TW202022059A - 用於製造可撓性顯示器之疊層結構以及使用其製造可撓性顯示器的方法 - Google Patents
用於製造可撓性顯示器之疊層結構以及使用其製造可撓性顯示器的方法 Download PDFInfo
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- TW202022059A TW202022059A TW108132801A TW108132801A TW202022059A TW 202022059 A TW202022059 A TW 202022059A TW 108132801 A TW108132801 A TW 108132801A TW 108132801 A TW108132801 A TW 108132801A TW 202022059 A TW202022059 A TW 202022059A
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Abstract
根據本發明,藉由使用在350℃以上的溫度下熱膨脹係數(CTE)為負數的聚醯亞胺膜作為用於分離可撓性基板與載體基板的剝離層,可利用由用以於可撓性基板上形成元件的高溫製程後可撓性基板與剝離層的殘留應力差異引起的分離(detach)現象,而容易地將可撓性基板自載體基板分離。藉此可不對形成於可撓性基板上的元件造成化學損傷或物理損傷並分離可撓性基板,從而可將進行剝離製程時可能產生的問題最小化。
Description
本發明是有關於一種包括可將可撓性基板自載體基板容易地分離的剝離層的疊層結構以及使用其製造可撓性顯示器的方法。
本發明主張基於2018年9月11日申請的韓國專利申請10-2018-0108219號的優先權的利益,且相應韓國專利申請的文獻所揭示的所有內容均作為本說明書的一部分而包含在內。
顯示裝置市場以容易大面積化、可薄型化及輕量化的平板顯示器(Flat Panel Display,FPD)為主正在迅速變化。於此種平板顯示器中,存在液晶顯示裝置(液晶顯示器(Liquid Crystal Display,LCD)),有機發光顯示裝置(有機發光顯示器(Organic Light Emitting Display,OLED))或電泳元件等。
特別是,最近為了進一步擴大此種平板顯示器的應用與用途,關於將可撓性基板應用於所述平板顯示器的所謂可撓性顯示器元件等備受關注。此種可撓性顯示器元件主要以智慧型電話等行動(mobile)機器為中心進行應用研究,並考慮逐漸擴大其應用領域。
但是,形成及處理塑膠基板上薄膜電晶體(TFTs on Plastic:TOP)等顯示器元件結構的製程在可撓性顯示器元件製造中是重要的核心製程。但是,由於包括此種可撓性顯示器元件的基板的可撓性,因此於直接將可撓性塑膠基板代替應用於現有的用於玻璃基板的元件製造製程來形成元件結構的過程中,至今仍存在許多製程上的問題。
特別是,由於可撓性基板內所包含的薄膜玻璃的情況因衝擊而容易破碎,因此以支撐玻璃(載體玻璃(carrier glass))上裝有薄膜玻璃的狀態實施用於顯示器的基板的製造製程。先前,於玻璃基板等載體基板上形成包含非晶矽等的犧牲層後,在其上形成可撓性基板。此後,於藉由載體基板支撐的可撓性基板上,藉由現有的用於玻璃基板的元件製造製程形成薄膜電晶體等元件結構。在此之後,藉由對載體基板等照射雷射或光,破壞所述犧牲層並分離形成有所述元件結構的可撓性基板,最終製造具有可撓性顯示器元件等的可撓性基板。
但是,於利用此種先前技術的製造方法中,於照射所述雷射或光的過程中,不僅存在元件結構受到影響而產生不良等擔憂,而且需要進行用於照射所述雷射或光的設備及單獨的製程,從而存在整體的元件製造製程變複雜且製造成本亦大幅升高的缺點。
進而,因包含非晶矽(a-Si)等的犧牲層與可撓性基板間的接著力不充分而於所述犧牲層與可撓性基板之間需要形成單獨的接著層等的情況多,該情形不僅使整體製程更加複雜,而且需要於更加苛刻的條件下進行雷射或光照射,從而會對元件的可靠性帶來不良影響的擔憂進一步增加。
[發明所欲解決之課題]
本發明欲解決的課題是提供一種用於製造具有與可撓性基板分離容易的剝離層的可撓性顯示器之疊層結構。
本發明的另一課題是欲提供一種使用所述疊層結構製造可撓性顯示器的方法。
[解決課題之手段]
本發明為了解決所述的課題,提供一種用於製造可撓性顯示器之疊層結構,包括:
載體基板;
剝離層,塗覆於所述載體基板上,且包含於350℃以上的溫度下熱膨脹係數(Coefficient of Thermal Expansion,CTE)具有負數值的聚醯亞胺;以及
可撓性基板層,形成於所述剝離層上。
根據一實施例,
所述剝離層具有第一面積,
所述可撓性基板層可具有大於所述第一面積的第二面積,且完全覆蓋所述剝離層。
