TW201505988A - 透明擴散性ｏｌｅｄ基材及製造此種基材之方法 - Google Patents
透明擴散性ｏｌｅｄ基材及製造此種基材之方法 Download PDFInfo
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Abstract
本發明提出一種透明擴散性OLED基材，其包含以下一連串之層：(a)由具有折射率介於1.45與1.65之間的無機玻璃所製成之透明平坦基材(1)，(b)包含無機粒子之粗糙的低指數層，該無機粒子係利用溶膠-凝膠無機黏結劑接附至該基材的一面，在無機黏結劑表面附近、表面上或自表面凸出之無機粒子造成以介於0.15與3微米之間所構成的算數平均偏差Ra為特徵之表面粗糙度，該無機粒子及無機黏結劑二者具有介於1.45與1.65之間的折射率；(c)由具有折射率介於1.8與2.1之間的琺瑯所製成之高指數層，其覆蓋該粗糙的低指數層；及一種製造此種擴散性OLED基材之方法。
Description
本發明提出一種製造用於有機發光二極體(OLED)之半透明的光散射性基材之新方法及以此種方法可獲得的基材。
OLED為光電元件，其包含具有夾在二個電極之間的螢光或磷光染料之有機層堆疊，該電極中之至少一者為半透明。當電壓施加於電極時，自陰極射出之電子及自陽極射出之電洞在有機層內重組，導致來自螢光/磷光層的發光。
一般已知自習知的OLED之光提取比較差，大部分的光經由總體內部反射而捕陷於高指數有機層及透明傳導層(TCL)內。總體內部反射不僅發生在高指數TCL與下方玻璃基材(折射率約1.5)之間的邊界處，亦在玻璃與空氣之間的邊界處。
依據估計，在不包含任何額外的提取層之習知的
OLED中，自有機層發射之光約60%補陷於TCL/玻璃之邊界處，額外20%的部份捕陷於玻璃/空氣之表面處，而僅約20%離開OLED進入空氣中。
已知利用在TCL與玻璃基材之間的光散射層來降低此光捕陷。此種光散射層具有接近於TCL指數的高折射率且含有複數個光擴散元件。
亦已知藉由組織化(texturing)在玻璃與OLED的高指數層之間的界面來增加光的輸出耦合(out-coupling)。
〝內部〞提取構件，亦常稱為〝內部提取層〞(IEL)的該二者包含在施加TCL及有機堆疊之前必須先平坦化的凹凸不平處。
WO2011/089343揭示包含以高指數玻璃塗層平坦化之至少一種組織化表面的OLED基材。經說明之基材係以酸蝕刻而組織化。使用強酸(特別為HF)的玻璃蝕刻為常用於使玻璃表面組織化之方法。然而，當在薄玻璃(厚度<1毫米)上進行時，此種濕式化學方法為複雜的製程。此技術僅容許每一製程步驟蝕刻兩面中的一面，因為玻璃板在蝕刻步驟期間必須保持在水平位置。而且，難以使粗糙度輪廓參數最優化，且尤其是HF的使用導致對環境及附近工作人員重要的安全問題。
申請者最近發展出有利於粗糙化玻璃基材的一或兩面之替代方法，該方法包含機械粗糙化(研磨lapping)。在2012年9月28日申請之歐洲申請案12306179.8中所
述之此方法比化學蝕刻還更低的危害性，容許更良好的粗糙度輪廓控制且有可能同時使基材的兩面粗糙化，由此以單一製程步驟製造透明OLED玻璃基材的內部及外部提取層(IEL及EEL)。
本發明提出又另一製造擴散性低指數玻璃基材之方法，該方法既不包含化學蝕刻步驟，亦不包含機械磨蝕步驟。構成本發明基礎的概念為利用低指數無機黏結劑黏結低指數無機粒子至低指數玻璃基材，相對於無機粒子的無機黏結劑之量足夠低，使得無機粒子自黏結劑表面凸出或至少在無機黏結劑表面上產生顯著的粗糙度。
接著將所得擴散性低指數基材進行一般已知使用高指數熔料的平坦化步驟，且接著可將所得平坦化擴散性基材以透明傳導層(TCL)塗佈及用作為OLED之光提取基材。
