TW201811964A - 填充奈米粒子之障壁黏著劑組成物 - Google Patents
填充奈米粒子之障壁黏著劑組成物 Download PDFInfo
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- TW201811964A TW201811964A TW106119990A TW106119990A TW201811964A TW 201811964 A TW201811964 A TW 201811964A TW 106119990 A TW106119990 A TW 106119990A TW 106119990 A TW106119990 A TW 106119990A TW 201811964 A TW201811964 A TW 201811964A
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/383—Natural or synthetic rubber
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/241—Polyolefin, e.g.rubber
- C09J7/243—Ethylene or propylene polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/005—Stabilisers against oxidation, heat, light, ozone
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- 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
- C09J2301/312—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 parameters being the characterizing feature
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Abstract
一種障壁黏著劑組成物,其包含聚異丁烯樹脂、經有機改質之奈米黏土及吸著劑奈米粒子。
Description
本發明係關於障壁黏著劑組成物及黏著劑障壁膜。
有機電子裝置需要阻隔濕氣與氧之保護,以提供適當長之壽命以用於商業應用。因此利用封裝材料來保護裝置免於接觸濕氣與氧。玻璃係一種常用之封裝材料,但玻璃顯著損害裝置之撓性。因此需要改用撓性障壁膜來代替玻璃。撓性障壁膜使撓性裝置以及更輕、更薄、更凹凸不平的堅硬裝置成為可能。
撓性障壁膜已經商業化用於有機電子裝置之通常用途。撓性障壁膜一般使用黏著劑層壓至要保護之裝置。因此重要的是黏著劑亦具有良好障壁性質,以最小化接合線邊緣之濕氣與氧入侵。一些障壁黏著劑,例如於美國專利申請案公開案第US 2014/0377554號(Cho等人)中所述者,包括奈米黏土作為「濕氣阻斷劑(moisture blocker)」。其他障壁黏著劑,例如於美國專利第6,936,131號(McCormick等人)中所述者,包括乾燥劑及/或吸氣劑材料以吸收及/或吸附氧氣及/或濕氣。
基於上述說明,吾等已了解,針對有特殊需求的有機電子裝置應用,諸如舉例來說:長壽命之有機發光二極體(OLED)顯示器,需要改良之障壁黏著劑。
簡言之,在一態樣中,本發明提供障壁黏著劑組成物,其包含聚異丁烯樹脂、經有機改質之奈米黏土及吸著劑奈米粒子。
如本文中所使用,用語「吸著劑(sorbent)」係指用於吸收或吸附液體或氣體(如氧氣或濕氣)的材料。
在另一態樣中,本發明提供障壁黏著劑組成物,其包含約50至約75wt.%之聚異丁烯樹脂,該聚異丁烯樹脂具有約300,000至約900,000g/mol之黏度平均分子量,約1至約10wt.%之經有機改質之奈米黏土,約1至約5wt.%之氧化鈣奈米粒子,以及約10至約25wt.%之增黏劑,以上皆係相對於該組成物之總重量計。
在又另一態樣中,本發明提供黏著劑障壁膜以及障壁黏著劑物品,該黏著劑障壁膜包含設置在一氣體障壁膜上之一層該障壁黏著劑組成物,而該障壁黏著劑物品包含設置在離型層之間之一層該障壁黏著劑組成物。
已經發現本發明之聚異丁烯黏著劑組成物,其填充有奈米黏土和吸附劑奈米粒子,相較於未填充的聚異丁烯黏著劑,或相較於填充有奈米黏土或吸附劑奈米粒子之一者的聚異丁烯黏著劑,提供障壁性質的顯著改善。令人意外的是,即使相較於具有較高負載的奈米黏土或吸附劑奈米粒子之一者的聚異丁烯黏著劑,亦觀察到此改善。
100‧‧‧障壁膜構造
110‧‧‧基材
120‧‧‧氣體障壁膜
130‧‧‧障壁黏著劑層
140‧‧‧離型襯墊
200‧‧‧障壁膜構造
210‧‧‧基材
220‧‧‧超障壁膜
230‧‧‧障壁黏著劑層
250‧‧‧有機電子裝置
260‧‧‧裝置基材
470‧‧‧玻璃基材
480‧‧‧鈣
圖1係障壁膜構造之示意圖。
圖2係經封裝之有機裝置之示意圖。
圖3係在實施例中使用的障壁膜構造之示意圖。
圖4係用於實施例中鈣測試之層壓構造之示意圖。
圖5係用於實施例中鈣測試之層壓構造之平面圖。
圖6係在加速老化條件下光學密度隨時間耗損之百分比圖。