根據一實施例,所述剝離層所包含的聚醯亞胺可包含含有聯苯四羧酸二酐(biphenyl-tetracarboxylic acid dianhydride,BPDA)的二酐與含有苯二胺(phenylene diamine,PDA)的二胺的聚合及硬化產物作為聚合成分。
另外,所述二酐可更包含均苯四甲酸二酐(pyromellitic dianhydride,PMDA),所述二胺可更包含2,3'-雙(三氟甲基)聯苯胺(2,3'-bis(trifluoromethyl)benzidine,TFMB)。
根據一實施例,所述酸二酐與二胺的組合可選自BPDA-PDA、BPDA-PMDA-PDA及BPDA-PDA-TFMB。
根據一實施例,所述剝離層所包含的聚醯亞胺可使二胺與二酐於與二酐相比、二胺以當量比計過量的條件下聚合及硬化製造而成。
根據一實施例,所述二酐與二胺的組合為BPDA-PDA-TFMB,且TFMB於整體二胺中可為5莫耳%以上。
根據一實施例,所述二酐與二胺的組合為BPDA-PMDA-PDA,且PMDA於整體二酐中可為5莫耳%以上。
根據一實施例,所述剝離層所包含的聚醯亞胺的熱分解溫度可為560℃以上。
根據一實施例,所述剝離層的厚度可為50 nm以上1 μm以下。
根據一實施例,所述可撓性基板層可包含於350℃以上的溫度下CTE具有正數值的聚醯亞胺。
本發明亦提供一種製造可撓性顯示器的方法,包含如下步驟:
於載體基板上形成包含於350℃以上CTE為負數的聚醯亞胺的剝離層的步驟;
於所述剝離層上形成可撓性基板層的步驟;
於所述可撓性基板層上形成元件的步驟;以及
將形成有所述元件的基板自所述剝離層剝離的步驟。
根據一實施例,所述剝離層以具有第一面積的方式形成於載體基板上,所述可撓性基板層以具有比所述第一面積大的第二面積且完全覆蓋所述剝離層的方式形成,所述元件可於所述剝離層與所述可撓性基板重疊的區域中形成於所述可撓性基板層上。
根據一實施例,剝離所述可撓性基板層的步驟可為在所述剝離層與所述可撓性基板重疊的區域的內側邊緣沿與所述載體基板垂直的方向切斷,從而將所述剝離層與所述可撓性基板層分離。
於一實施例中,於進行剝離製程時,將可撓性基板層自剝離層剝離的剝離強度可為0.05 N/cm以下。
於一實施例中,於自形成有所述剝離層的載體基板對所述聚醯亞胺基板層進行剝離製程時,可不經過在所述剝離層與可撓性基板層之間引起化學變化或物理變化的製程。
[發明的效果]
根據本發明的用於製造可撓性顯示器的疊層結構,藉由將在350℃以上的溫度下CTE(熱膨脹係數)為負數的聚醯亞胺用於用以分離可撓性基板與載體基板的剝離層,可利用經過用以於可撓性基板上形成元件的高溫製程並因可撓性基板與剝離層的殘留應力差異而產生分離(Detach)現象,而容易地將可撓性基板自載體基板分離。藉此可不對形成於可撓性基板上的元件造成化學損傷或物理損傷並分離可撓性基板,從而可將進行剝離製程時可能產生的問題最小化。
本發明可施加各種變化且可具有多種實施例,欲根據例示於附圖及詳細說明而詳細地對特定實施例進行說明。但是,應理解的是並非欲將本發明限定於特定的實施形態,本發明包括包含於本發明的思想及技術範圍的所有變換、均等物及代替物。於本發明的說明書中,於判斷出對相關習知技術的具體說明會使本發明的要旨變得含糊不清的情況時,省略對所述相關習知技術的詳細的說明。
於本說明書中,所有的化合物或官能基若未特別提及,則可為取代的或未經取代的化合物或官能基。此處,「取代的」意指包含於化合物或官能基的至少一個氫被選自由如下組成的群組中的取代基代替:鹵素原子、碳數為1至10的烷基、鹵化烷基、碳數為3至30的環烷基、碳數為6至30的芳基、羥基、碳個數為1至10的烷氧基、羧基、醛基、環氧基、氰基、硝基、胺基、磺酸基及其等的衍生物。
可撓性顯示器可因具有自由的形態且輕且薄、不破碎的特性而市場需求正在增加。於實現此種可撓性顯示器的過程中,主要使用包含耐熱性優異的BPDA-PDA的聚醯亞胺作為可撓性基板。
於形成此種可撓性顯示器的製程中,主要使用如下方法:於作為支撐基板的玻璃基板上形成如聚醯亞胺的高分子原材料的可撓性基板,在其上形成元件後,照射雷射(laser)將所述玻璃基板與可撓性基板之間分離。
但是,此種雷射分離(laser detach)技術的情況,於設備投資費用增加及雷射透過至塑膠基板的情況會對薄膜電晶體(Thin Film Transistor,TFT)元件帶來損傷而會產生產率下降。
本發明為了解決此種先前的問題,
提供一種用於製造可撓性顯示器之疊層結構,包括:
載體基板;
形成於所述載體基板上的、且包含於350℃以上的溫度下CTE具有負數值的聚醯亞胺的剝離層;以及
形成於所述剝離層上的可撓性基板層。
本發明亦提供一種製造可撓性顯示器的方法,包含如下步驟:
於載體基板上形成包含於350℃以上CTE為負數的聚醯亞胺的剝離層的步驟;
於所述剝離層上形成可撓性基板層的步驟;
於所述可撓性基板層上形成元件的步驟;以及
將所述可撓性基板層自形成有所述剝離層的載體基板剝離的步驟。
