JP2014500586A - 接着フィルム及びこれを利用した有機電子装置の封止方法 - Google Patents
接着フィルム及びこれを利用した有機電子装置の封止方法 Download PDFInfo
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- JP2014500586A JP2014500586A JP2013537605A JP2013537605A JP2014500586A JP 2014500586 A JP2014500586 A JP 2014500586A JP 2013537605 A JP2013537605 A JP 2013537605A JP 2013537605 A JP2013537605 A JP 2013537605A JP 2014500586 A JP2014500586 A JP 2014500586A
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- 229910000077 silane Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- YRGLXIVYESZPLQ-UHFFFAOYSA-I tantalum pentafluoride Chemical compound F[Ta](F)(F)(F)F YRGLXIVYESZPLQ-UHFFFAOYSA-I 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 150000003681 vanadium Chemical class 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09J7/00—Adhesives in the form of films or foils
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/29—Laminated material
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- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
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- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
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- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
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- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
- C09J2301/1242—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape the opposite adhesive layers being different
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- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/208—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive
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- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
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Abstract
Description
前記有機電子装置封止製品は、前記接着フィルムと有機電子装置との間に前記有機電子装置を保護する保護膜をさらに含むことができる。
本発明において有機電子装置の封止方法は、例えば、ガラスまたは高分子フィルムのような基板21上に真空蒸着またはスパッタリングなどの方法で透明電極を形成し、前記透明電極上に有機材料層を形成する。前記有機材料層は、正孔注入層、正孔輸送層、発光層、電子注入層及び/または電子輸送層を含むことができる。次に、前記有機材料層上に第2電極をさらに形成する。その後、前記基板21上の有機電子装置25の上部に前記有機電子者装置25をすべてカバーするように、前述の接着フィルム22を適用する。この際、前記接着フィルム22を適用する方法は、特に限定されず、例えば、基板21上に形成された有機電子装置25の上部に、本発明の接着フィルムの接着剤層をあらかじめ転写したカバー基板(例えば、ガラスまたは高分子フィルム)24を加熱、圧着などの方法で適用することができる。前記段階では、例えば、カバー基板24上に接着フィルム22を転写するとき、前述の本発明の接着フィルムを使用して、前記フィルムに形成された基材または離型フィルムを剥離した後、熱を加えながら、真空プレスまたは真空ラミネータなどを使用してカバー基板24上に転写することができる。この過程で、接着フィルムの硬化反応が一定の範囲以上で進行されれば、接着フィルム22の密着力や接着力が減少するおそれがあるので、工程温度を約100℃以下、工程時間を5分以内に制御することが好ましい。同様に、接着フィルム22が転写されたカバー基板24を有機電子装置に加熱圧着する場合にも、真空プレスまたは真空ラミネータを利用することができる。この段階での温度条件は、前述したように設定することができ、工程時間は、10分以内が好ましい。
