TW409150B - Evaporation apparatus, organic material evaporation source and method of manufacturing thin organic film - Google Patents
Evaporation apparatus, organic material evaporation source and method of manufacturing thin organic film Download PDFInfo
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經濟部智慧財產局員工消費合作社印製 五、發明說明（11) 在此場合，因爲蒸汽的放出立刻停止的緣故，可以進 行所請良好的「中止」的控制。此外，昂貴的有機薄膜材 料也不會浪費。結束有機薄膜形成作業，冷卻有機薄膜材 料時，也可以藉由將有機薄膜材料置於高壓環境中，使冷 卻速度變快。 根據實驗，在低壓環境即使加熱有機薄膜材料直到放 出蒸汽的溫度爲止，雖然會因爲有機薄膜材料的種類而有 些許不同，但只要周圍的環境壓力上升至1 3.3 P a ( 0.1 Torr)〜2.〇Xl03Pa(15 T o r r ) 程度的話，可以確認蒸汽不再被放出。 但是，壓力升高得太高的話，非活性氣體使用量會增 加，此外，真空排氣使其降低到低壓力爲止的時間也會變 長的緣故，所以在抑制蒸汽放出的場合，以將壓力調整爲 6 6 . 5 P a (0.5 Torr〉程度較佳。 另一方面，如此在高壓力環境將有機薄膜材料昇溫之 後，進行真空排氣降爲低壓力環境，而使放出蒸汽的場合 ，爲了提高有機薄膜的品質，以將壓力降低爲1,3 3 X l〇-4Pa(l.〇xl〇_6 To rr)以下，較佳者爲 降低至 1.33xl〇_5Pa (1.OxlO-7 Torr) 以下的壓力較佳。 因爲有機薄膜材料也會有吸附氣體或是水分的場合， 所以導入前述非活性氣體之前，將前述有機薄膜材料置於 真空環境，進行脫氣者佳。於脫氣時，其將有機薄膜材料 加熱至較其蒸發溫度更低的溫度爲止者較佳。 本紙張尺度適用中國國家標準（_CNS)A4規格（210x297公釐）-14 - (請先随讀背面之注意事項再填寫本頁) -------"•訂----r III11 409150 A7 B7 經濟部中央標準局員Η消費合作社印製 五、發明説明（彳) 發明所屬之技術領域 本發明係提供在成膜對象物的表面形成有機薄膜之有 機蒸鍍裝置、可以使用該有機蒸鍍裝置的有機蒸發源’以 及，適於形成有機薄膜的有機薄膜製造方法。 背景技術 從前的電子技術係以半導體爲中心而以無機物爲對象 的，但是近年來，開始注意到使用有機化合物的功能性有 機薄膜。 使用有機化合物的理由有以下種種優點： (1 )可以利用到較無機物更多樣的反應系/特性。 (2)可以藉由較無機物更低的能量來進行表面處理 〇 於利用功能性有機薄膜的例子有：有機電子螢光元件 '壓電感測器、焦電感測器、電氣羁緣膜等，這些例子中 ，有機電子螢光元件，由於可以利用作爲顯示器面板所以 被矚目，爲了要使顯示部分大口徑化，可以在大面積基板 上形成均一的有機薄膜的技術有很大的需求。 然而，於從前的有機薄膜製造工程，都是由供形成 A i薄膜或是S i 〇2薄膜等金屬薄膜或是無機薄膜之用的 真空蒸鍍裝置來轉用的，適於形成有機薄膜的蒸鍍裝置尙 未被開發出來。 此處，比較有機薄膜材料與無機薄膜材料的話，有機 薄膜材料具有以下的特徵： (請先閲讀背面之ii意事項再填寫本頁) 4T.Printed by the Employees' Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the Invention (11) In this case, because the steam release immediately stopped, you can perform the good “stop” control requested. In addition, expensive organic film materials are not wasted. When the organic thin film forming operation is finished and the organic thin film material is cooled, the organic thin film material may be placed in a high-pressure environment to increase the cooling speed. According to experiments, even if the organic thin film material is heated to a temperature at which steam is emitted in a low-pressure environment, although it is slightly different depending on the type of the organic thin film material, as long as the surrounding environmental pressure rises to 1 3.3 P a (0.1 Torr) ~ 2. 