於用作可撓性基板的聚醯亞胺膜於高溫下的CTE為負數的情況下,即若觀察到於高溫下收縮的跡象,則會於高溫的熱處理製程等中產生問題。根據本發明,藉由將此種表現出高溫下的收縮跡象的聚醯亞胺用作剝離層而並非可撓性基板,經過如元件形成製程的高溫製程並藉由收縮使可撓性基板與剝離層自然地剝離,從而無需進行如雷射製程的單獨的處理亦可容易地使可撓性基板自載體基板分離。
圖1a表示示出根據於350℃以上CTE具有正數值的聚醯亞胺膜的溫度的尺寸變化(dimension change)與殘留應力(stress)變化的曲線圖。
如圖1a所示,於將於350℃以上CTE為正數的聚醯亞胺用作剝離層的情況,於升溫過程中,應力減小(①),於350℃以上時表現出應力減小或保持的傾向(②③),之後於降溫過程中,表現出應力再次增加的狀況(④),此種應力變化狀況與通常的可撓性基板的根據溫度變化的翹曲變化狀況相同。因此,於將於350℃以上CTE為正數的聚醯亞胺用作剝離層的情況下,如圖1b所示根據應力變化的翹曲變化狀況,可撓性基板與剝離層相同,而可撓性基板與剝離層之間不產生分離。
相反,圖2a表示根據於350℃以上CTE具有負數值的聚醯亞胺膜的溫度的尺寸變化(dimension change)與殘留應力(stress)變化的曲線圖。如圖2a及圖2b所示,於將於350℃以上CTE為負數的聚醯亞胺剝離層的情況,於350℃以下的溫度中,應力減小(①)並表現出與可撓性基板相同的翹曲變化,但之後於350℃以上的溫度中,應力增加(②)而沿與可撓性基板相反方向產生翹曲,於此種過程中,可於可撓性基板與剝離層之間產生分離。之後,於降溫過程中,應力再次減小(③),但依然為保持分離的狀態,其因升溫時應力曲線與降溫時應力曲線的差異大而可得知。因此,即便於350℃以下時應力增加(④)而再次沿與可撓性基板相同的方向產生翹曲,所產生的分離亦依然存在,從而可使與可撓性基板的接著力下降。藉由此種方式產生的分離可於之後的製程中進一步變大或保持,使與可撓性基板的接著力下降,從而可使剝離變得容易。
於本發明中,所述CTE(熱膨脹係數)使用熱機械分析儀(Thermomechanical Analyzer)來測定,例如,是於100℃至460℃溫度範圍內以4 ℃/min的升溫速度進行第一次升溫製程後,之後於460℃至100℃的溫度範圍內以5 ℃/min的冷卻速度進行冷卻(cooling)後,使經冷卻的樣品於100℃至460℃下進行4 ℃/min的升溫的同時測定的值。於350℃以上的溫度範圍的CTE值具有負數意指於所述350℃以上的溫度範圍內,表示根據溫度變化的試樣的長度變化(尺寸變化(Dimension change,μm))的曲線的斜率表示為負數。
所述剝離層所使用的聚醯亞胺可包含含有聯苯四羧酸二酐(BPDA)的二酐與含有苯二胺(PDA)的二胺的聚合及硬化產物。
另外,所述二酐可更包含均苯四甲酸二酐(PMDA),所述二胺可更包含2,3'-雙(三氟甲基)聯苯胺(TFMB)。
根據一實施例,所述酸二酐與二胺的組合可選自BPDA-PDA、BPDA-PMDA-PDA及BPDA-PDA-TFMB。
此處簡稱意指如下。
BPDA:聯苯四羧酸二酐(biphenyl-tetracarboxylic acid dianhydride)
PDA:苯二胺(phenylene diamine)
PMDA:均苯四甲酸二酐(pyromellitic dianhydride)
TFMB:2,2'-雙(三氟甲基)聯苯胺(2,2'- bis(trifluoromethyl)benzidine)
所述聚醯亞胺可於二胺與二酐相比以當量比計過量的條件下聚合而成。例如,BPDA-PDA可使作為二胺的PDA與BPDA相比以當量比計過量的方式聚合而成。
BPDA-PMDA-PDA是以使PDA以比BPDA與PMDA之和的當量比過量的方式聚合而成,BPDA-PDA-TFMB可為使PDA與TFMB之和與PDA的當量比相比過量的方式聚合而成。
二胺與二酐相比以當量比計過量的條件可為例如二酐與二胺以0.9:1至0.99:1的莫耳比聚合。與二胺1莫耳相比,二酐的莫耳比可為0.95~0.99、或0.97~0.99、或0.98~0.99、或0.985~0.99。
通常,於將二胺以比二酐的當量比更多的量進行聚合及硬化而製造的聚醯亞胺用作可撓性基板的情況,在黏度及分子量穩定性方面有利,但於高溫下的CTE為負數,即觀察到收縮的跡象,因而具有於高溫的熱處理製程等中會產生不良的問題。例如,於高溫的熱處理製程之後誘發殘留應力,而存在會使如形成於可撓性基板上的無機膜的龜裂、膜的分離的各種不良產生的問題。根據本發明,藉由利用此種二胺過量的聚醯亞胺的高溫收縮跡象而用作用於載體基板與可撓性基板的分離的剝離層,從而可使高溫製程中形成元件的可撓性基板不經過如雷射照射製程或犧牲層形成及去除製程等引起化學變化或物理變化的製程,無損傷地自載體基板分離。
