TW201702058A - 雙重固化奈米結構轉移膜 - Google Patents
雙重固化奈米結構轉移膜 Download PDFInfo
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- TW201702058A TW201702058A TW105110139A TW105110139A TW201702058A TW 201702058 A TW201702058 A TW 201702058A TW 105110139 A TW105110139 A TW 105110139A TW 105110139 A TW105110139 A TW 105110139A TW 201702058 A TW201702058 A TW 201702058A
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- Prior art keywords
- transfer film
- polyfunctional
- acrylate
- epoxy
- layer
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Abstract
一種轉移膜,其包括具有一第一主要表面及相對之一第二主要表面之一模板層。該第二主要表面包括一結構化非平坦離型表面。一回填層係設置在該非平坦結構化表面上且與該非平坦結構化表面等形。該回填層包括第一交聯聚合物與複數種多官能性單體,其等係經由不同且獨立之固化機制固化。
Description
玻璃基材上之奈米結構及微結構係用於例如顯示器、照明、建築、及光伏裝置等多樣應用中。在顯示器裝置中,該等結構可用於光萃取或光分布。在照明裝置中,該等結構可用於光萃取、光分布、及裝飾效果。在光伏裝置中,該等結構可用於太陽能集中及防止反射。在大型玻璃基材上圖案化或以其他方式形成奈米結構及微結構可係困難且不具成本效益的。
已揭示一種在一奈米結構化犧牲模板層內部使用一結構化回填層作為微影蝕刻遮罩之層壓轉移方法。該回填層可為類玻璃材料。然而,此等方法需要從回填層上移除犧牲模板層,同時使該回填層之結構化表面保持實質上完整。該犧牲模板層通常採用使用氧氣電漿之乾式蝕刻製程、熱分解製程、或溶解製程移除。
本揭露係有關一種雙重固化結構化轉移膜。該結構化轉移膜係部分固化以形成穩定之黏性膜。此黏性膜係層壓在受體基材上,且完全固化以給予該受體基材穩定之奈米結構及/或微結構。該結構化轉移膜係藉由將第一多官能性單體或第二多官能性單體中之一者
固化來形成。該結構化轉移膜係層壓至受體基材,然後將該另一種多官能性單體固化以形成交叉穿透網絡。該第一多官能性單體係以自由基或陽離子固化機制中之一者固化,而該第二多官能性單體係以自由基或陽離子固化機制中之一者固化,其係與該第一多官能性單體固化機制不同且獨立。
在一態樣中,轉移膜包括具有第一主要表面及相對之第二主要表面之模板層。該第二主要表面包括結構化非平坦離型表面。回填層係設置在該非平坦結構化表面上且與該非平坦結構化表面等形。該回填層包括交聯環氧聚合物、複數種多官能性丙烯酸酯單體、與具有丙烯酸酯官能基與環氧官能基之分子。
在另一態樣中,轉移膜包括具有第一主要表面及相對之第二主要表面之一模板層。該第二主要表面包括結構化非平坦離型表面。回填層係設置在非平坦結構化表面上且與非平坦結構化表面等形。該回填層包括交聯丙烯酸酯聚合物、複數種多官能性環氧單體、與具有丙烯酸酯官能基與環氧官能基之分子。
在另一態樣中,物品包括轉移膜,其如本文中所說明般設置在受體基材上。
在一進一步態樣中,物品包括:受體基材,其具有受體表面;及透光層,其具有黏附至該受體表面之第一主要表面及相對之第二主要表面,該第二主要表面具有結構化非平坦表面。該透光層包括交聯環氧聚合物與交聯丙烯酸酯聚合物之交叉穿透網絡與複數種相容劑分子,該等相容劑分子具有鍵結至該交聯丙烯酸酯聚合物之丙烯
酸酯基團及鍵結至該交聯環氧聚合物之環氧基團。該透光層具有小於2%之霧度值及大於85%之可見光穿透率及高於攝氏200度之分解溫度。
這些以及多種其他特徵與優點將因研讀下面的詳細說明而明顯可知。
101‧‧‧載體
103‧‧‧結構化非平坦模板層;結構化非平坦離型表面
104‧‧‧離型襯墊
105‧‧‧未固化回填組成物;回填層
110‧‧‧受體基材
112‧‧‧助黏層
200‧‧‧OLED裝置
201‧‧‧玻璃基材
202‧‧‧高折射率層
205‧‧‧回填層
210‧‧‧濾色器層
211‧‧‧平坦層
由於結合隨附圖式與以下本揭露之各個實施例的實施方式可更完整理解本揭露,其中:圖1係製造雙重固化轉移膠帶與結構化受體基材之製程的示意圖;及圖2係例示性OLED裝置的示意圖。
下文實施方式將參考構成本說明書之一部分的隨附圖式,而且在其中以圖解說明的方式呈現數個具體實施例。應瞭解,可設想出並做出其他實施例而不偏離本揭露的範疇或精神。因此,以下之詳細敘述並非作為限定之用。
除非另有指明,本文中所用所有科學以及技術詞彙具本發明所屬技術領域中所通用的意義。本文所提出的定義是要增進對於本文常用之某些詞彙的理解,並不是要限制本揭露的範疇。
除非另有所指,本說明書及申請專利範圍中用以表示特徵之尺寸、數量、以及物理特性的所有數字,皆應理解為在所有情況下以「約(about)」一詞修飾之。因此,除非另有相反指示,否則在前
面說明書以及隨附申請專利範圍中所提出的數值參數為近似值,其可依據所屬技術領域中具有通常知識者運用在本文中所揭示之教示而獲得的所要特性而變。
由端點表述的數值範圍包括在該範圍之內包含的所有數字(例如,1至5包括1、1.5、2、2.75、3、3.80、4、及5)以及該範圍內的任何範圍。
如本說明書以及隨附申請專利範圍中所使用,除非內文明確地另有所指,單數形「一(a/an)」以及「該(the)」涵蓋具有複數種指稱物(referents)的實施例。
如本說明書以及隨附申請專利範圍中所使用,「或(or)」一詞一般是用來包括「及/或(and/or)」的意思,除非內文明確另有所指。
如本文中所使用,「具有(have,having)」、「包括(include,including)」、「包含(comprise,comprising)」或諸如此類係以其開放式意義使用,且一般意指「包括但不限於(including,but not limited to)」。應理解,「基本上由...組成(consisting essentially of)」、「由...組成(consisting of)」、以及類似用語係歸於「包含(comprising)」以及類似用語中。
在本揭露中:「固化(curing)」係指將近接之單體或聚合物的官能基交聯;
「光化輻射(actinic radiation)」係指可固化聚合物之輻射波長,其可包括紫外光、可見光、及紅外光波長且可包括來自光柵化雷射、熱數位成像、及電子束掃描的數位曝光。
「AMOLED」係指主動式矩陣有機發光二極體;「LED」係指發光二極體;「微結構(microstructure)」係指其最長尺寸範圍在從約0.1μm至約1000μm之結構。在本揭露中,奈米結構與微結構之範圍必然會重疊;「奈米結構(nanostructure)」係指其最長尺寸範圍在從約1nm至約1000nm之特徵。