〇Xl03Pa (15 Torr), it can be confirmed that steam is no longer emitted. However, if the pressure is raised too high, the amount of inert gas used will increase, and the time taken for the vacuum exhaust to reduce it to a low pressure will also be longer. Therefore, in order to suppress the release of steam, The adjustment is preferably 6 6. 5 Pa (0.5 Torr). On the other hand, after the organic thin film material is heated in a high pressure environment, the vacuum exhaust is reduced to a low pressure environment, and the steam is emitted in order to Improve the quality of the organic film to reduce the pressure to 1,3 3 X 10-4 Pa (1.0 x 10-10 Torr), preferably to 1.33 x 10-5 Pa (1.OxlO-7 The pressure below Torr) is better. Because organic thin film materials may also adsorb gas or moisture, it is better to degas the organic thin film material before introducing the inert gas. It is better to degas. It is better to heat the organic thin film material to a temperature lower than its evaporation temperature. This paper size is applicable to China National Standard (_CNS) A4 size (210x297 mm) -14-(Please read the note on the back first Matters refill this Page) ------- " Order ---- r III11 409150 A7 B7 Member of the Central Standards Bureau of the Ministry of Economy ΗPrinted by Consumer Cooperatives V. Description of Invention (彳) The technical field to which the invention belongs The invention is provided in Chengdu An organic vapor deposition device that forms an organic thin film on the surface of a film object, an organic vaporization source that can use the organic vapor deposition device, and an organic thin film manufacturing method suitable for forming an organic thin film. BACKGROUND ART In the past, electronic technology focused on semiconductors. Inorganic substances are targeted, but in recent years, functional organic thin films using organic