根據一實施例,BPDA-PMDA-PDA聚醯亞胺聚合時,PMDA可於整體二酐含量中包含5莫耳%以上、或8莫耳%以上、或10莫耳%以上,以及18莫耳%以下或15莫耳%以下。
另外,根據另一實施例,BPDA-PDA-TFMB聚醯亞胺聚合時,TFMB可於整體二胺含量中包含5莫耳%以上、或8莫耳%以上、或10莫耳%以上,以及18莫耳%以下或15莫耳%以下。
根據一實施例,用作所述剝離層的聚醯亞胺的熱分解溫度應比可撓性顯示器元件製程的溫度更高,例如,即便於達到500℃的高溫製程中亦不應分解,因此較佳可具有560℃以上的熱分解溫度。
根據一實施例,所述剝離層的硬化溫度可為350℃以上,較佳為可於400℃以上的溫度下硬化。藉由於350℃以上的溫度下硬化,從而可形成具有與可撓性基板不同的收縮現象的剝離層而使剝離更容易地進行。
所述剝離層的厚度可為50 nm以上1 μm以下,於剝離層的厚度比50 nm薄或比1 μm厚的情況,因根據溫度變化的收縮現象未充分表現而會難以進行剝離。剝離層的厚度可為70 nm以上、80 nm以上、或90 nm以上,且為800 nm以下、600 nm以下、400 nm以下、200 nm以下。
根據一實施例,於所述剝離製程中,對剝離層與可撓性基板層進行剝離的剝離強度可為0.05 N/cm以下、或0.04 N/cm以下、或0.03 N/cm以下。
為了於所述剝離層上形成可撓性基板層,於對可撓性基板用聚醯亞胺前驅物進行塗覆並硬化的製程中,會產生剝離層與可撓性基板層的分離(detach),藉由利用重覆進行用以形成元件的熱處理製程而增加所述分離(detach),從而可使可撓性基板層與剝離層的接著力下降。此時,所述熱處理製程可為350℃以上,且於重覆進行所述熱處理製程之後,剝離層與可撓性基板層的接著力(或剝離強度)可為0.05 N/m以下。
根據一實施例,形成於所述剝離層上的聚醯亞胺可撓性基板層於350℃以上的溫度下CTE具有正數值,較佳可為7 ppm/℃以下,更佳可為4 ppm/℃以下。藉由所述可撓性基板層於350℃以上的溫度下CTE具有正數值,且根據溫度變化的膜的變化狀況與剝離層不同而產生分離,從而可容易地發生剝離層與可撓性基板層的剝離。
根據本發明的一實施例的用於製造可撓性顯示器之疊層結構,可包含:
載體基板層;
形成於所述載體基板層上且具有第一面積的剝離層;以及
具有比所述第一面積大的第二面積且完全覆蓋所述剝離層的可撓性基板層。
圖3a及圖3b表示根據一實施例的疊層結構的平面圖及剖面圖。
參照圖3a與圖3b,於載體基板上形成剝離層,此時將剝離層的面積叫做第一面積。於所述剝離層上形成可撓性基板層,可撓性基板層以比所述剝離層的第一面積寬大的第二面積形成。即,所述可撓性基板層以完全覆蓋剝離層的形態形成,從而可存在所述載體基板與所述可撓性基板層直接相接的區域A。
此時,由於所述載體基板與可撓性基板層的接著力比所述可撓性基板與剝離層的接著力大,因此所述接著力亦可於進行元件形成製程的過程中提供製程穩定性。
即,即便於作為350℃以上的高溫的製程溫度下,因由剝離層的CTE變化產生的翹曲而使可撓性基板層與剝離層之間的接著力下降,因所述可撓性基板層與載體基板接著的區域A而於元件形成製程中亦不產生可撓性基板層與剝離層分離及移動,從而於高溫的製程溫度下亦可穩定地執行元件形成製程。
製造根據本發明的可撓性顯示器方法包含如下步驟:
於載體基板上形成具有第一面積的剝離層的步驟;
以具有比所述剝離層的第一面積大的第二面積且完全覆蓋剝離層的方式形成可撓性基板層的步驟;
於所述可撓性基板層上形成元件的步驟;以及
將形成有元件的可撓性基板自剝離層剝離的步驟。
將所述可撓性基板層剝離的步驟可為在所述剝離層與所述可撓性基板重疊的區域的內側邊緣沿與所述載體基板垂直的方向切斷,從而將所述剝離層與所述可撓性基板層分離。
形成於所述可撓性基板層上的元件在剝離層與所述可撓性基板重疊的區域中形成於可撓性基板層上對製程效率性方面而言較佳。
所述化學式1的X可為包含碳數為3至24的脂肪族環、或碳數為6至30的芳香族環的四價有機基團,具體而言可為包含芳香族環或脂肪族結構各自的環結構為剛性(rigid)的結構、即單環結構、各自的環以單鍵結合的結構、或者各自的環直接連接的多個環結構的四價有機基團,可例如為下述化學式3a至化學式3k的四價有機基團,但並不限定於此。
所述化學式3a至化學式3k的四價官能基中一個以上的氫原子亦可由選自由如下組成的群組中的取代基取代:碳數為1至10的烷基(例如,甲基、乙基、丙基、異丙基、第三丁基、戊基、己基等)、碳數為1至10的氟烷基(例如,氟甲基、全氟乙基、三氟甲基等)、碳數為6至12的芳基(例如苯基、萘基等)、磺酸基及羧酸基,且較佳為可由碳數為1至10的氟烷基取代。
在化學式3a至化學式3k中*表示結合部位。
