TWI666804B - 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
本發明係關於一種製備用於發光裝置之積層基材之方法，其包含：(a)提供介於1.45和1.65之間的折射指數之玻璃基材(1)，(b)將金屬氧化物層(2)塗覆在玻璃基材的一面上，(c)將折射指數至少1.7的玻璃料(glass frit)(3)塗覆在該金屬氧化物層(2)上，該玻璃料包含至少30重量%的Bi2O3，(d)所得經塗覆的玻璃基材於介於530℃和620℃之間的溫度燒製，藉此使得金屬氧化物與熔融玻璃料反應並形成具有多個球狀空隙(5)埋在琺瑯層之接近與玻璃基材之介面處之較低部分中的高指數琺瑯層(4)。
Description
本發明係關於製備用於有機發光二極體(OLED)之半透明散射光的玻璃基材之嶄新方法及藉此方法可得的基材。
OLED係光學元件，其包含有機層與螢光或磷光染料夾於兩個電極之間的有機層(其中至少一者半透明)之堆疊物。當電壓施於電極時，自陰極射出的電子和自陽極射出的電動在有機層內合併，得到自螢光/磷光層發射的光。
一般已經知道自慣用OLED萃出的光相當弱，大部分的光被高指數有機層和透明導電層(TCL)中的內部總反射所捕集。內部總反射不僅發生於介於高指數TCL和位於下方的玻璃基材(折射指數約1.5)之間的邊界，亦發生於介於玻璃和空氣之間的邊界。
根據估計，在不包含任何額外萃光層之慣用
OLED中，約60%自有機層發射的光在TCL/玻璃邊界處被捕集，另20%在玻璃/空氣表面處被捕集，僅約20%離開OLED進入空氣中。
已經知道降低藉由介於TCL和玻璃基材之間的光散射層減少此光截留。此光散射層具有具高折射指數(接近TCL折射指數)的透明基質並含有多個折射指數不同於基質的光散射元件。此高指數基質一般藉由熔化高指數玻璃料而得，藉此在低指數玻璃基材上得到薄的高指數琺瑯層。光散射元素可以在熔化步驟之前以固態粒子加至玻璃料中，在此熔化步驟期間內形成晶體或在此熔化步驟期間內形成氣泡。
也已經知道在施用和熔化高指數玻璃料之前，藉由介面的紋理化(即，在介於OLED的玻璃和高指數層之間的介面製造緩衝，例如藉低指數透明基材之蝕刻或重疊)，提高光之外偶合。
因為位於OLED基材和TCL之間，所以這些萃取方式二者通常被稱為“內部萃取層(IEL)”。
外部萃取層(EEL)，亦為此技術中習知者，以類似方式工作，但位於玻璃/空氣邊界。
在內部萃取層(IEL)領域中，本發明具有含氣泡之透明的高指數玻璃基板作為低指數擴散元件。此具有光擴散氣泡的IEL優於類似之具固態粒子的IEL的原因在於沒有大尺寸粒子自基質突出及在最終OLED產物中形成短路和/或內部電極漏電的風險。
但是，儘管沒有固態粒子存在，藉由簡單地將高指數玻璃料熔於低指數玻璃基材上，不易得到具有完美表面品質的擴散性琺瑯。事實上，在熔化步驟期間內形成的氣泡和在熔融基質中捕集的氣泡朝向表面上升，於此處破裂和整平。但是開啟或部分開啟氣泡，在完全整平之前於IEL表面處固化，製造似火山口的表面不規則性，其具有較尖銳的邊緣並導致內部電極漏電及最終OLED中的針孔。
EP 2 178 343 B1揭示用於具有內部萃取層(散射層)之OLED的半透明玻璃基材，其包含高指數玻璃基質和氣泡散射元件。根據此文件，因為開放的氣泡火山口，所以散射層表面沒有表面缺陷(參照[0026]至[0028]，和圖55)。但是，此文件且特別是[0202]的詳盡分析指出，此結果只是計算較低表層中的散射元件之不適切方法的人為因素所致。
申請人近期提出申請的南韓專利申請案第10-2013-0084314號(2013年7月17日)，在本申請案提出申請之前尚未發佈，揭示用於發光裝置的積層基材，其具有高度內聯的空隙系統位於介於低指數玻璃基材和高指數琺瑯之間的介面處。此散射層具有極高表面品質及低於0.1/cm2的開放氣泡密度，但有著與積層基材邊緣接觸的水或其他流體經由內聯空隙滲出於大面積的積層物上及，經由針孔，滲入有機層與螢光或磷光染料的堆疊物中，造成破壞該層的疑慮。