本發明方法容易實現，僅需要很簡單且一般已知的設備。一種超越EP 12306179.8中所述之研磨方法的顯著優點為其可用於非常大的表面。本發明方法更有利，因為其不減弱基材的機械強度，經大表面蝕刻或研磨之玻璃基材可觀察到不適用。
本發明的第一個發明標的為透明擴散性OLED基材，其包含以下一連串之元件或層：(a)由具有折射率介於1.45與1.65之間的無機玻璃
所製成之透明平坦基材；(b)包含無機粒子之粗糙的低指數層，該無機粒子係利用溶膠-凝膠無機黏結劑接附至基材的一面，在無機黏結劑表面附近、表面上或自表面凸出之無機粒子造成以介於0.15與3微米之間所構成的算數平均偏差Ra為特徵之表面粗糙度，無機粒子及無機黏結劑二者具有介於1.45與1.65之間的折射率；(c)由具有折射率介於1.8與2.1之間的琺瑯所製成之高指數層，其覆蓋該粗糙的低指數層(b)。
本發明亦提供一種製備如上文定義的擴散性基材之方法。
術語〝溶膠-凝膠無機黏結劑〞係指藉由溶膠-凝膠法而自小的前驅體(通常為金屬烷氧化物)獲得的無機固體。此方法包含將前驅體(例如，金屬四烷氧化物)轉化成膠態溶液(溶膠)，其逐步形成整合之聚合物網絡(凝膠)，接著將其乾燥及以燃燒進一步壓實。
本發明的OLED基材之低指數層係由其折射率(1.45-1.65)及其表面粗糙度輪廓，亦即由介於0.15與3微米之間所構成的算數平均偏差Ra(諸如在ISO 4287中之定義)所定義。
該粗糙度係由無機黏結劑表面附近、表面上或自表面凸出之無機粒子所造成。無機粒子未必一定要自無機黏結劑凸出，但是可埋入無機黏結劑層中，只要顯現於例如SEM截面圖中，低指數無機層的粗糙度或波紋度可歸因於
下層粒子，表面輪廓緊密地匹配存在/不存在的埋入之無機粒子。
在本發明所使用的無機粒子可為結晶、非晶形或半結晶粒子。該等粒子可為多少有一點銳利邊緣的任意形狀，但是較佳為有點球狀的粒子，沒有銳利的邊緣。
在較佳的實施態樣中，無機粒子為實體珠粒。此種珠粒較佳，超越呈任意形狀之銳利邊緣的粒子，因為珠粒輕易地擴展於基材表面上，由此加速形成薄的單層珠粒，而不是大尺寸化聚集物。沒有銳利邊緣的似球體粒子亦比呈任意形狀之粒子更輕易地平坦化。應瞭解空心珠粒不包含在本發明的無機粒子之定義中，因為內含的氣體不具有介於1.45與1.65之間所構成的折射率。
術語〝無機粒子〞(尤其在用於說明本發明方法時)包含以有機表面基團(諸如三烷基矽基)官能化之粒子。該有機表面基團在溶膠-凝膠無機黏結劑的燃燒步驟期間，或在形成高指數琺瑯層期間經歷熱分解及因此不再存在於最終產物中。
在本發明所使用的無機粒子(無論是否為球體)具有介於0.3微米與10微米之間的平均等效球體直徑((average equivalent spherical diameter)(由DLS所測量)、較佳為介於0.5微米與8微米之間、更佳為介於0.8微米與7微米之間，呈不規則形狀的粒子之等效球體直徑經定義為具有與無機粒子相同的體積之球體直徑。
然而，平均等效球體直徑不是唯一用於考慮挑選在本
發明使用的無機粒子之尺寸參數。無機粒子最好實質上沒有不僅能從無機黏結劑凸出，亦能從高指數琺瑯層凸出，接著能導致最終OLED中的漏電流之大尺寸化粒子。在本發明所使用的無機粒子因此實質上沒有具有大於15微米、較佳為大於12微米之等效球體直徑的粒子。
如已於上文所指定，玻璃基材、無機粒子及無機黏結劑全部皆具有約介於1.45與1.65之間所構成的相同折射率、較佳為介於1.50與1.60之間。
在本發明較佳的實施態樣中，無機粒子係選自矽石粒子。
為了從全部皆具有約相同的折射率之成分獲得擴散性基材，有必要產生及控制低指數無機層的表面粗糙度。如上文所述，低指數無機層應具有介於0.15與3微米之間所構成的算數平均偏差Ra、較佳為介於0.2與2微米之間。