所述化學式2的Y分別獨立地為碳數為4至30的脂肪族、脂環族或碳數為6至30的芳香族的二價有機基團,或者為其組合基團,自包含選自將脂肪族、脂環族或芳香族的二價有機基團直接連接、或藉由交聯結構彼此連接的二價有機基團中的結構的二胺衍生而成。例如,所述Y可為碳數為6至30的一環式或多環式芳香族、碳數為6至30的一環式或多環式脂環族、或者其中兩個以上以單鍵連接而成的結構,更具體而言,所述Y可為芳香族環或脂肪族結構形成有剛性(rigid)鏈結構者,例如可為包含單環結構、各自的環以單鍵結合的結構、或者各自的環直接連接的多個環結構的二價有機基團,例如可為下述化學式4a至化學式4k的二價有機基團,但並不限定於此。
所述化學式4a至化學式4k的二價官能基中,一個以上的氫原子亦可由選自由如下組成的群組中的取代基取代:碳數為1至10的烷基(例如,甲基、乙基、丙基、異丙基、第三丁基、戊基、己基等)、碳數為1至10的氟烷基(例如,氟甲基、全氟乙基、三氟甲基等)、碳數為6至12的芳基(例如苯基、萘基等)、磺酸基及羧酸基,且較佳為可由碳數為1至10的氟烷基取代。
在化學式4a至化學式4k中*表示結合部位。
根據一實施例,所述可撓性基板用聚醯亞胺可藉由使具有所述化學式1的結構的酸二酐的總莫耳量與化學式2的二胺的總莫耳量相比而以過量進行聚合而得到的前驅物進行硬化而獲得。
用於製造所述剝離層及可撓性基板用聚醯亞胺的酸二酐與二胺化合物的聚合反應可根據溶液聚合等通常的聚醯亞胺或其前驅物的聚合方法來實施。
所述反應可於無水條件下實施,可在所述聚合反應時的溫度為-75℃至50℃,較佳為0至40℃下實施。可以在將二胺類化合物溶解於有機溶劑的狀態下投入酸二酐的方式實施。
另外,作為可用於所述聚合反應的有機溶劑,具體而言可選自由如下組成的群組:γ-丁內酯、1,3-二甲基-咪唑啶酮、甲基乙基酮、環己酮、環戊酮、4-羥基-4-甲基-2-戊酮等酮類;甲苯、二甲苯、四甲基苯等芳香族烴類;乙二醇單乙醚、乙二醇單甲醚、乙二醇單丁醚、二乙二醇單乙醚、二乙二醇單甲醚、二乙二醇單丁醚、丙二醇單甲醚、丙二醇單乙醚、二丙二醇二乙醚、三乙二醇單乙醚等二醇醚類(溶纖劑);乙酸乙酯、乙酸丁酯、乙二醇單乙醚乙酸酯、乙二醇單丁醚乙酸酯、二乙二醇單乙醚乙酸酯、二丙二醇單甲醚乙酸酯、乙醇、丙醇、乙二醇、丙二醇、卡必醇、二甲基乙醯胺(dimethylacetamide,DMAc)、N,N-二乙基乙醯胺(diethylacetamide,DEAc)、二甲基甲醯胺(dimethylformamide,DMF)、二乙基甲醯胺(diethylformamide,DEF)、N-甲基吡咯啶酮(N-methyl pyrrolidone,NMP)、N-乙基吡咯啶酮(N-ethyl pyrrolidone,NEP)、N-乙烯基吡咯啶酮、1,3-二甲基-2-咪唑啶酮、N,N-二甲基甲氧基乙醯胺、二甲基亞碸、吡啶、二甲基碸、六甲基磷醯胺、四甲基脲、N-甲基己內醯胺、四氫呋喃、間二噁烷、p-二噁烷、1,2-二甲氧基乙烷、雙(2-甲氧基乙基)醚、1,2-雙(2-甲氧基乙氧基)乙烷、雙[2-(2-甲氧基乙氧基)]醚及其混合物。
另外,合成聚醯胺酸或聚醯亞胺的情況,為了使剩餘的聚胺基或酸酐基惰性化,可進一步添加末端密封劑,使分子末端與二羧酸酐或單胺反應密封聚醯亞胺的末端。
利用製造的聚醯亞胺前驅物組成物來製造聚醯亞胺的方法包含將所述聚醯亞胺前驅物組成物塗佈於基板的一表面進行熱處理而醯亞胺化的硬化步驟。
具體而言,聚醯亞胺前驅物組成物可為將聚醯亞胺前驅物溶解於所述有機溶劑中的溶液的形態,例如,在有機溶劑中合成聚醯亞胺前驅物的情況下,聚醯亞胺前驅物組成物可為聚合後獲得的聚醯亞胺前驅物溶液本身或進一步添加相同溶液而成,或亦可為利用其他溶劑對所述聚合後獲得的聚醯亞胺前驅物溶液進行稀釋而成。
考慮到所述聚醯亞胺前驅物組成物於進行膜形成製程時的塗佈性等的製程性,較佳為包含作為使其具有適當的黏度的量的固體成分,相對於聚醯亞胺前驅物組成物總重量,所述固體成分可包含5重量%至20重量%。另外,較佳為可以使所述聚醯亞胺前驅物組成物具有400 cP至50,000 cP的黏度的方式進行調節。此處,黏度可藉由美國材料試驗協會(American Society for Testing Materials,ASTM)D4287,ISO2884的標準方法進行測定。聚醯亞胺前驅物組成物的黏度可為小於400 cP,於聚醯亞胺前驅物組成物的黏度超過50,000 cP的情況,於製造利用所述聚醯亞胺前驅物組成物的顯示器基板時,流動性下降,從而於進行塗佈時,會導致不能均勻地塗佈等的製造製程上的問題。
作為所述載體基板,可使用玻璃、金屬基板或塑膠基板等而無特別限制,其中,亦可較佳為使用玻璃基板:於針對聚醯亞胺前驅物的醯亞胺化及硬化製程中,熱穩定性及化學穩定性優異,亦無需單獨的脫模劑進行處理,且可對硬化後形成的聚醯亞胺類膜無損傷且容易地進行分離。
又,可根據通常的塗佈方法實施所述塗佈及塗覆製程,具體而言可利用旋轉塗佈法、棒塗法、輥塗法、氣刀法、凹版法、反向輥法、吻輥法、刮刀法、噴塗法、浸漬法、或塗刷法等。其中,可更佳為藉由可進行連續製程、且可增加聚醯亞胺類樹脂的醯亞胺化率的流延(casting)法實施。