因此，有利地，提出用於OLED的積層基材，其類似於Saint-Gobain Glass France於2013年7月17日提出申請的南韓專利申請案第10-2013-0084314號中所描述者，其中在高指數琺瑯/玻璃基材層處內聯的空隙系統被彼此未連接的多個個別氣泡所取代並黏於該介面，基本上未上升至熔融高指數玻璃料表面。
申請人訝異地發現到，當施用玻璃料且其熔化未直接與玻璃基材接觸而是在事先塗覆於該玻璃表面上的薄金屬氧化物層上時，在熔融高指數玻璃料的較低層中形成大量的個別氣泡，黏於位於下方的玻璃基材，基本上未上升至表面。
本申請案之標的係製造用於發光裝置之積層基材之方法，其至少包含以下四個步驟：(a)提供折射指數(λ=550nm處)介於1.45和1.65之間的玻璃基材，(b)將金屬氧化物層塗覆在玻璃基材的一面上，(c)將折射指數(λ=550nm處)至少1.7的玻璃料(glass frit)塗覆在該金屬氧化物層上，(d)所得經塗覆的玻璃基材於高於玻璃料的Littleton的溫度燒製，藉此使得金屬氧化物與熔融玻璃料反應並形成高指數琺瑯層，該層具有多個球狀空隙埋在琺瑯層之接近與玻璃基材之介面處之較低部分中。
本申請案的另一標的係藉以上方法可得的積層基材，該積層物包含(i)具有折射指數介於1.45和1.65之間的玻璃基材，(ii)高指數玻璃琺瑯層，其折射指數(550nm處)至少1.7，其特徵在於多個球狀空隙埋在高指數琺瑯層之接近琺瑯層與位於下方的玻璃基材的介面處，至少95%、較佳地至少99%、更佳地基本上所有的球狀空隙所具有的直徑明顯小於琺瑯層的一半厚度且位於高指數琺瑯層之接近與位於下方的玻璃基材的介面之下半部。
步驟(a)中提出的玻璃基材係礦物玻璃(例如鈉鈣玻璃)之扁平的半透明或透明基材，其通常具有介於0.1和5mm之間、較佳介於0.3和1.6mm之間的厚度。其透光率(ISO9050標準，illuminant D65(TLD)，如ISO/IEC 10526標準之定義，考慮ISO/IEC 10527定義的標準色度觀察CIE 1931)較佳地儘量高且基本上高於80%、較佳地高於85%或甚至高於90%。
本發明之方法的步驟(b)中，藉任何適當方法，金屬氧化物薄層塗覆於扁平玻璃積材的一面上，較佳地藉反應性或非反應性磁控管濺射、原子層澱積(ALD)或溶膠潤濕塗覆。該金屬氧化物層可覆蓋玻璃基材一面的全表面。替代的具體實施例中，基材的僅部分表面經金屬氧化物層塗覆。特別感興趣的是以圖案化的金屬氧化物層塗
覆基材，以製備具有非均勻萃取圖案的最終積層基材。
不希望被任何理論所限，申請人認為在燒製步驟(d)期間內，藉介於金屬氧化物和覆蓋的高指數玻璃料之間的反應生成光散射球狀空隙。尚未完全闡釋該反應的特定本質。認為O2氣體被含括作為反應產物。大部分的球狀空隙並非只是在熔化-固化步驟期間內埋在玻璃料中的氣泡，此如EP 2 178 343 B1中所述者，而是在燒製步驟期間內生成的氣泡。
事實上，申請人觀察發現，相較於玻璃料層直接塗覆在裸露的玻璃基材上的區域，在玻璃料層塗覆於金屬氧化物層上的區域中之球狀空隙的密度明顯較高。
對於金屬氧化物層的厚度沒有特定限制，只要其提供足夠的反應性組份以在所得琺瑯的下半部中生成大量球狀空隙即可。幾奈米的金屬氧化物層只能夠驅動所欲球狀空隙之形成。
金屬氧化物層較佳地具有介於5和80nm之間、更佳地介於10和40nm之間，且又更佳地介於15和30nm之間的厚度。
本申請案提出申請的同時，申請人以實驗顯示至少三種金屬氧化物，即，TiO2、Al2O3、ZrO2，導致形成接近玻璃料介面的球狀空隙。嫻於此技術者，未背離本發明之精神，可輕易地以不同的金屬氧化物(如Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3和SnO2或其混合物)代替這些金屬氧化物，以完成申請人的實驗操作及發現額
外的金屬氧化物適用於本發明之方法。
因此，金屬氧化物較佳地選自TiO2、Al2O3、ZrO2、Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3和SnO2和其混合物。
