TW575699B - Low pressure vapor phase deposition of organic thin films - Google Patents

Low pressure vapor phase deposition of organic thin films Download PDF

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TW575699B
TW575699B TW87118943A TW87118943A TW575699B TW 575699 B TW575699 B TW 575699B TW 87118943 A TW87118943 A TW 87118943A TW 87118943 A TW87118943 A TW 87118943A TW 575699 B TW575699 B TW 575699B
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organic
film
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Stephen R Forrest
Paul E Burrows
Vladimir S Ban
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Univ Princeton
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45561—Gas plumbing upstream of the reaction chamber
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
    • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/321—Metal complexes comprising a group IIIA element, e.g. Tris (8-hydroxyquinoline) gallium [Gaq3]
    • H10K85/324—Metal complexes comprising a group IIIA element, e.g. Tris (8-hydroxyquinoline) gallium [Gaq3] comprising aluminium, e.g. Alq3
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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    • H10K85/631—Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine
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    • Y10S261/00—Gas and liquid contact apparatus
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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Electroluminescent Light Sources (AREA)
  • Physical Vapour Deposition (AREA)
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  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)

Description

575699 五、發明說明（l) ---------- 美國政府^^ 本發明係受1 _ τ Αη 果國政府貧助，合約號碼F49620 - 92- J-05 24(普妓甘6， 室）提休斯頓大學），由美國空軍〇SR(科技研究辦公 至 八’美國政府享有本發明之特定權利。 發明範圍 ^發明係關於光學品質薄膜之製造方法，特別是使用於 非線性光學裝置與有機光發射裝置之此種薄膜的低壓製造 方法。 JL明背景 、有機电％發光乃是迅速成長之技術，因被認為是具潛力 的顯不用裝置而受到激勵，有機光發射裝置（OLEDs)可達 到額外的3%量子效率，而且在視亮度下之使用壽命可達 1 0，〇 〇 〇小時之等級。目前已知有小分子與塑膠基材之 ^肋^兩者，但高分子基底之裝置具因使用旋轉沉積技術 =有簡單與廉價之優點，相較之下，通常使用真空熱蒸發 =製造小分子裝置，其製造成本比旋轉沉積技術為高， ED結構與製造技術於本文所參考之第㈣96/19?92號 利已有提供。 〜 有機蒸氣氣相沉積（0VPD)之使用已進步到用在許多且、、既 力的光電裝置如顯示裝置之小分子量有機層能夠低價^ 尺寸的沉積，0VPD方法如本文所參考之美國專利第、 5:‘5 54’220 號，由Forrest 等；S. R. F〇rrest 等所提出之 以有機蒸氣沉積生成的有機鹽薄膜之強化第二諧波生 〜長距結構次序” 68 Appl. Phys. Lett.i 326 ( 1 9 9 6 ).