本發明之障壁黏著劑組成物包含聚異丁烯樹脂。該聚異丁烯樹脂一般具有約40,000至約2,600,000g/mol之黏度平均分子量。在一些實施例中該聚異丁烯樹脂具有約300,000至約900,000g/mol之黏度平均分子量。在一些實施例中,該樹脂系統包含黏度平均分子量係約300,000至約500,000g/mol、約350,000至約450,000g/mol、或約400,000g/mol之第一聚異丁烯樹脂與(b)黏度平均分子量係約700,000至約900,000g/mol、約650,000g/mol至約850,000g/mol、或約800,000g/mol之第二聚異丁烯樹脂之摻合物。
黏度平均分子量(Mv)一般係基於施陶丁格(Staudinger)指數。施陶丁格指數Jo(cm3/g)係通過烏氏(Ubbelohde)黏度計的毛細管I從20℃的流動時間計算。
Jo=ηsp/c(1+0.31×ηsp)cm3/g(Schulz-Blaschke方程式)
ηsp=t/to-1(特定黏度)
t=溶液的流動時間,以Hagenbach-Couette校正
to=溶劑的流動時間,以Hagenbach-Couette校正
c=溶液濃度為g/cm3
黏度平均分子量係根據式Jo=3.06*10-2*Mv 0.65計算。
在一些實施例中,該樹脂系統包含相對於該樹脂系統之總重量約65至約85wt.%之聚異丁烯樹脂。在一些實施例中,該樹脂系統包含相對於該樹脂系統之總重量約15至約35wt.%、約20至約30wt.%、或約25wt.%之第一聚異丁烯樹脂。在一些實施例中,該樹脂系統包含相對於該樹脂系統之總重量約40至約60wt.%、約45至約55wt.%、或約50wt.%之第二聚異丁烯樹脂。
聚異丁烯樹脂通常係在主鏈或側鏈中具有聚異丁烯樹脂骨架之樹脂。在一些實施例中,聚異丁烯樹脂實質上係異丁烯之均聚物,諸如舉例來說:可以商標名稱OPPANOL(BASF AG)與GLISSO-PAL(BASF AG)購得之聚異丁烯樹脂。適合的可商購之聚異丁烯樹脂之實例包括OPPANOL B15(Mv=85,000)、OPPANOL B50(Mv=400,000)、OPPANOL B50SF與穩定劑(Mv=400,000)、OPPANOL N50(Mv=425,000)、OPPANOL N50SF與穩定劑(Mv=425,000)、OPPANOL B80(Mv=800,000)及OPPANOL N80(Mv=800,000)。在一些實施例中,聚異丁烯樹脂包含異丁烯之共聚物,諸如舉例來說:合成橡膠,其中異丁烯係與另一種單體共聚合。合成橡膠包括丁基橡膠,其係主成分異丁烯與少量異戊二烯之共聚物,諸如舉例來說:可以商標名稱VISTANEX(Exxon Chemical Co.)與JSR BUTYL (Japan Butyl Co.,Ltd.)購得之丁基橡膠。合成橡膠亦包括主成分異丁烯與苯乙烯、正丁烯、或丁二烯之共聚物。在一些實施例中,可使用異丁烯均聚物與丁基橡膠之混合物。其它有用的共聚物包括苯乙烯-異丁烯二嵌段共聚物(SIB)及苯乙烯-異丁烯-苯乙烯三嵌段共聚物(SIBS),可以商標名稱SIBSTAR(Kaneka Corporation)獲得。
例如:第一聚異丁烯樹脂可包含異丁烯之均聚物且第二聚異丁烯可包含丁基橡膠,或者第一聚異丁烯可包含丁基橡膠且第二聚異丁烯可包含異丁烯之均聚物。第一與第二聚異丁烯樹脂各可包含超過一種樹脂。
聚異丁烯樹脂通常具有類似氫化環脂族烴樹脂之溶解度參數(SP值,用於表徵化合物極性之指數),且展現與氫化環脂族烴樹脂(若使用時)良好之相容性(亦即混溶性),因此可以形成透明膜。此外,聚異丁烯樹脂具有低的表面能,因此使得黏著劑可被塗展至黏附體上,並且最小化在界面處之空隙產生。此外,聚異丁烯樹脂的玻璃轉移溫度與透濕性低,因此適合作為黏著劑封裝組成物之基底樹脂。
聚異丁烯樹脂可具有所需之黏彈性質,其通常可用於賦予黏著劑封裝組成物所需之流動程度。可使用應變流變儀(strain rheometer)來測定各種不同溫度下之彈性(儲存)模數G’,與黏性(損耗)模數G”。然後使用G’與G”來判定比值tan(δ)=G”/G’。通常,tan(δ)值越高,材料越像黏性材料,tan(δ)值越低,材料越像彈性固體。在一些實施例中,可選擇聚異丁烯樹脂,以使得當黏著劑封裝 組成物在約70℃至約110℃下時,該組成物具有在相對低頻率下至少約0.5之tan(δ)值。依此方式,該組成物即可充份流經凹凸不平表面且極少或沒有空氣截留。
本發明之障壁黏著劑組成物可選地亦包括增黏劑。通常,增黏劑可為可提高黏著劑封裝組成物之膠黏性之任何化合物或化合物之混合物。希望的是,增黏劑不提高透濕性。增黏劑可包含氫化烴樹脂、部分氫化烴樹脂、非氫化烴樹脂、或其組合。較佳地,增黏劑包含氫化石油樹脂。在一些實施例中,黏著劑組成物包含相對於該組成物之總重量約15至約35wt.%、約20至約30wt.%、或約25wt.%之增黏劑。
增黏劑之實例包括但不限於:基於氫化萜之樹脂(例如:以商品名稱CLEARON P、M與K(Yasuhara Chemical)購得之樹脂);氫化樹脂或基於酯之氫化樹脂(例如:以下列商品名稱購得之樹脂:FORAL AX(Hercules Inc.);FORAL 105(Hercules Inc.);PENCEL A(Arakawa Chemical Industries.Co.,Ltd.);ESTERGUM H(Arakawa Chemical Industries Co.,Ltd.);與SUPER ESTER A(Arakawa Chemical Industries.Co.,Ltd.);歧化樹脂或基於酯之歧化樹脂(例如:以商品名稱PINECRYSTAL(Arakawa Chemical Industries Co.,Ltd.)