帶有圖案化或非圖案化薄金屬氧化物層的玻璃基材面接著以高指數玻璃料塗覆。
該玻璃料的折射指數較佳地介於1.70和2.20之間、更佳地介於1.80和2.10之間。
高指數玻璃料有利地包含至少30重量%、較佳地至少50重量%且更佳地至少60重量%的Bi2O3。
可選擇玻璃料，以具有介於450℃和570℃之間的熔點(Littleton點)及應使得得到的琺瑯具有1.8至2.1的折射指數。
較佳玻璃料具有以下組成：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%
典型的具體實施例中，玻璃料粒子(70-80重量%)與20-30重量%的有機媒質(乙基纖維素和有機溶劑)
混合。藉網版印刷或縫隙模具塗覆，所得玻璃粒膏之後施用在經金屬氧化物塗覆的玻璃基材上。所得層藉由在120-200℃的溫度加熱而乾燥。有機黏合劑(乙基纖維素)於介於350-440℃之間的溫度燒除，燒製步驟，即，高指數玻璃料之熔化，得到最終琺瑯，此於介於530℃和620℃之間、較佳地介於540℃和600℃之間的溫度進行。
所得琺瑯具有算術平均偏差Ra(ISO 4287)低於3nm的表面糙度，此藉AFM在10μm×10μm的區域上測得。
塗覆在金屬氧化物層上之高指數玻璃料的量通常介於20和200g/m2之間、較佳地介於25和150g/m2之間、更佳地介於30和100g/m2之間、且最佳地介於35和70g/m2之間。
在燒製步驟(d)中，玻璃料受熱至高於玻璃料的Littleton溫度，造成玻璃料熔化，玻璃料的組份與位於下方的金屬氧化物的組份反應，在反應區形成球狀空隙。在最終固化的琺瑯塗層中，通常無法清楚地區分原始金屬氧化物層和玻璃料層。最可能地，金屬氧化物層與玻璃料熔合，局部形成組成略為不同的玻璃料。因此，無法指定這兩層的各自厚度。包含多個球狀空隙(散射元件)埋於其中之固化的琺瑯層(下文中稱為“高指數琺瑯層”)的總厚度較佳地介於3μm和25μm之間、更佳地介於4μm和20μm之間且最佳地介於5μm和15μm之間。
本發明之最令人訝異的特點之一係觀察發現
在燒製期間內形成於玻璃料層(與金屬氧化物之反應區)底部的氣泡不會在熔融玻璃相中朝向其表面上升，而是維持於相當接近介於所得琺瑯和位於下方的玻璃基材之間的介面之處。散射元件的“維持於下方”使得固化的高指數琺瑯具極佳的表面品質，沒有因為固化的開口氣泡而形成之似火山口的凹陷。
為有效地維持球狀空隙接近高指數琺瑯層底部及防止其上升至表面，步驟(d)的燒製溫度不應過高且燒製步驟的期間不應過長。
燒製步驟(d)的期間較佳地介於3和30分鐘之間、更佳地介於5和20分鐘之間。
無須贅言，本發明中使用的高指數玻璃料和自彼得到的琺瑯應較佳地實質上無固態散射粒子(如晶狀SiO2或TiO2粒子)。此粒子常作為內部萃取層的散射元件，但須要額外的平面化層，因此，所不欲地提高萃取層的總厚度。
如以上已解釋者，在燒製步驟期間內形成的球狀空隙非隨機地遍佈於高指數琺瑯層的厚度，而是主要位於“下”半部，即，接近該琺瑯層與位於下方的玻璃基材的介面處。為完全埋在琺瑯層中，球狀空隙當然必須比琺瑯層的厚度小得多。至少95%、較佳地至少99%、且更佳地基本上所有的球狀空隙所具有的直徑小於琺瑯層的一半厚度且位於高指數琺瑯層之接近與位於下方的玻璃基材之介面的下半部。“位於高指數琺瑯層的下半部”是指至少
80%的空隙體積位於琺瑯層中間平面的下方。
球狀空隙所具有的平均等效球直徑(average equivalent spherical diameter)介於0.2μm和8μm之間、較佳地介於0.4μm和4μm之間、更佳地介於0.5μm和3μm之間。
球狀空隙隨機地分佈在對應於事先經金屬氧化物層塗覆之玻璃基材表面的全區域上。為有效地散射自含有螢光或磷光染料的有機層的堆疊物發出的光，球狀空隙的密度較佳地介於104和25.106/mm2之間、更佳地介於105和5.106/mm2之間。