compounds have begun to be noticed. The reasons for using organic compounds have the following advantages: (1) More diverse reaction systems / characteristics than inorganic substances can be used. (2) Surface treatment can be performed with lower energy than inorganic substances. Examples of functional organic thin films are: organic electronic fluorescent elements' piezoelectric sensors, coke inductors, electrical barrier films, etc. In these examples, organic electronic fluorescent devices have attracted attention because they can be used as display panels. In order to make the display portion larger, There is a great demand for a technology for forming a uniform organic thin film on an area substrate. However, in the previous organic thin film manufacturing processes, it was used to form metal films such as Ai thin films or S i 02 thin films or inorganic thin films. The vacuum evaporation device suitable for the formation of organic thin films has not been developed. Here, when comparing organic thin film materials with inorganic thin film materials, organic thin film materials have the following characteristics: (Please read first (Please fill in this page on the back of ii) 4T.
Mr >. 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公餐） 經濟部中央標準局員工消費合作社印製 409150 ^ 五、發明説明（2 ) (1 )有機薄膜材料的蒸汽壓較高，就蒸發源溫度而 言，金屬蒸發源需要6 〇 〇。1〇〜2 0 0 0 t：程度的高溫， 而有機薄膜材料的蒸發源溫度則爲〇°C (有時還會到達零 .下的溫度）〜4 0 0°C之間，有很多材料會在2 Ot〜 4 0 〇°C的溫度範圍內引起分解。也就是說，在蒸發時以 進行精密的溫度控制爲佳。 在形成金屬薄膜時，一般使用的是將電子束照射於金 屬蒸發源的電子束式（E/B )蒸鍍裝置，但是對於有機 薄膜材料而言能量太高，被電子束照射到的話就會被分解 掉。 (2 )有機薄膜材料之中也有形態是粉體的，但是一 般而言，粉體狀材料的熱傳導性較差，特別是要在真空中 加熱的話，由於真空的絕熱效果而使得昇溫與冷卻不易進 行，會在控制溫度與實際溫度之間產生延遲。 '另一方面，如此的粉狀體材料，一旦蒸發源的溫度上 昇之後，僅靠輻射冷卻的話是不容易冷下來，即使停止加 熱也無法立即停止蒸發。而會有所謂蒸發的「中止」不佳 的問題。 (3 )有機薄膜材料因爲蒸汽壓高’所以吸附於低溫 的真空槽的槽壁上的有機薄膜材料’會由於真空槽的溫度 上昇而脫離（再蒸發），如果脫離粒子混入有機薄膜中的 話，會使有機薄膜的特性劣化° (4 )有機薄膜材料裡頭容易吸附水分的物質很多’ 吸附水分之後會產生變質而影響特性。此外在形成多層有 (請先閲讀背面之注意事項再填寫本頁) 釘. P. 本紙張尺度適用中國國家標準（CMS ) A4规格（210X297公釐） -5- Ί Ί 經濟部中央標準局員工消費合作社印製 409150 五、發明説明（3 ) 機薄膜時，將水分取入有機薄膜內的話，也會有引起界面 特性變化的可能。特別是，作成有機電子螢光元件或壓電 /焦電元件等功能性元件的場合，會使得最終的性能缺陷 〇 (5 )金屬蒸發源，在蒸發時具有方向性，其方向依 照餘弦法則（COS LAW)從蒸發源出發、具有幾乎完全 直進的性質，但是在有機薄膜材料的蒸發源，則會有接近 擴散程度的迂迴混入現象。 (6 )形成蒸鍍重合膜的場合，有必要使同時蒸鍍的 2個有機薄膜材料的組成比依照化學量論比的必要。在組 成比偏離了化學量論比的場合，壓電/焦電元件失去其功 能，或者是降低其功能。爲了使組成比符合化學量論比， 必須要精密控制成膜的速度。 _如以上所述，有機薄膜材料在操作上有很多困難處。 從前所使用的真空蒸鍍裝置的蒸發源有以.下數種（第8圖 (a)〜（e))，由於上述的有機薄膜材料的性質，或 是被要求的有機薄膜的特性，各種蒸發源皆不適用。 (A)以金屬形成蒸發源容器1 0 1，直接通電加熱 ，使薄膜材料蒸發的方式（第8圖（a):直接電阻加熱 形式） 此種方式，在融解金屬的溫度區域具有優異的溫度安 定性，但是在蒸發有機薄膜村料的溫度區域其溫度安定性 與控制性都不佳。亦即，有機化合物蒸汽（有機薄膜材料 的蒸汽）的產生速度變得不安定。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閱讀背面之法$項再填寫本頁) 钉- Μ 經濟部中央標準局員工消費合作社印製 409150 A7 B7 五、發明説明（4 ) 此外.，有機薄膜材料之中，有的會使金屬腐蝕，有的 會與金屬起反應，所以對於構成容器的金屬具有腐蝕性/ 反應性的有機薄膜材料不能夠使用。 (B)蒸發源容器111、121周圍置電阻加熱體 1 、122，藉由通電加熱的方式間接加熱，使薄膜 材料蒸發的方式（第8圖（b):錐籃形式；第8圖（c ):K細胞形式）。 此種方式，在融解金屬的溫度區域具有優異的溫度安 定性，但是在蒸發有機薄膜材料的溫度區域其溫度安定性 與控制性都不佳。亦即，有機化合物蒸汽的產生速度變得 不安定。 此外’此種方式的電阻加熱體1 1 2，一般使用金屬 裸線材，但是.有機薄膜材料與無機薄膜材料相比，容易產 生赶迴混入的現象。有機薄膜材料中含有金屬鉗合物的場 合’還會有電阻加熱體1 1 2間產生短路的可能。 此外’ K細胞形式的蒸發源因爲構造複雜，內部淸掃 不易’薄膜材料無法完全除去。亦即，蒸發源容器1 1丄 、1 2 1內的薄膜材料要交換爲不同種類的薄膜材料時， 之前留下的薄膜材料有可能會成爲污染。 (C )使用由石英等透光性材料所構成的蒸發源容器 1 3 1 ’藉由紅外線登1 3 3輻射加熱薄膜材料使其蒸發 的方式C第8圖（d ):燈光加熱型蒸發源）。 此種方式，在低溫具有優異的溫度控制性，但是因爲 蒸發源容器131的比熱容量很大，所以控制溫度與實際 (請先閱讀背面之注意事項再填窝本頁) 41 公 7 29. 409150 A7 __ ______. B7 五、發明説明（5 ) 薄膜材料的溫度之間會產生溫度差。另一方面，在測定薄 _材料自身的溫度而進行控制的場合，容易引起溫度過熱 ’有引起有機薄膜材料分解之虞= 此外，爲了要使從紅外線燈1 3 3所射出的熱線（紅 外線）透過，蒸發源容器1 3 1有必要以石英等透明材料 來構成，透明材料在淸掃或交換時容易產生破損。 進而，由於蒸發源容器1 3 1的長期使用而使透明材 料起霧，使得紅外線的透過強度因位置的不同而有所不同 ’就熱傳導率很差的有機薄膜材料而.言，有引起局部過熱 之虞。 此外，有機薄膜材料之中，有的會因特定波長的光線 而變質，這種有機材料不能夠以此方式產生蒸汽。 (D)將電子線1 4 5照射於薄膜材料，使其蒸發的 方式（第8圖（e ):電子線E / B槍）。 用電子線1 4 5照射的話有機薄膜材料會分解，所以 不能夠應用。 經濟部中央標準局員工消費合作社印製 如以上所說明的，使無機系薄膜材料蒸發的從前技術 (A )〜（D )方式，並不能夠完全適用於有機薄膜材料 。特別是由於有機薄膜材料的溫度過熱所導致的分解問題 ，或是有機薄膜材料加熱的困難性，都是無機系薄膜材料 所沒有的問題，而有待解決。 本發明係爲了解決上述先行技術的問題而發明者，其 目的在於提供昇溫時不會產生溫度過熱，有機薄膜材料的 主成份不會熱分解，可以在短時間內使溫度變化達到所要 -8 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） 經濟部中央標準局員工消費合作社印製 40915G_^___ 五、發明説明（6 ) 的溫度之技術。 此外，還以提供在蒸鍍時以外1抑制有機薄膜材料的 蒸汽的產生，可以有效利用有機薄膜材料的技術爲目的。 此外，在有機薄膜材料爲液體狀的時候，還以提供對 於如此的有機薄膜材料，可以一定的溫度加熱，而且容易 操作的有機材料用蒸發源爲目的。 發明槪要 本發明具有真空排氣系，真空槽，有機蒸發源，藉由 前述真空排氣系將前述真空槽內真空排氣，控制被容納於 前述有機蒸發源內的有機薄膜材料的溫度使其產生蒸汽， 以於被配置在前述真空槽內的成膜對象物表面形成有機薄 膜的方式被構成的蒸鍍裝置，於前述真空槽被接續著氣體 導入系，以將非活性氣體導入前述真空槽內的方式構成的 蒸鍍裝置。 