購得之樹脂;基於二環戊二烯之氫化樹脂,其係藉由石油腦(petroleum naphtha)經過熱分解所產生之C5餾份(如:戊烯、異戊二烯、胡椒鹼、與1,3-戊二烯)共聚合所得到之C5-型石油樹脂之氫化樹脂(例如:以下列商品名稱購得之樹脂:ESCOREZ 5300與5400 系列(Exxon Chemical Co.);EASTOTAC H(Eastman Chemical Co.));基於經芳族改質之二環戊二烯之部分氫化樹脂(例如:以商品名稱ESCOREZ 5600(Exxon Chemical Co.)購得之樹脂);氫化C9-型石油樹脂所產生之樹脂,C9-型石油樹脂係藉由石油腦經過熱分解所產生之C9餾份(如:茚、乙烯基甲苯、與α-或β-甲基苯乙烯)共聚合製得(例如:以商品名稱ARCON P或ARCON M(Arakawa Chemical Industries Co.,Ltd.)購得之樹脂);由上述C5餾份與C9餾份共聚合之石油樹脂氫化所得之樹脂(例如:以商品名稱IMARV(Idemitsu Petrochemical Co.)購得之樹脂)。
非氫化烴樹脂包括C5、C9、C5/C9烴樹脂、聚萜樹脂、經芳族改質之聚萜樹脂或松香衍生物。若使用非氫化烴樹脂,一般會與另一種氫化或部分氫化之增黏劑組合使用。
在一些實施例中,增黏劑包含氫化烴樹脂,特別是氫化環脂族烴樹脂。氫化環脂族烴樹脂之具體實例包括ESCOREZ 5340(Exxon Chemical)。在一些實施例中,氫化環脂族烴樹脂係基於二環戊二烯之氫化樹脂,因為其低透濕性與透明度。可用於黏著劑封裝組成物之氫化環脂族烴樹脂一般具有約200至5,000g/mol之重量平均分子量。在另一實施例中,氫化環脂族烴樹脂之重量平均分子量係約500至3,000g/mol。若重量平均分子量超過5,000g/mol,則可能造成不良膠黏性,或可能降低與聚異丁烯樹脂之相容性。
增黏劑可能具有至少部分地隨著組成物之黏著性、利用溫度、生產容易度、及類似者而異之軟化溫度或軟化點(環球法軟化 溫度)。環球法軟化溫度通常可係約50至200℃。在一些實施例中,環球法軟化溫度係約80至150℃。若環球法軟化溫度低於80℃,增黏劑可能因電子裝置發光時所產生之熱造成分離與液化。這會造成直接使用黏著劑封裝組成物封裝之有機電致發光裝置的有機層諸如發光層之劣化。另一方面,若環球法軟化點超過150℃,增黏劑之添加量太低,以致無法得到令人滿意之重要特性改良。
在一些實施例中,增黏劑包含氫化烴樹脂,特別是氫化環脂族烴樹脂。氫化環脂族烴樹脂之具體實例包括ESCOREZ 5300及ESCOREZ 5340(Exxon Chemical)。在一些實施例中,氫化環脂族烴樹脂係基於二環戊二烯之氫化樹脂,因為其低透濕性與透明度。可用於黏著劑封裝組成物之氫化環脂族烴樹脂一般具有約200至5,000g/mol之重量平均分子量。在另一實施例中,氫化環脂族烴樹脂之重量平均分子量係約500至3,000g/mol。若重量平均分子量超過5,000g/mol,則可能造成不良膠黏性,或可能降低與聚異丁烯樹脂之相容性。
本發明之障壁黏著劑組成物包括經有機改質之奈米黏土。奈米黏土一般係可經陽離子取代之礦物質,其已經過有機改質劑處理,而可與樹脂系統相容。在一些實施例中,奈米黏土之最長尺寸係約100至約1000nm。
合適之奈米黏土材料包括例如以下地質類別中之該等黏土材料:膨潤石、高嶺土、伊萊石(illite)、綠泥石、蛇紋石、鎂鋁海泡石、坡縷石、蛭石、海綠石、海泡石、以及混層黏土。膨潤石可包 括例如微晶高嶺石、膨土、葉蠟石、水輝石、皂石、鋅膨潤石、囊脫石、滑石、拜萊石、以及鉻嶺石。高嶺土可包括例如高嶺石、狄克石、珍珠石、葉蛇紋石、多矽高嶺石、多水高嶺石、印得石(indellite)以及纖蛇紋石。伊利石包括例如漂雲母、白雲母、鈉雲母、金雲母以及黑雲母。綠泥石可包括例如柯綠石、葉綠泥石、片鋁綠泥石、鋁綠泥石、斜綠泥石以及斜鎂綠泥石。混層黏土可包括例如板石及蛭石黑雲母(vermiculitebiotite)。此等層化黏土礦物之變異體及同形取代物(isomorphic substitution)提供獨特的應用。較佳係使用微晶高嶺石、膨土、或其組合。
用於黏土的合適之有機改質劑包括例如:具有二甲基苯甲基氫化獸脂四級銨離子、雙(氫化獸脂)二甲基四級銨離子、甲基獸脂雙-2-羥基乙基四級銨離子、二甲基氫化獸脂2-乙基己基四級銨離子、或二甲基去氫化獸脂四級銨離子者。
障壁黏著劑組成物一般包含相對於該組成物之總重量約1至約10wt.%、或約2至約5wt.%之該經有機改質之奈米黏土。
本發明之障壁黏著劑組成物亦包括吸附劑奈米粒子,諸如奈米尺寸乾燥劑及/或吸氣劑以吸附及/或吸收氧氣及/或濕氣。
適合的乾燥劑之實例包括脫水金屬鹵化物、鹽、矽酸鹽、氧化物、氫氧化物、鹵化物、硫酸鹽、過氯酸鹽、碳酸鹽及活性碳。具體實例包括氯化鈷、氯化鈣、溴化鈣、氯化鋰、氯化鋅、溴化鋅、二氧化矽(矽膠)、氧化鋁(活性氧化鋁)、硫酸鈣、硫酸銅、碳酸鉀、碳酸鎂、二氧化鈦、膨土、酸性黏土、高嶺石、矽藻土(黏 土礦物)氧化矽鋁、沸石、二氧化矽、氧化鋯、活性碳、五氧化磷、硫酸鎂及鹼土金屬氧化物,諸如氧化鋇、氧化鈣、氧化鐵及氧化鎂。
適合的吸氣劑之實例包括細散金屬,諸如Al、Fe、Mg及Mn。
在一些實施例中,氧化鈣係較佳吸著劑材料。在一些實施例中,吸著劑材料具有不大於約200nm(例如,約1nm至約200nm)之平均粒子大小。
障壁黏著劑組成物一般包含相對於該組成物之總重量約0.5至約10wt.%、或約1至約5wt.%之該吸附劑奈米粒子。
在一些實施例中,本發明之障壁黏著劑組成物係基於溶劑之黏著劑。任何可溶解樹脂之有用溶劑均可使用。合適溶劑實例包括庚烷、甲苯、二甲苯、苯、乙基苯、與己烷(較佳為庚烷、甲苯、或其組合。在一些實施例中,較佳的是溶劑具有低於約200℃之沸點。
