TWI507448B - 透明聚亞醯胺基板及其製造方法 - Google Patents
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Description
本發明係關於一種在可撓性電子裝置中作為覆蓋基板的透明聚亞醯胺基板和其製造方法。
近年來,新一代的顯示器中,可彎曲的電子裝置備受關注,包括可撓性有機發光二極體,可撓性的太陽能電池(PV)、輕便顯示器、可撓性密封材料、彩色電泳顯示器(EPD)、塑膠液晶顯示器、觸控面板(TSP)、有機太陽能電池(OPVs)等。為了製造可彎曲的可撓性顯示器並保護其中的元件,有必要使用新型的可撓性覆蓋基板來代替傳統的玻璃基板。此外,新型基板需要具有高硬度、低濕度性、高耐化學性和高光透射性來保護包括在顯示器中的元件。
對於作為這種可撓性顯示器的覆蓋基板材料,各種高硬度的塑膠基板正被研究作為候選材料,而其中一種具有高硬度的透明聚醯亞胺薄膜也正被考慮作為主要的候選材料。
過去,為增強聚亞醯胺的硬度以作為可撓性電子裝置的覆蓋基板材料,係在透明薄膜上形成丙烯酸類或環氧類的有機固化層,但是這種固化層不夠柔韌,在彎曲時表面容易開裂。
韓國專利公開第10-2012-0078514號(公佈於2012年7月10日)揭露了一種具有耐溶劑性和高耐熱性的透明聚亞醯胺基板,此可撓性基板材料係在透明聚亞醯胺薄膜的一表面或兩表面上形成氧化矽層。這種基板具有良好的耐溶劑性、透光度、黃度和熱性能等諸多優點,但只有氧
化矽層是無法提供覆蓋基板所需之足夠的抗劃傷性。
本發明的目的在於提供一種透明聚亞醯胺基板,其具有良好抗劃傷性以避免可撓性電子裝置在使用時被刮傷,因此可作為可撓性電子裝置的覆蓋基板材料。
在一實施例中,本發明提供一種透明聚亞醯胺基板,包括一透明聚亞醯胺薄膜以及一形成在該透明聚亞醯胺薄膜的至少一表面上的聚異氰酸酯(polyisocyanate)固化層,該聚異氰酸酯每一分子含有一丙烯酸酯基以及2~5個異氰酸酯基。
在一個特定之關於本發明透明聚亞醯胺基板的實施例中,聚異氰酸酯可為下面的化學式1所示的異氰酸酯化合物,其具有一丙烯酸酯基。
在本發明的一個較佳實施例中,鑒於透明聚亞醯胺基板的硬度和柔韌性,上述固化層的厚度可為1.0~20.0μm。
在本發明實施例中之透明聚亞醯胺基板為提高耐溶劑性、透水性以及光學性,可進一步於透明聚亞醯胺薄膜和固化層之間形成一氧化矽層,該氧化矽層的單元結構是由下面的化學式2所表示。
;其中,m和n分別表示0~10的整數。
在本發明的一個較佳實施例中,鑒於透明聚亞醯胺基板的耐溶劑性和柔韌性,上述固化層的厚度可為0.3~2.0μm。
在本發明的一個實施例中,提供了一種製造透明聚亞醯胺薄膜的方法,其步驟包括:在一透明聚亞醯胺薄膜的至少一個表面上塗佈每一分子含有一丙烯酸酯基和2~5個異氰酸酯基所構成的聚異氰酸酯溶液,之後乾燥該塗佈的溶液以形成一塗層;以及固化該塗層以形成一固化層。
根據本發明一個較佳實施例的製造方法,該聚異氰酸酯是由上述化學式1所表示。
鑑於紫外線的固化性,含有上述聚異氰酸酯的溶液可包括安息香醚類光引發劑、二苯甲酮光引發劑或兩者結合而成的光引發劑。
根據本發明一個較佳實施例的製造方法,形成上述固化層的步驟是用312nm或365nm的短波長紫外線以1500~10000J/m2
的劑量照射
該塗層。
在本發明的較佳實施例中,一種製造透明聚亞醯胺基板的方法,在塗佈含有聚異氰酸酯的溶液步驟之前,可進一步先:塗佈含有聚矽氮烷的溶液;乾燥該塗佈的溶液;以及固化該聚矽氮烷以形成一氧化矽層。
根據一個特定實施例中的製造方法,上述聚矽氮烷的單元結構可由下面的化學式3所表示。
;其中,m和n分別為0~10的整數。