苐4頁 575699 發明說明（2) —— 及P F r ^ · bUrrows等所提出之“有機蒸氣沉積：具高光學 、会性之有機薄膜生成之新方法，，156 j. 〇f crystal Growth 9 1 ( 1 9 9 5 )均有詳述。 結^PD方法使利用載體氣體傳送原材料至基材上，氣體凝 = 所要的薄膜，例如〇VPD技術已使用於光學非線性 (Das 鹽二+曱基礦酸4,-二曱基胺基-N-曱基-4—偶氮| & I由可蒸發之先驅物一碘化4,-二曱基胺基-N-曱基 im偶ί 4-(DASI)及對—甲苯石黃酸甲基酷（曱苯續酸酯、 n /、、二由載體氣體傳送至已加熱之基材上，此時， 解成4-二甲基胺基一4_偶氮基（DAS) ’隨後DAS與 MT反應而於基材上形成DAST。 由於可控制在極端不同的蒸-氣壓下材料的共沉積，〇vpD 1 ^為=精密化學計量生成多成分薄膜的唯一方法，然而 I成大i壓Γ實施0PVD方法，薄膜在大氣壓或近大氣壓下 ά a ’a因氣相成核作用與擴散限制生成製程而使得薄膜 較為粗糖並有不均句的表面形態。成-發明概沭 本發明提供一種在次大氣壓下於基材上生成一具有優異 、面（1貝之有機薄膜的方法與裝置，一方面，本發明包括 於,材上製備有機薄膜之方法，it匕方法包含以下步驟：提 二：ί有機先驅物，而先驅物為蒸氣相狀態；纟在次大氣 =/、子在有基材下多種先驅物發生反應而於基材上形成薄 ，一另一方面，本發明包含以此一方法所製成的薄膜，另 夕方面’本發明包含一用以促進在次大氣壓下有機先驅
575699
五、發明說明（3) 物之反應以於基材表面形成有機薄膜的裝置。 、本發明之一項優點為提供一可精確控制各成分含量之多 成分有機薄膜。 f發明之另一項優點為提供一具有平滑表面之均勻的有 壯本發月之另一項優點為提供低壓有機蒸氣相沉積方法與 衣置’用來生成有機光發射材料與光學非線性鹽之薄膜。 本發明之另一項優點為提供低壓有機分子束沉積方法與 裝置’用來形成有機光發射材料與光學非線性鹽之薄膜。 本發明尚有一項優點為提供一可於大型基材面積上形成 均勻的有機材料沉積之方法與裝置。 凰例說明 - 圖1為依據本發明具體實施例之LPOVPD反應室。 圖2為依據本發明具體實施例之〇MVD反應室。 圖3表示依據本發明具體實施例之連續式低壓基材沉積 有機材料之裝置。 。圖4A與4B分別為依據本發明具體實施例之反應氣體分散 斋的平面與剖面圖。 圖5為依據本發明具體實施例之滾輪基材搬送機構的侧
視圖。 詳述 本發明提供一種在次大氣壓下於基材上生成一具有優異 表面性質之有機薄膜的方法與裝置，本發明之此一方法稱 之為低壓有機蒸氣沉積（LPOVPD)，本發明之LPOVPD方法容
第6頁 575699 分有機薄膜 粗糙度之優 之具體實施 含反應室， 圓柱狀且有 長度為約45 或石英。— 置於圓管36 堝14直接置 上，掛禍1 4 器1 8來加熱 有機先驅物 氣流3 0流經 驅物蒸氣沿 性氣體如氮 特性之氣體 亦為惰性氣 過多反應物 槽2 4經由調 徑30與38， 器3 2、流量 此傳送至反 節器40、流 此傳送至其 的沉積，此 異表面性質 例的LPOVPD 如反應管1 2 適當的尺寸 公分，反應 内含第一有 内並放置在 於反應管1 2 利用緊密包 或冷卻，控 材料熱分解 圓管3 6並進 著反應管1 2 、氦、氬、 ，如氫、氨 體’使用此 會有額外的 節閥2 6傳送 並流入反應 計3 4以及快 應管1 2之一 量計4 2以及 中含有第二 反應室1 0 並伸入至 ，例如實 管1 2可使 機先驅物 接近反應 之上或置 圍在反應 制坩堝1 4 或昇華， 入反應室 流至排氣 氪、氤、 五、發明說明（4) 許精確控制多成 特性為如低表面 一依據本發明 示，反應室1 〇包 内，反應管1 2為 直徑為1 0公分、 適的材料如破璃 口容器如坩堝工4 端20。另外，掛 隔板或是圓管之 區域加熱/冷卻 坩堝1 4内的第一 之惰性載體氣體 ;的第-有機先 性载體氣體為惰 氣體，而具還原 有機材料而言 於燒除不兩 而要的 3性氣體從氣 至少兩個、土 t ^ ]调峨動路 3包含壓力調節 ，载體氣體每 Γ包含壓力調 ，栽體氣體經 外’本發明之薄膜 如圖1所 反應室 驗裝置之 用任何合 材料之開 管1 2的一 於其中的 管1 2之多 之溫度使 一受調節 内，所造 端2 2，惰 氖等一類 及曱烷等，對許多 類還原氣體通常對 幫助。 管件2 8，以傳送到 管1 2。一流動路徑 速切換閥3 5之系 2 0 ’另一流動路 快速切換閥3 9之系 有機先驅物材料48 575699 五、發明說明（5) ' --- 之起’包器4 6，為能幫助第二有機先驅物材料4 8之溫度控 制，將起泡器46部份浸入容器52内之液浴5〇中，來自氣槽 2 4之!^性氣體呈氣泡狀通過第二有機先驅物材料4 8後進入 反應吕1 2，在此一程序中，圓管54必須維持在足夠高的溫 度以避免已揮發之第二有機先驅物48在從起泡器流至 室時再次凝結。 ~ 、任=進入反應管12之先驅物的量藉由製程參數如溫度、 載體氣體之流量以及反應物之溫度來控制，Lp〇vpD方法使 兩壓力質量流量控制器提供精確計量，不受先驅物的墓氣 壓與化學物性所影響，因此本方法容許根據所生產的薄膜 所需要比例之特性差異明顯之材料組合。 先驅物氣流利用快速切換閥3 5與3 9可幾乎立即開與關， 此類閥導引先驅物氣流至反應室1 2或至旁通線（未顯示）， 所以在任意時間内，可將不同的先驅物氣流輪入反應管工2 以得到不同組成與特性，閥39調節載體氣體流入起泡器46 的量，閥3 5與3 9容許快速變換進入反應管1 2之反應物:以 變換所生成薄膜之物性與組成，例如，可生成Α β A B、 ABCABC、ABABCAB與ABCDABCD-型態之薄膜，其中各字母代 表不同的分子層或組成。 真空泵66與控制節流閥68在排氣口 62處連接至反靡室 1 〇，大部份有機蒸氣並不沉積於基材5 8，而是；疑、纟士於安置 在真空泵66上游之捕集阱64，捕集阱64包含如液鮮氣或天 然氟碳油，節流閥68調節反應室1 〇的壓力，合適^ ^力計 連接至反應室，此壓力計附有電子回饋來控制節流闊6 8 ^