就垂直於基材之任意平面的方向觀之(投射圖)，球狀空隙較佳地佔據事先經金屬氧化物層塗覆之基材之至少20%、更佳地至少25%的表面及最多80%、更佳地最多70%的表面。
如可由出示根據本發明之積層基材的截面之圖2見到者，幾乎所有的球狀空隙與位於下方的玻璃基材接觸，藉此形成與該玻璃基材接觸之個別空隙的單層。該空隙可以彼此非常接近或甚至彼此接觸但未彼此連接。藉此有效地阻礙流體(如水或其他溶劑)以液體或氣體形式滲出，因此有效地阻礙自本發明的積層基材周圍進入。自本發明之積層基材製造的OLED因此對於水或溶劑的敏感度遠不及南韓專利申請案第10-2013-0084314中描述的積層基材。
本發明之積層基材可作為製造底部發射的
OLED的半透明基材。底部發射OLED包含帶有半透明電極(通常是陽極)的半透明基材、和光反射電極(通常是陰極)。自發光有機層的堆疊物發射的光係直接經由半透明陽極和基材發射或先藉陰極朝向和通過半透明的陽極和基材反射。
發光有機層堆疊物積層之前，透明導電層(電極層)必須因此塗覆在內部萃取層頂部上。較佳具體實施例中，本發明之積層基材因此進一步包含在高指數琺瑯層上的透明導電層，此導電層較佳地直接與琺瑯層接觸或塗覆在中間層(例如阻擋層或保護層)上。
較佳具體實施例中，本發明之方法此進一步包含將透明的導電層(TCL)塗覆於高指數琺瑯層上的額外步驟。此層較佳地為透明的導電氧化物，如ITO(氧化銦錫)。此TCL之形成可以根據嫻於此技術者熟知的慣用方法(如磁控管濺射)進行。
1‧‧‧玻璃基材
2‧‧‧金屬氧化物層
3‧‧‧玻璃料
4‧‧‧高折射琺瑯層
5‧‧‧球狀空隙
6‧‧‧透明導電層
圖1係流程圖，出示製造本發明之積層基材之方法。
圖2係掃描電子顯微(SEM)照片，出示根據本發明之積層基材的截面圖。
圖3出示根據本發明之以上實例1、2和3各者的投射圖(左)和截面圖(右)。
圖1中，步驟(a)中先施用扁平的透明玻璃基材1。步驟(b)中，接著藉磁控管濺射，將金屬氧化物層2塗覆在此基材的一面上。下一步驟(步驟(c))中，施用高指數玻璃料層3，此例如藉網版印刷包括玻璃料和有機介質(聚合物和有機溶劑)的膏進行。
所得帶有金屬氧化物層2和玻璃膏層3的基材之後在步驟(d)中逐步加熱以先蒸發有機溶劑，之後燒除有機聚合物及最終熔合玻璃料粉末，以得到高指數琺瑯層4。在此最終加熱步驟期間內，自介於金屬氧化物和玻璃料之間的反應，在玻璃料層底部形成球狀空隙5。球狀空隙黏在高指數琺瑯4介面且不會上升至琺瑯層表面。之後，在步驟(e)中，將透明的導電層6塗覆於高指數琺瑯4的平坦表面上。
在圖2的SEM照片上，深灰色玻璃基材被淡灰色的高指數琺瑯層所覆蓋。單層球狀空隙完全埋於其中且位於與介於玻璃基材和覆於其上的琺瑯之間的介面接觸之處。所示積層基材尚未包含透明導電層。可看出高指數琺瑯層表面完美地平整且沒有似火山口的表面不規則性。
0.7mm鈉鈣玻璃片經TiO2先質溶液旋塗。經塗覆的玻璃片之後於150℃的溫度處理10分鐘以蒸發溶劑，及之後於約400℃的溫度1小時以使得TiO2層緻密
化。
所得經TiO2塗覆的玻璃片以包含75重量%的高指數玻璃料(Bi2O3-B2O3-ZnO-SiO2)和25重量%的有機介質(甲基纖維素和有機溶劑)的膏進行網版印刷並進行乾燥步驟(於150℃ 10分鐘)。
之後，基材於570℃燒製約10分鐘，得到含有多個球狀空隙的高指數琺瑯層(12μm)。
藉TiO2層厚度提高的三個不同樣品的影像分析，測定球狀空隙的平均尺寸和覆蓋率(被球狀空隙佔據之經TiO2塗覆的表面區域)。
以下表出示球狀空隙的平均尺寸、覆蓋率、和所得基材的濁度比，此以提高量的TiO2與將高指數玻璃料直接塗覆在鈉鈣玻璃上的負對照組作比較。
負對照組的高指數琺瑯層沒有球狀空隙位於琺瑯層底部。
提高金屬氧化物的量造成在玻璃/琺瑯介面處形成的球狀空隙的平均尺寸、空隙佔據的區域和所得IEL層的濁度比提高。
這些實驗數據清楚指出，在琺瑯層底部的球狀空隙源自於金屬氧化物層與覆蓋於其上的高指數玻璃料
之交互作用。