本揭露係關一種雙重固化結構化轉移膜。該結構化轉移膜係部分固化以形成一穩定之黏性膜。此黏性膜係層壓在一受體基材上,且完全固化以給予該受體基材穩定之奈米結構及/或微結構。該轉移膜利用塗佈在一結構化襯墊之形貌上的可雙重固化之樹脂配方。該樹脂之第一固化階段形成一穩定之黏性膜,該黏性膜呈該結構化襯墊之相反圖案,且具有可以一離型襯墊覆蓋以供運送與隨後之層壓的一平坦頂部表面。該黏性膜之該平坦表面可抵靠一受體基材層壓及固化,以使樹脂完全固化,並增強黏附至該受體基材,然後可移除該結構化襯墊以在該受體基材上留下一結構(奈米結構及/或微結構)。所得結構由於交叉穿透及交互反應之聚合物網絡,而係熱穩定(具有高於攝氏100度或高於攝氏200度或高於攝氏250度之熱分解溫度)且對溶劑具有優異抗性。該第一固化機制不同於且獨立於該第二固化機
制。在許多實施例中,該第一固化類型為陽離子固化機制而該第二固化機制為自由基固化機制。在其他實施例中,該第一固化機制為自由基固化機制而該第二固化機制為陽離子固化機制。一項實施例包括熱陽離子第一階段固化,然後為光化輻射(UV)自由基固化,以將該層壓結構完全固化至該基材。可雙重固化之樹脂配方包括環氧組分、丙烯酸酯組分、及包括環氧官能基與丙烯酸酯官能基之相容劑分子。該環氧組分可係多官能性分子,而該丙烯酸酯組分可係多官能性分子。轉移膜及基材上所得結構(透光層)具有小於2%或小於1%之霧度值及大於85%之可見光透射性。雖然未如此限制本揭露,但透過討論下文提供之實例,將獲得對本揭露之各種態樣之理解。
揭示結構化層壓轉移膜與結構化層壓轉移方法,以使用層壓製造結構化固體表面。該等方法涉及膜、層、或塗層之複製,以形成結構化模板層(亦稱為「結構化非平坦模板層(structured non-planar template layer)」)。該複製可使用對微複製技術具有通常知識者已知之任何微複製技術針對母版(master)進行。此等技術可包括例如:預聚合物樹脂之壓紋、澆注、與固化(使用熱或光化學起始法),或熱熔擠壓法。通常微複製法涉及對著一模板澆注光可固化預聚合物溶液,後續對該預聚合物溶液進行光聚合。在本揭露中,「奈米結構化(nanostructured)」係指具有之特徵小於1μm、小於750nm、小於500nm、小於250nm、100nm、小於50nm、小於10nm、或甚至小於5nm之結構。「微結構化(microstructured)」係指具有之特徵小於1000μm、小於100μm、小於50μm、或甚至小於5μm之結構。階
層(hierarchical)係指具有超過一種大小規格之結構,包括帶有奈米結構之微結構(例如:具有奈米規格蛾眼抗反射特徵之微透鏡)。層壓轉移膜已揭示於例如:申請者之待審公告申請案US 2014/0021492中,標題為「STRUCTURED LAMINATION TRANSFER FILMS AND METHODS」。
圖1係製造雙重固化轉移膠帶與結構化受體基材之製程的示意圖。結構化非平坦模板層103係形成或設置於載體101上,如上所述。結構化非平坦模板層103包括一離型表面,在許多實施例中,該離型表面係一種採用例如電漿增強化學氣相沉積法沉積之離型薄塗層(未顯示)。在一些實施例中,釋離性質可係該結構化模板層所固有。
隨後以未固化回填組成物105塗佈所得結構。未固化回填組成物105緊密接觸結構化非平坦模板層103。該回填組成物包括多官能性環氧單體、多官能性丙烯酸酯單體、及具有丙烯酸酯官能基與環氧官能基之相容分子。在許多實施例中,該回填組成物係至少95% wt之單體與相容分子或至少98% wt之單體與相容分子或實質上係單體與相容分子。
多官能性環氧單體、多官能性丙烯酸酯單體具有不同且獨立之固化機制。因此,未固化回填組成物可包括陽離子起始劑與自由基起始劑。在一項實例中,多官能性環氧單體具有陽離子固化機制,而多官能性丙烯酸酯單體具有獨立之自由基固化機制。
在一實施例中,多官能性丙烯酸酯單體具有光自由基(經由UV光與游離基光起始劑)固化機制,而多官能性環氧單體具有陽離子熱(經由加熱與熱酸發生劑)固化機制。在另一實施例中,多官能性丙烯酸酯單體具有熱自由基(經由加熱與熱酸發生劑)固化機制,而多官能性環氧單體具有光-陽離子(經由UV光與游離基光起始劑)固化機制。
有三個階段與形成最終膜物品相關聯。階段A(或A-階段)係定義為開始配方,其中沒有或幾乎沒有發生固化。階段B(或B-階段)係定義為其中該兩組可固化基團中的第一者係經固化且固化程度足以產生具有可在所需表面處作用為壓敏性黏著劑之一膜之狀態(部分固化)。階段C(或C-階段)係定義為其中該兩組可固化基團中的第二者係經固化且固化程度已可讓該膜維持模板圖案並從模板釋離之狀態(完全固化)。
在例示性實施例中,該轉移膜係藉由將多官能性環氧單體固化來形成,以形成其中分散有多官能性丙烯酸酯單體之交聯環氧聚合物。此部分固化(或b-階段)膜具有之彈性模數值小於0.3×105Pa,其可為多種不同表面提供長時間穩定之類壓敏性黏著劑之黏性。此外,此部分固化(或b-階段)膜對結構化非平坦模板層103具有良好之完全潤溼(wet-out)與黏著性。
部分固化(或b-階段)膜應具有的模數值不超過達爾奎斯特標準(Dahlquist Criterion)(當於室溫下,在約1Hz之頻率下測量時為0.3×105Pa或3×106達因/cm2),其可為多種不同表面提供長時間
穩定之類壓敏性黏著劑之黏性。此係黏性之標準,且係以探討此現象之科學家命名為「達爾奎斯特黏性標準(Dahlquist Criterion for tack)」(參見Dahlquist,C.A.述於Adhesion Fundamentals and Practice,The Ministry of Technology(1966)McLaren and Sons,Ltd.,London)。超過此模數,經觀察會在分離時出現小的拉張變形而發生黏著失敗。
在其他例示性實施例中,該轉移膜係藉由將多官能性丙烯酸酯單體固化來形成,以形成其中分散有多官能性環氧單體之交聯丙烯酸酯聚合物。此部分固化(或b-階段)膜在60℃之加工溫度下具有接近上述達爾奎斯特標準之彈性模數,其可為多種不同表面提供長時間穩定之類壓敏性黏著劑之黏性。此外,b-階段膜具有為室溫或低於室溫的玻璃轉變溫度,有助於膜「完全潤溼」至受體基材上。此外,此部分固化(或b-階段)膜對結構化非平坦模板層103具有一些黏著性。
在許多實施例中,該部分固化(或b-階段)膜具有小於2%或小於1%之霧度值、及大於85%或大於90%之可見光透射性。在許多實施例中,該部分固化(或b-階段)膜具有小於攝氏30度或小於攝氏25度或小於攝氏20度之玻璃轉變溫度。
一旦形成穩定的部分固化(或b-階段)膜,即可施加一可選的離型襯墊104至該穩定的部分固化(或b-階段)膜上,以在運送及隨後的加工期間用於保護。離型襯墊104可設置在回填層105之一平坦主要表面上,其中回填層105將離型襯墊104與結構化非平坦
離型表面103分隔。將該可選之離型襯墊104從該穩定的部分固化(或b-階段)膜分離,之後再將該轉移膜層壓至受體基材110上。
可選地可將受體基材110塗佈助黏層112,以幫助該穩定的部分固化(或b-階段)膜黏附並產生完全固化之結構化透光層。助黏層112可以任何適用之方式形成,諸如旋塗法、浸塗法、噴塗法、電漿聚合法或經由其他沉積製程。
將該穩定的部分固化(或b-階段)膜層壓在受體基材110上。將此層壓膜固化,以將其餘多官能性單體交聯,並形成交叉穿透之交聯聚合物網絡,界定一完全固化結構化層。隨後可將該完全固化結構化層從結構化非平坦模板層103釋離。