在一些實施例中,溶劑佔總障壁黏著劑組成物之約40至約95wt.%、約65至約95wt.%、約70至約90wt.%、約75至約85wt.%、或約80wt.%。
本發明之障壁黏著劑組成物可藉由所屬技術領域具有通常知識者已知的各種不同方法製備。例如:障壁黏著劑組成物可藉由徹底混合上述組分來製備。混合該組成物時,可使用任意混合機,如:捏合機或擠壓機。在一些實施例中,組成物可藉由例如下述製備:製備樹脂系統與溶劑之混合物,分散該經有機改質之奈米黏土及 吸附劑奈米粒子至溶劑中,接著組合該樹脂混合物與該奈米黏土粒子分散液。
本發明之障壁黏著劑組成物展現良好之可見光穿透率及低霧度。在一些實施例中,障壁黏著劑組成物具有約90%或更高之可見光穿透率。在一些實施例中,障壁黏著劑組成物具有約3%或更小之霧度。
本發明之障壁黏著劑組成物一般係不可固化或非反應性組成物。不可固化組成物係有利的,因為其等不需要使用移動性(migratory)物種,如:起始劑。其等亦消除可傷害下伏裝置之高溫固化之需求。組成物可為例如:基於溶劑之乾燥黏著劑、壓敏性黏著劑、接觸黏著劑、或熱熔性黏著劑。較佳地,組成物係基於溶劑之乾燥黏著劑,其在乾燥時硬化。當溶劑蒸發時黏度提高,黏著劑組成物即硬化。
本發明之障壁黏著劑組成物可藉用任何可用之塗佈製程施加至基材、裝置、或任何裝置組件。基於溶劑之乾燥黏著劑一般藉由刷子、輥、珠粒或條帶(ribbon)、或噴灑施加。障壁黏著劑組成物可塗佈至適當基材上,以形成障壁黏著劑物件。
障壁黏著劑組成物可例如:塗佈至氣體障壁膜上並允許其乾燥,以形成黏著劑障壁膜。氣體障壁膜具有低的氧通透性,可用於協助防止物品(如:食品、電子產品、與藥品)與氧接觸而劣化。一般而言,食品級氣體障壁膜具有在20℃與65%相對濕度下小於約1cm3/m2/天之氧穿透率。較佳地,氣體障壁膜亦具有障壁濕氣之性質。
聚合氣體障壁膜實例包括乙基乙烯基醇共聚物(EVOH)膜,如:聚乙烯EVOH膜與聚丙烯EVOH膜;聚醯胺膜,如:共擠壓之聚醯胺/聚乙烯膜、共擠壓之聚丙烯/聚醯胺/聚丙烯膜;與聚乙烯膜,如:低密度、中密度、或高密度聚乙烯膜,與共擠壓之聚乙烯/乙基乙烯基乙酸酯膜。聚合氣體障壁膜亦可經金屬化,例如:在聚合物膜上塗佈一薄層金屬,如:鋁。
無機氣體障壁膜實例包括包含氧化矽、氮化矽、氧氮化矽、氧化鋁之膜、類鑽石膜、類鑽石玻璃與箔(foil),如:鋁箔。
較佳地,氣體障壁膜係可撓。在一些應用中,亦較佳係該氣體障壁膜係可見光透射的。如本文中所使用,用語「可見光透射(visible light-transmissive)」意指在可見光光譜部分(例如:在400nm與700nm之間)之平均透射率係至少約80%,較佳為至少約88%或90%。
在一些應用中,需要免於濕氣與氧之保護。在特別敏感之應用中,可能需要「超障壁膜(ultra-barrier film)」。超障壁膜一般具有在23℃與90%RH下小於約0.005cc/m2/天之氧穿透率,及在23℃與90%RH下小於約0.005g/m2/天之水蒸氣穿透率。
一些超障壁膜係多層膜,其包含設置在聚合物層之間之無機可見光透射性層。一種合適的超障壁膜之實例包含一可見光透射性無機障壁層,該無機障壁層設置在玻璃轉化溫度(Tg)高於或等於熱安定化聚對苯二甲酸乙二酯(HSPET)之聚合物之間。
許多種Tg高於或等於HSPET之聚合物可被採用。形成合適高Tg聚合物之可揮發性單體尤佳。較佳地,第一聚合物層之Tg高於PMMA,更佳地Tg為至少約110℃,又更佳地至少約150℃,且最佳地至少約200℃。可用於形成第一層之尤佳單體包括胺甲酸酯丙烯酸酯(例如:CN-968,Tg=約84℃,與CN-983,Tg=約90℃,二者均購自Sartomer Co.)、丙烯酸異莰酯(例如:SR-506,購自Sartomer Co.,Tg=約88℃)、二新戊四醇五丙烯酸酯(例如:SR-399,購自Sartomer Co.,Tg=約90℃)、與苯乙烯摻合之環氧丙烯酸酯(例如:CN-120S80,購自Sartomer Co.,Tg=約95℃)、二-三羥甲基丙烷四丙烯酸酯(例如:SR-355,購自Sartomer Co.,Tg=約98℃)、二乙二醇二丙烯酸酯(例如:SR-230,購自Sartomer Co.,Tg=約100℃)、1,3-丁二醇二丙烯酸酯(例如:SR-212,購自Sartomer Co.,Tg=約101℃)、五丙烯酸酯(例如:SR-9041,購自Sartomer Co.,Tg=約102℃)、新戊四醇四丙烯酸酯(例如:SR-295,購自Sartomer Co.,Tg=約103℃)、新戊四醇三丙烯酸酯(例如:SR-444,購自Sartomer Co.,Tg=約103℃)、乙氧基化(3)三羥甲基丙烷三丙烯酸酯(例如:SR-454,購自Sartomer Co.,Tg=約103℃)、乙氧基化(3)三羥甲基丙烷三丙烯酸酯(例如:SR-454HP,購自Sartomer Co.,Tg=約103℃)、烷氧基化三官能性丙烯酸酯(例如:SR-9008,購自Sartomer Co.,Tg=約103℃)、二丙二醇二丙烯酸酯(例如:SR-508,購自Sartomer Co.,Tg=約104℃)、新戊二醇二丙烯酸酯(例如:SR-247,購自Sartomer Co.,Tg=約107℃)、乙氧 基化(4)雙酚a二甲基丙烯酸酯(例如:CD-450,購自Sartomer Co.,Tg=約108℃)、環己烷二甲醇二丙烯酸酯(例如:CD-406,購自Sartomer Co.,Tg=約110℃)、甲基丙烯酸異莰酯(例如:SR-423,購自Sartomer Co.,Tg=約110℃)、環狀二丙烯酸酯(例如:SR-833,購自Sartomer Co.,Tg=約186℃)、與參(2-羥基乙基)異氰脲酸酯三丙烯酸酯(例如:SR-368,購自Sartomer Co.,Tg=約272℃)、上述甲基丙烯酸酯之丙烯酸酯、與上述丙烯酸酯之甲基丙烯酸酯。