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575699 五、發明說明（7) 堝14、14N在反應管12内可以隔板或圓管方式垂直堆疊來 處理額外的先驅物，根據欲沉積之有機薄膜，可單獨使用 一個或多個流通路徑3 0、3 8或其任何組合，來提供必需的 先驅物材料。 本發明之方法可用來由蒸氣先驅物反應而沉積許多不同 的有機薄膜，其中，“反應”認定為先驅物反應物形成不 同的反應產物，或亦可認為先驅物材料形成供給者一受體 或賓一主關係。例如，根據本發明，用表列的先驅物之反 應而形成下列NL 0材料之薄膜： 薄膜材料 第一先驅物 第二先驅物 甲苯磺酸45-二甲基胺基-N-甲基-4-偶氮：|(DAST) 4’- _^甲基胺基-4-偶氮 fe(DAS) - 甲基偶氮i(MT) 甲烷磺酸4’-二甲基胺基-4-甲基偶氮fe(DASM) 甲烷磺酸甲基酯(MM) 4，-二甲基胺基-4-偶氮4 (DAS) 三氟曱院磺酸4’-二甲基胺 基-4-甲基偶MS:(DASM) 三氟甲烷磺酸甲基酯 (MfM) 4，-二甲基胺基-4-偶氮fe (DAS) 甲苯磺酸4’-二甲基胺基-N-甲基-4-偶氮ft(DAST) 甲基偶氮fc(MT) 硫酚4’-二甲基胺基-4-甲 基偶氮氐(DASTh) 甲苯磺酸4’-甲氧基-4-甲 基偶氮S(MeOST) 甲基偶氮&(ΜΤ) 4，-甲氧基斗甲基偶氮fe (MeOS) 甲苯磺酸4’-二甲基胺基-N-甲基-4-偶氮 fi：(DAST) 甲基偶氮&MT) 碘化4’-二甲基胺基-4-甲 基偶氮 i(DAS(Et)I) 甲苯磺酸4’-二甲基胺基-N-甲基-4-偶氮£(DAST) 甲基偶氮：fe(MT) 氫氧化4’-二甲基胺基-4-甲基偶氮 l：(DAS(Et)OH) 甲苯磺酸4’-二甲基胺基-4-乙醯偶氮S：(DAAST) 乙醯偶氮έ(ΑΤ) 4’-—•甲基胺基-4-偶氮έ (DAS) 三氟乙酸二甲基胺基-4-乙醯偶氮fe(DASAf) 三氟甲烷磺酸甲基酯 (MAf) 4’-二甲基胺基-4-偶氮:| (DAS)
第10頁 575699 五、發明說明（8) 在另一與用來製造OLED之光發射材料較為相 中，先驅物係由如 tetrathlsferlvalene(TFF)^7^列 (卿所組成’經混合後形成沉積又 材上的电何轉移錯合物丁 TF—TCNQ。4 一（二二、基 ^基胺基苯乙稀基）—I咲。南（4加至高流甲吾 ίϋ二人ΐ 的客體分子稀釋於主體基質分子中以 形成早一冷光層，其他客體分子範5 基-21Η，23Η-卩卜吩（τρρ)、紅螢稀、dcm2、豆辛^四本 :…推雜物至單-基質達成有效的多色變=做Π c" ιιϋ中’雙層光發射袭置係由電洞傳送層 # Α α-4,4,-雙“-(卜聯苯基）-Ν-苯基-胺基] ^本基^ ^-NPD)或MTDATA，積層於光發射層（"EL")如 力隹^也1本基雙—（8_羥基4啉）鋁（（AlQ2)，-0Ph)或其已摻 ^的組合之上所構成，HTL與EL兩者輪流生成至所要的厚 再於該有機層上生成附加層或使用如三甲基銦、 二曱基鎵寺類之有機金屬源金屬接觸層。 柄Ϊ ί Ϊ L所不之裝置與方法，本發明包含-如圖2所示之 二 μ至7〇 ’反應室70包含一已修改之超高真空室71與 允—J輪(未顯示）之真空泵連接至閥72，典型的真 ^ ^ ^至壓1〇δ—1 0_U，使用反應室7 0沉積有機層 nMvt王稱為有機分子束蒸氣沉積（0MVD)，雖SLP0VPD與 均使用次大氣壓來沉積有機層，其主要的不同點為後
575699 五、發明說明（9) 者’分子平均自由經相冬 之下，LPOVPD之平均Π大於反應室70的尺寸，相較 容許從注入器形L = t於氣體反應室尺寸，0_ 备&丄 円扣向性分子“束”至基材，而可精密 動悲控刮成獏的膜厚、純度盘型皞。 上來盛Ϊ第一先驅物75之起泡器74，起泡器74置於 $二…、、’亚次、:包在溫度控制液浴80中。高純度惰性載體 7' = # ί /包通過第—先驅物7 5並帶走個別蒸氣經過加熱管 進入真空室71。在真空室η内，先驅物 制如Α卻Γ| ^而撞擊基材8 5，基材8 5則為附有溫度控 釗如冷部劑入口 8 1的方式。 I Ϊ =二71 I選擇性地附加至少一個納得生（Knudsen)或 1 ” 含有第二先驅物88，κ—元件86為一均勻加熱 熱爐兩來在真空下滲透蒸發物，例如，加熱K- 則以八ίL解DASI或其他先驅物並昇華生成的das，而das 僅简：…”方式注入反應室7〇 ’另夕卜，K—元件86亦可 進入？ΠΪ氣口以稀釋分子物種因加熱而昇華或蒸發 κ |ρ之/辰又此稀釋程序對於如藉由控制液浴8 0與 —^件86的溫度以及載體氣體78至起泡器74的〇^1 〜主糸統特別有甩。 43 3 始4二θ日體3來監視，旋轉試樣承載器90以確保先驅物的 ‘ 1st Ϊ與反應，先驅物材料之沉積進一步藉由可遮斷分 子束83與89之快門87來控制。