算數平均偏差Ra係於ISO 4287中定義。其可藉由樣品橫截面之掃描電子顯微法(SEM)、表面輪廓量測法或3D雷射顯微法測量。
為了獲得具有適合的表面粗糙度及滿意的機械抗性二者的無機層，重要的是適當地選擇相對於無機粒子的無機黏結劑量。若使用太高的無機黏結劑量，則無機粒子完全地埋入所得低指數無機黏結劑基質中且不產生介於0.15與3微米之間必要的表面粗糙度(Ra)。另一方面，若相對於無機粒子的無機黏結劑量太低，則無機黏結劑的黏結
強度太弱且所得無機層在處置時過度脆弱及容易受損。
申請者發現由介於0.2與4之間(較佳為介於0.4與3之間)所構成的無機粒子對乾溶膠物質之重量比造成低指數層之適合的表面粗糙度及機械抗性。詞組〝溶膠乾物質〞係指自溶膠所獲得的冷凝之立體無機網絡的乾重量。
最終的低指數無機層亦可以無機粒子對無機黏結劑之體積比特徵化，其較佳地由介於0.3與3之間所構成、較佳為介於0.5與2之間、且更佳為介於0.7與1.5之間。
在低指數無機層(b)上的高指數琺瑯(c)應該具有足以完全覆蓋及平坦化其粗糙度輪廓的厚度。
高指數層的厚度最好由介於3微米與20微米之間所構成、較佳為介於4微米與15微米之間、且更佳為介於5微米與12微米之間。高指數層的厚度為低指數層之粗糙度輪廓與高指數層之粗糙度輪廓的中間線之間的平均距離(如在ISO 4287,3.1.8.1中之定義)。
高指數層之表面粗糙度較佳地應儘可能的低，且高指數琺瑯最好具有少於3奈米之算數平均偏差Ra、更佳為少於2奈米、且最佳為少於1奈米。
高指數層較佳地實質上沒有分散於其中的擴散性元件，尤其沒有分散於其中的擴散性固體粒子。事實上可能不希望此種擴散性固體粒子自高指數層表面凸出及造成最終OLED中的漏電流。
攜帶以高指數玻璃玻料(frit)平坦化之低指數無機層(低指數粒子+溶膠-凝膠無機黏結劑)的所得平坦玻璃
基材通常具有介於75與98%之間所構成的霧度、較佳為介於85與97%之間、且更佳為介於87與95%之間。霧度值可以光學分光光度計測量，如PE Lambda 950或Varian Carry 5000，但是亦可以更快且更便宜的專用裝置，如BYK測霧計。
在較佳的實施態樣中，本發明的透明擴散性OLED基材進一步包含較佳地與高指數琺瑯層(c)直接接觸的透明導電層(d)。可用作為OLED之陽極的此種透明傳導層為先前技藝所熟知。最常使用的材料為ITO(氧化銦錫)。透明傳導層應該具有至少80%之透光率及介於1.8與2.2之間的折射率。其總厚度通常由介於50與400奈米所構成。
如上文所述，本發明亦提出用於製備本發明的OLED基材之方法。
該方法包含以下一連串之步驟：(1)提供由具有折射率介於1.45與1.65之間的無機玻璃所製成之透明平坦基材；(2)將具有折射率介於1.45與1.65之間的無機粒子分散在具有折射率介於1.45與1.65之間的無機黏結劑之至少一種前驅體的溶膠中；(3)將所得分散液施加至基材的一面上；(4)將所得層以加熱乾燥及燒製，從而獲得包含無機粒子及無機黏結劑之透明粗糙的低指數層；(5)將具有折射率介於1.8與2.1之間的高指數玻璃
玻料層施加至該粗糙的低指數層上；(6)將玻璃玻料乾燥及熔化，以獲得覆蓋粗糙的低指數層之具有折射率介於1.8與2.1之間所構成的高指數琺瑯層。
在步驟(1)中所提供的平坦玻璃基材通常具有介於0.1與5毫米之間的厚度、較佳為介於0.3與1.6毫米之間。
在步驟(2)，將如先前所述之無機粒子分散在無機黏結劑之至少一種前驅體的溶膠中。該前驅體較佳地選自由下列者所組成之群組：矽酸鈉、矽酸鉀，矽酸鋰、四-烷氧基矽烷(alcoxysilane)、較佳為四-乙氧基矽烷、烷氧化鈦、烷氧化鋁、烷氧化鋯或其混合物。烷氧化鋯及烷氧化鈦係以低至不足以超過最終無機黏結劑的最大折射率(1.65)之量用在與其他的前驅體之摻合物中。