第一聚合物層可藉由施加一層單體或寡聚物至基材,以及使該層交聯以原位形成聚合物來形成,例如,藉由閃蒸及氣相沉積輻射可交聯單體,隨後使用例如電子束設備、UV光源、放電設備、或其他合適裝置進行交聯。可藉由冷卻支撐物來改良塗佈效率。單體或寡聚物亦可使用習知塗佈方法,如:輥塗法(例如:凹版輥塗佈)或噴塗法(例如:靜電噴塗)施加至基材,然後如上述說明進行交聯。第一聚合物層亦可藉由施加一層於溶劑中含有寡聚物或聚合物之層,以及乾燥該經施加之層以移除溶劑來形成。若希望提供在高溫下具有玻璃態之聚合層,且玻璃轉化溫度高於或等於HSPET時,亦可採用電漿聚合法。最佳的是,第一聚合物層係藉由閃蒸及氣相沉積及隨後的原位交聯形成,其說明於例如:美國專利第4,696,719號(Bischoff)、第4,722,515號(Ham)、第4,842,893號(Yializis等人)、第4,954,371號(Yializis)、第5,018,048號(Shaw等人)、第5,032,461號(Shaw等人)、第5,097,800號(Shaw等人)、第5,125,138號(Shaw等人)、第5,440,446號(Shaw等人)、第 5,547,908號(Furuzawa等人)、第6,045,864號(Lyons等人)、第6,231,939號(Shaw等人)、以及第6,214,422號(Yializis);公開之PCT申請案WO 00/26973(Delta V Technologies,Inc.);D.G.Shaw and M.G.Langlois,「A New Vapor Deposition Process for Coating Paper and Polymer Webs」,6th International Vacuum Coating Conference(1992);D.G.Shaw and M.G.Langlois,「A New High Speed Process for Vapor Depositing Acrylate Thin Films:An Update」,Society of Vacuum Coaters 36th Annual Technical Conference Proceedings(1993);D.G.Shaw and M.G.Langlois,「Use of Vapor Deposited Acrylate Coatings to Improve the Barrier Properties of Metallized Film」,Society of Vacuum Coaters 37th Annual Technical Conference Proceedings(1994);D.G.Shaw,M.Roehrig,M.G.Langlois and C.Sheehan,「Use of Evaporated Acrylate Coatings to Smooth the Surface of Polyester and Polypropylene Film Substrates」,RadTech(1996);J.Affinito,P.Martin,M.Gross,C.Coronado and E.Greenwell,「Vacuum deposited polymer/metal multilayer films for optical application」,Thin Solid Films 270,43-48(1995);以及J.D.Affinito,M.E.Gross,C.A.Coronado,G.L.Graff,E.N.Greenwell and P.M.Martin,「Polymer-Oxide Transparent Barrier Layers」,Society of Vacuum Coaters 39th Annual Technical Conference Proceedings(1996)。
各聚合物層之平滑性與連續性及其對下伏層之黏著性係較佳地藉由適當前處理來增強。較佳的前處理方案採用在適當反應性或非反應性氣氛存在下放電(例如,電漿、輝光放電、電暈放電、介電障壁放電、或大氣壓放電);化學前處理或火燄前處理。此等前處理有助於讓下伏層之表面更具接受性(receptive),以形成後續施加之聚合層。電漿前處理係特佳。亦可利用另一種組成上不同於高Tg聚合物層之黏著性促進層覆在下伏層之頂部上,以改良層間黏著性。黏著性促進層可係例如另一聚合層或含金屬層,諸如金屬、金屬氧化物、金屬氮化物、或金屬氮氧化物之層。黏著性促進層可具有數nm(例如1或2nm)至約50nm之厚度,若需要時可以更厚。
第一聚合物層的所欲化學組成與厚度將部分取決於支撐物的本質與表面形貌。厚度較佳係足以提供平滑、無缺陷表面,以供後續施加第一無機障壁層。例如:第一聚合物層可具有數nm(例如:2或3nm)至約5μm之厚度,若需要時可以更厚。
一或多個由具有Tg高於或等於HSPET之聚合物層分隔開之可見光透射無機障壁層位於第一聚合物層之頂部上。此等層可分別稱為「第一無機障壁層」、「第二無機障壁層」、與「第二聚合物層」。若需要時,可存在其他無機障壁層與聚合物層,包括Tg不高於或等於HSPET之聚合物層。然而較佳的是,各對相鄰之無機障壁層僅利用Tg高於或等於HSPET之聚合物層分隔開,且更佳的是僅利用Tg高於PMMA之聚合物層分隔開。