圖2係例示性OLED裝置200濾色器層210的示意圖。可將回填層205(部分或完全固化)設置於濾色器層210上或耦合至濾色器層210。一或多層諸如平坦層211可將濾色器層210耦合至回填層205(部分或完全固化)。可將玻璃基材201耦合至濾色器層210之相對側。可在回填層205(部分或完全固化)之結構化表面上設置高折射率層202(例如:R.I.大於1.6)。未繪示OLED之功能層,但咸了解,此等層可相鄰於所繪示之描述性OLED裝置200層之任一側。
完全固化結構化層具有小於2%或小於1%之霧度值、及大於85%或大於90%之可見光透射性、及高於攝氏150度或高於攝氏200度或高於攝氏250度之玻璃轉變溫度。完全固化結構化層可稱為「結構化透光層(structured light transmission layer)」且在攝氏100
度或更高溫度下穩定、或在攝氏150度或更高溫度下穩定、或在攝氏200度或更高溫度下穩定、或在攝氏250度或更高溫度下穩定達至少10分鐘。完全固化結構化層可係對溶劑穩定的且阻抗IPA、MEK、甲苯、庚烷、甲氧基丙醇、及其他溶劑。完全固化結構化層可係機械上穩定的,例如能夠在水及/或IPA中承受音波10min。該完全固化之結構化層可具有約1.5±0.1之可見光折射率。
在一些實施例中,先將環氧單體固化形成轉移膜後,再將丙烯酸酯單體固化形成交叉穿透該交聯環氧聚合物之交聯丙烯酸酯聚合物,界定一完全固化結構化層。在一些此等實施例中,該交聯環氧聚合物係經由陽離子機制固化(b-階段),而該多官能性丙烯酸酯單體係經由自由基機制固化(c-階段)。
在一些實施例中,先將丙烯酸酯單體固化形成轉移膜後,再將環氧單體固化形成交叉穿透該交聯丙烯酸酯聚合物之交聯環氧聚合物,界定一完全固化結構化層。在其他實施例中,該交聯丙烯酸酯聚合物係經由自由基機制固化(b-階段),而該多官能性環氧單體係經由陽離子機制固化(c-階段)。
在許多實施例中,該完全固化結構化層中存在具有鍵結至該交聯丙烯酸酯聚合物之丙烯酸酯基團及鍵結至該交聯環氧聚合物之環氧基團的複數種相容劑分子。
「聚官能性丙烯酸酯(polyfunctional acrylate)」或「多官能性丙烯酸酯(multifunctional acrylate)」組分可為脂族聚羥基化合物與(甲基)丙烯酸之反應產物。
(甲基)丙烯酸為不飽和羧酸,其等包括例如彼等由下列基本化學式代表者:
其中R為氫原子或甲基。
聚官能性(亦即多官能性)丙烯酸酯可為單體或寡聚物。用語「單體(monomer)」係指有能力與相同或其他單體依形成長鏈(聚合鏈或巨分子)之方式形成化學鍵之小(低分子量)分子。用語「寡聚物(oligomer)」係指有能力從其等與相同或其他寡聚物依形成更長聚合鏈之方式形成化學鍵之具有2至10個重複單位之聚合物分子(例如:二聚物、三聚物、四聚物等等)。單體與寡聚物之混合物亦可作為聚官能性丙烯酸酯組分使用。較佳者係該聚官能性丙烯酸酯組分為單體。
代表性聚官能性丙烯酸酯單體包括但不限於例如:乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、己二醇二丙烯酸酯、三乙二醇二丙烯酸酯、三羥甲丙烷三丙烯酸酯、乙氧基化三羥甲丙烷三丙烯酸酯、甘油三丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇三甲基丙烯酸酯、季戊四醇四丙烯酸酯、季戊四醇四甲基丙烯酸酯、及新戊基二
醇二丙烯酸酯。亦可使用不同類型之聚官能性丙烯酸酯之混合物或組合。本文中所使用之用語「丙烯酸酯(acrylate)」包括丙烯酸酯與甲基丙烯酸酯。
適用之市售聚官能性丙烯酸酯包括商標名稱為「SR351」之三羥甲丙烷三丙烯酸酯、商標名稱為「SR454」之乙氧基化三羥甲丙烷三丙烯酸酯、商標名稱為「SR295」之季戊四醇四丙烯酸酯、商標名稱為「SR833S」之環己烷二羥甲基二丙烯酸酯、及商標名稱為「SR247」之新戊基二醇二丙烯酸酯,且所有此等商品均可購自Sartomer Co.,Exton,Pa。
聚官能性丙烯酸酯單體可迅速固化成網絡,因為每個單體上均有可用之多重官能基。若僅有一個丙烯酸酯官能基,會在材料固化時產生線性無網絡之分子。在本發明中,以具有二個或更多個官能基之聚官能性丙烯酸酯較佳,可促進及加速形成所欲之聚合網絡。
回填層或透光層可具有任何適用量之聚官能性丙烯酸酯。在許多實施例中,回填層或透光層具有40至90% wt之聚官能性丙烯酸酯。在一些實施例中,回填層或透光層具有60至80% wt之聚官能性丙烯酸酯。
適用之環氧樹脂包括具有至少一個環氧乙烷環(亦即
可利用開環反應聚合)之任何有機化合物。此等材料泛稱為環氧化物,包括單體與寡聚合環氧化物二者,且可為脂族、環脂族、或芳香族。其等可為液體或固體或其掺合物。此等材料通常每個分子平均具有至少兩個環氧基團(較佳為每個分子具有超過兩個環氧基團)。聚合性環氧化物包括具有末端環氧基團之線性聚合物(例如:聚氧烷二醇之二縮水甘油醚)、具有環氧乙烷單元架構之聚合物(例如:聚丁二烯聚環氧化物)、及具有側接環氧基團之聚合物(例如:甲基丙烯酸環氧丙酯聚合物或共聚物)。
適用之環氧樹脂包括彼等包含環己烯氧化物基團者,如:環氧環己烷羧酸酯,以3,4-環氧環己基甲基-3,4-環氧環己烷羧酸酯、3,4-環氧-2-甲基環己基甲基-3,4-環氧-2-甲基環己烷羧酸酯、與雙(3,4-環氧-6-甲基環己基甲基)己二酸酯為代表。此性質之適用環氧化物之更詳細列表可參見美國專利第3,117,099號,其以引用方式併入本文中。
其他特別適用之環氧樹脂包括如下式之縮水甘油醚單體:
其中R’為烷基或芳基,且n為2至6之整數。實例為由多元酚與過量氯醇(如:環氧氯丙烷)反應得到之多元酚之縮水甘油醚,例如:2,2-雙-2,3-環氧丙氧丙氧酚丙烷之二縮水甘油醚。可用於操作本發明之此類環氧化物之其他實例說明於美國專利第3,018,262號,其以引用方式併入本文中。
可自市售商品取得許多種適用之環氧樹脂。特定言之,容易取得之環氧化物包括八伸癸基氧化物、表氯醇、苯乙烯氧化物、乙烯基環己烯氧化物、縮水甘油、縮水甘油基-甲基丙烯酸酯、雙酚A之二縮水甘油醚(例如:彼等以下列商標名稱取得者:「EPON 828」、「EPON 1004」、與「EPON 1001F」(得自Shell Chemical Co.)、與「DER-332」與「DER-334」(得自Dow Chemical Co.))、雙酚F之二縮水甘油醚(例如:「ARALDITE GY281」(來自Ciba-Geigy))、乙烯基環己烯二氧化物(例如:具有商標名稱「ERL 4206」(來自Union Carbide Corp.))、3,4-環氧環己基-甲基-3,4-環氧環己烯羧酸酯(例如:具有商標名稱「ERL-4221」(來自Union Carbide Corp.))、2-(3,4-環氧環-己基-5,5-螺-3,4-環氧)環己烷-偏二烷(例如:具有商標名稱「ERL4234」(來自Union Carbide Corp.))、己二酸雙(3,4-環氧-環己基)酯(例如:具有商標名稱「ERL-4299」(來自Union Carbide Corp.))、二戊烯二氧化物(例如:具有商標名稱「ERL4269」(來自Union Carbide Corp.))、環氧化聚丁二烯(例如:具有商標名稱「OXIRON 2001(來自FMC Corp.))、含環氧官能基之聚矽氧樹脂、環氧矽烷(例如:β-3,4-環氧環己基乙基三-甲氧基矽烷與γ-縮水
甘油基氧丙基三甲氧基矽烷,可自Union Carbide取得商品)、阻燃劑環氧樹脂(例如:具有商標名稱「DER-542」、溴化雙酚型環氧樹脂(來自Dow Chemical Co.)、1,4-丁二醇二縮水甘油基醚(例如:具有商標名稱「ARALDITE RD-2」(來自Ciba-Geigy))、基於氫化雙酚A-表氯醇之環氧樹脂(例如:具有商標名稱「EPONEX 1510」(來自Shell Chemical Co.))、及苯酚-甲醛清漆之聚縮水甘油基醚(例如:具有商標名稱「DEN-431」與「DEN-438」(來自Dow Chemical Co.))。