但し、接着フィルムの第2領域より第1領域の接着剤層が有機電子装置に当接するように(有機電子装置が保護膜を備える場合には、保護膜に当接するように)接着フィルムを有機電子装置に適用する。
1.第1領域溶液製造
シラン変性エポキシ樹脂(KSR−177、KUKDO化学)200g及びフェノキシ樹脂(YP−50、東都化成)150gを反応器内に投入し、メチルエチルケトンで希釈した。その後、反応器の内部を窒素で置換し、製造された溶液を均質化した。
水分吸着剤としてCaO(Aldrich)70gをメチルエチルケトンに30wt%の濃度で投入して水分吸着剤溶液を製造し、前記溶液をボールミル工程によって24時間ミーリングした。また、これとは別に、常温で反応器にシラン変性エポキシ樹脂(KSR−177、KUKDO化学)200g及びフェノキシ樹脂(YP−50、東都化成)150gを投入し、メチルエチルケトンで希釈した。その後、反応器の内部を窒素で置換し、製造された溶液を均質化した。前記均質化された溶液にあらかじめ準備した水分吸着剤溶液を投入し、硬化剤であるイミダゾール(四国化成)4gを投入した後、1時間高速撹拌し、第2領域の溶液を製造した。
前記準備した第1領域の溶液を離型PETの離型面にコンマコッターを使用して塗布し、乾燥器で130℃に3分間乾燥し、厚さが15μmの接着層を形成した。
前記準備した第2領域の溶液を離型PETの離型面にコンマコッターを使用して塗布し、乾燥器で130℃に3分間乾燥し、厚さが30μmの接着層を形成した。
前記第1領域及び第2領域の接着層をラミネートし、多層の接着フィルムを製造した。
前記実施例1の接着フィルム製造過程で、第1領域溶液にCaO 7gを添加し、第2領域溶液には、CaO 62gを添加したことを除いて、実施例1と同一の方法で多層構造の接着フィルムを製造した。
前記実施例1の接着フィルム製造過程で、第1領域溶液にCaO 14gを添加し、第2領域溶液には、CaO 56gを添加したことを除いて、実施例1と同一の方法で多層構造の接着フィルムを製造した。
前記実施例1と同様の接着フィルム製造過程で実施するが、実施例1の第1領域フィルム組成だけよりなる厚さ45μmの接着フィルムを製造した。
前記実施例1と同様の接着フィルム製造過程で実施するが、実施例1の第2領域フィルム組成だけよりなる厚さ45μmの接着フィルムを製造した。
前記実施例1の接着フィルム製造過程で、第1領域溶液にCaO 28gを添加し、第2領域溶液には、CaO 42gを添加したことを除いて、実施例1と同一の方法で多層構造の接着フィルムを製造した。
前記実施例1の接着フィルム製造過程で、シラン変性エポキシ樹脂をアクリル粘着剤樹脂に代替したことを除いて、実施例1と同一の方法で多層構造の接着フィルムを製造した。
前記実施例1の接着フィルム製造過程で、シラン変性エポキシ樹脂をブタジエン変性エポキシ樹脂に代替したことを除いて、実施例1と同一の方法で多層構造の接着フィルムを製造した。
実施例1〜3及び比較例1〜5の接着フィルムの水分遮断特性を調査するために、カルシウムテストを進行した。具体的には、100mm×100mmサイズのガラス基板上にカルシウム(Ca)を5mm×5mmのサイズ及び100nmの厚さで9個(9 spot)蒸着し、実施例1〜3及び比較例1〜3の接着フィルムが転写されたカバーガラスを各カルシウム蒸着箇所に真空プレス(vacuum press)を使用して、80℃で1分間加熱圧着した。その後、高温乾燥器内で100℃に3時間硬化させた後、11mm×11mmのサイズに封止されたカルシウム(Ca)の試験片をそれぞれ切断した。得られた試験片を恒温恒湿チャンバで85℃の温度及び85%R.H.の環境に放置した後、水分浸透による酸化反応によってカルシウムが透明になり始めた時点を評価し、下記表1に示した。
実施例1と比較例4及び5の接着フィルムの硬化性樹脂に対する透湿度(WVTR;water vapor transmission rate)を測定した。透湿も測定は、シラン変性エポキシ樹脂、アクリル粘着剤樹脂及びブタジエン変性エポキシ樹脂を硬化させて厚さ80μmのフィルム形状に製造した後、38℃及び100%の相対湿度下でMOCON社の機器を使用して前記フィルムの厚さ方向に対して測定した。その結果を下記表2に示した。
実施例1〜3及び比較例1〜3の接着フィルムを利用して3インチの有機発光パネルを製造して恒温恒湿チャンバで85℃の温度及び85%R.H.の環境に放置した後、有機蒸着膜が破壊される現象を観察し、下記表3に示した。
ガラスに有機電子装置の保護膜として使用されるシリコーンナイトライド(SiNx)を1μmの厚さで蒸着した。SiNx蒸着膜の上に実施例1〜3及び比較例1〜3の接着フィルムを熱圧着して硬化し、85℃の温度及び85%R.H.の環境に放置した後、SiNx蒸着膜に化学的変化が発生したかをFT−IRを利用して分析した。その結果は、下記表4に示し、実施例1及び比較例2の接着フィルムに対するFT−IR分析結果は、図6及び図7に示した。図6とは異なって、図7では、SiNx蒸着膜の化学的成分変異が発生したことが分析された。水分反応性吸着剤が水和反応によって強い塩基として作用し、保護膜(SiNx蒸着膜)に化学的損傷が発生したことを確認することができる。
