TW201726864A - 填充奈米黏土之障壁黏著劑組成物 - Google Patents
填充奈米黏土之障壁黏著劑組成物 Download PDFInfo
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- TW201726864A TW201726864A TW105126162A TW105126162A TW201726864A TW 201726864 A TW201726864 A TW 201726864A TW 105126162 A TW105126162 A TW 105126162A TW 105126162 A TW105126162 A TW 105126162A TW 201726864 A TW201726864 A TW 201726864A
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- barrier
- adhesive
- resin
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- adhesive composition
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Classifications
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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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
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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
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- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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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]
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- B32B2307/7244—Oxygen barrier
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/01—High molecular weight, e.g. >800,000 Da.
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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
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- 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
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- 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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-
- 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
- C09J2423/00—Presence of polyolefin
- C09J2423/001—Presence of polyolefin in the barrier 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
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- C09J2467/006—Presence of polyester in the substrate
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H10K50/80—Constructional details
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
一種障壁黏著劑組成物,其包含樹脂系統及經有機改質之奈米黏土。該樹脂系統包含(a)具有約300,000至約500,000g/mol之黏度平均分子量之第一聚異丁烯樹脂、(b)具有約700,000至約900,000g/mol之黏度平均分子之第二聚異丁烯樹脂、及(c)增黏劑。
Description
本發明係關於填充奈米黏土之障壁黏著劑組成物且關於包含一層該黏著劑之黏著障壁膜。
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,如說明於例如:美國專利申請公開案第US 2014/0377554號(Cho等人),包括奈米黏土作為「濕氣封阻劑(moisture blocker)」。
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,在一個態樣中,本發明提供障壁黏著劑組成物,其包含樹脂系統及經有機改質之奈米黏土。該樹脂系統包含(a)具有約300,000至約500,000g/mol之黏度平均分子量之第一聚異丁烯樹脂、(b)具有約700,000至約900,000g/mol之黏度平均分子之第二聚異丁烯樹脂、及(c)增黏劑(tackifier)。