575699 五、發明說明（10) 反應室7 0可u 1 7 1之壓力以、、^擇性地包含冷卻遮罩9 1來協助維持真空室 、& 1減夕先驅物材料之再蒸發，而較佳為包含隔板 y z以避免先驅你从 — 初材枓移動而彼此污染。 、* f f至7〇可加裝許多如圖1所示之LP0VPD反應室的如快 、 、閥 方通官線等類之相同附件，反應室7 0可裝設多 :元件與起泡器以用來於基材85上沉積多種先驅物材 二.至7 〇争乂佳為包含一試樣裝填用之“裝載閘，，9 4， 之‘力門95與真空泵96，以避免換料時造成真空室 、〃圖1之裝置可選擇性修改為可於大面積基材表面上連續 =積有機層，如圖3之範例說明，圖3之裝置包含多個真空 室如裝填室146、有機層沉積室150與152、接觸沉積室154 =及卸載室1 56。舉例來說，各沉積室為圖1之LPOVPD反應 至10 ’基材137以輪送帶148傳送，經過處理室15〇、152、 154與156，在圖3之具體實施例中，處理室15〇、152、與 U4分別包含輻射加熱源158、16〇與162以避免有機蒸氣的 凝結，雖然在圖3中只有2個有機層沉積室丨5 〇與丨5 2，但可 視需求加入額外的沉積室。在由裝填室丨46傳送至有機層 >儿積室1 5 0與1 5 2以及由接觸沉積室1 5 4傳送至卸載室1 5 6 時，基材1 3 7會先經過氣閉鎖（未顯示）以避免提昇沉積室 150、1 52與1 54的真空度。而關於〇LED的範例中，沉積室 150與1 52分別用來沉積TPd與Ah，沉積室154則用來沉^ Mg : Ag接點層。 、 圖3範例之沉積室150、152與丨54分別包含一沉積有機先
第13頁 575699 五、發明說明（11)
"用之反應物氣體分散器（RGD)108，如圖4A與4B之詳 ^ RGD 108為圖1與圖2之有機先驅物傳送機構的另一種 '兩來提供氣幕UO'UO, 、120，，與 120，，，，RGD 108可確保多曹女地& … 有機先驅物之沉積，有機先驅物在維持分 人 /1"積於各許發生反應之基材上，RGD 108包 含加執哭1 ? 9° 第二載體氣體進氣口 112與氣體歧管132， 口二器122避免有機先驅物材料的過早凝結，rgd ι〇8之上 二弟一載體氣體進氣口 114與分散板11()，第一載體氣體進 =口1j 4供應载有具低揮發性如MT之第一有機先驅物的氣 _’、第一載體氣體經由分散板丨丨〇進入反應室内，分散板 11 〇為如網目、、破璃填充材料或孔狀不鏽鋼板，流經分散 板110 =氣流被RGD 108所遮蔽，RGD 108使具低蒸氣壓如 DAS之第二有機先驅物的氣體成一平面氣幕120，含有第二 有機先驅物的第二載體氣體於進氣口 112進氣並導向氣體 歧管132，氣體歧管132為一空心管，具有一排孔13，，用 ^供給第二載體氣體至環繞於氣體歧管132之環狀穴126， 第二載體氣體經由細縫丨36離開RGD 1〇8，而形成平面氣幕 的形狀。 氣幕120由TPD蒸氣所構成，氣幕丨2〇，由Uq3蒸氣所構成 以及，氣幕120’’由可產生導電表面如聚咯或有機金屬化 合物所構成’如果需要的話，控制或調節0LED之發光顏色 可由沉積室1 52之額外的RGI)裝置1〇8產生摻雜物蒸氣的氣 幕1 20’ ’ ’來調整A1 q3層的合適摻雜量。 圖1、圖2或圖3之裝置可使用一“滾輪—至_滾輪，，基材
第14頁 575699 五、發明說明（12) 傳送系統來選擇性地修改，如圖5所千 一 統適合於大面積、彈性基材上沉積有、\圖5所示之傳送系 ⑽以高分子板或金屬薄片製成，並有由機/膜如基枓 182，於基材180上之有機先驅物沉^由凌輪“I傳，至滚輪 1 80脫離滾輪丨8 i而暴露於圖i之反應' 77別發曰生於/基材 圖3之分子束或氣幕，;袞輪181與18;用^ J 圖2與 =黑動，如變速馬達，基材180由滚輪181傳送至滾輪f f 的速度代表形成於基材180上的有機薄膜之膜厚。 明本發明進一步參照下列不受此限之範例來做進一步的說 範例1 使用圖1之裝置，有機光發射材料層生成於已預塗 化銦錫（ITO)透明層之玻璃與彈性聚酯基材，ιτ〇形成裳乳 之電極，其厚度分別為玻璃的1 7 0 0埃以及聚§旨的1 2 0 0 ^罝 :得之電極阻抗分別為10Ω與60Ω，玻璃基材以清潔劑邀 去離子水之溶液於超音波槽浴中清洗，再以hl，卜三氣/甲 烷做蒸浴，接著以丙酮沖洗，最後以異丙醇沖洗。為避免 暴露於有機溶劑所造成的損傷，彈性基材僅以清潔劑與里 丙醇沖洗。 、
玻璃基材置於反應管1 2内溫度為接近220它的位置，第 層 >儿積於I T 0表面的是電洞傳送材料τ p d，特定地，τ p d 蒸氣藉由氮氣載體氣體從掛禍14載送至基材a，tpd生成 條件包含：源頭溫度為2 〇 〇 ± 5。(：，氮氣載體氣體流量為 lOOsccm，反應室壓力為0· 50托與生成時間為2〇分鐘。氮
