JP2014500813A - 多層フィルム及びこれを含む光電池モジュール - Google Patents
多層フィルム及びこれを含む光電池モジュール Download PDFInfo
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- JP2014500813A JP2014500813A JP2013538635A JP2013538635A JP2014500813A JP 2014500813 A JP2014500813 A JP 2014500813A JP 2013538635 A JP2013538635 A JP 2013538635A JP 2013538635 A JP2013538635 A JP 2013538635A JP 2014500813 A JP2014500813 A JP 2014500813A
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- multilayer film
- acrylate
- reactive functional
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Abstract
Description
剥離強度は、ASTM D1897に準拠して、試験片を10mmの幅で切断した後、4.2mm/secの速度及び180度の剥離角度で剥離しながら測定した。
クロスカット試験基準であるASTM D3002/D3359の規格に準拠して、クロスカットテストを行った。具体的に、試験片を1mmの間隔で横及び縦方向にそれぞれ11列ずつカッターを利用して切断し、横及び縦がそれぞれ1mmの100個の正方形格子を形成した。その後、Nichiban社のCT−24接着テープを前記切断面に付着した後、取り外すとき、一緒に剥がれた面の状態を測定し、下記基準にして評価した。
〈クロス−ハッチ接着力評価基準〉
5B:剥がれた面がない場合
4B:剥がれた面が全体面積に対して5%以内の場合
3B:剥がれた面が全体面積に対して5〜15%の場合
2B:剥がれた面が全体面積に対して15〜35%の場合
1B:剥がれた面が全体面積に対して35〜65%の場合
0B:ほぼ大部分が剥がれた場合
実施例及び比較例で製造された多層フィルム(基材の両面をフッ素系重合体/反応性官能基を含有するアクリル系重合体を含む樹脂層でコーティング)を85℃及び85%R.H.の条件が維持されるオーブンに1,000時間、2,000時間または3,000時間放置した後、接着力の変化を観察した。本明細書で単位「R.H.」は、相対湿度を意味する。
実施例及び比較例で製造された多層フィルム(基材の両面をフッ素系重合体/反応性官能基を含有するアクリル系重合体を含む樹脂層でコーティング)を2気圧、121℃及び100%R.H.の条件が維持されるオーブンに50時間、75時間または100時間放置した後、接着力の変化を観察した。
基材層の準備
両面にアクリルプライマー処理が施されたPET(poly(ethylene terephthalate)、厚さ:250μm)フィルム(コーロング社製)の表面をコロナ処理を行った。
フッ素系重合体及び反応性官能基を含有するアクリル系重合体の混合物を製造するために、下記表1のように多様なフッ素系重合体を準備した。下記表1には、実施例と比較例に使用するフッ素系重合体の分子量及び融点を示す。
樹脂層用コーティング液の製造
ジメチルホルムアミド(DMF:N、N−dimethyl formamide)600gとメチルエチルケトン(MEK:Methylethyl ketone)200gに前記製造例1で準備した重合体5(ビニリデンフルオライド(VDF;Vinylidene fluoride)及びクロロトリフルオロエチレン(CTFE;Chlorotrifluoro ethylene)を85:15(VDF:CTFE)の重量比率で重合された形態で含む共重合体)120g、前記製造例1で準備した重合体2(VDF及びヘキサフルオロプロピレン(HFP;Hexafluoropropylene)を88:12(VDF:HFP)の重量比率で重合された形態で含む共重合体60g、メチルメタクリレート(MMA):グリシジルメタクリレート(GMA):ブチルメタクリレート(BMA):スチレン(ST)の重量比が49.5:35.5:10:5であるエポキシ基を含むアクリル系重合体(エポキシ当量400g)20gをあらかじめ溶解させて第1コーティング液を準備した。