在另一態樣中,本發明提供障壁黏著劑組成物,其包含樹脂系統、經有機改質之奈米黏土、及溶劑。該樹脂系統包含(a)約15至約35wt.%之第一聚異丁烯樹脂,該第一聚異丁烯樹脂具有約300,000至約500,000g/mol之黏度平均分子量、(b)約40至約60wt.%之第二聚異丁烯樹脂,該第二聚異丁烯樹脂具有約700,000至約900,000g/mol之黏度平均分子、及(c)約15至約35wt.%之增黏劑,以上皆係相對於該樹脂系統之總重量計。
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。
當本發明之障壁黏著劑組成物施加至超障壁膜時,該經塗佈之超障壁膜構造具有實質上改良之障壁性能。如本文中所使用,用語「超障壁膜(ultra-barrier film)」意指具有在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/天之水蒸氣穿透率之膜。
然而令人驚訝的是,填充奈米黏土之障壁黏著劑本身,並未展現顯著優於未填充之對照黏著劑之性能。同樣地,當較低級障壁膜(例如:食品級障壁膜)經本發明之填充奈米黏土之障壁黏著劑塗佈時,其障壁性能相較於經未填充之對照黏著劑塗佈時並未展現顯著改良。
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
220‧‧‧超障壁膜
230‧‧‧障壁黏著劑層
250‧‧‧有機電子裝置
260‧‧‧裝置基材
570‧‧‧玻璃基材
580‧‧‧鈣
圖1係障壁膜構造之示意圖。
圖2係封裝有機裝置之示意圖。
圖3係塗佈填充黏土之障壁黏著劑之超障壁膜之示意圖。
圖4係用於剝離測試的樣本之構造之示意圖。
圖5係用於鈣測試之層壓構造之示意圖。
圖6係光密度隨時間耗損之百分比圖。
圖7代表鈣測試樣品上有食品級障壁膜構造層壓之照片。
圖8係光密度隨時間耗損之百分比圖。
圖9代表鈣測試樣品上有超障壁膜構造層壓之照片。
本發明之障壁黏著劑組成物包含樹脂系統,該樹脂系統包含聚異丁烯樹脂。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。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。
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。合適之市售聚異丁烯樹脂實例包括OPPANOL B50(Mv=400,000)與OPPANOL B80(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。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。
本發明之樹脂系統亦包括增黏劑。通常,增黏劑可為可提高黏著劑封裝組成物之膠黏性(tackiness)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,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 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亦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。
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。
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;更佳為庚烷)。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至溶劑中,接著組合該樹脂混合物與該奈米黏土分散液。
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、或約2%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,氣體障壁膜係撓性。在一些應用中,亦較佳係該氣體障壁膜係可見光穿透性。如本文中所使用,用語「可見光穿透性(visible light-transmissive)」意指在可見光光譜部分(例如:在400nm與700nm之間)之平均穿透率係至少約80%,較佳為至少約88%或90%。
在一些應用中,需要阻隔濕氣與氧之保護。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。令人驚訝地發現,當使用本發明之障壁黏著劑組成物塗佈超障壁膜時,超障壁膜之障壁性能有實質上的改良。
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穿透性層。一種合適的超障壁膜之實例包含一可見光穿透性無機障壁層,該無機障壁層設置在玻璃轉移溫度(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,且玻璃轉移溫度高於或等於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);PCT專利申請公開案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。
一或多個利用Tg高於或等於HSPET之聚合物層分隔開之可見光穿透性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穿透性與撓性。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。
撓性可見光穿透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之橫剖面結構,障壁膜構造100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、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,障壁膜構造200包括超障壁膜220與障壁黏著劑層230。