在一些實施例中,脲類係選自雙取代脲類。在一些實施例中,咪唑類係選自:1-N經取代-咪唑類、2-C經取代-咪唑類、及金屬咪唑酸鹽類,如說明於美國專利4,948,449中者,其具有高於200℃之熔點。合適之固化劑為可自市售商品取得,可以商標名稱CUREZOL 2PHZ-S、CUREZOL 2MZ-AZINE、及CUREZOL 2MA-OK得自Air Products and Chemicals;以商標名稱ARADUR 3123得自Huntsman Advanced Materials;及以商標名稱OMICURE U-35及OMICURE U-52得自CVC Thermoset Specialties。為達到快速固化,通常同時需要起始劑與活化劑。當調配兩部分系統時,其中一部分將包含起始劑,而另一部分將包含活化劑。
可使用之活化劑係由三級胺、胺/醛(或酮)縮合物、氫硫基化合物、或過渡金屬化合物組成。適用之三級胺的實例為:N,N-二甲基苯胺、N,N-二乙基苯胺、N,N-二甲基-對-甲苯胺、N,N-二乙基-對-甲苯胺、或N,N-二異丙基-對-甲苯胺。氫硫基化合物之實例
為:2-氫硫基苯并咪唑、烯丙硫脲、與伸乙基硫脲。適用之胺/醛縮合物的實例為:苯胺/丁醛、丁胺/苯甲醛、及丁胺/二苯乙二酮。過渡金屬化合物之實例為:環烷酸銅、環烷酸鐵;環烷酸鈷、環烷酸鎳、環烷酸錳;辛酸銅;己酸鐵、丙酸鐵;氧化銅、氧化錳、氧化釩、二氧化鉬;與氧化釩(乙醯丙酮酸鹽)2、及氧化鉬(乙醯丙酮酸鹽)2。
回填層或透光層可具有任何適用量之聚官能性環氧樹脂。在許多實施例中,回填層或透光層具有0.1至25% wt之聚官能性環氧樹脂。在一些實施例中,回填層或透光層具有10至20% wt之聚官能性環氧樹脂。
可使用一些分子使存在於轉移膜中之兩個不同相可以相容。此等分子一般具有至少一個由該兩相中之各官能基代表之官能基團。代表性分子可例如具有一個末端環氧基團及一個末端丙烯酸酯基團。此等分子之實例包括部分丙烯酸化雙酚A二縮水甘油醚(亦稱為「CN-153」Sartomer Corp,Exton,PA)、丙烯酸2-羥基丁基環氧丙基酯(「4-HBAGE」Nippon Kasei Chemical,Tokyo,Japan)、(甲基)丙烯酸環氧丙基酯、甲基丙烯酸3,4-環氧環己基甲基酯(市售名稱為「CYCLOMER M100」(Daicel Corp,Osaka,Japan))。除了具有兩個在化學上相似於轉移膜中之相的基團外,相容劑分子中之一個官能基團亦可能可以與轉移膜中之相之一者產生化學反應。舉例而言,已知具有一級羥基官能基之分子會與環氧化物官能基產生化學反應。因
此,可使用具有末端羥基官能基及末端丙烯酸酯官能基之分子。此等分子之實例包括季戊四醇四丙烯酸酯(「SR444」Sartomer,Exton,PA)。
其他寡聚物包括丙烯酸化環氧化物,諸如環氧樹脂之二丙烯酸化酯,例如:雙酚A環氧樹脂之二丙烯酸化酯。可自市售商品取得之丙烯酸化環氧化物的實例包括可以商標名稱「CMD 3500」、「CMD 3600」、及「CMD 3700」得自Radcure Specialties之環氧化物。
其他同時具有環氧基與丙烯酸酯官能基之適用化合物說明於例如美國專利第4,751,138號(Tumey等人)中,其以引用方式併入本文中。
回填層或透光層可具有任何適用量之相容劑分子。在許多實施例中,回填層或透光層具有5至40% wt之相容劑分子。在一些實施例中,回填層或透光層具有10至35% wt之相容劑分子。在其他實施例中,回填層或透光層具有15至25% wt之相容劑分子。
另一種量化回填層或透光層中之相容劑分子的方式為將環氧材料與相容劑材料相關連、或以相容劑材料置換環氧材料。相容劑分子可為環氧材料之1至100%莫耳當量。相容劑分子可依1:1莫耳比置換環氧材料。
回填層或透光層可具有任何適用量之聚官能性丙烯酸酯、聚官能性環氧樹脂、及相容劑分子。在許多實施例中,回填層或
透光層具有40至90% wt之聚官能性丙烯酸酯、1至30% wt之聚官能性環氧樹脂、及5至40% wt之相容劑分子。
該第一多官能性單體係以自由基或陽離子固化機制中之一者固化,而該第二多官能性單體係以自由基或陽離子固化機制中之一者固化,其係與該第一多官能性單體固化機制不同且獨立。自由基固化機制可係熱或光-游離基固化機制。陽離子固化機制可係熱或光-陽離子固化機制。
以自由基可固化聚官能性丙烯酸酯組分為例,將自由基起始劑添加至回填材料中係適用的,但應了解,亦可使用電子束源起始並產生自由基。基於樹脂組分之總量計,自由基起始劑較佳添加量為0.1至3.0%重量比。當曝露至紫外光時可產生自由基來源之適用光起始劑的實例包括但不限於:有機過氧化物、偶氮化合物、苯醌、二苯基甲酮、亞硝基化合物、醯基鹵化物、腙類、氫硫基化合物、吡喃鹽(pyrylium)化合物、三醯基咪唑類、醯基膦氧化物、雙咪唑類、氯烷基三嗪類、苯偶姻醚類、二苯乙二酮縮酮、硫雜蒽酮(thioxanthones)、與乙醯苯衍生物,及其混合物。當曝露至可見光照射時可產生自由基之來源之光起始劑的實例說明於美國專利第4,735,632號中,其以引用方式併入本文中。用於以紫外光產生自由基之較佳起始劑為可自Lamberti Corporation(Gallarate-VA-Italy)購得之起始劑,商標名稱為「ESACURE ONE」。
促進環氧樹脂聚合之固化劑可經熱或光活化;亦即,該固化劑可為受到光化輻射(具有電磁光譜中紫外光或可見光部分之波長之輻射)或加熱而活化之觸媒。適用之陽離子觸媒會產生催化環氧樹脂聚合之酸。應了解,用語「酸(acid)」可包括質子酸或路易氏酸(Lewis acid)。此等陽離子起始劑可包括具有鎓陽離子與金屬或擬金屬之含鹵素之錯合陰離子的茂金屬鹽。其他適用之陽離子觸媒包括具有有機金屬錯合陽離子與金屬或擬金屬之含鹵素之錯合陰離子的茂金屬鹽,其進一步說明於美國專利第4,751,138號(例如:第6欄第65行至第9欄第45行),其以引用方式併入本文中。另一種實例為有機金屬鹽與鎓鹽,其說明於美國專利第4,985,340號(第4欄第65行至第14欄第50行);歐洲專利申請案306,161;306,162,其等均以引用方式併入本文中。又另其他陽離子觸媒包括有機金屬錯合物之離子性鹽,其中該金屬係選自週期表第IVB、VB、VIB、VIIB及VIIIB族之元素,其說明於歐洲專利申請案109,581,其亦以引用方式併入本文中。另一種可產生適用於固化之熱活化酸之鎓鹽的實例已知為「CXC-1612」,其係一種來自King Industries(Norwalk,CT)之六氟銻酸銨鹽。
此概念下可使用其他可能之正交固化規程。舉例而言,一般可利用鉑化合物催化SiH與不飽和碳-碳(烯、炔)之間之氫矽化反應。另一種實例為一般利用鉑化合物催化SiH與SiOH之間之醇解反應。另一種適用之實例為SiX經SiOH之親核性取代,其中X為鹵素、肟、羧酸酯、烷氧化物,其經常利用一族列酸或鹼、錫與鈦化合
物進行催化。亦可使用自由基(例如:過氧化物、UV或電子束)來起始SiCH3與SiCH3之間之反應。所有此等均說明於Michael Brook,Silicon in Organic,Organometallic and Polymer Chemistry,Wiley Interscience,2000,pg 282-291中。