根據本發明一個較佳實施例之製造透明聚亞醯胺基板的方法,其中,固化聚矽氮烷的氧化矽層的步驟可在200~300℃的溫度下進行熱處理來固化形成。
本發明提出了一種具有抗劃傷性、耐溶劑性、透水性和柔韌性的透明聚亞醯胺基板,這種基板可以作為可撓性電子裝置的覆蓋基板。
下面將對本發明進行詳述。
依據本發明的一種透明聚亞醯胺基板,其包括形成在一透明聚亞醯胺薄膜的至少一表面上含有丙烯酸酯基之聚異氰酸酯化合物的固化層,這種固化層可以作為硬塗層。
聚異氰酸酯化合物是指每一個分子中具有多個異氰酸酯基的有機化合物,並且這種化合物每一個分子中所含有的異氰酸酯基數量以不超過5個為較佳。
這種聚異氰酸酯化合物可以和含有羥基的丙烯酸樹脂反應形成含有丙烯酸酯基的聚異氰酸酯化合物。含有丙烯酸酯基的聚異氰酸酯化合物可以經由交聯而提供一有較佳物理特性的塗層。
如果含有丙烯酸酯基的聚異氰酸酯化合物中的異氰酸酯基數目超過5個,雖有利於提高硬度,但隨著交聯度的提高,彎曲性就會降低,而此彎曲性卻是可撓性覆蓋薄膜的重要物理性質。在每一個分子中含有2個異氰酸酯基的聚異氰酸酯化合物例子中,包括二異氰酸酯單體,例如:二異氰酸甲苯酯(tolylene diisocyanate)、二異氰酸萘酯(naphthalene diisocyanate)、二異氰酸二甲苯酯(xylylene diisocyanate)和降莰烯二異氰酸酯(norbornene diisocyanate)。上述二異氰酸酯單體可以和含有羥基的丙烯酸樹脂反應形成具丙烯酸酯基的二異氰酸酯化合物。
在其他例子中,每一個分子中含有3個以上異氰酸酯基的聚異氰酸酯化合物可以和含有羥基的丙烯酸樹脂反應以形成化學式1所示的聚異氰酸酯。
化學式1所示的聚異氰酸酯含有一丙烯酸酯基,固化後可提高固化層的物理特性,尤其是耐劃傷性。
此種含有一丙烯酸酯基的聚異氰酸酯所形成的固化層,其厚度以1.0-20.0μm為較佳,為確保薄膜具有高於鉛筆H值的硬度,固化層的厚度以1μm以上為較佳,而為防止固化層降低透明聚亞醯胺基板的柔韌性,固化層的厚度較佳在20.0μm以下。
此種含有一丙烯酸酯基的聚異氰酸酯是在透明聚亞醯胺薄
膜上塗佈含有丙烯酸酯基的聚異氰酸酯溶液,並乾燥後固化所得到。
在透明聚亞醯胺薄膜的一表面或兩表面上塗佈時,可以選擇噴塗、棒塗、旋塗或浸塗中的某一適當的方法來實施。
固化過程可藉由紫外線方式來固化,因此含有丙烯酸酯基的溶液中也可含有光引發劑。光引發劑中可包括安息香醚類光引發劑、二苯甲酮光引發劑或兩者結合的光引發劑。
紫外線固化條件是以312nm或365nm的短波長紫外線於1500~10000J/m2
的劑量下照射來進行固化。
同時,本發明的透明聚亞醯胺基板,也包括在透明聚亞醯胺薄膜和上述固化層(即硬塗層)之間形成以化學式2的單元結構所構成的氧化矽層。
在透明聚亞醯胺薄膜的一表面或兩表面上形成無機氧化矽層,可使薄膜表面具有良好的耐溶劑性和高耐熱性。當化學式1中的n或m為0而為純無機層時,可以發揮最大耐溶劑性和高耐熱性。在某些情況下,為提高透明聚亞醯胺基板的柔韌性,化學式1中的n或m較佳是1以上,且是長度適當的烷基鏈。但當n或m為10以上時,由於塗層溶液中的二氧化碳粒子的疏水性,會在塗佈時產生結塊現象。
上述氧化矽層的厚度以0.3-2.0μm為較佳,厚度在0.3μm以上是為了確保有適當的耐溶劑性,而在2.0μm以下是為了避免降低透明聚亞醯胺的柔韌性。
因此,形成有氧化矽層的透明聚亞醯胺基板具有較高的光透射度、低黃度和低滲水性的優點。而低滲水性是保護TFT和OLED裝置暴露在潮濕環境下的必要特性。
當氧化矽層形成在本發明之透明聚亞醯胺基板的表面時,其表面粗糙度(即RMS)可達2nm以下,因此基板表面是平坦的。此平坦表面在形成電極或TFT時可以促進載體的流動。
本發明之製造透明聚亞醯胺基板的方法,其步驟包括在一透