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。
這些實例僅用於闡釋之目的,並非意圖限制隨附申請專利範圍之範疇。實例及說明書其餘部分中之所有份數、百分比、比率等皆依重量計,除非另有說明。所使用之溶劑與其他試劑得自Sigma-Aldrich Chemical Company,St.Louis,MO,除非另有其他說明。
Escorez 5300氫化石油烴樹脂係購自ExxonMobil Chemical Company(Houston,TX)。Clearon P105得自Yasuhara Chemical(Fuchu-city,Japan)。具有下列式量之聚異丁烯:(i)400,000g/mol(Oppanol B50 SF);(ii)800,000g/mol(Oppanol B80);(iii)1,110,000g/mol(Oppanol B100)係得自BASF(Florham Park,NJ)。Exxon Butyl 268丁基橡膠係得自ExxonMobil Chemical(Houston,TX)。庚烷與甲苯係購自VWR International(Radnor,PA)。二甲苯係得自EMD(Gibbstown,NJ)。SKC-12N與SKC-02N離型襯墊之卷係購自SKC Haas(Seoul,Korea)。M74F離型襯墊之卷係得自
Siliconature(Godega di Sant’Urbano,Italy)。Aldrich 682640表面改質之奈米黏土係購自Sigma-Aldrich(Saint Louis,MO)。Claytone APA親有機物膨土、Claytone AF親有機物膨土、與Cloisite-20微粒化奈米黏土係得自BYK(Wesel,Germany)。
先將聚異丁烯與丁基橡膠聚合物樹脂切成約1吋立方體。此等樹脂立方體隨後與增黏劑一起加至庚烷或甲苯中,且所得配方於滾輪上混合1至2週。此作業所使用之基於聚異丁烯之黏著劑溶液說明於表1,且表1中「聚合樹脂」一欄所列之「份」係以重量計之份數。
將微晶高嶺石黏土分散在有機溶劑中,其係以如表2所示之固體wt%直接添加黏土粉末至庚烷或甲苯中。然後,採用下列方式之一,將黏土混合至甲苯或庚烷溶劑中:
(i)IKA® T25數位化Ultra-Turrax高剪切混合機(IKA® Works,Inc.,Wilmington,NC),依指定旋轉速率及指定時間進行,或(ii)Sonics Vibra Cell VCX750超音波振盪器(Sonics & Materials Inc.,Newtown,CT),依指定振幅及指定時間長度進行。
製備PE13至PE22時,將表2之微晶高嶺石黏土分散液與表1之基於聚異丁烯之聚合物溶液組合,並於滾輪上混合1週。所得之經奈米黏土填充之基於聚異丁烯之黏著劑配方概述於表3。
使用三種不同膜基材:多孔性聚丙烯支撐膜(F1);3M食品級氧化物障壁膜(F2);及3M FTB3-50(3M Company,Maplewood,MN)超障壁膜(F3)。此等膜基材之性質概述於表4。
製備手塗樣本時,使用檯面型缺口棒塗佈機,將黏著劑混合物塗佈在SKC-12N離型襯墊上。將經塗佈之樣本放置於80℃烘箱中20分鐘,以移除溶劑。此等樣本之乾燥厚度係25μm。然後將M74F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。CE2與EX8之黏著劑係直接塗佈在3M食品級障壁膜(F2)上,並於80℃下乾燥20分鐘。然後將M74F離型襯墊層壓至黏著劑。
製備樣本EX3與EX9時,使用配備有缺口棒之Hirano試驗塗佈機,將黏著劑混合物塗佈在SKC-12N離型襯墊上。黏著劑於80℃烘箱中乾燥1分鐘,再於另一個烘箱中,於130℃下乾燥1分
鐘。此等樣本之乾燥厚度係25μm。然後將M74F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。
將黏著劑從離型襯墊轉移至多孔性聚丙烯膜(F1)上,以進行整體水蒸氣穿透率(WVTR)測試;轉移至3M食品級障壁膜(F2)上,以進行鈣測試;及轉移至3M超障壁膜(F3)上,以進行剝離測試、剪切測試、與鈣測試。塗佈黏著劑之障壁膜構造之示意圖係提供於圖3。此作業中所測試之所有經塗佈樣本之概述係提供於表5。表5中「黏著劑說明資訊」一欄中之比值為重量比。
使用根據ASTM D1876之T-剝離測試進行剝離測試。從離型襯墊轉移25μm黏著劑並層壓在兩片障壁膜F3之間,使得此等障壁膜片材上之障壁塗層面向黏著劑,如圖4圖解說明。根據ASTM D1876,在將黏著劑轉移至障壁膜之後,有2小時停留時間。於室溫下評估寬度0.5"之樣本。剝離測試係使用裝有SPA2-02 T-剝離夾具之IMASS SP-2000剝離測試機(IMASS,Inc.,Accord,MA)進行。進行三次重覆測量,取平均值報告。
剪切測試係根據ASTM D3654/D3654M程序A完成。轉移25μm黏著劑至障壁膜,其中障壁塗層面向黏著劑。然後將背襯黏著劑之障壁膜黏附至不銹鋼板。使用於23℃與50%RH下之CREX Research Systems(Saint Paul,MN)剪切測試架評估剪切黏著性能。各樣本吊掛1kg重量,並記錄黏著劑內聚失效之時間。進行三次重覆測量,取平均值報告。
黏著劑配方之透濕性係使用Mocon Permatran-W機型1/50 G(Mocon,Inc.,Minneapolis,MN)測試。此等實驗係在40℃與100% RH下,使用50cm2樣本面積完成。樣本係藉由將25μm厚度之黏著劑板塊轉移至多孔性聚丙烯膜(F1)上來製備。然後將樣本對
摺,使得兩片多孔性聚丙烯膜之間有50μm之黏著劑。接著將此等樣本置入Permatran儀器中進行測試。