接著將所得漿液以已知的方法施加於平坦基材的一面上，諸如以浸漬塗佈、滾筒塗佈、旋轉塗佈、狹縫式塗佈。
將溶膠相的溶劑蒸發且使乾燥進行燃燒步驟。在步驟(4)中的乾燥及燃燒最好在至少100℃之溫度下加熱進行、較佳為100℃至300℃、更佳為110至200℃。當所使用的無機粒子為攜帶有機表面基團(諸如三烷基矽基)的經有機改質之粒子時，則烘烤應在高至足以達成該等表面基團之熱分解的溫度下執行。
在步驟(5)，接著將高指數玻璃玻料以任何適合的
方法施加於經烘烤之低指數粗糙層上，諸如網印、噴霧塗佈、棒塗佈、滾筒塗佈、狹縫式塗佈及旋轉塗佈玻璃粒子之水性或有機懸浮液。適合的高指數玻璃玻料及塗佈且燃燒該等熔料之方法的說明可見於例如EP 2 178 343中。
玻璃玻料應經選擇而具有介於450℃與570℃之間所構成的熔點且應該導致琺瑯具有1.8至2.2之折射率。
較佳的玻璃玻料具有下列組成：Bi2O3：55-75重量%
BaO：0-20重量%
ZnO：0-20重量%
Al2O3：1-7重量%
SiO2：5-15重量%
B2O3：5-20重量%
Na2O：0.1-1重量%
CeO2：0-0.1重量%
在典型的實施態樣中，將玻璃玻料粒子(70-80重量%)與20-30重量%之有機媒劑(乙基纖維素及有機溶劑)混合。接著將所得玻料糊以網印法或狹縫式塗佈法施加於經塗佈之擴散性玻璃基材上。將所得層在120-200℃之溫度下加熱而乾燥。將有機黏結劑(乙基纖維素)在介於350-440℃之間的溫度下燒盡，且得到最終琺瑯的燃燒步驟係在介於510℃與610℃之間的溫度下進行、較佳為介於520℃與600℃之間。
當以AFM在10微米×10微米之面積上測量時，顯
示所得琺瑯具有少於3奈米之算數平均偏差Ra(ISO 4287)的表面粗糙度。
塗佈於粗糙化表面上的高指數玻璃玻料量通常由介於20與200公克/平方公尺之間所構成、較佳為介於25與150公克/平方公尺之間、更佳為介於30與100公克/平方公尺之間、且最佳為介於35與70公克/平方公尺之間。
在本發明中所使用的高指數玻璃玻料及由其所生成之琺瑯較佳地實質上沒有固體散射粒子，諸如SiO2或TiO2結晶粒子。此種粒子常被用作為高指數散射層中的散射元件，但是通常需要額外的平坦化層，由此增加高指數塗層的總厚度。
以高指數琺瑯平坦化之擴散性基材特別用作為底部發射OLED之基材。在施加有機發光層堆疊之前，必須先將透明傳導層施加於高指數琺瑯頂部上。
在較佳的實施態樣中，本發明方法因此進一步包含以透明傳導層(較佳為透明傳導性氧化物)塗佈自步驟(6)所生成之高指數琺瑯的額外步驟。此種TCL的形成可根據習知的方法進行，諸如磁控濺鍍。
圖1及2顯示粗糙的低指數層在燃燒之後及以高指數玻料平坦化之前的SEM顯微照片。
將具有2.5微米之平均直徑的20公克經有機改質之矽石珠粒分散在150公克2-甲氧基丙醇中且以超音波分散。將30公克Xenios® Surface Perfection(Evonik GmbH)添加至此分散液中。接著將所得分散液以浸漬塗佈法施加於清潔的玻璃基材上且在120℃下經約1分鐘乾燥。接著將經塗佈之乾燥基材以5℃/分鐘之速率加熱至500℃之溫度且在此溫度下燒製5分鐘。
圖1及2顯示粗糙的低指數層在燃燒之後及以高指數玻料平坦化之前的SEM顯微照片。可看出球體粒子係以相當緊密填充的單層形式擴展於玻璃基材上。
接著將所得低指數粗糙層以高指數玻料漿液(n=1.90)經網印法塗佈。將塗層在150℃下乾燥且在IR爐中以545℃進行10分鐘燃燒。
Claims (15)