無機障壁層不一定要相同。可採用各種不同的無機障壁材料。較佳無機障壁材料包括金屬氧化物、金屬氮化物、金屬碳化物、金屬氮氧化物、金屬硼氧化物、與其組合,例如:氧化矽諸如二氧化矽、氧化鋁諸如礬土、鈦氧化物諸如二氧化鈦、銦氧化物、錫氧化物、氧化銦錫(「ITO」)、鉭氧化物、鋯氧化物、鈮氧化物、碳化硼、碳化鎢、碳化矽、氮化鋁、氮化矽、氮化硼、氮氧化鋁、氮氧化矽、氮氧化硼、硼氧化鋯、硼氧化鈦、與其組合。氧化銦錫、氧化矽、氧化鋁、與其組合係尤佳之無機障壁材料。ITO係一類特別的陶瓷材料實例,在適當選擇各元素構成分之相對比例下,可變成具有導電性。無機障壁層較佳係使用膜金屬化技術領域中所採用之技術形成,如:濺鍍(例如:陰極或平面磁控濺鍍)、蒸鍍(例如:電阻式或電子束蒸鍍)、化學氣相沉積、原子層沉積、電鍍、與類似方法。無機障壁層最佳係使用濺鍍例如反應性濺鍍來形成。相較於較低能量技術諸如習知化學氣相沉積製程,當藉由高能量沉積技術諸如濺鍍形成無機層時,已觀察到增強的障壁性質。各無機障壁層之平滑性與連續性及其與下伏層之黏著性可藉由前處理(例如:電漿前處理)來增強,如上述關於第一聚合物層之前處理。
無機障壁層不一定要具有相同厚度。各無機障壁層的所欲化學組成與厚度將部分取決於下伏層的本質與表面形貌以及障壁總成的所欲光學性質。無機障壁層較佳係足夠厚以呈連續性,且足夠薄以確保障壁總成及含有該總成之物件將具有所欲程度之可見光透射性 與可撓性。較佳地,各無機障壁層之物理厚度(相對於光學厚度)係約3至約150nm,更佳係約4至約75nm。
分隔第一、第二與任何其他無機障壁層之第二聚合物層不一定相同,且不一定要全部具有相同厚度。可採用各種不同的第二聚合物層材料。較佳的第二聚合物層材料包括如上述關於第一聚合物層之材料。較佳地,第二聚合物層係如上述關於第一聚合物層之說明,藉由閃蒸及氣相沉積及隨後的原位交聯施加。較佳地,亦可在形成第二聚合物層之前採用如上述之前處理(例如:電漿前處理)。第二聚合物層的所欲化學組成與厚度將部分取決於(多個)下伏層的本質與表面形貌。第二聚合物層之厚度較佳係足以提供平滑、無缺陷表面,以供後續施加無機障壁層。一般而言,第二聚合物層可具有低於第一聚合物層之厚度。例如:各第二聚合物層可具有約5nm至約10μm之厚度,若需要時可以更厚。
可撓可見光透射性超障壁膜與其製造係說明於例如:美國專利第7,940,004號(Padiyath等人),其以引用方式併入本文中。
市售超障壁膜包括例如:可購自3M Company之FTB 3-50與FTB 3-125。
可在基材上提供已塗佈一層本發明之黏著劑障壁組成物之氣體障壁膜。基材較佳係撓性及可見光穿透性。合適之基材材料包括有機聚合材料,如:聚對苯二甲酸乙二酯(PET)、聚丙烯酸酯、聚碳酸酯、聚矽氧、環氧樹脂、聚矽氧官能化環氧樹脂、聚酯,如:Mylar (製造商E.I.du Pont de Nemours & Co.)、聚醯亞胺,如:Kapton H或Kapton E(製造商du Pont)、Apical AV(製造商Kanegafugi Chemical Industry Company)、Upilex(製造商UBE Industries,Ltd.)、聚醚碸(PES,製造商Sumitomo)、聚醚醯亞胺、聚萘二甲酸乙二酯(PEN)、聚甲基丙烯酸甲酯、苯乙烯/丙烯腈、苯乙烯/馬來酸酐、聚甲醛、聚乙烯基萘、聚醚醚酮、聚芳基醚酮、高Tg氟聚合物(例如:DYNEONTM六氟丙烯、四氟乙烯、與乙烯之HTE三聚物)、聚α-甲基苯乙烯、聚芳基酸酯、聚碸、聚伸苯基氧化物、聚醯胺亞胺、聚醯亞胺、聚酞醯胺、聚乙烯、與聚丙烯。亦可利用無色聚醯亞胺、環狀烯烴共聚物、與環狀烯烴共聚物。較佳地,該基材包含PET。
圖1顯示例示性障壁膜構造100之横剖面結構,障壁膜構造包含基材110、氣體障壁膜120(較佳為超障壁膜)、與障壁黏著劑層130。在一些實施例中,障壁黏著劑層具有約5至約50μm之厚度。在一些實施例中,障壁膜構造具有約20至約250μm之厚度。
在一些實施例中,障壁黏著劑層之外表面可採用如:離型襯墊(140)之方式保護。可使用任何有用之離型襯墊,諸如舉例來說:經離型劑(例如:聚矽氧樹脂)處理之膜或片材。終端使用者可移除離型襯墊,以將障壁構造黏附至要保護之裝置。
或者,本發明之障壁黏著劑可設置在兩個離型襯墊之間,以提供給終端使用者。
本發明之障壁膜構造可用於保護OLED顯示器與固態照明、太陽能電池、電泳與電致變色顯示器、薄膜電池組(battery)、量子點裝置、感測器(例如,觸控感測器)、與其他有機電子裝置以阻隔氧與濕氣。其等特別適合需要阻隔氧與濕氣,且需要撓性與良好光學穿透性之用途。
圖2顯示本發明之障壁膜構造被用於封裝有機電子裝置,諸如舉例來說OLED。有機電子裝置250係設置在裝置基材260上。有機電子裝置250係使用障壁膜構造200與裝置基材260封裝,該障壁膜構造包括超障壁膜220、障壁黏著劑層230與基材210。
本發明之目的與優點將以下列實例進一步闡述,然而在這些實例中所引述之特定材料與用量以及其他的條件及細節,皆不應被視為對本發明之過度限制。除非另外註明,否則以下實例中所報導之所有份數、百分比、及比均以重量計。除非另外註明,否則試劑係購自Sigma Aldrich Company,St.Louis,MO。
使用BYK Gardner Haze-Gard Plus(BYK-Gardner USA,Inc.,Columbia,MD)獲得透射率、清晰度、及霧度數據。