明聚亞醯胺薄膜的至少一表面上塗佈含有聚異氰酸酯的溶液,該聚異氰酸酯每一分子含有一丙烯酸酯基以及2~5個異氰酸酯基;之後乾燥該塗佈的溶液以形成塗層;以及固化所述塗層以形成一固化層。
當在透明聚亞醯胺薄膜的一個表面上塗佈的聚矽氮烷固化後,化學式3單元結構中的胺基(-NH-)被轉換成化學式2單元結構中的醚基(-O-),從而形成了氧化矽層。此時,較佳的固化方法是在200~300℃的溫度下進行熱處理。
在熱固化方法中,聚矽氮烷易形成具有網狀結構的氧化矽膜。而且該膜的硬質性使其具有良好的耐化學性和耐熱性。
在選擇熱固化方法的情況下,可以在200~300℃的溫度下對聚矽氮烷進行熱處理。
當熱處理的溫度在200℃以上時,可以縮短固化聚矽氮烷以形成氧化矽膜所需的時間,在300℃以下時,可以防止透明聚亞醯胺薄膜和氧化矽層之間因熱膨脹係數不同而產生的變形。
傳統在表面上形成無機物的沉積方式,如PECVD或濺射,由於有限的真空設備,因而具有沉積區域受限的缺點。但本發明方法中固化所塗佈的溶液以形成無機層的方法,具有在大氣壓下可經由簡單鑄製方式,在大區域內連續操作的優點。
該聚矽氮烷包括上述化學式3的單元結構,而且重均分子量為3,000-5,000g/mol。
所述分子量是根據凝膠滲透層析法(gel permeation chromatograph,GPC)(S-3580,SYKAM RI)的標準物質換算後的重均分子量。將待測的聚合物溶解在濃度為0.1wt%的THF中後,取50ML加入GPC中。GPC的流動相使用25mM溴化銀和3mM H3
PO4
在THF:MEK(1:1)中,以1mL/min的流速,在50℃下進行分析。所用的層析柱是由兩根Styragel HR 5ET和1根Styragel HR 4E互相串聯而成。所用的檢測器是Sykam RI S-3580,且測量溫度達到50℃。
化學式3中的m和n可根據最終形成的氧化矽性質來決定。而且,聚矽氮烷的重均分子量在3000以上才能確保具有良好的耐溶劑性和高耐熱性,重均分子量在5000以下才能確保溶液均勻的覆蓋性。
在透明聚亞醯胺薄膜的一表面或兩表面上塗佈含有聚矽氮烷溶液的過程,可以選擇噴塗、棒塗、旋塗或浸塗中的某一適當的方法來實施。
以下以本發明的實施例進行詳細說明。
<製造實施例1>
1-1:聚亞醯胺粉末的製造
在內置攪拌器、設有氮氣注入口、滴液漏斗、溫度調節器和冷卻器的1L反應器中,沖入氮氣和加入832g的N,N-二甲基乙醯酸(DMAc),在反應器內部的溫度調整至25℃的狀態下,把64.046g(0.2mol)的雙三氟甲基聯苯胺(bistrifluoromethyl benzidin,TFDB)溶解於反應器中的溶液,並將溫度維持在25℃。隨後在該溶液中加入31.09g(0.07mol)的2,2-雙(3,4-二羧基苯基)六氟丙烷二酐(2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride,6FDA)和8.83g(0.03mol)的聯苯四羧酸二酐(biphenyl tetracarboxylic dianhydride,BPDA),於25℃下攪拌一預定時間。之後,添加20.302g(0.1mol)的對酞醯氯(terephthaloyl chloride,TPC)以獲得13wt%固體濃度的聚醯胺酸溶液。接下來,在該溶液中加入25.6g吡啶(pyridine)和33.1g乙酸酐(acetic anhydride)後,於25℃下攪拌30分鐘,再於70℃下攪拌1小時。之後將其冷卻至室溫,並以20L甲醇進行沉澱。將沉澱出的固體過濾並搗碎後,在100℃的真空狀態下乾燥6小時,獲得111g固體粉末狀的聚亞醯胺。
1-2:聚亞醯胺薄膜的製造