- 一種透明擴散性OLED基材，其包含以下一連串之元件或層：(a)由具有折射率介於1.45與1.65之間的無機玻璃所製成之透明平坦基材(1)，(b)包含無機粒子之粗糙的低指數層，該無機粒子係利用溶膠-凝膠無機黏結劑接附至該基材的一面，在無機黏結劑表面附近、表面上或自表面凸出之無機粒子造成以介於0.15與3微米之間所構成的算數平均偏差Ra為特徵之表面粗糙度，該無機粒子及無機黏結劑二者具有介於1.45與1.65之間的折射率；(c)由具有折射率介於1.8與2.1之間的琺瑯所製成之高指數層，其覆蓋該粗糙的低指數層。
- 根據申請專利範圍第1項之基材，其中該無機粒子具有介於0.3微米與10微米之間、較佳為介於0.5微米與8微米之間、更佳為介於0.8微米與7微米之間的平均等效球體直徑(average equivalent spherical diameter)。
- 根據申請專利範圍第1或2項之基材，其中該無機粒子為實體珠粒。
- 根據申請專利範圍第1或2項之基材，其中該無機粒子實質上沒有具有大於15微米、較佳為大於12微米之等效球體直徑的粒子。
- 根據申請專利範圍第1或2項之基材，其中該基材、低指數琺瑯及無機粒子之折射率係由介於1.50與 1.60之間所構成。
- 根據申請專利範圍第1或2項之基材，其中該高指數層之厚度係由介於3微米與20微米之間、較佳為介於4微米與15微米之間、且更佳為介於5微米與12微米之間所構成。
- 根據申請專利範圍第1或2項之基材，其中該高指數層之表面粗糙度具有低於3奈米、更佳為低於2奈米、且最佳為低於1奈米之算數平均偏差Ra。
- 根據申請專利範圍第1或2項之基材，其中該高指數層實質上沒有分散於其中的擴散性元件，尤其沒有分散於其中的擴散性固體粒子。
- 根據申請專利範圍第1或2項之基材，其中該無機粒子係選自矽石粒子。
- 根據申請專利範圍第1或2項之基材，其進一步包含在該高指數琺瑯層上的透明導電層。
- 根據申請專利範圍第1或2項之基材，其中該無機粒子對無機黏結劑之體積比係由介於0.3與3之間、較佳為介於0.5與2之間、且更佳為介於0.7與1.5之間所構成。
- 一種製備根據前述申請專利範圍中任一項之透明擴散性基材的方法，其包含以下一連串之步驟：(1)提供由具有折射率介於1.45與1.65之間的無機玻璃所製成之透明平坦基材；(2)將具有折射率介於1.45與1.65之間的無機粒子 分散在具有折射率介於1.45與1.65之間的無機黏結劑之至少一種前驅體的溶膠中；(3)將該所得分散液施加至該基材的一面上；(4)將該所得層以加熱乾燥及燒製，從而獲得包含無機粒子及無機黏結劑之透明粗糙的低指數層；(5)將具有折射率介於1.8與2.1之間的高指數玻璃玻料(frit)層施加至該粗糙的低指數層上；(6)將該玻璃玻料乾燥及熔化，以獲得覆蓋該粗糙的低指數層之具有折射率介於1.8與2.1之間所構成的高指數琺瑯層。
- 根據申請專利範圍第12項之方法，其中該無機黏結劑之至少一種前驅體係選自由下列者所組成之群組：矽酸鈉、鉀或鋰、四-烷氧基矽烷(alcoxysilane)、烷氧化鈦、烷氧化鋁、烷氧化鋯。
- 根據申請專利範圍第12項之方法，其中在步驟(4)之該乾燥及燒製係藉由在至少100℃、較佳為100℃至300℃、更佳為110至200℃之溫度下加熱來進行。
- 根據申請專利範圍第12項之方法，其中該無機粒子具有介於0.3微米與10微米之間、較佳為介於0.5微米與8微米之間、更佳為介於0.8微米與7微米之間的平均等效球體直徑。
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| ??13168341.9 | 2013-05-17 | ||
| EP13168341.9A EP2803644B1 (en) | 2013-05-17 | 2013-05-17 | Transparent diffusive oled substrate and method for producing such a substrate |