前記あらかじめ準備した基材上に前記樹脂層用コーティング液をコンマリバース(comma reverse)方式で塗布した。具体的に、乾燥後の厚さが約20〜30μmとなるように間隔を調節してコーティングした後、コーティングされた基材をそれぞれの長さが2mであり、温度が80℃、170℃及び170℃に調節された3個のオーブンに1m/minの速度で順次に通過させて樹脂層を形成した。その後、樹脂層の反対面に同様にコーティングを行い、PETフィルムの両面にフッ素系重合体及びエポキシ基を含有するアクリル系重合体がコーティングされた多層フィルムを製造した。
二酸化チタンを使用しないことを除いて実施例1と同一の方法で多層フィルムを製造した。
樹脂層用コーティング液の製造時に含まれるフッ素系重合体の種類及び配合比と二酸化チタンの含量を下記表2に示された方式に変更したことを除いて、実施例1と同一の方法で多層フィルムを製造した。
商業的に販売されているイソボルタ(Isovolta)社のIcosolar 2442製品を多層フィルムとして使用した。前記Icosolar 2442製品は、押出工程で製造されたPVF(poly(vinylfluoride))フィルム(厚さ38μm)を接着剤を利用してPETフィルムの両面にラミネートした製品である。
商業的に販売されているイソボルタ(Isovolta)社のIcosolar 3469製品を多層フィルムとして使用した。前記Icosolar 3469製品は、キャスティング工程で製造されたPVFフィルム(厚さ25μm)を接着剤を利用してPETフィルムの両面にラミネートした製品である。
前記実施例1〜10及び比較例1及び2の多層フィルムに対して、湿熱(damp heat)試験を行った後、180度剥離強度及びクロス−ハッチテストをそれぞれ行った。具体的には、それぞれの多層フィルムを85℃及び85%R.H.の条件のオーブンでそれぞれ1000時間、2000時間または3000時間放置した後、180度剥離強度及びクロス−ハッチテストを行い、剥離力の変化を評価した。前記評価結果を下記表4に示した。
コーティング液の製造過程でフッ素系重合体をビニリデンフルオライド(VDF)の単一共重合体であるポリビニリデンフルオライド(PVDF:Polyvinylidene fluoride、重合体7)を使用し、フッ素系重合体及びアクリル系重合体の相対的な量を調節し、下記表5のようにエポキシ当量を変更したこととミルベースに含まれる二酸化チタンの含量を80gに変更したことを除いて、実施例1と同一の方式で多層フィルムを製造した。
コーティング液の製造過程でアクリル系重合体として非反応性アクリル重合体であるポリメチルメタクリレート(PMMA:Polymethylmethacrylate)を使用したことを除いて、それぞれ実施例13、15及び17と同一の方式で多層フィルムを製造した。
前記実施例11〜21及び比較例3〜8の多層フィルムに対して、PCT(Pressure cooker test)を行った後、180度剥離強度及びクロス−ハッチテストをそれぞれ行った。具体的には、それぞれの多層フィルムを2気圧、121℃及び100%R.H.の条件でそれぞれ25時間、50時間または75時間放置した後、180度剥離強度及びクロス−ハッチテストを行い、その結果を下記表6に示した。
コーティング液の製造過程でフッ素系重合体を分岐ビニリデンフルオライド(VDF)の単一共重合体である重合体6を使用し、フッ素系重合体及びアクリル系重合体の相対的な量を調節し、下記表7のようにエポキシ当量を変更したことを除いて、実施例11と同一の方式で多層フィルムを製造した。
前記実施例22〜32及び比較例9〜11の多層フィルムに対して、PCT(Pressure cooker test)を行った後、180度剥離強度及びクロス−ハッチテストをそれぞれ行った。具体的には、それぞれの多層フィルムを2気圧、121℃及び100%R.H.の条件でそれぞれ25時間、50時間または75時間放置した後、180度剥離強度及びクロス−ハッチテストを行い、その結果を下記表8に示した。
コーティング液の製造過程でフッ素系重合体を分岐ビニリデンフルオライド(VDF)の単一共重合体である重合体6を使用し、アクリル系重合体をメチルメタクリレート(MMA):グリシジルメタクリレート(GMA):ブチルメタクリレート(BMA):スチレン(ST)の重量比が56.3:23.7:13.3:6.7であるエポキシ基を含むアクリル系重合体(エポキシ当量600g)を使用し、フッ素系重合体及びアクリル系重合体の相対的な量を調節し、下記表9のようにエポキシ当量を変更したことを除いて、実施例11と同一の方式で多層フィルムを製造した。