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氣載體氣體流量為lOOsccm時，其系統雷諾數為〜5〇()， 不刼作是在層流區域，TPD層生成之厚度介於丨⑽_3⑽埃 产沉積之後，降低接近TPD掛堝的溫度，並關閉相關的、。 彳，九流，接著藉由打開分離的氮氣管線將蒸氣由掛瑪 14N二入至反應室12内以生成電子傳送層—，ai 件包含：源頭溫度為247 ±8t，氮氣載體氣體流量為条 5〇sccm，反應至壓力為0.65托與生成時間為1〇分鐘，在h 積TPD與Alqs二者時，使用水冷不鏽鋼基材承載器來維匕 基材贩度為15C，AlQ3層生成之厚度介於7〇〇 — η〇〇埃。 沉積ΑΙΑ層後，基材移出反應室並以熱蒸鍍一Mg:Ag丁貝 部接點，再蒸鍍一 1 0 0 0埃之保護金層而完成。 於沉積時使用低壓可使有機層具平滑且均勻的表面， 如，TPD與A1Q3層以原子力顯微鏡測量，其RMS粗糙度分 為6-8埃與9-1丨埃，所製成的叽肋裝置具有一電流—電壓 特性，其中於低電壓時I(XV，於高電壓時1工”，而[與^關 係之功率定律變化的開啟電壓VT為約6 V。 範例2 使用圖1之裝置製造一NL0膜，MT48導入至3〇立方公分之 起泡器46，其溫度藉由矽油浴5〇維持在接近8〇。—1〇〇它， 使用II氣中產生氣泡’目而載送MT蒸氣經由玻璃管 進入反應管12内含有置於反應管12底部的msi之坩堝14 丽接，近5公分^位置，反應管12的壓力維持在約1〇_2托， MS瘵氣與MT瘵氣反應而於基材58上形成MST之固體薄 膜基材5 8則以基材底板6 〇支撐著，過剩未反應之mt蒸氣
575699 五、發明說明（14) 則由排氣管62排出，因而形成DAST膜，可以用於如井與 關之上。 、予開 本發明使用低壓沉積技術來製造具優異表面性質與精 組成之有機薄膜，雖然本發明的許多具體實施例於文^， 述，但並不受具體實施例所限，例如對熟知此項技菽 # 對具體實施例思考出修改，但仍為本發明之申嗜直 ^ 明号刊部If] 的精神與想法所涵蓋。 111 本發明與下列專利共同申請專利：“高可靠性、高效 率、整合有機光發射裝置與其製備方法”，序I ·· n > 0 8/774, 1 1 9 (專利日期·· 1 99 6年12月23日）；“多色LEd 新材料”，序號：08/85 0, 2 64 (專利日期：1997年5月2之 曰）；“以有機自由基為基礎之電子傳送與光發射層”， 序號：08/7 7 4, 1 20 (專利日期：！ 9 9 6年12月23日）· ‘‘夕^ 顯示裝置]，序號：08/ 772,333 (專利日期：1 9 9 6年12夕月巴 23曰），紅色發光有機光發射裝置（LED)，，，序贫. 〇8/774,〇87(專利日期：1 99 6年12月23日）；“堆^有 發射裝置用驅動電路”，序號：08/ 792, 05 0 (專利i日期： Π 9 7年2月3曰）’高效率有機光發射裝置結構，，，序 號：08/7 72, 3 32 (專利曰期：1 9 9 6年12月23 積、非高分子彈性有機光發射裝置”， 9,319(專利日期：1 9 9 7 y月23日）二‘且 年2月3日“谁田士序遽 ，（專利日期：1997 年2月3曰），堆贅有機光發射裝置，，，序铁· 0 8/ 792,046 (專利日期· 1(^7主9 曰q m 』· 1997年2月3曰）；“高對比透明有
575699 五、發明說明（15) 機光發射裝置顯示器，，，序號：〇8/821，38 0 (專利日期： 1 9 9 7年3月2 0日）；“含有5 ~羥基—啉之金屬錯合物為基 質材料之有機光發射裝置”，序號：08/838, 0 9 9 (專利曰 期·· 1 9 97年8月1 5日）；“具高亮度之光發射裝置”，序 號：0 8 /844, 3 53 (專利日期：1 9 9 7年4月18日）；“有機半 導體雷射’序號：60/046,061(專利日期：1997年5月9 曰）；“有機半導體雷射”，序號：〇 8/859,468 (專利曰 期·· 1 9 9 7年5月1 9曰）；“飽和全彩堆疊有機光發射裝 置’序號：08/858,994(專利日期：1997年5月20日）； 含有電洞射入強化層之有機光發射裝置”，序號·· 08/865,491(專利日期：1997年5月29日）；“導電層之電 漿處理”，序號：PCT/US97 / 1 0 2 52 (專利日期：1 9 9 7年6月 1 2曰；“製造有機多彩顯示裝置之薄膜，，專利申請中，序 號·Ρ(：Τ/υ897/1〇289(專利日期·· 1997 年 6 月 12 曰）；“雙 異種結構紅外線與縱向孔表面發射有機雷射，，，序號： 6 0/ 0 5 3, 1 7 6 (專利日期：1 9 9 7年7月18日）；“含有熱安定 非對稱電荷載體材料之0LED ” ，序號：08/9^,029(專利 日期：199,7年9月8日）；“0LED之堆疊與螢光轉換器之光 毛射裝‘置’序就· 〇 8 / 9 2 5，4 0 3 (專利日期：1 9 9 7年9月9 曰），有機光發射裝置之沉積氧化銦錫層之改良方法，， ，序號· 08/928,800(專利日期：1997年9月12日）； “OLED之發光層中之阿内酯相關摻雜物，，，序號： 0 8/ 948, 1 3 0 (專利曰期：1 9 9 7年1〇月9曰）；“使用非金屬 陰極之高透過有機光發射裝置，，，（專利日期·· 1 9 9 7年11 575699 五、發明說明（16)