12 接着剤層
14 カバーフィルム
21 基板
22 接着フィルム
12a、22b 第1領域
12b、22b 第2領域
13、23 水分吸着剤
24 カバー基板
25 有機電子装置
26 保護膜
Claims (25)
- 有機電子装置を封止する接着フィルムであって、
前記接着フィルムは、硬化性樹脂及び水分吸着剤を含む硬化性ホットメルト型接着剤層を含み、
前記硬化性ホットメルト型接着剤層は、有機電子装置の封止時に有機電子装置と接触する第1領域と有機電子装置と接触しない第2領域とを含み、前記接着剤層内の全体水分吸着剤の質量を基準にして、前記第1領域には、0〜20%、前記第2領域には、80〜100%の水分吸着剤を含む接着フィルム。 - 前記硬化性ホットメルト型接着剤層は、常温での粘度が106dyne/cm2以上である、請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、硬化状態で透湿度が50g/m2・day以下である、請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、熱硬化型樹脂、光硬化型樹脂またはデュアル硬化型樹脂である、請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、グリシジル基、イソシアネート基、ヒドロキシ基、カルボキシル基、アミド基、エポキシド基、環状エーテル基、スルフィド基、アセタール基及びラクトン基から選択される1つ以上の硬化性官能基を含む、請求項1に記載の接着フィルム。
- 前記硬化性樹脂が分子構造内に環状構造を含むエポキシ樹脂である、請求項1に記載の接着フィルム。
- 前記硬化性樹脂がシラン変性エポキシ樹脂である、請求項1に記載の接着フィルム。
- 前記水分吸着剤は、水分反応性吸着剤、物理的吸着剤、またはその混合物である、請求項1に記載の接着フィルム。
- 前記水分反応性吸着剤がアルミナ、金属酸化物、金属塩または五酸化リンであり、前記物理的吸着剤は、シリカ、ゼオライト、ジルコニア、チタニアまたはモンモリロナイトである、請求項8に記載の接着フィルム。
- 前記水分反応性吸着剤が、P2O5、Li2O、Na2O、BaO、CaO、MgO、Li2SO4、Na2SO4、CaSO4、MgSO4、CoSO4、Ga2(SO4)3、Ti(SO4)2、NiSO4、CaCl2、MgCl2、SrCl2、YCl3、CuCl2、CsF、TaF5、NbF5、LiBr、CaBr2、CeBr3、SeBr4、VBr3、MgBr2、BaI2、MgI2、Ba(ClO4)2及びMg(ClO4)2よりなる群から選択された1つ以上である、請求項9に記載の接着フィルム。
- 前記接着剤層の第2領域は、硬化性樹脂100重量部に対して、1重量部〜100重量部の水分吸着剤を含む、請求項1に記載の接着フィルム。
- 前記接着剤層の第1領域は、硬化性樹脂100重量部に対して、0重量部〜20重量部の水分吸着剤を含む、請求項1に記載の接着フィルム。
- 前記接着剤層は、フィラーをさらに含む、請求項1に記載の接着フィルム。
- 前記フィラーがクレイ、タルク及び針状シリカよりなる群から選択された1つ以上である、請求項13に記載の接着フィルム。
- 前記接着剤層は、硬化性樹脂100重量部に対して、1重量部〜50重量部のフィラーを含む、請求項13に記載の接着フィルム。
- 前記接着剤層は、硬化剤をさらに含む、請求項1に記載の接着フィルム。
- 前記硬化剤は、アミン系化合物、イミダゾール系化合物、フェノール系化合物、リン系化合物または酸無水物系化合物である、請求項16に記載の接着フィルム。
- 前記接着剤層は、硬化性樹脂100重量部に対して、1重量部〜10重量部の硬化剤を含む、請求項16に記載の接着フィルム。
- 前記接着剤層は、高分子量樹脂をさらに含む、請求項1に記載の接着フィルム。
- 基板と;前記基板上に形成された有機電子装置と;前記有機電子装置を封止する請求項1〜19のいずれかに記載の接着フィルムを含み、前記接着フィルムの接着剤層の第1領域が前記有機電子装置をカバーしている有機電子装置封止製品。
- 前記有機電子装置が有機発光ダイオードである、請求項20に記載の有機電子装置封止製品。
- 上部に有機電子装置が形成された基板に請求項1〜19のいずれかに記載の接着フィルムを、前記接着フィルムの接着剤層の第1領域が前記有機電子装置をカバーするように適用する段階と;前記接着剤層を硬化する段階と;を含む有機電子装置の封止方法。
- 前記接着フィルムを前記有機電子装置に適用する段階は、接着フィルムのホットロールラミネート、熱圧着(hot press)または真空圧着方法で行う、請求項22に記載の有機電子装置の封止方法。
- 前記接着フィルムを前記有機電子装置に適用する段階は、50℃〜90℃の温度で行う、請求項22に記載の有機電子装置の封止方法。
- 前記硬化段階は、70℃〜110℃の温度範囲で加熱するか、またはUVを照射して行う、請求項22に記載の有機電子装置の封止方法。
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