可利用潛伏性固化系統使環氧部分交聯,只要符合b-階段與c-階段膜之光學與物理性質即可。適用於本揭露之潛伏性固化系統包括彼等習用於固化環氧樹脂組成物並形成交聯聚合物網絡者,包括醯肼類,諸如胺基二醯肼、己二酸二醯肼、異酞基二醯肼;胍類,諸如四甲基胍;及二氰基二醯胺。
其用量將隨不同樹脂而變化,且通常提供之量可以在所欲時間長度內有效達成實質上完全固化。基於一份可固化之環氧組成物的總重量計,根據本揭露之典型組成物包括約1至10重量%之潛伏性硬化劑。將了解,固化組成物之最終性質將大幅受到分別由潛伏性硬化劑造成之交聯與環氧鏈伸長之相對量之影響。
在一些實施例中,潛伏性固化系統具有二或更多種潛伏性加速劑,該二或更多種潛伏性加速劑選自經取代之脲類、經取代之咪唑類、及其組合中之至少一者。在一些實施例中,可與樹脂混溶之第一固化劑之組分可預先掺合,然後加至熱可固化環氧樹脂中。在一些實施例中,該等可與樹脂混溶之第一固化劑之組分可分開加至該熱可固化環氧樹脂中。
本文中所揭示之轉移膜(或「層壓轉移膜」)可用於多種不同目的。舉例而言,該等轉移膜可用於轉移OLED(有機發光二極體)裝置中之結構化層,以改善OLED之效率或光提取。
該等層壓轉移膜之另一種例示性應用為用於圖案化在顯示器玻璃、光伏玻璃元件、LED晶圓、矽晶圓、藍寶石晶圓、建築玻璃、金屬、非織物、紙、或其他基材之內表面或外表面上之數位光學元件,包括菲涅爾微透鏡片(microfresnel lens)、繞射光學元件、全像術光學元件、及在Kress、與P.Meyrueis之Applied Digital Optics,Wiley,2009,B.C.第2章中所揭示之其他數位光學元件。
該等層壓轉移膜亦可用於玻璃表面上產生裝飾效果。舉例而言,在裝飾性晶體小面之表面上賦予虹彩可能係所欲的。特定言之,該等玻璃結構可用於功能性或裝飾性應用中,諸如交通工具用玻璃、建築用玻璃、玻璃餐具、藝術品、顯示器信號、與珠寶或其他附件。可使用本文中所揭示之方法轉移所埋置之結構來改善玻璃結構之耐用性。此外,可在此等玻璃結構上施加塗層。此可選之塗層可係相對薄的,以避免負面影響玻璃結構之性質。此等塗層之實例包括親水性塗層、疏水性塗層、保護性塗層、抗反射塗層、及類似者。
襯墊或載體基材或膜可以一撓性膜實施,為轉移膜及其他層提供機械性支撐。載體膜的一項實例為聚苯二甲酸乙二酯(PET)。
在一些實施例中,載體可包括紙、離型塗佈紙、非織物、織物(織品)、金屬膜、及金屬箔。
包含多種熱固性或熱塑性聚合物的多種聚合膜基材適合作為載體使用。載體可為單一層或多層膜。可作為載體層膜的聚合物之說明性實例包括(1)氟化聚合物,例如聚(三氟氯乙烯)、聚(四氟乙烯-共六氟丙烯)、聚(四氟乙烯-共-全氟(烷基)乙烯基醚)、聚(偏二氟乙烯-共六氟丙烯);(2)具有鈉或鋅離子之離子性乙烯共聚物聚(乙烯-共-甲基丙烯酸),例如SURLYN-8920以及SURLYN-9910,可從美國德拉瓦州威明頓的E.I.duPont Nemours公司購得;(3)低密度聚乙烯如低密度聚乙烯、線性低密度聚乙烯、與非常低密度聚乙烯、增塑性乙烯基鹵化物聚合物如增塑性聚(氯乙烯);(4)聚乙烯共聚物,包括酸官能性聚合物,例如聚(乙烯-共-丙烯酸)「EAA」、聚(乙烯-共-甲基丙烯酸)「EMA」、聚(乙烯-共-順丁烯二酸)以及聚(乙烯-共-反丁烯二酸);丙烯酸官能性聚合物,例如聚(乙烯-共-烷基丙烯酸酯)其中烷基為甲基、乙基、丙基、丁基等等、或CH3(CH2)n-其中n為0至12,以及聚(乙烯-共-醋酸乙烯酯)「EVA」;以及(5)(例如)脂族聚胺基甲酸酯。載體層一般係烯烴聚合材料,一般包含至少50wt-%之具有2至8個碳原子的烯烴,以乙烯及丙烯最常被採用。其他本體層(body layers)包括例如聚(萘二甲酸乙二酯)、聚碳酸酯、聚(甲基)丙烯酸酯(例如聚甲基丙烯酸甲酯或「PMMA」)、聚烯(例如聚丙烯或「PP」)、聚酯(例如,聚對苯二甲酸乙二酯或「PET」)、聚醯胺、聚醯亞胺、酚樹脂、
二醋酸纖維素、三醋酸纖維素(TAC)、聚苯乙烯、苯乙烯-丙烯腈共聚物、環狀烯烴共聚物、環氧化物(epoxies)以及類似物。
受體基材的實例包括諸如顯示器母體玻璃、發光母體玻璃、建築玻璃、板玻璃、卷玻璃、及撓性玻璃(可使用於卷對卷製程)的玻璃。撓性卷玻璃的實例為來自Corning Incorporated的WILLOW玻璃產品。受體基材之其他實例包括金屬,諸如金屬片與箔。受體基材之其他實例包括藍寶石、矽、二氧化矽、及碳化矽。另一其他實例包括織物、非織物、及紙。
其他例示性受體基材包括擔體晶圓(support wafer)上之半導體材料。這些受體基材的尺寸可超過半導體晶圓主模板的尺寸。目前所製造之最大晶圓具有300mm之直徑。使用在本文中揭示的方法製成的層壓轉移膜,其橫向尺寸可大於1000mm且卷長度可為數百公尺。在一些實施例中,該受體基材可有約620mm乘以約750mm、約680mm乘以約880mm、約1100mm乘以約1300mm、約1300mm乘以約1500mm、約1500mm乘以約1850mm、約1950mm乘以約2250mm、或約2200mm乘以約2500mm或甚至更大的尺寸。長卷長度之橫向尺寸可大於約750mm、大於約880mm、大於約1300mm、大於約1500mm、大於約1850mm、大於約2250mm、或甚至大於約2500mm。典型尺寸具有約1400mm的最大圖案化寬度,及約300mm的最小寬度。該等大尺寸可能藉由使用卷對卷加工
與圓柱型主模板的組合而得。具有這些尺寸的膜可用來對整個大型數位顯示器(例如:對角55吋的顯示器,尺寸為寬52吋、高31.4吋)賦予奈米結構。
受體基材可選擇性地在將施加層壓轉移膜的該受體基材的該側包括一緩衝層。緩衝層之實例揭示於美國專利第6,396,079號(Hayashi等人)中,該案以引用方式併入本文中,如同完整陳述般。緩衝層的一個類型是SiO2薄層,如K.Kondoh等人於J.of Non-Crystalline Solids 178(1994)189-98及T-K.Kim等人於Mat.Res.Soc.Symp.Proc.Vol.448(1997)419-23中所揭示者。
本發明所揭示之轉移製程的一特別優點為賦予結構給具有大表面之受體表面如顯示器素玻璃或建築玻璃的能力。該等受體基材的尺寸超出半導體晶圓主模板的尺寸。層壓轉移膜的大尺寸可能藉由使用卷對卷加工與圓柱型主模板的組合而得。
本發明所揭示之轉移製程的另一優點為賦予結構給不平坦受體表面的能力。由於轉移膠帶的撓性形態,受體基材可為彎曲、折彎扭曲或具有凹或凸的特徵。
受體基材亦可包括汽車玻璃、薄片玻璃、撓性電子基材如電路化撓性膜、顯示器背板、太陽能玻璃、金屬、聚合物、聚合物複合件以及纖維玻璃。
模板層係對回填層賦予結構之層。其係由模板材料製成。模板層可經由例如壓紋、複製製程、擠壓、澆注、或表面結構化形成。結構化表面可包括奈米結構、微結構、或階層式結構。在一些實施例中,模板層可與圖案化、光化圖案化、壓紋、擠壓、及共擠壓相容。
模板層可包括光可固化材料,其在複製製程期間具有低黏度,接著可被快速固化以形成一「鎖在(locking in)」該複製奈米結構、微結構或階層式結構內的永久交聯聚合網絡。在光聚合作用領域中具有通常知識者已知之任何光可固化樹脂都可被用來作為模板層。用於模板層的樹脂在使用所揭示之結構化膠帶期間必須能夠在交聯時自回填層離型;或應能相容於離型層的應用(請見下方)與施加離型層的製程。此外,用於模板層的樹脂必須能與如上文所討論之助黏層的應用相容。