月3日），代理人列表绝 金屬陰極之高透過有乂°°20/4°(暫f以及“使用非 、、有機先發射裝置，，，（專利日期：丨9 97 年月5日），代理人列表編號：j 〇〇2〇/44，各共同申請專 利案之王文於本文中列為參考，所提出之發明與案美國專 利第08/354, 674 、 08/613,207 、 08/632, 322 與08/693, 359 號以及暫定第60/010,013 、60/024,001 、60/025,501 號共 同申請專利，各共同申請專利案之全文於本文中列為參 考。
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Claims (1)

  1. 揮發第一有機小分子物質於該第一載體氣流中； 將該第一載體氣流通過一裝置，其中該裝置之内壁係 足夠高溫，以避免該第一有機小分子物質之冷凝作用； 於0.001托（torr)至100托之壓力下，將該第一載體氣 流通過一基材；及 澱積該第一有機小分子物質於基材上，以於基材上形 成含該第一有機小分子物質之第一膜。 2. 根據申請專利範圍第1項之方法，其中該壓力係自0. 1 托至1 0托。 3. 根據申請專利範圍第1項之方法，其中該第一載體氣 流係選自由氮氣、氬氣、氦氣、氖氣、氪氣及氙氣所組成 之群。 4. 根據申請專利範圍第1項之方法，其中該第一有機小 分子物質係選自由三（8-喹啉）鋁、N，N’ -二苯基-N，Ν’ -雙（3-甲苯基）-1，1’-雙苯基-4，4’ -二胺、α-4，4’ -雙 [N-(l -萘基）-Ν-苯基-胺]雙苯基、4,4’ ，4Π-參[Ν-（3-甲 苯基）-Ν -苯基-胺基]三苯基胺及雙-(8 -羥喹啉基）鋁氧苯 基所組成之群。 5. 根據申請專利範圍第1項之方法，其中該第一膜係具 有少於11埃（angstroms)之RMS表面粗糙度。 6. 根據申請專利範圍第1項之方法，其中該第一膜係包 含N，N’ -二苯基-N，N’-雙（3 -甲苯基）-1，1’ -雙苯基-4，
    O:\55\55921-920730.ptc 第24頁 575699 _案號87118943 今# 月 日 修正_ 六、申請專利範圍 4,-二胺。 7.根據申請專利範圍第1項之方法，其中該方法進一步 包含： 揮發第二有機小分子物質於第二載體氣流中；及 將該第二載體氣流與該第一載體氣流摻合； 其中該澱積步驟包括澱積該第二有機小分子物質於基 材上，以使該第一膜包含第一有機小分子物質及第二有機 小分子物質。 8 .根據申請專利範圍第7項之方法，其中該壓力係自0. 1 托至1 0托。 9 .根據申請專利範圍第7項之方法，其中該第一膜係併 入一有機光放射裝置中。 1 0 .根據申請專利範圍第1項之方法，其中該方法進一步 包含： 揮發第三有機小分子物質於第三載體氣流中； 於0.001托（torr)至100托之壓力下，將該第三載體氣 流通過第一膜；及 澱積該第三有機小分子物質於第一膜上，以於第一膜 上形成含該第三有機小分子物質之第二膜。 1 1 .根據申請專利範圍第1 0項之方法，其中該壓力係自0 . 1托至1 0托。 1 2 .根據申請專利範圍第9項之方法，其中該第二膜係併 入一有機光放射裝置中。 1 3 ·根據申請專利範圍第9項之方法，其中該第二膜係包
    O:\55\55921-920730.ptc 第25頁 575699 _案號87118943 h〕月 日 修正_ 六、申請專利範圍 含參（8 -喹啉）铭。 1 4 · 一種製造有機膜之方法，其包含： 提供包含一或多種揮發性第一有機小分子物質之第一 載體氣流； 將該第一載體氣流通過一裝置，其中該裝置之内壁係 足夠高溫，以避免該一或多種第一有機小分子物質之冷凝 作用； 於自0. 0 0 1托至1 0 0托之壓力下，將該第一載體氣流曝 置於基材上； 澱積該一或多種揮發性第一有機小分子物質於該基材 上，以於基材上形成第一膜，該第一膜係包含一或多種揮 發性第一有機小分子物質； 提供一包含一或多種揮發性第二有機小分子物質之第 二載體氣流； 將該第二載體氣流通過一裝置，其中該裝置之内壁係 足夠高溫，以避免該一或多種第二有機小分子物質之冷凝 作用； 於自0 · 0 0 1托至1 0 0托之壓力下，將該第二載體氣流曝 置於該基材上之第一膜上； 澱積該一或多種揮發性第二有機小分子物質於該第一 膜上，以於該基材之第一膜上形成第二膜，該第二膜係包 含一或多種揮發性第二有機小分子物質。 1 5 ·根據申請專利範圍第1 4項之方法，其中該一或多種揮 發性第一有機小分子物質係包含單一第一有機小分子物
    O:\55\55921-920730.ptc 第26頁 575699 _案號87118943 Q月 日 修正_ 六、申請專利範圍 ' 質。 1 6 ·根據申請專利範圍第1 4項之方法，其中該一或多種揮 發性第一有機小分子物質係包含二或多種第一有機小分子 物質。 1 7.根據申請專利範圍第1 4項之方法，其中該一或多種揮 發性第二有機小分子物質係包含單一第二有機小分子物 質。 1 8.根據申請專利範圍第1 4項之方法，其中該一或多種揮 發性第二有機小分子物質係包含二或多種第二有機小分子 物質。 1 9.根據申請專利範圍第1 4項之方法，其中該第一及第二 膜係併入有機光放射裝置中。 2 0 ·根據申請專利範圍第1 9項之方法，其中該第一及第二 膜之一係一光放射層。 2 1 .根據申請專利範圍第2 0項之方法，其中該光放射層係 包含參（8 -喹琳）鋁。 2 2.根據申請專利範圍第1 9項之方法，其中該第一及第二 膜之一係一電洞轉移層。 2 3.根據申請專利範圍第2 2項之方法，其中該電洞轉移層 係包含N，N’-二苯基_N，N’-雙（3-甲苯基）-1，Γ -雙苯基 - 4，4 ’ - 二胺。 2 4 ·根據申請專利範圍第1 9項之方法，其中該第一及第二 膜之一係光放射層，而另一則為電洞轉移層。 2 5 .根據申請專利範圍第2 4項之方法，其中該光放射層係