藉由將障壁總成層壓到已經沉積元素鈣的玻璃上以產生測試樣品,以測試障壁總成防止濕氣或水蒸氣輸送的能力。然後將這些樣品暴露於升高的溫度和濕度,並測量由於元素鈣與水的反應引起的光學密度損失。先於80℃真空中烘烤各障壁總成,以確保除去任何殘留的濕氣。鈣(反射性金屬)係經過加熱沉積在玻璃板之指定區域上,如正方形之陣列。將各障壁總成放置在四個鈣正方形上之玻璃板上(稱為像素),並層壓該總成以提供測試樣品。使用Epson v750 Professional掃描測試樣本及Aphelion影像分析軟件來分析該掃描,測量各新製成之測試樣品的各鈣像素的光學密度。各樣品隨後保持放置在60℃及90%相對濕度下之環境腔室中加速老化。頭三天中,每天測量光學密度二次。然後每天測量光學密度一次,直到光學密度為初 始光學密度之50%為止。水蒸氣輸送率(WVTR)係與鈣像素的光學密度達到其初始值之50%所需時間成反比。該關係由以下方程式描述:
其中 d Ca 係鈣層的厚度; ρ Ca 係鈣的密度; t i 係時間;係水的莫耳數; n Ca 係鈣的莫耳數;係水的分子量;以及, MW Ca 係鈣的分子量。
將Bulk Oppanol B80及Oppanol B50SF聚異丁烯聚合物樹脂切成約1吋(2.5cm)立方體。然後將稱重的這些樹脂立方體在甲苯中與Escorez 5300增黏劑在封蓋的玻璃罐中混合。黏著劑混合物的重量比為在足夠的甲苯中兩份Oppanol B80、一份Oppanol B50SF、及一份Escorez 5300,以提供25wt.%的溶液。將所得配方用滾筒式混合器混合2週直至溶液均勻。
奈米粒子係氧化鈣奈米粉(CaO)及Claytone APA(「黏土」),以表2中提供的重量比加入到甲苯中。將奈米粒子直接以5wt.%的固體添加到甲苯中,然後使用Sonics Vibra Cell VCX750超音波振盪器(Sonics & Materials Inc.,Newtown,CT)以18至20%的振幅分散20分鐘。
以表3中提供的重量比將製備實例2至4之奈米粒子分散液與製備實施例1之聚異丁烯系聚合物溶液組合。將所得配方用滾筒式混合器混合一週。將所得溶液用甲苯稀釋至達到20wt.%固體的最終固體含量。
為了製備黏著劑膜,使用檯面型缺口棒塗佈機將製備實施例5至9的經奈米粒子填充之黏著劑配方施用於SKC-12N離型襯墊。將該經塗佈的離型襯墊置於80℃的烘箱中20分鐘以除去溶劑,提供具有12微米厚度的黏著劑膜。之後,將M74F或SKC-02N離型襯墊層壓至黏著劑,使得黏著劑夾在兩個離型襯墊之間。然後藉由去除M74F或SKC-02N離型襯墊將黏著劑轉移到3M FTB3-50超障壁膜中,並將黏著劑層壓到超障壁膜的障壁層側以提供障壁總成。表4中提供用於製造測試的障壁總成的黏著劑的組成物。包含聚異丁烯但不含奈米粒子的黏著劑在表中稱為PIB。
加速老化測試樣品 如圖3至5所示(其中470、570是玻璃基材及480、580是鈣)製備和測試用於加速老化測試的樣品且描述於先前濕氣障壁測試中。加速老化測試樣品結果總結在表5及圖6中。如表5所示,相較於未填充的黏著劑(比較例1),含有兩種奈米粒子類型(比較例2至5)中的任一種的測試樣品達到50%光學密度耗損的時間更長。相較於僅含有10wt.%黏土或僅含有1wt.%CaO 的比較例,包含5wt.%黏土與1wt.%CaO組合的實施例顯示出增加的達到50%光學密度耗損的時間。加速老化300小時後,分化變得明顯。
本文所引用之公開案的完整揭露之全文係併入本文以供參照,如同其個別併入一般。本發明中的各種修改與變更對於所屬技術領域中具有通常知識者將為顯而易見且不悖離本發明之範圍與精神。應理解,本發明不意欲受到本文所提出之說明性實施例及實例過度地限制,且此等實例及實施例僅係以舉例方式呈現,其中本發明之範疇僅意欲由本文提出如下之申請專利範圍所限制。
Claims (29)
- 一種障壁黏著劑組成物,其包含:(a)聚異丁烯樹脂;(b)經有機改質之奈米黏土;以及(c)吸著劑奈米粒子。
- 如請求項1之障壁黏著劑組成物,其中該奈米黏土係膨土奈米黏土或微晶高嶺石奈米黏土。
- 如請求項1或2之障壁黏著劑組成物,其中該奈米黏土之最長尺寸係約100至約1000nm。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該奈米黏土係經四級銨離子改質。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該等吸著劑奈米粒子包含金屬氧化物。
- 如請求項5之障壁黏著劑組成物,其中該等吸著劑奈米粒子包含氧化鈣。
- 如請求項6之障壁黏著劑組成物,其中該氧化鈣具有不大於約200nm之平均粒子大小。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該樹脂系統包含黏度平均分子量係約40,000至約2,600,000g/mol之第一聚異丁烯樹脂。
- 如請求項8之障壁黏著劑組成物,其中該樹脂系統包含黏度平均分子量係約300,000至約900,000g/mol之第一聚異丁烯樹脂。
- 如前述請求項中任一項之障壁黏著劑組成物,其包含相對於該組成物之總重量約1至約10wt.%之該經有機改質之奈米黏土。
- 如請求項10之障壁黏著劑組成物,其包含相對於該組成物之總重量 約2至約5wt.%之該經有機改質之奈米黏土。
- 如前述請求項中任一項之障壁黏著劑組成物,其包含相對於該組成物之總重量約0.5至約10wt.%之該等吸著劑奈米粒子。
- 如請求項12之障壁黏著劑組成物,其包含相對於該組成物之總重量約1至約5wt.%之該等吸著劑奈米粒子。
- 如前述請求項中任一項之障壁黏著劑組成物,其進一步包含溶劑。
- 如前述請求項中任一項之障壁黏著劑組成物,其進一步包含紫外光阻斷劑。
