
実施例5
実施例5は、フルオロポリマーコーティング中の相溶性の架橋接着性ポリマーの組成の関数としての未改質高分子基材フィルムへのフルオロポリマーコーティングの接着をさらに実証する。表7は、未改質PET表面上に形成されたときのPVFマトリックス中のポリカーボネートウレタン網状構造についての接着結果を示す。ポリカーボネートウレタンは、Desmodur(登録商標)N−3300イソシアネート官能性架橋剤と反応させた、ポリカーボネートジオール、Desmophen(登録商標)C−2200(Bayer MaterialScience)に由来する。用いた手順は、ポリエステルウレタンについて上に記載されたものと同じものである。全てのサンプルは、ポリカーボネートジオールに対して当量のイソシアネート架橋剤を使用し、PVFの100部当たり0.02部のジブチルスズジラウレートを使用した。Desmophen(登録商標)C−2200は形式上、1,6−ヘキサンジオール・プラス炭酸から誘導される2000MWポリカーボネートである。結果は、顔料の不存在下に低濃度のポリカーボネートウレタンでの強い接着を示す。
表8は、100部PVF当たり1部ポリカーボネートおよびポリカーボネートジオールに対して当量の架橋剤で実施例5におけるようにポリカーボネートウレタンブレンド調合物への白色顔料の添加についての接着結果を示す。結果は、顔料がこの調合物で接着結合の形成を妨害し得ることを明確に示す。
表9は、実施例5および6に記載された、しかし顔料の存在を可能にするタイプの調合物についての接着結果を示す。当量を超えるイソシアネート官能性架橋剤と組み合わせてポリカーボネートジオールの量を増やすと、顔料を許容し、かつ、ポリカーボネートウレタン/PVFブレンド物と未改質PETウェブとの間の強い接着結合を依然として提供する調合物を生成する。10部ポリカーボネートジオールおよび30部白色顔料で、最良の結合は、ポリカーボネートジオールに対して150〜200モル%の架橋剤の範囲で達成される。
実施例8は、商業上実用的な条件下でのコーティング法を実証する。加えて、本実施例は、太陽電池バックシート試験に共通している***的な熱および湿気条件を切り抜ける耐久性のある結合を生成するのに十分な加熱の重要性を示す。これらのサンプルの全てが、150モル%か200モル%かのいずれかのポリイソシアネート架橋剤(Desmodur(登録商標)N−3300)と組み合わせてPVFに対して10部のポリカーボネートジオール(Desmophen(登録商標)C−2200)を有する。加えて、それぞれは、100部PVF当たり0.02部ジブチルスズジラウレート触媒および30部白色顔料を使用した。コーティング混合物を、リバース・グラビア法を用いて未改質3ミルPETウェブ(Melinex(登録商標)377)に塗布し、次に3−ゾーン浮上オーブン中でベーキングした。それぞれ5フィート長さのオーブンゾーンを、コーティング前に300°F/350°F/430°Fに調節した。ライン速度を5〜30フィート毎分に変えた。
3ミルPET/1ミルコーティング/26ミルEVA/125ミルガラスパネル。
Claims (4)
- 高分子基材フィルムを、
フッ化ビニルのホモポリマーおよびコポリマーから選択されたフルオロポリマー、
溶剤、
ポリエステル、ポリエステルウレタン、ポリカーボネート、ポリカーボネートウレタン、ポリアクリレート、アクリルポリウレタン、ポリエーテル、ポリエーテルウレタン、エチレンビニルアルコールコポリマー、エチレンビニルアルコールコポリマーウレタン、ポリアミド、ポリアミドウレタン、ポリアミドウレア、ポリアクリルアミド、ポリアクリルアミドウレタンおよびそれらの組み合わせから選択される、相溶性の架橋可能な接着性ポリマー、ならびに
架橋剤
を含む液体フルオロポリマーコーティングで被膜する工程と、
架橋ポリマー網状構造を前記フルオロポリマーコーティング中に形成するために前記相溶性の架橋可能な接着性ポリマーを架橋させる工程と、
前記溶剤を前記フルオロポリマーコーティングから除去する工程と、
前記フルオロポリマーコーティングを前記高分子基材フィルムに接着させる工程と
を含む、多層フィルムの形成方法。 - 高分子基材フィルムと、
高分子基材フィルム上の、
フッ化ビニルのホモポリマーおよびコポリマーから選択されたフルオロポリマー、ならびに
ポリエステル、ポリエステルウレタン、ポリカーボネート、ポリカーボネートウレタン、ポリアクリレート、アクリルポリウレタン、ポリエーテル、ポリエーテルウレタン、エチレンビニルアルコールコポリマー、エチレンビニルアルコールコポリマーウレタン、ポリアミド、ポリアミドウレタン、ポリアミドウレア、ポリアクリルアミド、ポリアクリルアミドウレタンおよびそれらの組み合わせから選択される、相溶性の架橋接着性ポリマーを含むフルオロポリマーコーティングと
を含むフルオロポリマー被膜フィルムであって、
前記高分子基材フィルムが、前記相溶性の架橋接着性ポリマーと相互作用して前記高分子基材フィルムへの前記フルオロポリマーコーティングの結合を促進する官能基を含む、フルオロポリマー被膜フィルム。 - 高分子基材フィルムがポリエステル、ポリアミド、ポリイミド、またはそれらの任意の組み合わせを含む、請求項2に記載のフルオロポリマー被膜フィルム。
- 請求項2に記載のフルオロポリマー被膜フィルムを含む太陽電池モジュール用のバックシート。
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- 2008-04-11 US US12/101,413 patent/US8168297B2/en active Active
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US8025928B2 (en) | 2011-09-27 |
EP2468829A1 (en) | 2012-06-27 |
AU2008244557A1 (en) | 2008-11-06 |
US8168297B2 (en) | 2012-05-01 |
US20110086954A1 (en) | 2011-04-14 |
AU2008244557B2 (en) | 2013-11-14 |
CA2680847C (en) | 2015-03-31 |
KR20100015554A (ko) | 2010-02-12 |
EP2139962A2 (en) | 2010-01-06 |
US20080261037A1 (en) | 2008-10-23 |
CN101663367A (zh) | 2010-03-03 |
WO2008133848A3 (en) | 2009-01-15 |
CN101663367B (zh) | 2013-05-29 |
KR101553188B1 (ko) | 2015-09-14 |
JP2010526886A (ja) | 2010-08-05 |
WO2008133848A2 (en) | 2008-11-06 |
KR20140096388A (ko) | 2014-08-05 |
ES2570607T3 (es) | 2016-05-19 |
ES2537383T3 (es) | 2015-06-08 |
CN103275570B (zh) | 2015-08-19 |
US20110086172A1 (en) | 2011-04-14 |
CA2680847A1 (en) | 2008-11-06 |
EP2468829B1 (en) | 2015-03-18 |
EP2139962B1 (en) | 2016-02-17 |
CN103275570A (zh) | 2013-09-04 |
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