    O:\55\55921-920730.ptc 第27頁 575699 _案號87118943 月 日 修正_ 六、申請專利範圍 包含參（8 -喹啉）鋁，且該電洞轉移層係包含Ν，Ν’ -二苯基 -Ν，Ν’-雙（3_甲苯基）- 1，Γ -雙苯基-4，4’-二胺。 2 6 .根據申請專利範圍第1 4項之方法，其中該基材包括聚 合物膜材料、玻璃材料或半導體材料。 2 7 .根據申請專利範圍第1 4項之方法，其中該基材包括銦 氧化錫。 2 8 .根據申請專利範圍第2 7項之方法，其中該基材係一塗 覆銦氧化錫之聚酯。 29. —種製造有機膜之方法，其包含： 提供包含一或多種揮發性第一有機小分子物質之載體 氣流； 將該載體氣流通過一裝置，其中該裝置之内壁係足夠 高溫，以避免該一或多種第一有機小分子物質之冷凝作 用； 於自0 . 0 0 1托至1 0 0托之壓力下，將該載體氣流曝置於 基材上；及 澱積該一或多種揮發性第一有機小分子物質於該基材 上，以於基材上形成一層膜，該膜係包含一或多種揮發性 第一有機小分子物質。 3 0 .根據申請專利範圍第2 9項之方法，其中該膜係光放射 層。 3 1 .根據申請專利範圍第3 0項之方法，其中該膜係包含單 一第一有機小分子物質。 3 2 .根據申請專利範圍第3 0項之方法，其中該膜係包含二
    O:\55\55921-920730.ptc 第28頁 575699 案號 87118943 六、申請專利範圍
    月 曰 修正 或多種第一有機小分子物質。 3 3 .根據申請專利範圍第3 0項之方法，其中該壓力係自0. 1托至1 0托。 3 4.根據申請專利範圍第3 0項之方法，其中該壓力係自0 . 0 0 1托至0 . 1托。 3 5 .根據申請專利範圍第3 0項之方法，其中該壓力係自0 . 0 0 1托至1 0托。 3 6 .根據申請專利範圍第3 0項之方法，其中該壓力係自0 . 1托至1 0 0托。 3 7.根據申請專利範圍第3 0項之方法，其中該壓力係自1 0 托至1 0 0托。 3 8.根據申請專利範圍第3 0項之方法，其中該基材係經冷 卻。 3 9 .根據申請專利範圍第30項之方法，其中該基材包括聚 合物膜材料、玻璃材料或半導體材料。 4 0 .根據申請專利範圍第3 0項之方法，其中該基材包括銦 氧化錫。 4 1 .根據申請專利範圍第3 0項之方法，其中該基材係一塗 覆銦氧化錫之聚醋。 4 2 .根據申請專利範圍第3 0項之方法，其中該基材係經塗 覆銦氧化錫之聚酯，其係進一步塗覆一層電洞轉移層。 4 3. —種用以於基材上物理性氣相澱積含有機小分子物質 的膜之裝置，該裝置包含： 一澱積反應室；
    O:\55\55921-920730.ptc 第29頁 575699 _案號87118943 今^年月 日 修正_ 六、申請專利範圍 ] 與該澱積反應室可行流體交換的至少一條流體通路， 該流體通路包含： (i )載體氣流來源， (i i )有機小分子物質流，及 (i i i )流速控制器； 放置於該澱積反應室中之基材固定器；及 可與該澱積反應室行流體交換之真空泵，其係以於該 澱積反應室中提供0.001托（torr)至100托之壓力。 4 4.根據申請專利範圍第4 3項之裝置，其中該流速控制器 包括壓力調節器。 4 5 .根據申請專利範圍第4 3項之裝置，其中該流速控制器 包括一流速計。 4 6 .根據申請專利範圍第4 3項之裝置，其中該流速控制器 包括一交換閥。 4 7.根據申請專利範圍第4 3項之裝置，其中該澱積反應室 係具有加熱牆。 4 8 .根據申請專利範圍第4 3項之裝置，其中該澱積反應室 係具有一或多個輻射熱源。 4 9 .根據申請專利範圍第4 3項之裝置，其進一步包括一實 質上包圍該殿積反應室之加熱器。 5 0 ·根據申請專利範圍第4 9項之裝置，其中該加熱器係多 區域加熱器/冷卻器。 5 1 .根據申請專利範圍第4 3項之裝置，其中該基材固定器 係經冷卻。
    O:\55\55921-920730.ptc 第30頁 575699 _案號87118943 年？ 月 曰_^_ 六、申請專利範圍 1 5 2 .根據申請專利範圍第5 1項之裝置，其中該基材固定器 係包含控溫區隔器。 5 3 .根據申請專利範圍第4 3項之裝置，其中該有機小分子 物質來源係含該有機小分子物質之開放式容器。 5 4.根據申請專利範圍第5 3項之裝置，其中該開放式容器 係經加熱。 5 5 .根據申請專利範圍第4 3項之裝置，其中該裝置係包含 二或多條流體通路。 5 6 . —種用以於基材上物理性氣相澱積含有機小分子物質 的膜之裝置，該裝置包含： 一殿積反應室； 用以加熱該澱積反應室之裝置； 將有機小分子物質蒸氣導入該澱積反應室之裝置； 於該澱積反應室中冷卻基材之裝置； 用以維持該澱積反應室中之壓力於自〇 . 〇 0 1托至1 0 0托 間之範圍内之裝置。 57. —種製造有機膜之方法，其包含： 提供一基材； 提供二或多種有機先質分子； 使該有機先質分子於介於1 0 - 8至1 0 - 1 1托間之壓力 下、於該基材之存在下反應，以形成該有機膜。 5 8.根據申請專利範圍第5 7項之方法，其中該二或多種有 機先質分子係藉由將載體氣體起泡而通過該有機先質分子 而製造。