取0.03g(0.03wt%)表面有羥基(OH)的非結晶二氧化矽粒子,以0.1%濃度分散在N,N-二甲基乙醯胺(DMAc)中,並以超音波處理至溶劑變透明。之後把前述100g固體粉末狀的聚醯亞胺溶解到670g的N,N-二甲基乙醯胺中而具有13wt%的濃度。把所得溶液塗在不銹鋼板上,並壓鑄
成340μm的厚度後,在130℃下以熱風乾燥30分鐘。將形成的薄膜剝下,並用銷釘固定在框架上。然後把該框架放入真空乾燥爐中,緩慢由100℃至300℃下加熱2個小時,之後再緩慢冷卻。從框架上將薄膜分離,即獲得聚亞醯胺薄膜。聚亞醯胺薄膜最後再進行300℃下30分鐘的熱處理。此時製造出的聚亞醯胺薄膜的厚度為50μm,具有88%的平均光透射率和數值為3.0的黃度。根據TMA-方法在50~250℃下測定的平均熱膨脹係數(CTE)為20ppm/℃。
<比較實施例1>
以製造實施例1中所得到的聚亞醯胺薄膜作為比較實施例1。
<比較實施例2>
化學式3中的m和n分別為0時,把重均分子量為2000g/mol的聚矽氮烷(MOPS-1800,Az材料)溶解在二丁醚中形成濃度為2wt%的溶液,並將該溶液以線狀塗佈在比較實施例1中的無色透明聚亞醯胺薄膜的一表面,然後在約80℃下進行乾燥,形成了厚度為300nm的聚矽氮烷層。
接著,將聚矽氮烷層在室溫中靜置約5分鐘後,在250℃左右進行熱固化以形成氧化矽層,即可製造出具有無色透明的聚亞醯胺薄膜/氧化矽層結構的基板。
<比較實施例3>
進行與上述比較實施例2中把聚矽氮烷溶液塗在無色透明的聚亞醯胺薄膜的一表面上的相同方式,但係塗於兩表面,製造出具有氧化矽層/無色透明的聚亞醯胺薄膜/氧化矽層結構的基板。
<實施例1>
使用浸塗機把包括化學式1中含丙烯酸酯的聚異氰酸酯(m=2,n=2,R1
為甲基,R2
為乙基)和光引發劑(3wt%,Chempia,PI981)的塗液塗佈在上述比較實施例1中無色透明的聚亞醯胺薄膜的一表面上,並在約80℃下乾燥,得到了厚度為10μm的塗層。然後使用312nm和365nm波長的紫外線以100mw/cm2
照射塗層10秒,即可製造出具有無色透明聚亞
醯胺薄膜/含丙烯酸酯的聚異氰酸酯固化層結構的無色透明聚亞醯胺薄膜。
<實施例2>
以上述實施例1的方法,但係在無色透明聚亞醯胺薄膜兩表面上形成固化層,以製造出具有含丙烯酸酯的聚異氰酸酯固化層/無色透明的聚亞醯胺薄膜/含丙烯酸酯的聚異氰酸酯固化層結構的無色透明聚亞醯胺薄膜。
<實施例3>
取比較實施例2中在一表面上形成有氧化矽層的無色透明聚亞醯胺薄膜,以實施例1相同的方法,於氧化矽層上形成含有丙烯酸酯的聚異氰酸酯固化層,而製造出具有無色透明聚亞醯胺薄膜/氧化矽層/含丙烯酸酯的聚異氰酸酯固化層結構的基板。
<實施例4>
取比較實施例3中在二個表面上形成有氧化矽層的無色透明聚亞醯胺薄膜,以實施例1相同的方法,於氧化矽層上分別形成含有丙烯酸酯的聚異氰酸酯固化層,而製造出具有含丙烯酸酯的聚異氰酸酯固化層/氧化矽層/無色透明的聚亞醯胺薄膜/氧化矽層/含丙烯酸酯的聚異氰酸酯固化層結構的基板。
以實施例和比較實施例中所製造出的無色透明聚亞醯胺薄膜將以下述方式測量其表面硬度、光學性能和其他物理特性。
按以下方法測定物理特性,結果如下表1所示。
(1)平均光透率(%)
使用分光光度計(CU-3700D,KONICA MINOLTA)來測定350-700nm範圍內的平均光透率。
(2)黃度
使用分光光度計(CU-3700D,KONICA MINOLTA)來測定黃度。
(3)滲水性(g/m2
*天)
使用滲透計(MOCON/US/Aquatran-model-1)來測滲水性(WVTR)。
(4)鉛筆硬度
使用自動鉛筆硬度測定計測量,將負載1kg的三菱鉛筆以180mm/min的速度在薄膜上畫5次50mm後,判斷表面完全沒有刮痕的鉛筆硬度。