前記実施例33〜43及び比較例12及び13の多層フィルムに対して、PCT(Pressure cooker test)を行った後、180度剥離強度及びクロス−ハッチテストをそれぞれ行った。具体的には、それぞれの多層フィルムを2気圧、121℃及び100%R.H.の条件でそれぞれ25時間、50時間または75時間放置した後、180度剥離強度及びクロス−ハッチテストを行い、その結果を下記表10に示した。
11 樹脂層
12 基材
Claims (31)
- 基材と;
前記基材上に形成され、フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層と;を含む多層フィルムであって、
前記樹脂層の全体重合体に対する反応性官能基の当量が30,000以下である多層フィルム。 - 前記反応性官能基は、カルボキシ基、アミド基、アミノ基、エポキシ基、ヒドロキシ基、酸無水物基、イソシアネート基、スルホン酸基、アジリジン基、アミン基、ユリア基、リン酸基、シアノ基、シアネート基、イミダゾール基、オキサゾリン基及びイミン基よりなる群から選択された1つ以上である、請求項1に記載の多層フィルム。
- 前記反応性官能基を含有するアクリル系重合体は、(メタ)アクリレート、アルキル(メタ)アクリレート及びイソボニル(メタ)アクリレートよりなる群から選択される1種以上と反応性官能基を含有する1種以上の単量体との共重合体である、請求項1に記載の多層フィルム。
- 前記アルキル(メタ)アクリレートは、メチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート、n−ブチル(メタ)アクリレート、s−ブチル(メタ)アクリレート、t−ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、ヘキシル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、n−オクチル(メタ)アクリレート、イソオクチル(メタ)アクリレート、n−ノニル(メタ)アクリレート、イソノニル(メタ)アクリレート、n−デシル(メタ)アクリルレート、イソデシル(メタ)アクリレート、n−ドデシル(メタ)アクリレート、n−トリデシル(メタ)アクリレート及びn−テトラデシル(メタ)アクリレートよりなる群から選択された1種以上である、請求項3に記載の多層フィルム。
- 前記反応性官能基を含有する単量体は、カルボキシ基含有単量体、アミド基含有単量体、アミノ基含有単量体、エポキシ基含有単量体、ヒドロキシ基含有単量体、酸無水物基含有単量体、イソシアネート基含有単量体、スルホン酸基含有単量体、アジリジン基含有単量体、アミン基含有単量体、ユリア基含有単量体、リン酸基含有単量体、シアノ基含有単量体、シアネート基含有単量体、イミダゾール基含有単量体、オキサゾリン基含有単量体及びイミン基含有単量体よりなる群から選択される1種以上である、請求項3に記載の多層フィルム。
- 前記反応性官能基を含有する単量体は、カルボキシ基含有単量体、エポキシ基含有単量体またはオキサゾリン基含有単量体である、請求項3に記載の多層フィルム。
- 前記反応性官能基を含有する単量体は、グリシジル(メタ)アクリレート、グリシジルアルキル(メタ)アクリレート、(メタ)アクリル酸、イソシアネートアルキル(メタ)アクリレート、(メタ)アクリロニトリル、シクロヘキシルマルレイミド、ヒドロキシアルキル(メタ)アクリレート、マレイン酸無水物、p−トルエンスルホン酸、リン酸、(メタ)アクリルアミド、アミノアルキル(メタ)アクリレート、ビニルイミダゾール、及び2−イソプロフェニル−2−オキサゾリンよりなる群から選択される1種以上である、請求項3に記載の多層フィルム。
- 前記反応性官能基を含有するアクリル系重合体は、重合性単量体をさらに含む共重合体である、請求項3に記載の多層フィルム。
- 前記重合性単量体は、スチレン、クロロスチレン、クロロメチルスチレンまたはメチルスチレンである、請求項8に記載の多層フィルム。