    O:\55\55921-920730.ptc 第31頁 575699 _案號87118943 Q月曰 修正_ 六、申請專利範圍 1 5 9 .根據申請專利範圍第5 7項之方法，其中該二或多種有 機先質分子係藉由將該有機先質分子於納得生（Knuds en) 元件而製造。 6 0 .根據申請專利範圍第5 7項之方法，其中該有機膜係非 線性光學膜。 6 1 .根據申請專利範圍第6 0項之方法，其中該有機先質分 子之一係選自由4’ _二曱基胺-4 -偶氮英，硫紛4’ -二甲基 胺-4-偶甲基氮芪，4’-甲氧胺-4-甲基偶氮芪，4’ -二甲基 胺-4-乙基偶氮萬碳及4’ -二甲基胺-4-乙基偶氮英氫氧化 物所組成之群。 6 2 .根據申請專利範圍第6 0項之方法，其中該有機先質分 子之一係選自由甲基偶氮芪，甲烷磺酸酯，三氟甲烷磺酸 酯，乙醯甲苯磺酸酯以及三氟乙酸甲酯所組成之群。 6 3.根據申請專利範圍第60項之方法，其中該非線性光學 膜係選自由甲苯磺酸4’-二甲基胺-N-甲基-4 -偶氮芪，甲 烷磺酸4’-二甲基胺-4-曱基偶氮芪，三氟甲烷磺酸4’ -二 甲基胺-4-甲基偶氮芪，甲苯磺酸4’ -甲氧基-4-甲基偶氮 ，甲苯磺酸4’-二曱基胺-4-乙醯偶氮芪及三氟乙酸4’-二甲基胺-4-甲基偶氮芪所組成之群。 6 4.根據申請專利範圍第5 7項之方法，其中該有機膜係一 透光層。 6 5 .根據申請專利範圍第5 7項之方法，其中該有機膜包含 一電價轉移錯合物。 6 6.根據申請專利範圍第6 5項之方法，其中該二或多種有
    O:\55\55921-920730.ptc 第32頁 575699 _案號87118943 月 日 修正_ 六、申請專利範圍 機先質分子係包含士61：『3七11丨3€6『1¥316116及7，7，8，8-四氰 基喹啉二甲烷。 6 7.根據申請專利範圍第5 7項之方法，其中該有機膜包含 一存在於母體分子基質中之客體分子。 6 8 .根據申請專利範圍第6 7項之方法，其中該母體分子係 選自由三（8 -喹啉）鋁及雙- (8 -羥喹啉）鋁氧苯所組成之 群。 6 9.根據申請專利範圍第6 7項之方法，其中該客體分子係 選自由4-（二氰亞甲基）-2-甲基-6(p -二甲基胺苯乙烯 基）-411_哌喃，5，10，15,20-四苯基-2111，2311-樸吩， DCM2，橡皮烯及香豆素所組成之群。 7 0 .根據申請專利範圍第5 7項之方法，其中該基材包含聚 合物膜材料’玻璃材料或半導體材料。 7 1 .根據申請專利範圍第57項之方法，其中該基材包含一 聚茚滿氧化鈦層。 7 2.根據申請專利範圍第7 1項之方法，其中該基材包含一 經聚茚滿氧化鈦塗覆之聚酯。 7 3.根據申請專利範圍第7 2項之方法，其中該基材包含一 經聚茚滿氧化鈦塗覆之聚酯，其係進一步塗覆一層電洞轉 移層。 7 4.根據申請專利範圍第5 7項之方法，其中該基材包含一 電洞轉移層。 7 5.根據申請專利範圍第5 7項之方法，其中該基材係經旋 轉0
    O:\55\55921-920730.ptc 第33頁 575699 第087118943號專利申請案 中文圖式替換頁(92年7月）
    〇
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KR20060034312A (ko) 2006-04-21
US20040007178A1 (en) 2004-01-15
DE69827293T2 (de) 2006-02-02
JP2013177692A (ja) 2013-09-09
AU1412499A (en) 1999-06-07
EP1032722B1 (en) 2004-10-27
US20070131172A1 (en) 2007-06-14
WO1999025894A1 (en) 1999-05-27
KR20010024652A (ko) 2001-03-26
US6558736B2 (en) 2003-05-06
JP4890592B2 (ja) 2012-03-07
JP5371837B2 (ja) 2013-12-18
US20020155230A1 (en) 2002-10-24
JP2016104913A (ja) 2016-06-09
KR100606325B1 (ko) 2006-07-31
US20010002279A1 (en) 2001-05-31
EP1032722A4 (en) 2001-09-12
US20100104753A1 (en) 2010-04-29
US20150114296A1 (en) 2015-04-30
JP2010159497A (ja) 2010-07-22
US6337102B1 (en) 2002-01-08
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KR100585286B1 (ko) 2006-05-30
DE69827293D1 (de) 2004-12-02

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