- 如前述請求項中任一項之障壁黏著劑組成物,其進一步包含增黏劑。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該聚異丁烯樹脂包含異丁烯共聚物。
- 如請求項17之障壁黏著劑組成物,其中該聚異丁烯樹脂包含丁基橡膠。
- 一種障壁黏著劑組成物,其包含:(a)約50至約75wt.%之聚異丁烯樹脂,該聚異丁烯樹脂具有約300,000至約900,000g/mol之黏度平均分子量,(b)約1至約10wt.%之經有機改質之奈米黏土,(c)約1至約5wt.%之氧化鈣奈米粒子,以及(d)約10至約25wt.%之增黏劑,以上皆係相對於該組成物之總重量計。
- 一種黏著劑障壁膜,其包含設置在一氣體障壁膜上之一層如前述請求項中任一項之障壁黏著劑組成物。
- 如請求項20之黏著劑障壁膜,其中該氣體障壁膜係一超障壁膜,該超障壁膜具有在23℃與90% RH下小於約0.005cc/m 2/天之氧穿透率,及在23℃與90% RH下小於約0.005g/m 2/天之水蒸氣穿透率。
- 如請求項21之黏著劑障壁膜,其中該超障壁膜係一多層膜,該多層膜包含設置在聚合物層之間的一無機可見光穿透性層。
- 如請求項20至22中任一項之黏著劑障壁膜,其進一步包含相對該層該障壁黏著劑組成物而設置在該氣體障壁膜上之一基材。
- 如請求項23之黏著劑障壁膜,其中該基材包含聚對苯二甲酸乙二酯。
- 如請求項20至24中任一項之黏著劑障壁膜,其進一步包含相對該氣體障壁膜而設置在該層該障壁黏著劑組成物上之一離型層。
- 一種經囊封之有機電子裝置,其包含囊封一薄膜裝置之如請求項1至19中任一項之障壁黏著劑組成物。
- 如請求項26之經囊封之有機電子裝置,其中該裝置係一OLED。
- 一種經囊封之觸控感測器,其包含囊封一觸控感測器之如請求項1至19中任一項之障壁黏著劑組成物。
- 一種障壁黏著劑物品,其包含設置在離型層之間之一層如請求項1至19中任一項之障壁黏著劑組成物。
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CN (1) | CN109415607B (zh) |
TW (1) | TW201811964A (zh) |
WO (1) | WO2017218500A1 (zh) |
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WO2020187681A1 (en) | 2019-03-15 | 2020-09-24 | Henkel Ag & Co. Kgaa | Sulfone-resin containing gas-barrier adhesive |
JP6864139B1 (ja) * | 2020-06-25 | 2021-04-28 | デンカ株式会社 | ブチルゴム系粘着剤組成物、粘着テープ、屋根用防水シート及び接合体 |
JP7153104B2 (ja) * | 2020-06-25 | 2022-10-13 | デンカ株式会社 | ブチルゴム系粘着剤組成物、粘着テープ、屋根用防水シート及び接合体 |
CN113376916B (zh) * | 2021-06-25 | 2022-05-31 | 绍兴迪飞新材料有限公司 | 一种智能动态调光膜及其制备方法和应用 |
CN113930188B (zh) * | 2021-09-30 | 2023-02-03 | 四川北尚新材料科技有限公司 | 一种水下粘弹体防腐胶及其制备方法、水下粘弹体防腐胶带 |
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- 2017-06-13 JP JP2018565698A patent/JP2019523804A/ja active Pending
- 2017-06-13 CN CN201780037231.1A patent/CN109415607B/zh active Active
- 2017-06-13 WO PCT/US2017/037197 patent/WO2017218500A1/en unknown
- 2017-06-13 US US16/309,835 patent/US11034865B2/en active Active
- 2017-06-13 KR KR1020187037425A patent/KR102407014B1/ko active IP Right Grant
- 2017-06-15 TW TW106119990A patent/TW201811964A/zh unknown
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WO2017218500A1 (en) | 2017-12-21 |
US11034865B2 (en) | 2021-06-15 |
EP3472254A1 (en) | 2019-04-24 |
KR20190019960A (ko) | 2019-02-27 |
US20200181460A1 (en) | 2020-06-11 |
CN109415607B (zh) | 2022-08-09 |
CN109415607A (zh) | 2019-03-01 |
KR102407014B1 (ko) | 2022-06-10 |
JP2019523804A (ja) | 2019-08-29 |
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