(5)附著性(用膠帶進行100次的黏合與拆開)
依照標準測量方式(ASTM D3359),進行100次膠帶測試法來測定附著性。
(6)彎曲性
把基板圍繞在直徑為10mm的圓形工具上反覆進行纏繞並鬆開,以肉眼或顯微鏡觀察膜是否破裂。如果出現少量破裂的現象即不具有彎曲性,沒有***現象即測定為具有彎曲性。
(7)抗劃傷性
使用鋼絲絨在負載500g的情況下,以50mm/s的速度在基板上反覆摩擦5OO次後,以肉眼或光學顯微鏡來測定劃痕的數量。如果沒有劃痕就用「◎」來表示,少於1~5條就用「△」來表示,而超過5條就用「X」來表示。
(8)耐溶劑性
分別把塗層浸入表2所示的有機溶劑中,進行30分鐘的浸漬試驗來測定其耐溶劑性。以肉眼觀察,如果外觀上沒有變化且化學測試前後的RMS差值小於1nm以「◎」來表示,如果外觀上沒有變化且化學測試前後的RMS差值大於1nm以「○」來表示,若表面出現白濁或斑點現象則以「X」來表示,實驗結果如表2所示。
根據表1中的資料,將表面形成有氧化矽層的比較實施例2和3與表面不做任何處理的比較實施例1比較後可知,其光透射率、黃度等物性得到了提升,而表面形成含有丙烯酸酯的聚異氰酸酯固化層的實施例1到4,則可以確認抗劃傷性有明顯的提高。特別是在實施例3和4中,在含有丙烯酸酯的聚異氰酸酯固化層下含有氧化矽層時,其滲水性測試有最佳的結果。
根據表2中實施例和比較實施例的耐溶劑性測試結果可知,實施例1到4和比較實施例2到3中對所有溶劑的耐溶劑性在外觀上沒有變化,且化學測試前後測定出的RMS差值小於1nm,但比較實施例1中部分溶劑的測定結果並不佳。
Claims (10)
- 一種透明聚亞醯胺基板,包括:一透明聚亞醯胺薄膜;以及一固化層,係聚異氰酸酯經由光引發劑所引發之固化反應所形成,其中,該聚異氰酸酯係形成在該透明聚亞醯胺薄膜的至少一表面上,而該聚異氰酸酯係如化學式1所示:
- 如申請專利範圍第1項所述之透明聚亞醯胺基板,其中該固化層的厚度為1.0~20.0μm。
- 如申請專利範圍第1項所述之透明聚亞醯胺基板,其中該透明聚亞醯胺薄膜和固化層之間進一步形成有一氧化矽層,該氧化矽層具有化學式2所示的單元結構: ;其中,m和n分別為0~10的整數。
- 如申請專利範圍第3項所述之透明聚亞醯胺基板,其中該氧化矽層的厚度為0.3-2.0μm。
- 一種製造透明聚亞醯胺基板的方法,其步驟包括:在一透明聚亞醯胺薄膜的至少一表面上塗佈含有光引發劑及聚異氰酸酯的溶液,之後乾燥該塗佈的溶液以形成一塗層;以及固化該塗層以形成一固化層,其中,該聚異氰酸酯係如化學式1所示:
- 如申請專利範圍第5項所述之製造透明聚亞醯胺基板的方法,其中該光引發劑包括一選自安息香醚類光引發劑、二苯甲酮光引發劑以及兩者結合所組成群組的光引發劑。
- 如申請專利範圍第5項所述之製造透明聚亞醯胺基板的方法,其中該固化塗層以形成固化層的步驟,係以312nm或365nm短波長的紫外線於1500-10000J/m2 劑量下來照射該塗層。
- 如申請專利範圍第5項所述之製造透明聚亞醯胺基板的方法,其中在該塗佈含有聚異氰酸酯溶液的步驟之前,進一步先:塗佈含有聚矽氮烷的溶液;乾燥該塗佈的溶液;以及固化該聚矽氮烷以形成一氧化矽層。
- 如申請專利範圍第8項所述之製造透明聚亞醯胺基板的方法,其中該聚矽氮烷具有化學式3所示的單元結構,而該氧化矽層具有化學式2所示的單元結構:化學式2 ;其中,m和n分別為0~10的整數;;其中,m和n分別為0~10的整數。
- 如申請專利範圍第8項所述之製造透明聚亞醯胺基板的方法,其中該固化該聚矽氮烷以形成該氧化矽層的步驟係在200~300℃中熱處理該聚矽氮烷。
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