- 前記フッ素系重合体は、ビニリデンフルオライド(VDF、Vinylidene Fluoride)、ビニルフルオライド(VF、Vinyl Fluoride)、テトラフルオロエチレン(TFE、Tetrafluoroethylene)、ヘキサフルオロプロピレン(HFP、Hexafluoropropylene)、クロロトリフルオロエチレン(CTFE、chlorotrifluoroethylene)、トリフルオロエチレン、ヘキサフルオロイソブチレン、ペルフルオロブチルエチレン、ペルフルオロメチルビニルエーテル(PMVE、perfluoro(methylvinylether))、ペルフルオロエチルビニルエーテル(PEVE、perfluoro(ethylvinylether))、ペルフルオロプロピルビニルエーテル(PPVE)、ペルフルオロメチルビニルエーテル(PMVE)、ペルフルオロ−2、2−ジメチル−1、3−ジオキソール(PDD)及びペルフルオロ−2−メチレン−4−メチル−1、3−ジオキソラン(PMD)よりなる群から選択された1つ以上の単量体を重合された形態で含む単独重合体、共重合体またはこれらの混合物を含む、請求項1に記載の多層フィルム。
- 前記フッ素系重合体は、ビニルフルオライドを重合された形態で含む単独重合体または共重合体;またはビニリデンフルオライドを重合された形態で含む単独重合体または共重合体;またはこれらの混合物である、請求項1に記載の多層フィルム。
- 前記フッ素系重合体は、ビニリデンフルオライド(VDF)またはビニルフルオライド(VF)と、テトラフルオロエチレン、ヘキサフルオロプロピレン、クロロトリフルオロエチレン、トリフルオロエチレン、ヘキサフルオロイソブチレン、ペルフルオロブチルエチレン、ペルフルオロメチルビニルエーテル、ペルフルオロエチルビニルエーテル、ペルフルオロプロピルビニルエーテル(PPVE)、ペルフルオロメチルビニルエーテル(PMVE)、ペルフルオロ−2、2−ジメチル−1、3−ジオキソール(PDD)及びペルフルオロ−2−メチレン−4−メチル−1、3−ジオキソラン(PMD)よりなる群から選択された1つ以上の共単量体を含む共重合体またはこれらの混合物である、請求項1に記載の多層フィルム。
- 前記共単量体の含量は、0.5〜50重量%である、請求項12に記載の多層フィルム。
- 前記フッ素系重合体の重量平均分子量は、50,000〜1,000,000である、請求項1に記載の多層フィルム。
- 前記フッ素系重合体の融点が80℃〜175℃である、請求項1に記載の多層フィルム。
- 前記フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層の反応性官能基を含有するアクリル系重合体の含量が50重量%以下である、請求項1に記載の多層フィルム。
- 前記基材は、アルミニウム、鉄;またはポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)またはポリブチレンテレフタレート(PBT)の単一シート、積層シートまたは共押出物である、請求項1に記載の多層フィルム。
- 前記基材の少なくとも一面にプラズマ、コロナ、プライマー、カップリング剤処理及び熱処理のうちから選択された1つ以上の処理が形成される、請求項1に記載の多層フィルム。
- 前記基材の厚さは、50〜500μmである、請求項1に記載の多層フィルム。
- 前記フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層の厚さは、3〜50μmである、請求項1に記載の多層フィルム。
- 前記フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層は、顔料、充填剤、UV安定剤、熱安定剤または障壁粒子をさらに含む、請求項1に記載の多層フィルム。
- 前記フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層は、樹脂組成物を塗布して形成されるコーティング層である、請求項1に記載の多層フィルム。
- 基材と;前記基材上に形成され、フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層と;を含み、前記樹脂層の全体重合体に対する反応性官能基の当量が30,000以下である光電池用裏面シート。
- 基材上にフッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層を形成する段階を含み、
前記樹脂層の全体重合体に対する反応性官能基の当量が30,000以下であることを特徴とする多層フィルムの製造方法。 - 前記フッ素系重合体及び反応性官能基を含有するアクリル系重合体を含む樹脂層の形成段階は、フッ素系重合体、反応性官能基を含有するアクリル系重合体及び沸点が200℃以下の溶媒を含む樹脂組成物を基材上にコーティングする段階を含む、請求項24に記載の多層フィルムの製造方法。