圖3出示根據本發明之以上實例1、2和3各者的投射圖(左)和截面圖(右)。
Claims (14)
- 一種製備用於發光裝置之積層基材之方法，其至少包含以下步驟：(a)提供於550nm的折射指數介於1.45和1.65之間的玻璃基材(1)，(b)將金屬氧化物層(2)塗覆在玻璃基材的一面上，該金屬氧化物選自TiO2、Al2O3、ZrO2、Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3和SnO2和彼等之混合物，(c)將於550nm的折射指數至少1.7的玻璃料(glass frit)(3)塗覆在該金屬氧化物層(2)上，該玻璃料包含至少30重量%的Bi2O3，(d)所得經塗覆的玻璃基材於介於530℃和620℃之間的溫度燒製，藉此使得金屬氧化物與熔融玻璃料反應並形成高指數琺瑯層(4)，該層具有多個球狀空隙(5)埋在琺瑯層之接近與玻璃基材之介面處之較低部分中。
- 如申請專利範圍第1項之方法，其中該金屬氧化物層具有介於5和80nm之間的厚度。
- 如申請專利範圍第1項之方法，其中該玻璃料的折射指數介於1.70和2.20之間。
- 如申請專利範圍第1項之方法，其中該玻璃料包含至少50重量%的Bi2O3。
- 如申請專利範圍第1項之方法，其中該玻璃料包含至少60重量%的Bi2O3。
- 如申請專利範圍第1項之方法，其中該高指數玻璃料之熔化(fusing)係於介於540℃和600℃之間的溫度進行。
- 如申請專利範圍第1項之方法，其進一步包含(e)將透明的導電層(TCL)塗覆於高指數琺瑯層(4)上。
- 一種可藉申請專利範圍第1至7項中任一項之方法得到的積層基材，其包含：(i)具有折射指數介於1.45和1.65之間的玻璃基材(1)，(ii)高指數玻璃琺瑯層(4)，其包含至少30重量%的Bi2O3且於550nm的折射指數至少1.7，其特徵在於多個球狀空隙(5)埋在高指數琺瑯層之接近琺瑯層與位於下方的玻璃基材的介面處，至少95%的球狀空隙所具有的直徑明顯小於琺瑯層的一半厚度且位於高指數琺瑯層之接近與位於下方的玻璃基材(1)的介面(7)之下半部且與位於下方的玻璃基材接觸。
- 如申請專利範圍第8項之積層基材，其中該球狀空隙所具有的平均等效球直徑(average equivalent spherical diameter)介於0.2μm和8μm之間。
- 如申請專利範圍第8項之積層基材，其中該高指數琺瑯層的厚度介於3μm和25μm之間。
- 如申請專利範圍第8項之積層基材，其中至少99%的球狀空隙所具有的直徑明顯小於琺瑯層的一半厚度。
- 如申請專利範圍第8項之積層基材，其中基本上所有的球狀空隙所具有的直徑明顯小於琺瑯層的一半厚度。
- 如申請專利範圍第8項之積層基材，其中該球狀空隙形成個別空隙單層，其與位於下方的玻璃基材(1)接觸。
- 如申請專利範圍第8項之積層基材，其進一步包含(iii)在高指數琺瑯層(4)上的透明導電層(6)。
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| EP2178343A1 (en) * | 2007-07-27 | 2010-04-21 | Asahi Glass Co., Ltd. | Translucent substrate, method for manufacturing the translucent substrate, organic led element and method for manufacturing the organic led element |
| US20110001159A1 (en) * | 2008-03-18 | 2011-01-06 | Asahi Glass Company, Limited | Substrate for electronic device, layered body for organic led element, method for manufacturing the same, organic led element, and method for manufacturing the same |