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| EP2814078B1 (en) | 2013-06-14 | 2016-02-10 | Saint-Gobain Glass France | Transparent diffusive oled substrate and method for producing such a substrate |
| WO2016160911A1 (en) * | 2015-03-31 | 2016-10-06 | Corning Incorporated | Waveguides comprising light scattering surfaces and display devices comrpising the same |
| EP3353583A1 (en) * | 2015-09-23 | 2018-08-01 | Corning Incorporated | Oled light extraction using nanostructured coatings |
| US11327205B2 (en) | 2019-07-29 | 2022-05-10 | Viavi Solutions Inc. | Encapsulated diffuser |
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| EP2814078B1 (en) * | 2013-06-14 | 2016-02-10 | Saint-Gobain Glass France | Transparent diffusive oled substrate and method for producing such a substrate |
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| EP2803644B1 (en) | 2018-08-08 |
| RU2015153822A (ru) | 2017-06-22 |
| KR20160009029A (ko) | 2016-01-25 |
| EP2803644A1 (en) | 2014-11-19 |
| EP2996995A1 (en) | 2016-03-23 |
| RU2656264C2 (ru) | 2018-06-04 |
| RU2015153822A3 (zh) | 2018-04-02 |
| TWI622562B (zh) | 2018-05-01 |
| CN105189383B (zh) | 2018-08-10 |
| US10147894B2 (en) | 2018-12-04 |
| ES2695052T3 (es) | 2018-12-28 |
| JP6495894B2 (ja) | 2019-04-03 |
| WO2014183993A1 (en) | 2014-11-20 |
| MY175975A (en) | 2020-07-19 |
| KR102142437B1 (ko) | 2020-08-07 |
| JP2016524788A (ja) | 2016-08-18 |
| CN105189383A (zh) | 2015-12-23 |
| US20160072083A1 (en) | 2016-03-10 |
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