塗佈黏著劑之測試基材先於80℃真空中焙烤,直到移除濕氣為止。反射性金屬鈣係經過加熱沉積在玻璃基材之指定區域上(例如:正方形之陣列)。將背襯黏著劑之膜設置在塗佈鈣之玻璃基材上,並層壓此夾心體。圖5提供此層壓物件之示意圖(其中570係玻璃基材,且580係鈣),及一些約略之層厚度。各實例中之黏著劑厚度為25μm。在初始時間點,使用密度計測定光密度。樣本隨後保持在60℃/90%相對濕度下之環境腔室中加速老化。頭三天中,每天測量光密度二次。然後每天測量光密度一次,直到光密度為初始光密度之50%為止。水蒸氣穿透率(WVTR)係與光密度達到其初始值之50%所需時間成正比。用於鈣測試之障壁膜為3M FTB3-50超障壁膜(F3)或3M食品級障壁膜(F2)。
填充黏土之實例EX13至EX22與未填充之黏著劑對照樣本CE5至CE7之剝離與剪切數據提供於表6。表6中,「黏著劑說明資訊」一欄中之比值為重量比。通常,當添加奈米黏土至黏著劑時,剝離黏著性強度下降,而剪切黏著性強度則隨著黏土填料之添加
而上升。此等樣本之黏著劑性能通常在膜與基材之層壓上可接受之範圍內。EX19未進行剝離力之測試。
兩種填充黏土之黏著劑與兩種未填充之黏著劑對照組之WVTR數據提供於表7中。WVTR值係使用於40℃與100% RH下操作之MOCON Permatran-W機型1/50 G測量。測試樣本包含50μm厚之黏著劑層夾在多孔性聚丙烯膜(F1)之間。添加奈米黏土填料至PIB黏著劑CE1不造成WVTR下降,EX24與EX25均出現WVTR值高於CE8之特徵。
如上述準備背襯黏著劑之食品級障壁膜樣本之鈣測試障壁性能數據,且概述於表8與圖6及圖7。表8呈現背襯黏著劑之食品級障壁膜樣本CE10與EX26達到50%光耗損之時間。該等數據係於溫度60℃及相對濕度90%之環境腔室中使用鈣測試取得。圖6係表8所說明之樣本之光密度隨時間耗損之百分比圖。有空心正方形記號之粗線係在3M食品級障壁膜上之未填充之聚異丁烯黏著劑(CE10)。有內填星狀記號之線係在3M食品級障壁膜上之已填充之聚異丁烯黏著劑(EX26)。有實心正方形記號之線係在3M超障壁膜上之對照PIB障壁黏著劑。圖7呈現鈣上有表8所述之食品級障壁膜構造層壓之照片。(a)組係使用未填充之聚異丁烯黏著劑CE10所製成之樣本在時間零的照片;(b)組係使用已填充奈米黏土之聚異丁烯黏著劑EX26所製成之樣本在時間零的照片;(c)組係使用未填充之聚異丁烯黏著劑CE10所製成之樣本在9小時的照片;而(d)組係使用已填充奈米黏土之聚異丁烯黏著劑EX26所製成之樣本在9小時的照片。
改用10wt%填充黏土之黏著劑代替標準PIB黏著劑,並未改良層壓之食品級障壁膜之性能。圖6中代表樣本之光密度百分
比隨時間變化之曲線幾近疊合,且兩種樣本所測得達到50%光耗損之時間均為七小時。此外,圖7提供之鈣正方形陣列之照片均類似。所有此等數據均顯示,CE2與EX8之障壁性能沒有區別。此結論令人驚訝,因為根據JP2012193335與US20140377554之教示,添加微晶高嶺石黏土填料至層壓黏著劑時,將會改良該等具有寬廣障壁性能範圍之障壁膜構造之性能。
背襯黏著劑之超障壁膜之鈣測試障壁性能數據概述於表9及圖6及圖7。表9中所有樣本均包含填充奈米黏土之黏著劑施加至單層超障壁膜,如圖5所示。該等數據係於溫度60℃及相對濕度90%之環境腔室中使用鈣測試取得。圖8係表9所說明之樣本之光密度隨時間耗損之百分比圖。有空心正方形記號之線係在3M超障壁膜上之具有藉由高剪切混合分散之奈米黏土的聚異丁烯黏著劑(EX27)。有內填星狀之正方形記號之線係在3M超障壁膜上之具有藉由超音波分散之奈米黏土的聚異丁烯黏著劑(EX28)。有實心正方形記號之藍線係在3M超障壁膜上之對照障壁黏著劑(CE11加UV阻斷劑)。圖9呈現
鈣上有超障壁膜構造層壓之照片。(a)組係使用未填充之聚異丁烯黏著劑CE11加UV阻斷劑所製成之樣本在時間零的照片;(b)係使用已填充奈米黏土之聚異丁烯黏著劑EX28所製成之樣本在時間零的照片;(c)係使用未填充之聚異丁烯黏著劑CE11加UV阻斷劑所製成之樣本在360小時的照片;(d)係使用已填充奈米黏土之聚異丁烯黏著劑EX28所製成之樣本在360小時的照片;(e)係使用未填充之聚異丁烯黏著劑CE11加UV阻斷劑所製成之樣本在959小時的照片;及(f)係使用已填充奈米黏土之聚異丁烯黏著劑EX28所製成之樣本在959小時的照片。
當添加微晶高嶺石黏土至黏著劑配方中時,不同於黏著劑本身之WVTR測量及食品級層壓體之鈣測試數據,此等樣本顯示顯著改良障壁性能。每一個背襯25μm厚度已填充黏土之黏著劑之超障壁樣本達到50%光耗損之時間,皆比層壓25μm厚度未填充之對照黏著劑之類似超障壁樣本(CE11與CE12)更長。PIB樣本達到50%光耗損之時間的增加,從含2wt%奈米黏土填料之EX30之增加27%,至含10wt%奈米黏土填料之EX28之增加183%。
對照樣本(與CE11相同,惟黏著劑含有一些UV阻斷劑)、EX27、與EX28之光密度數據提供於圖8。從約150小時開始,EX27與EX28之兩條曲線明顯低於未填充之黏著劑對照樣本之曲線。此等較低曲線指示較長之鈣壽命與改良之障壁性能。EX28樣本中之黏土係使用超音波分散,而EX27中之黏土則使用高剪切混合機分散。EX28相較於EX27具有改良性能,表示超音波係製備填充黏土之障壁黏著劑之較佳方案。
未填充之對照樣本(CE11加UV阻斷劑)與EX28之鈣正方形陣列的照片提供於圖9。未填充之對照組之鈣正方形曝露在60℃/90% RH環境下959小時後,幾乎完全消失,其係水蒸氣穿透障壁構造並與鈣反應之結果。反之,EX28之鈣正方形即使曝露在60℃/90% RH環境下959小時後,仍保持大致完整。此等影像顯示,使用填充黏土之PIB黏著劑層壓至基材之超障壁膜,相較於使用標準PIB黏著劑層壓之超障壁膜,具有優異之障壁性能。此性能並未見於食品級氧化物障壁膜構造。
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。
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
Claims (25)
- 一種障壁黏著劑組成物,其包含樹脂系統及經有機改質之奈米黏土,該樹脂系統包含:(a)第一聚異丁烯樹脂,該第一聚異丁烯樹脂具有約300,000至約500,000g/mol之黏度平均分子量;(b)第二聚異丁烯樹脂,該第二聚異丁烯樹脂具有約700,000至約900,000g/mol之黏度平均分子;及(c)增黏劑。