可用來作為模板層的聚合物亦包括下列:苯乙烯丙烯腈共聚物;苯乙烯(甲基)丙烯酸酯共聚物;聚甲基丙烯酸甲酯;聚碳酸酯;苯乙烯順丁烯二酐共聚物;有核半結晶聚酯;聚萘二甲酸乙二酯之共聚物;聚醯亞胺;聚醯亞胺共聚物;聚醚醯亞胺;聚苯乙烯;間規聚苯乙烯;聚伸苯醚;環狀烯烴聚合物;以及丙烯腈、丁二烯和苯乙烯的共聚物。一種較佳的聚合物係Lustran SAN Sparkle材料,可從Ineos ABS(USA)Corporation購得。用於輻射固化模板層的聚合物包括經交聯的丙烯酸酯諸如多官能性丙烯酸酯或環氧化物以及摻合單官能性和多官能性單體的丙烯酸化胺基甲酸酯。
圖案化結構化模板層可藉由下列形成:沉積一層輻射可固化組成物至輻射透射載體之一個表面上,以提供具有暴露表面的一層,使該層與具有預成形表面的一母版(master)接觸,該預成形表面帶有一圖案,該圖案能賦予一經精確成形及定位的交互式功能性不連續性之三維微結構(包括遠端表面部分及臨近下壓表面部分)至該載體上的輻射可固化組成物層的暴露表面,該接觸在充足的接觸壓力下以將該圖案賦予至該層,當輻射可固化組成物層與母版的圖案化表面相接觸時,經由載體(carrier)暴露該可固化組成物至充足輻射量以固化該組成物。此澆注與固化製程以連續方式進行,其使用一卷載體、沉積一層可固化材料至該載體上、對著主體工具層壓該可固化材料、並使用光化輻射對著該工具固化該可固化材料。接著可捲起所得之有圖案化、結構化模板設置於其上之載體之卷。此方法揭示於例如US 6,858,253號(Williams等人)中。
對於擠壓或壓紋模板層,可根據要賦予的頂部結構化表面之特定形貌,來選擇組成模板層的材料。一般而言,材料係經選擇以使結構在材料固化前完全被複製。這將部分取決於在擠壓製程中材料所保持的溫度及用來賦予頂部結構化表面的工具溫度,以及進行擠壓的速度。一般而言,用於頂層之可擠壓的聚合物具有小於約140℃的Tg,或介於約85℃到約120℃之間的Tg,以便能在大多數操作條件下被擠壓複製並壓紋。在一些實施例中,載體膜和模板層可同時共擠壓。此實施例需要至少兩層的共擠壓,即一聚合物頂層和另一聚合物底層。若頂層包含第一可擠壓聚合物,則第一可擠壓聚合物可具有小
於約140℃之Tg或自約85℃至約120℃之Tg。若頂層包含第二可擠壓聚合物,則可作用為載體層之第二可擠壓聚合物具有小於約140℃之Tg或約85℃至約120℃之Tg。其他性質(如分子量及熔融黏度)亦應考慮並且取決於所使用之特定聚合物或多個聚合物。亦應選擇用在模板層的材料,以提供與載體間之良好黏著性,使得在該轉移膜的生命週期內,兩層間的分層(delamination)降至最低。
該擠壓或共擠壓之模板層可經澆鑄至一母版卷(工具)上,該母版卷可賦予該模板層圖案化結構。可以批次方式或以持續性卷對卷製程進行。此外,回填層可擠壓到經擠壓或共擠壓之模板層上。在一些實施例中,所有三層即載體、模板、及回填層可經一次共擠壓,只要回填層可在加工後與模板層分開即可。
可用作模板層聚合物的有用聚合物,包括一或多種選自由下列所組成之群組的聚合物:苯乙烯丙烯腈共聚物;苯乙烯(甲基)丙烯酸共聚物;聚甲基丙烯酸甲酯;苯乙烯順丁烯二酐共聚物;有核半結晶聚酯;聚萘二甲酸乙二酯之共聚物;聚醯亞胺;聚醯亞胺共聚物;聚醚醯亞胺;聚苯乙烯;間規聚苯乙烯;聚伸苯醚;以及丙烯腈、丁二烯和苯乙烯的共聚物。能作為第一擠壓式聚合物之特別有用的聚合物包括稱為TYRIL共聚物的苯乙烯丙烯腈共聚物,能從Dow Chemical公司購得;樣品包括TYRIL 880以及125。其他可作為模板層聚合物之特別有用的聚合物包括苯乙烯順丁烯二酸酐共聚物DYLARK 332與苯乙烯丙烯酸酯共聚物NAS 30,二者皆可從Nova
Chemical購得。與成核劑混合的聚對苯二甲酸乙二酯亦適用,成核劑諸如矽酸鎂、乙酸鈉或亞甲雙(2,4-二-三級丁基酚)酸磷酸鈉。
模板層可係犧牲的手段,意即其將在稍後從構造中移除,如揭示在申請者於2012年7月20日申請之待審公開案第2014/0021492號、標題為「STRUCTURED LAMINATION TRANSFER FILMS AND METHODS」中之模板層。然而,製造所揭示之轉移膠帶及其所製成物品之方法並不需要犧牲該模板層。
模板層係自回填層移除。減少回填層與模板層之黏著性的一種方法為施加離型塗層至該膜。施加離型塗層至模板層表面的一方法為電漿沉積法。寡聚物可被用來產生電漿交聯離塗層。該寡聚物在塗佈前可為液體形式或固體形式。一般而言,該寡聚物具有大於1000的分子量。而且寡聚物的分子量通常小於10,000,使得該寡聚物不會太具揮發性。分子量大於10,000的寡聚物通常過於不揮發,導致塗佈過程形成液滴。在一實施例中,寡聚物的分子量大於3000且小於7000。在另一實施例中,寡聚物的分子量大於3500且小於5500。通常寡聚物具有提供低磨擦表面塗佈之特性。合適的寡聚物包括含聚矽氧的烴類、含三烷氧基矽烷的反應性聚矽氧、芳香烴、脂肪烴、氟化物以及其組合。例如,合適的樹脂包括但不限於二甲基矽酮、烴基底聚醚、氟化物聚醚、乙烯四氟乙烯和氟矽酮。氟矽烷表面化學、真空沉積及表面氟化亦可用來提供離型塗層。
電漿聚合薄膜組成一與習用聚合物不同之材料類別。在電漿聚合物中,聚合係隨機的,交聯程度非常高,且所產生的聚合物膜與對應之「習用」聚合物膜非常不同。因此,電漿聚合物被所屬技術領域中具有通常知識者視為一獨特不同類別的材料,且可用於所揭示的物品中。
此外,有其他方法可將離型塗層施加至模板層上,包括但不限於起霜(blooming)、塗佈、共擠壓、噴霧塗佈、電塗或浸塗。
助黏層可用任何能強化轉移層對受體基材黏性但不會實質上不利影響轉移膜之性能的材料實現。回填層之例示性材料亦可用於助黏層。適用於所揭示物品與方法中的助黏材料包括光阻劑(正向及負向)、自組裝單層、矽烷耦合劑、及巨分子。在一些實施例中,矽倍半氧烷可作用為助黏層。其他例示性材料可包括苯并環丁烷、聚醯亞胺、聚醯胺、聚矽氧、聚矽氧烷、聚矽氧混合聚合物、(甲基)丙烯酸酯、與其他經各式反應基官能化的矽烷或巨分子,諸如環氧化物、環硫化物、乙烯基、羥基、烯丙氧基、(甲基)丙烯酸酯、異氰酸酯、氰酯、乙醯氧基、(甲基)丙烯醯胺、硫醇、矽烷醇、羧酸、胺基、乙烯醚、酚、醛、烷基鹵化物、桂皮酸酯、疊氮化物、氮丙啶、烯烴、胺甲酸酯、醯亞胺、醯胺、炔烴、及該等基團的任何衍生物或組合。此外,已發現可以商標名稱「SILQUEST A174」購自Momentive,Inc(Waterford,NY)之專賣矽烷表面改質劑尤其適用。
回填層可選擇性地以暫時的離型襯墊覆蓋。離型襯墊可於操作時保護該圖形化結構化回填,且當需要時可被輕易移除,以便將結構化回填或部分結構化回填轉移至受體基材。適用於所揭示轉移膜的例示性襯墊係揭示於PCT專利申請公開案第WO 2012/082536號(Baran等人)中。
襯墊可以係撓性的或剛性的。其係撓性較佳。一合適的襯墊(可撓性襯墊較佳)通常至少為0.5密耳厚,且通常不超過20密耳厚。該襯墊可為在其第一表面上設置有一離型塗層的背襯。離型塗層可以可選地設置在其第二表面。若此背襯係用於呈卷形式的轉移物品,則第二離型塗層具有較第一離型塗層為低的離型值(release value)。適合作用為剛性襯墊的材料包括金屬、金屬合金、金屬基質複合物、金屬化塑膠、無機玻璃及玻璃化有機樹脂、成形陶瓷及聚合物基質強化複合物。