又,可按照以最終製造的聚醯亞胺類膜具有適合於剝離層或顯示器基板用的厚度的厚度範圍,而將所述聚醯亞胺前驅物溶液塗佈至基板上。
於塗佈所述聚醯亞胺前驅物組成物後,於進行硬化製程之前,可更選擇性地實施用以去除存在於聚醯亞胺前驅物組成物內的溶劑的乾燥製程。
可根據通常的方法實施所述乾燥製程,具體而言可於140℃以下,或80℃至140℃的溫度下實施。若乾燥製程的實施溫度小於80℃,則乾燥製程變長,於超過140℃的情況,醯亞胺化急劇進行,從而難以形成具有均勻的厚度的聚醯亞胺膜。
進而,可藉由於80℃至450℃溫度下的熱處理來進行所述硬化製程。所述硬化製程亦可於所述的溫度範圍內於各種溫度下進行多步驟加熱處理。又,進行所述硬化製程時,硬化時間並不特別限定,作為一例,可實施3分鐘至30分鐘。
又,於所述硬化製程後,為了提高聚醯亞胺膜內聚醯亞胺樹脂的醯亞胺化率而形成具有所述的物性特徵的聚醯亞胺類膜,亦可更選擇性地實施後續的熱處理製程。
較佳為於200℃以上、或200℃至450℃下於1分鐘至30分鐘的持續時間內實施所述熱處理製程。又,所述後續的熱處理製程亦可實施一次,或亦可按照兩次以上的多步驟實施。具體而言,可按照包含於200℃至220℃下的第一熱處理、300℃至380℃下的第二熱處理及400℃至450℃下的第三熱處理的三個步驟實施。
所述可撓性基板層所包含的聚醯亞胺可具有約360℃以上的玻璃轉移溫度。如上所述,由於具有優異的耐熱性,包含所述聚醯亞胺的膜針對於元件製造製程中附加的高溫的熱亦可保持優異的耐熱性及機械特性。
[用於實施發明的形態]
以下,對本發明的實施例進行詳細說明,以使本發明所屬技術領域中具有通常知識者可容易地實施。但是,本發明可表現為各種不同的形態,且並不限定於此處所說明的實施例。
>製造例1> BPDA-對苯二胺(para phenylenediamine,pPDA)(98.9:100)聚醯亞胺聚合
於流通有氮氣流的攪拌機內填充100 g有機溶劑NMP(N-甲基-2-吡咯啶酮)後,於將反應器的溫度保持為25℃的狀態下使6.243 g(57.726 mmol)的對苯二胺(p-PDA)溶解。於相同的溫度下向所述p-PDA溶液添加16.797 g(57.091 mmol)的3,3',4,4'-聯苯四羧酸二酐(s-BPDA)與56.96 g的NMP,並於固定時間內溶解並攪拌來聚合聚醯胺酸,從而製造聚醯亞胺前驅物。
以使根據所述反應製造的聚醯亞胺前驅物的固體成分濃度為12.8重量%的方式添加所述有機溶劑來製造聚醯亞胺前驅物溶液。
>製造例2> BPDA-PMDA-pPDA(88.9:10:100)聚醯亞胺聚合
於流通有氮氣流的攪拌機內填充100 g有機溶劑NMP(N-甲基-2-吡咯啶酮)後,於將反應器的溫度保持為25℃的狀態下使6.364 g(58.849 mmol)的對苯二胺(p-PDA)溶解。於相同的溫度下向所述p-PDA溶液添加15.393 g(52.316 mmol)的3,3',4,4'-聯苯四羧酸二酐(s-BPDA)、1.289 g(5.885 mmol)的均苯四甲酸二酐(PMDA)與56.96 g的NMP,並於固定時間內溶解並攪拌來聚合聚醯胺酸,從而製造聚醯亞胺前驅物。
以使根據所述反應製造的聚醯亞胺前驅物的固體成分濃度為12.8重量%的方式添加所述有機溶劑來製造聚醯亞胺前驅物溶液。
>製造例3> BPDA-pPDA-TFMB(98.9:90:10)聚醯亞胺聚合
於流通有氮氣流的攪拌機內填充100 g有機溶劑NMP(N-甲基-2-吡咯啶酮)後,於將反應器的溫度保持為25℃的狀態下使5.335 g(49.332 mmol)的對苯二胺(p-PDA)與1.775 g(5.481 mmol)的2,3'-雙(三氟甲基)聯苯胺(TFMB)溶解。於相同的溫度下向所述p-PDA與TFMB溶液添加15.950 g(54.221 mmol)的3,3',4,4'-聯苯四羧酸二酐(s-BPDA)與56.96 g的NMP,並於固定時間內溶解並攪拌來聚合聚醯胺酸,從而製造聚醯亞胺前驅物。
以使根據所述反應製造的聚醯亞胺前驅物的固體成分濃度為12.8重量%的方式添加所述有機溶劑來製造聚醯亞胺前驅物溶液。
>製造例4> BPDA-pPDA(100:98.9)聚醯亞胺聚合
於流通有氮氣流的攪拌機內填充100 g有機溶劑NMP(N-甲基-2-吡咯啶酮)後,於將反應器的溫度保持為25℃的狀態下使6.142 g(56.800 mmol)的對苯二胺(p-PDA)溶解。於相同的溫度下向所述p-PDA溶液添加16.898 g(57.432 mmol)的3,3',4,4'-聯苯四羧酸二酐(s-BPDA)與56.96 g的NMP,並於固定時間內溶解並攪拌來聚合聚醯胺酸,從而製造聚醯亞胺前驅物。
以使根據所述反應製造的聚醯亞胺前驅物的固體成分濃度為12.8重量%的方式添加所述有機溶劑來製造聚醯亞胺前驅物溶液。