- 如請求項1之障壁黏著劑組成物,其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.%之該第一聚異丁烯樹脂。
- 如請求項1或2之障壁黏著劑組成物,其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.%之該第二聚異丁烯樹脂。
- 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.%之該增黏劑。
- 如前述請求項中任一項之障壁黏著劑組成物,其包含相對於該樹脂系統及該奈米黏土之總重量約2至約15wt.%之該奈米黏土。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該增黏劑係氫化石油樹脂。
- 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。
- 如請求項7之障壁黏著劑組成物,其包含相對於該障壁黏著劑組成物之總重量約70至約90wt.%之溶劑。
- 如請求項7或8之障壁黏著劑組成物,其中該溶劑包含庚烷、甲苯、或其組合。
- 如請求項8之障壁黏著劑組成物,其中該溶劑包含庚烷。
- 如前述請求項中任一項之障壁黏著劑組成物,其中該奈米黏土係膨土(bentonite clay)或微晶高嶺石奈米黏土。
- 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,其具有約90%或更大之光學穿透性。
- 如前述請求項中任一項之障壁黏著劑組成物,其具有約3%或更小之霧度。
- 一種障壁黏著劑組成物,其包含樹脂系統、經有機改質之奈米黏土、及溶劑,該樹脂系統包含:(a)約15至約35wt.%之第一聚異丁烯樹脂,該第一聚異丁烯樹脂具有約300,000至約500,000g/mol之黏度平均分子量,(b)約40至約60wt.%之第二聚異丁烯樹脂,該第二聚異丁烯樹脂具有約700,000至約900,000g/mol之黏度平均分子,及(c)約15至約35wt.%之增黏劑,以上皆係相對於該樹脂系統之總重量計。
- 如請求項16之障壁黏著劑組成物,其包含相對於該樹脂系統及該奈米黏土之總重量約2至約15wt.%之該奈米黏土。
- 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18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/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。
- 如請求項19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19之黏著劑障壁膜,其中該超障壁膜係一箔(foil)。
- 如請求項18至21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22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18至23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上之一離型層。
- 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17中任一項之障壁黏著劑組成物。
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JP (1) | JP2018529803A (zh) |
KR (1) | KR102579723B1 (zh) |
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CN107925010B (zh) | 2015-08-17 | 2020-11-06 | 3M创新有限公司 | 阻挡膜构造 |
JP2019523804A (ja) * | 2016-06-16 | 2019-08-29 | スリーエム イノベイティブ プロパティズ カンパニー | ナノ粒子充填バリア接着剤組成物 |
CN110536945B (zh) | 2017-04-21 | 2022-04-29 | 3M创新有限公司 | 阻隔性粘合剂组合物和制品 |
US11591501B2 (en) | 2017-12-06 | 2023-02-28 | 3M Innovative Properties Company | Barrier adhesive compositions and articles |
CN109694518B (zh) * | 2018-12-27 | 2022-01-28 | 四川东方绝缘材料股份有限公司 | 一种双键聚合物量子点膜及其制备方法 |
CN111718683A (zh) * | 2019-03-21 | 2020-09-29 | 日胜化工股份有限公司 | 无溶剂聚氨酯接着剂及双涂布无溶剂聚氨酯接着剂 |
CN114316843A (zh) * | 2020-09-29 | 2022-04-12 | 上海飞凯材料科技股份有限公司 | 一种临时粘合剂及其应用和应用方法 |
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KR102579723B1 (ko) | 2023-09-15 |
CN107922805A (zh) | 2018-04-17 |
CN107922805B (zh) | 2020-09-15 |
US10738224B2 (en) | 2020-08-11 |
JP2018529803A (ja) | 2018-10-11 |
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WO2017031074A1 (en) | 2017-02-23 |
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