| US20120313134A1 (en) * | 2010-01-22 | 2012-12-13 | Saint-Gobain Glass France | Glass substrate coated with a high-index layer under an electrode coating, and organic light-emitting device comprising such a substrate |
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| WO2018032351A1 (en) * | 2016-08-16 | 2018-02-22 | Zhejiang Kaiying New Materials Co., Ltd. | Thick-film paste for front-side metallization in silicon solar cells |
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| EP2178343A1 (en) * | 2007-07-27 | 2010-04-21 | Asahi Glass Co., Ltd. | Translucent substrate, method for manufacturing the translucent substrate, organic led element and method for manufacturing the organic led element |
| US20110001159A1 (en) * | 2008-03-18 | 2011-01-06 | Asahi Glass Company, Limited | Substrate for electronic device, layered body for organic led element, method for manufacturing the same, organic led element, and method for manufacturing the same |
| US20120313134A1 (en) * | 2010-01-22 | 2012-12-13 | Saint-Gobain Glass France | Glass substrate coated with a high-index layer under an electrode coating, and organic light-emitting device comprising such a substrate |
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| WO2016008685A1 (en) | 2016-01-21 |
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| MY181429A (en) | 2020-12-21 |
| RU2017104776A3 (zh) | 2018-12-25 |
| EP2975008A1 (en) | 2016-01-20 |
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| CN106488893B (zh) | 2020-08-07 |
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| EP2975008B1 (en) | 2017-03-01 |
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