>製造例5> BPDA-pPDA-PA(98.9:100:2.2)聚醯亞胺聚合
於流通有氮氣流的攪拌機內填充100 g有機溶劑NMP(N-甲基-2-吡咯啶酮)後,於將反應器的溫度保持為25℃的狀態下使6.192 g(57.259 mmol)的對苯二胺(p-PDA)溶解。於相同的溫度下向所述p-PDA溶液添加16.661 g(56.629 mmol)的3,3',4,4'-聯苯四羧酸二酐(s-BPDA)與56.96 g的NMP,並於固定時間內溶解並攪拌來聚合聚醯胺酸,從而製造聚醯亞胺前驅物。之後向所述聚醯胺酸溶液投入0.187 g(1.260 mmol)的鄰苯二甲酸酐(phthalic anhydride,PA),並於固定時間內攪拌製造聚醯亞胺前驅物。
以使根據所述反應製造的聚醯亞胺前驅物的固體成分濃度為12.8重量%的方式添加所述有機溶劑來製造聚醯亞胺前驅物溶液。
>製造例6> BPDA-PMDA-pPDA(90:10:98.9)聚醯亞胺聚合
除使BPDA-PMDA-pPDA的莫耳比改變,使二酐當量比過量之外,以與製造例2相同的方法製造聚醯亞胺前驅物溶液。
>製造例7> BPDA-pPDA-TFMB(100:88.9:10)聚醯亞胺聚合
除使BPDA-pPDA-TFMB的莫耳比改變,使二酐當量比過量之外,以與製造例3相同的方法製造聚醯亞胺前驅物溶液。
>實驗例1>
將於製造例1至製造例7中製造的各個聚醯亞胺前驅物溶液旋轉塗佈於玻璃基板。將塗佈有聚醯亞胺前驅物溶液的玻璃基板放置於烘箱並以6 ℃/min的速度進行加熱,於400℃下保持10分鐘進行硬化製程。於硬化製程結束後,將玻璃基板浸入水中以剝除形成於玻璃基板上的膜,並在烘箱中以100℃進行乾燥,來製造厚度為6 μm的聚醯亞胺的膜。
針對所製造的聚醯亞胺膜,以如下所述的方法測定熱膨脹係數(CTE)及熱分解溫度並示於表1。
>熱膨脹係數測定>
將各個聚醯亞胺膜準備成5 mm×20 mm大小後,利用附件將試樣裝載於TA公司的Q400設備中。使實際測定的膜的長度統一為16 mm。將拉伸膜的力設定為0.02 N,並於100℃~460℃的溫度範圍內以4 ℃/min的升溫速度進行第一次升溫製程,之後於460℃~100℃的溫度範圍內以5 ℃/min的冷卻速度進行冷卻(cooling)。之後,於100℃~460℃內以4 ℃/min的升溫速度對經冷卻的各個樣品進行加熱(heating),並藉由熱機械分析儀(thermomechanical analyzer,TMA)測定樣品的熱膨脹變化。將根據由所述加熱引起的溫度變化的樣品的尺寸變化狀況示於圖1a,將於所述溫度範圍內測定的熱膨脹係數示於下述表1。
>熱分解溫度測定>
利用TA儀器(instruments)公司迪斯卡沃瑞(Discovery)TGA對在氮環境下聚合物的重量減少率為1%時的溫度進行測定。
根據所述表1的結果可知,二胺與二酐相比而為過量的製造例1至製造例3的聚醯亞胺膜的CTE為負數,但製造例4至製造例7的膜的CTE表現為正數。於製造例4、製造例6及製造例7的情況下,與二胺相比而二酐過量,於製造例5的情況下,與二酐(BPDA)相比而二胺(pPDA)過量,但添加末端密封劑(PA)而最終酸成分比二胺的含量多。
>實施例1>
利用溶劑對於製造例1中製造的聚醯亞胺前驅物溶液進行稀釋以使固體成分濃度為3 wt%後,旋轉塗佈至玻璃基板的一部分。將塗佈有聚醯亞胺前驅物溶液的玻璃基板放置於烘箱並於常溫下開始以6 ℃/min的速度進行加熱(200℃、350℃、及400℃),於最終硬化溫度下保持10分鐘形成最終厚度為0.1 μm的剝離層。
為了形成可撓性基板層,以完全覆蓋形成於玻璃基板的剝離層的方式旋轉塗佈製造例4的聚醯亞胺前驅物溶液。將塗佈有聚醯亞胺前驅物溶液的玻璃基板放置於烘箱並以6 ℃/min的速度進行加熱,於120℃下保持10分鐘,於400℃下保持55分鐘,形成厚度為10 μm的可撓性基板層,獲得疊層結構。
>實施例2及實施例3>
除利用於製造例2及製造例3中製造的聚醯亞胺前驅物溶液分別形成剝離層之外,以與實施例1相同的方法製造疊層結構。
>比較例1至比較例4>
除利用於製造例4及製造例7中製造的聚醯亞胺前驅物溶液分別形成剝離層之外,以與實施例1相同的方法製造疊層結構。
>剝離力測試>
針對於實施例及比較例中製造的疊層結構,在將完全覆蓋有剝離層的可撓性基板層切割為寬度10 mm及長度100 mm的矩形形態後,抓住切割的可撓性基板的邊緣部分,利用質地分析儀(Texture Analyzer)(TA,XT plus,穩定微系統(Stable microsystems))測定以50 mm/min的速度進行剝除時所用的力。測定結果示於表2。