例示性襯墊材料包括紙及聚合材料。例如,撓性背襯包括經密緻化的牛皮紙(例如可從Loparex North America,Willowbrook,IL購得者)、聚合物塗佈紙,例如聚乙烯塗佈牛皮紙及聚合膜。合適的聚合膜包括聚酯、聚碳酸酯、聚丙烯、聚乙烯、纖維素、聚醯胺、聚醯亞胺、聚矽氧烷、聚四氟乙烯、聚對苯二甲酸乙二酯、聚氯乙烯、聚碳酸酯或其組合。亦可使用非織造或織造襯墊。非織造或織造襯墊的實施例可結合離型塗層。CLEARSIL T50離型襯墊(塗佈聚矽
氧的2密耳聚酯膜襯墊,可從美國維吉尼亞州馬丁斯維爾的Solutia/CP Films公司購得)及LOPAREX 5100離型襯墊(塗佈氟矽酮的2密耳聚酯膜襯墊,可從美國威斯康辛州哈蒙德的Loparex公司購得)皆為實用的離型襯墊實例。
襯墊的離型塗層可為含氟材料、含矽材料、氟聚合物、矽氧聚合物、或從包含具有12至30個碳原子之烷基的(甲基)丙烯酸烷基酯之單體所衍生的聚(甲基)丙烯酸酯。在一個實施例中,烷基可係支鏈。有用的氟聚合物及聚矽氧聚合物的說明性實例可見於美國專利第4,472,480號(Olson)、第4,567,073號及第4,614,667號(二者皆為Larson等人)。有用的聚(甲基)丙烯酸酯的說明性實例可見於美國專利申請公開案第2005/118352號(Suwa)。移除襯墊不應造成該回填層表面位相(surface topology)的不利改變。
用於轉移膜之樹脂可包含可選之添加劑,以改善或維持多種不同條件下之性能。此等可包括光起始劑、聚合抑制劑、受阻胺光穩定劑、敏化劑、抗氧化劑、觸媒、分散劑、均化劑、及類似者。
用於轉移膜之樹脂可包含無機填料材料,以增強機械、熱、黏著性、或光學之性能。舉例而言,可使用氧化矽奈米粒子來增強樹脂之硬度而不犧牲透光性。可使用金屬氧化物奈米粒子來修飾塗
層之折射率而不犧牲樹脂層之透光性。此等之實例包括由氧化鋯、氧化鈦、氧化鉿、及類似者製成之奈米粒子。該等奈米粒子可以適當配體來官能化,以增強其與用於轉移膜中之樹脂之相容性。此等之實例可包括有機醇類、羧酸類、有機矽烷類、及類似者。
本揭露之目的及優點係藉由以下之實例來進一步說明,但不應過度解讀這些實例中詳述的特定材料及其用量、以及其他條件而限制本揭露。
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。所使用的溶劑及其他試劑係得自Sigma-Aldrich Chemical Company,St.Louis,Missouri,除非另有說明。
使用丙酮與異丙醇完全清洗玻璃片,並使用無塵室擦拭布擦乾。將玻璃片曝露在YES G1000系統之氧氣電漿(O2=60sccm,時間=3分鐘,RF=300W)中,移除任何殘留之烴汙染並暴露出表面矽烷醇基團。將玻璃片在>100C烘箱中維持脫水,直到可以使用時為止,然後置入已含3滴3-甲基丙烯醯氧丙基三甲氧矽烷(「SILQUEST A-174」)之乾燥器中,然後置入80度C之烘箱中達4小時。從乾燥器中取出後,觀察到水接觸角之變化,此表示有單層矽烷沉積。使用丙酮與異丙醇洗除未與玻璃片共價鍵結之任何矽烷。實例#1不需要在玻璃片上沉積SILQUEST A-174助黏劑。
基礎膜係2-mil PET,以包含UVACURE 1500與TMPTA之50/50掺合物及1% OMAN 071光起始劑的UV固化底層前處理。複製之樹脂為SR 399與SR238之75/25掺合物與含有1% Darocur 1173、1.9%三乙醇胺、0.5% OMAN 071、及0.3%亞甲藍之光起始劑包裝。樹脂之複製係於20fpm下,以137度F之工具溫度進行。來自以600W/in操作的Fusion「D」燈的輻射穿透該膜以在樹脂與工具接觸時固化該樹脂。從工具上移除複合膜,該膜的圖案化側係在與加熱至華氏100度的冷卻卷接觸時,使用以360W/in操作的Fusion「D」燈經後UV固化。該微結構包含具有多種間距(400、500、及600nm)之光繞射圖案。
將複製之模板膜以流速250標準cc/min(SCCM)的氬氣、25毫托的壓力、及1000瓦特的RF功率前處理達30秒。隨後,將樣本暴露於四甲基矽烷(TMS)電漿,TMS流速為150SCCM,但不添加氧;此對應於氧對矽大約為0之原子比。腔室中的壓力為25毫托,且使用1000瓦特的RF功率達10秒。
將上表2所示之樹脂配方添加至聚丙烯杯中,於Speed Mixer混合機(Flacktek,Landrum,SC)中以2500rpm混合30秒,直到均質為止。使用具有5mil間隙之凹口棒,將該等配方塗佈在上述之微結構化離型襯墊上。將該等膜在烘箱中以120℃乾燥4分鐘,直到膜形成黏性凝膠為止。切出膜區塊,使用手動壓輥層壓至玻璃片,於60℃對流加熱烘箱中預焙烤30分鐘,建立黏著性後,使用Fusion H燈泡以強度300W/in依30呎/分鐘進行UV固化2次。將玻璃/膜工具堆疊置回120℃烘箱中,進行後製熱焙烤,以完成固化製程,然後移除微結構化離型工具,在基材上留下微結構化工具膜之反轉圖案。
使用霧度計(BYK Gardiner,商標名稱「BYK Hazegard Plus,Columbia,MD」),基於ASTM D1003-11測量透射性、霧度、及清晰度之平均%。
剝離奈米結構化之工具膜後,黏附在基材上之完全固化奈米結構形成肉眼可見之光繞射圖案。將玻璃片置於氮氣下之加熱板上,設定100℃達15分鐘。取得玻璃片在測試之前與之後之圖像,逐一比較各片之光繞射圖案。若奈米結構經過所有此等測試後所觀察到之光繞射沒有出現變化,則視該樹脂配方為「通過」。若樣本通過,則對同一個樣本接著進行相同程序,但進行加熱至高達230℃。
剝離黏附力為在特定角度與移除速率下,從測試板上移除已塗佈之撓性材料時所需之力。先使用異丙醇清潔玻璃,再施加膜。將樣本切成1”寬之長條。層壓後及測試前,將樣本於室溫23℃及相對濕度50%下平衡15分鐘。使用IMASS 2100滑動/剝離測試機(Slip/Peel Tester,IMASS,Inc.,Accord,MA),在12in/min之拉伸速度(crosshead speed)下背向剝離180度時,測量剝離黏附力。所報告之剝離黏附力係三次重覆之平均值,以每吋之盎司值表示。
使用凹口棒,以5mil之乾厚度將樹脂配方塗佈在離型襯墊上,然後如上述於120℃下固化。然後多層手動塗層係經層壓在彼等自身之上,以達到30mil之乾厚度。將TA Instruments(New
Castle,DE)Discovery Hybrid Rheometer從-65至170℃以1rad/sec操作,黏著劑係在直徑8mm之平行板之間。
所有實例與比較例均於Fusion UV處理器(Hereus,Gaithersburg,MD)中,使用H-燈泡與1J/cm2之曝光劑量,利用紫外線固化至C-階段。
測量玻璃轉變溫度時,將固化膜切成寬5mm,夾在TA Instruments Q800 Dynamic Mechanical Analyzer分析儀(DMA)中。該實驗係以拉伸模式於0℃至250℃之溫度範圍內,於5微米之拉張變形幅度、1Hz之頻率、及2℃/min之加熱速率下進行。玻璃轉變溫度係以黏彈性比值曲線(tan delta curve)之峰值來界定。
將數片完全固化樹脂(各約2mg)置入Q500 Thermogravimetric Analyzer分析儀(來自TA Instruments(New Castle,DE))內之空鋁盤中。選擇之加熱速率為10℃/min,直到550℃。分解溫度係以樹脂分解至其原始重量之95%時之溫度來界定。
使用線性熱塑性聚合物結合多官能性丙烯酸酯膠黏劑,製備比較例1及比較例2。將此等比較例與使用交聯環氧化物結合多官能性丙烯酸酯膠黏劑及助黏劑之實例1及實例2比較。進行測試,以檢測膜之B-階段之黏附性質及膜之C-階段之高溫性能。