- 前記沸点が200℃以下の溶媒は、アセトン、メチルエチルケトン、ジメチルホルムアミド及びジメチルアセトアミドよりなる群から選択される1種以上を含む、請求項25に記載の多層フィルムの製造方法。
- 前記樹脂層を形成する前に、前記基材の少なくとも一面にプラズマ、コロナ、プライマー、カップリング剤処理及び熱処理のうちから選択された1つ以上の処理を行う段階をさらに含む、請求項24に記載の多層フィルムの製造方法。
- 前記コーティング段階に引き続いて、乾燥する段階をさらに行う、請求項25に記載の多層フィルムの製造方法。
- 乾燥は、200℃以下の温度で30秒〜30分間行う、請求項28に記載の多層フィルムの製造方法。
- 請求項1〜22に記載の多層フィルムを含む光電池用裏面シート。
- 請求項23または30に記載の光電池用裏面シートを含む光電池モジュール。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2010-0111751 | 2010-11-10 | ||
KR20100111751 | 2010-11-10 | ||
KR1020110115306A KR101411682B1 (ko) | 2010-11-10 | 2011-11-07 | 다층 필름 및 이를 포함하는 광전지 모듈 |
KR10-2011-0115306 | 2011-11-07 | ||
PCT/KR2011/008462 WO2012064082A2 (ko) | 2010-11-10 | 2011-11-08 | 다층 필름 및 이를 포함하는 광전지 모듈 |
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KR20130135780A (ko) * | 2012-05-31 | 2013-12-11 | 주식회사 엘지화학 | 다층 필름 및 이를 포함하는 광전지 모듈 |
KR101630011B1 (ko) * | 2012-06-01 | 2016-06-13 | 주식회사 엘지화학 | 태양전지용 보호필름 및 이를 포함하는 태양전지 |
WO2013180552A1 (ko) * | 2012-06-01 | 2013-12-05 | 주식회사 엘지화학 | 친환경 광전지 모듈용 백시트 및 이의 제조방법 |
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KR101489996B1 (ko) | 2012-09-12 | 2015-02-12 | (주)엘지하우시스 | 고내후성 아크릴계 다층 필름 및 그 제조 방법 |
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JP2015073048A (ja) * | 2013-10-04 | 2015-04-16 | 積水化学工業株式会社 | 太陽電池保護シート、及び、太陽電池モジュール |
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CN103269853B (zh) | 2016-06-29 |
TWI469869B (zh) | 2015-01-21 |
EP2639060B1 (en) | 2018-10-03 |
TW201228833A (en) | 2012-07-16 |
EP2639060A2 (en) | 2013-09-18 |
JP6011817B2 (ja) | 2016-10-19 |
KR20120050381A (ko) | 2012-05-18 |
US9379264B2 (en) | 2016-06-28 |
WO2012064082A3 (ko) | 2012-07-19 |
KR101411682B1 (ko) | 2014-06-26 |
US20130247984A1 (en) | 2013-09-26 |
CN103269853A (zh) | 2013-08-28 |
WO2012064082A2 (ko) | 2012-05-18 |
EP2639060A4 (en) | 2015-08-26 |
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