根據以上的結果可知,根據包括由與二酐的當量比相比過量的方式使用二胺來製造的聚醯亞胺前驅物形成的剝離層的實施例的疊層結構與比較例的疊層結構不同,在將最終硬化溫度提高到350℃以上的情況,表現出0.05 N/cm以下的低的剝離力。另外,可知比較例1的疊層結構由相同的製造例4的聚醯亞胺前驅物組成物製造剝離層與可撓性基板層,於最終硬化溫度為350℃以上的情況下亦保持相當高的接著力。藉此,可知於使可撓性基板層的塗覆面積大於剝離層以完全覆蓋剝離層的情況,可撓性基板層與支撐基板(玻璃基板)直接接觸,即便於高的熱處理製程中亦可無可撓性基板層的分離現象(detach)而進行穩定的製程。
以上,詳細地對本發明內容的特定的部分進行了記述,對本發明所屬技術領域內具有通常知識者而言應明白的是,此種具體的記述僅為較佳的實施方式,並不藉此限制本發明的範圍。因此,本發明的實質的範圍藉由隨附的申請專利範圍與其等同物來定義。
A:區域
圖1a及圖1b是示出於剝離層的CTE為正數的情況下、根據溫度變化的尺寸變化及殘留應力變化的曲線圖(圖1a)以及示出疊層結構的翹曲變化的概略圖(圖1b)。
圖2a及圖2b是示出於剝離層的CTE為負數的情況下、根據溫度變化的尺寸變化及殘留應力變化的曲線圖(圖2a)以及示出疊層結構的翹曲變化的概略圖(圖2b)。
圖3a及圖3b是用以說明將形成有元件的可撓性基板自根據本發明的一實施例的用於製造可撓性基板的疊層結構剝離的製程的平面圖(圖3a)及剖面圖(圖3b)。
Claims (15)
- 一種用於製造可撓性顯示器之疊層結構,包括: 載體基板; 剝離層,形成於所述載體基板上,且包含於350℃以上的溫度下熱膨脹係數(CTE)具有負數值的聚醯亞胺;以及 可撓性基板層,形成於所述剝離層上。
- 如申請專利範圍第1項所述的用於製造可撓性顯示器之疊層結構,其中所述剝離層具有第一面積, 所述可撓性基板層具有大於所述第一面積的第二面積,且完全覆蓋所述剝離層。
- 如申請專利範圍第1項所述的用於製造可撓性顯示器之疊層結構,其中所述剝離層所包含的聚醯亞胺包含二胺與二酐,在與二酐相比,二胺以當量比計過量的條件下聚合及硬化的產物。
- 如申請專利範圍第1項所述的用於製造可撓性顯示器之疊層結構,其中所述剝離層包含含有聯苯四羧酸二酐(BPDA)的二酐與含有苯二胺(PDA)的二胺的聚合及硬化產物。
- 如申請專利範圍第4項所述的用於製造可撓性顯示器之疊層結構,其中二酐能夠更包含均苯四甲酸二酐(PMDA),二胺更包含2,3'-雙(三氟甲基)聯苯胺(TFMB)。
- 如申請專利範圍第5項所述的用於製造可撓性顯示器之疊層結構,其中酸二酐與二胺的組合選自聯苯四羧酸二酐-苯二胺(BPDA-PDA)、聯苯四羧酸二酐-均苯四甲酸二酐-苯二胺(BPDA-PMDA-PDA)及聯苯四羧酸二酐-苯二胺-2,3'-雙(三氟甲基)聯苯胺(BPDA-PDA-TFMB)。
- 如申請專利範圍第6項所述的用於製造可撓性顯示器之疊層結構,其中二酐與二胺的組合為聯苯四羧酸二酐-苯二胺-2,3'-雙(三氟甲基)聯苯胺(BPDA-PDA-TFMB),且2,3'-雙(三氟甲基)聯苯胺(TFMB)於整體二胺中為5莫耳%以上。
- 如申請專利範圍第6項所述的用於製造可撓性顯示器之疊層結構,其中二酐與二胺的組合為聯苯四羧酸二酐-均苯四甲酸二酐-苯二胺(BPDA-PMDA-PDA),且均苯四甲酸二酐(PMDA)於整體二酐中為5莫耳%以上。
- 如申請專利範圍第1項所述的用於製造可撓性顯示器之疊層結構,其中所述剝離層的厚度為50 nm以上1 μm以下。
- 如申請專利範圍第1項所述的用於製造可撓性顯示器之疊層結構,其中所述可撓性基板層包含於350℃以上的溫度下熱膨脹係數具有正數值的聚醯亞胺。
- 一種製造可撓性顯示器的方法,包含如下步驟: 於如申請專利範圍第1項至第10項中任一項所述的用於製造可撓性顯示器之疊層結構所包含的所述可撓性基板層上形成元件的步驟;以及 將形成有所述元件的所述可撓性基板層自所述剝離層剝離的步驟。
- 如申請專利範圍第11項所述的製造可撓性顯示器的方法,其中所述剝離層以具有所述第一面積的方式形成於所述載體基板上, 所述可撓性基板層以具有比所述第一面積大的所述第二面積且完全覆蓋所述剝離層的方式形成, 所述元件於所述剝離層與所述可撓性基板重疊的區域中形成於所述可撓性基板層上。
- 如申請專利範圍第12項所述的製造可撓性顯示器的方法,其中剝離所述可撓性基板層的步驟為在所述剝離層與所述可撓性基板重疊的所述區域的內側邊緣沿與所述載體基板垂直的方向切斷,從而將所述剝離層與所述可撓性基板層分離。
- 如申請專利範圍第11項所述的製造可撓性顯示器的方法,其中於進行剝離製程時,將所述可撓性基板層自所述剝離層剝離的剝離強度為0.05 N/cm以下。
- 如申請專利範圍第11項所述的製造可撓性顯示器的方法,其中於自形成有所述剝離層的所述載體基板對所述聚醯亞胺基板層進行所述剝離製程時,不經過在所述剝離層與所述可撓性基板層之間引起化學變化或物理變化的製程。
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