使用上述測試方法#2中說明之熱穩定性測試進行初步篩選。在比較例1中,於100℃下達15分鐘後,觀察到來自微結構之光繞射已消失。此樹脂將被排除於以後之加工與分析之外。比較例#2通過100℃熱穩定性焙烤測試,但未通過230℃熱穩定性測試。實例1與實例2通過兩種測試並進一步評估。
由通過100℃微結構熱穩定性測試之完全固化樹脂樣本進行透射性與霧度量測、玻璃轉變溫度、及熱分解溫度分析。結果顯示於表4。所有樹脂配方均顯示高透射性及低霧度。此等樹脂配方之間之主要差異在於其熱分解溫度。使用熱塑性組分之CE1在215℃時開始分解,而由該微結構所造成之光繞射在230℃時完全消失。E1與E2二者均具有高於300℃之分解溫度。高的分解溫度結合高於150℃之玻璃轉變溫度,結果為增強了高溫結構性能。CE2顯示兩個玻璃轉變溫度,一個在2度C而第二個在168度C,因此CE2具有至少一個小於攝氏150度之玻璃轉變溫度。
表5顯示B-階段膜之剝離黏附力、玻璃轉變溫度、及平行板流變儀測試結果。結果顯示E1與E2相較於CE2,具有較高之儲存模數及亦較高之玻璃轉變溫度值(高於150度C)。E1與E2亦具有低於CE2之剝離黏附力值。然而,已驚人地發現E1與E2可以具有組合性質,即在部分固化時可以在受體基材上潤溼之黏附性質、及在基材上完全固化及從工具膜模型中取出時可以維持高溫結構性能。
因此,揭示雙重固化奈米結構轉移膜之實施例。
在此特以引用之方式將本文所引述之所有參考文件以及出版品之全文明示納入本揭露中,除非其內容可能與本揭露直接抵觸。雖在本文中是以具體實施例進行說明及描述,但所屬技術領域中具有通常知識者將瞭解可以各種替代及/或均等實施來替換所示及所描述的具體實施例,而不偏離本揭露的範疇。本申請案意欲涵括本文所
討論之特定具體實施例的任何調適形式或變化形式。因此,本揭露意圖僅受限於申請專利範圍及其均等者。本文所揭示之實施例僅為說明性目的而非限制性。
101‧‧‧載體
103‧‧‧結構化非平坦模板層;結構化非平坦離型表面
104‧‧‧離型襯墊
105‧‧‧未固化回填組成物;回填層
110‧‧‧受體基材
112‧‧‧助黏層
Claims (26)
- 一種轉移膜,其包含:模板層,其具有第一主要表面及相對之第二主要表面,該第二主要表面包含結構化非平坦離型表面;回填層,其設置在該非平坦結構化表面上且與該非平坦結構化表面等形,該回填層包含:交聯環氧聚合物;及複數種多官能性丙烯酸酯單體。
- 如請求項1之轉移膜,其中該交聯環氧聚合物與該等多官能性丙烯酸酯單體具有不同且獨立之固化機制,且該回填層包含陽離子起始劑與自由基起始劑。
- 如請求項1之轉移膜,其中該回填層包含具有丙烯酸酯官能基與環氧官能基之分子。
- 如請求項1之轉移膜,其中該轉移膜具有小於攝氏25度之玻璃轉變溫度值。
- 如請求項1之轉移膜,其中該交聯環氧聚合物包含環脂族多官能性環氧基團。
- 如請求項1之轉移膜,其中該等多官能性丙烯酸酯單體包含環脂族多官能性丙烯酸酯基團。
- 如請求項1之轉移膜,其中該交聯環氧聚合物具有可經由陽離子機制固化之環氧部分,且該等多官能性丙烯酸酯單體可經由自由基機制固化。
- 如請求項1之轉移膜,其進一步包含設置在該回填層之平坦主要表面上之離型襯墊,其中該回填層係介於該離型襯墊與該結構化非平坦離型表面之間。
- 一種轉移膜,其包含:模板層,其具有第一主要表面及相對之第二主要表面,該第二主要表面包含結構化非平坦離型表面;回填層,其設置在該非平坦結構化表面上且與該非平坦結構化表面等形,該回填層包含:交聯丙烯酸酯聚合物;複數種多官能性環氧化物單體。
- 如請求項9之轉移膜,其中該交聯丙烯酸酯聚合物與該等多官能性環氧化物單體具有不同且獨立之固化機制,且該回填層包含陽離子起始劑與自由基起始劑。
- 如請求項9之轉移膜,其中該回填層包含具有丙烯酸酯官能基與環氧官能基之分子。
- 如請求項9之轉移膜,其中該轉移膜具有小於攝氏25度之玻璃轉變溫度值。
- 如請求項9之轉移膜,其中該交聯丙烯酸酯聚合物包含多官能性環脂族丙烯酸酯基團。
- 如請求項9之轉移膜,其中該等多官能性環氧單體包含多官能性環脂族環氧基團。
- 如請求項9之轉移膜,其中該交聯丙烯酸酯聚合物具有可經由自由基機制固化之丙烯酸酯部分,且該等多官能性環氧單體可經由陽離子機制固化。
- 如請求項9之轉移膜,其進一步包含設置在該回填層之平坦主要表面上之離型襯墊,其中該回填層係介於該離型襯墊與該結構化非平坦離型表面之間。
- 一種物品,其包含:如請求項1之轉移膜,其設置在受體基材上。
- 如請求項17之物品,其中該受體基材包含玻璃或藍寶石。
- 如請求項17之物品,其中該受體基材包含有機發光二極體濾色器元件。
- 一種物品,其包含:如請求項9之轉移膜,其設置在受體基材上。
- 如請求項20之物品,其中該受體基材包含玻璃或藍寶石。
- 如請求項20之物品,其中該受體基材包含有機發光二極體濾色器元件。
- 一種物品,其包含:受體基材,其具有受體表面;透光層,其具有黏附至該受體表面之第一主要表面與相對之第二主要表面,該第二主要表面具有結構化非平坦表面,該透光層包含:交聯環氧聚合物與交聯丙烯酸酯聚合物之交叉穿透網絡;及複數種相容劑分子,其等具有鍵結至該交聯丙烯酸酯聚合物之丙烯酸酯基團及鍵結至該交聯環氧聚合物之環氧基團;該透光層具有小於2%之霧度值及大於85%之可見光穿透率及高於攝氏250度之分解溫度。
- 如請求項23之物品,其中該交聯環氧聚合物包含多官能性環脂族環氧基團。
- 如請求項23之物品,其中該交聯丙烯酸酯聚合物包含多官能性環脂族丙烯酸酯基團。
- 如請求項23之物品,其中該受體基材包含有機發光二極體濾色器元件。
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EP (1) | EP3277495B1 (zh) |
JP (1) | JP2018512307A (zh) |
KR (1) | KR101882643B1 (zh) |
CN (1) | CN107454871B (zh) |
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- 2016-03-25 EP EP16717733.6A patent/EP3277495B1/en active Active
- 2016-03-25 CN CN201680018989.6A patent/CN107454871B/zh active Active
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US20160288450A1 (en) | 2016-10-06 |
WO2016160560A1 (en) | 2016-10-06 |
EP3277495A1 (en) | 2018-02-07 |
KR101882643B1 (ko) | 2018-07-26 |
CN107454871B (zh) | 2020-09-11 |
KR20170125998A (ko) | 2017-11-15 |
EP3277495B1 (en) | 2021-01-27 |
JP2018512307A (ja) | 2018-05-17 |
CN107454871A (zh) | 2017-12-08 |
US10106643B2 (en) | 2018-10-23 |
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