在此場合，將真空槽內真空排氣後，導入非活性氣體 ，可以將有機蒸發源內的有機薄膜材料至於非活性氣體環 境中=接著，控制有機薄膜材料的溫度的場合，在有機薄 膜材料的周圍產生非活性氣體的對流，結果，與有機蒸發 材料被置於真空環境的場合相比，可以加快昇溫速度或是 降溫速度。特別是在有機薄膜材料爲粉體的場合，非活性 氣體侵入粉體的粒子間具有熱媒體的作用，因爲構成粉體 的粒子間的熱傳導率變大，所以提高有機薄膜材料的溫度 控制性，此外，有機薄膜材料的局部過熱或是溫度過高的 (請先閲讀背面之洼意事項再填寫本頁) —i. 本紙張尺度適用中國國家標準（CNS ) A4規格（210父297公嫠） -9 - 409150 at _ B7 五、發明説明（7 ) 情形變得不容易發生，可以防止有機薄膜材料的分解。 本發明的蒸鍍裝置，具有容器、氣體閥、放出口：其 構成方式係以使前述氣體閥爲開狀態的話，前述容器的內 部環境與外部環境相接；將前述氣體閥關閉的話，可以遮 斷前述容器的內部環境與前述外部環境的相連的方式構成 的。 在此有機蒸發源的場合，將非活性氣體導入真空槽內 之後，關閉氣體閥，可以將有機薄膜材料置於非活性氣體 環境中。 一般而言，在非活性氣.髓環境中的有機化合物蒸汽的 產生量，較真空環境中者爲少，所以在非活性氣體環境中 進行有機薄膜材料的加熱/冷卻的話，因爲於其間，由有 機薄膜材料產生蒸汽的情形會被抑制的緣故，所以不會發 生在形成薄膜時無法利用到的無效的蒸汽，可以提高有機 薄膜材料的使用效率，降低製造成本。 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注$項再填寫本頁) ->- 在真空環境下，即使有機薄膜材料被加熱到產生蒸汽 的溫度爲止的場合，也可以藉由非活性氣體的壓力而使其 在非活性氣體環境中不產生蒸汽。也就是說，有機薄膜材 料在非活性氣體環境中被昇溫之後，進行真空排氣的話， 可以不放出無效的蒸汽，而形成有機薄膜。 在此場合，預先將有機蒸發源以可以接續氣體導入系 的方式構成，在關閉前述氣體閥的狀態下導入非活性氣體 至前述容器內的話，在將真空槽內置於真空環境的狀態， 可以將有機薄膜材料置於非活性氣體環境。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X2.97公釐） -10- 409150 a7 ______B7__ 五、發明説明（8 ) 也就是說，不需要爲了抑制蒸汽的放出，.而將非活性 氣體導入容積大的真空槽內。 在此場合，使真空排氣系可以接續於有機蒸發源，在 關閉前述氣體閥的狀態，使前述容器內部可以真空排氣， 而將導入的非活性氣體真空排氣之後，可以打開氣體閥。 也就是說，可以接續真空排氣系的有機蒸發源的場合 ，使成爲可以接續氣體導入系，在關閉前述氣體閥的狀態 可以導入氣體至前述容器內的方式構成者爲佳。 此外，有機薄膜的蒸汽，如果冷卻的話就會析出，所 以本發明的有機蒸發源的場合，至少在前述容器與前述放 出口之間，設加熱手段，可以使蒸汽直到被放出到真空槽 內爲止都不會冷卻下來。 經濟部中央標準局貝工消費合作社印製 另一方面，從液體狀的有機薄膜材料產生蒸汽的場合 ，於有機蒸發源設內部被配置液體狀的有機薄膜材料的容 器，及內部爲熱媒體的流動路徑的熱媒體循環路徑*將前 述熱媒體循環路徑預先配置於前述容器周圍的話，可以藉 熱媒體將容器全體均一地加熱或是冷卻，所以可以提高有 機薄膜材料的均熱性。 在此場合，設有控制前述熱媒體於指定的溫度的熱媒 體源，以可以將前述容器內的有機薄膜材料加熱或是冷卻 的方式構成的話，因爲液體狀的有機薄膜材料與被控制溫 度的熱媒體之間進行熱交換的緣故，所以可以精密地控制 有機蒸發材料的溫度上升或是冷卻。特別是在昇溫時’因 爲有機薄膜的溫度不會較熱媒體的溫度還要高’所以不會 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -11 - 經濟、哪中央標準局貝工消費合作社印製 40915Q at B7 五、發明説明（9 ) 產生有機薄膜局部過熱的狀態。 此外，因爲不藉由熱輻射線進行加熱的緣故，所以不 會因爲容器起霧而使得有機蒸發材料被不均勻地加熱。而 且，因爲容器材料並不被要求須具備透明性，所以可以使 用熱傳導效率高的陶瓷材料來製作。也就是說，操作.變得 更爲容易。 此有機蒸發源，前述容器構成爲內側容器與外側容器 之雙重構造，前述內側容器與前述外側容器之間可以作爲 前述熱媒體循環路徑。 在此場合，因爲有機薄膜材料與熱媒體之間，是透過 內側容器的壁面進行熱交換的緣故，所以熱交換的效率.很 高，結果提高了溫度控制性。 又，於前述外側容器的周圍配置絕熱材的話，可以更 進一步提高熱效率或是溫度控制性。 本發明之有機蒸發源的前述容器，係被構成爲內側容 器與外側容器之雙重構造，前述內側容器與前述外側容器 之間被作爲前述熱媒體循環路徑的場合，接觸熱媒體源， 藉由該熱媒體源，可以將前述熱媒體循環路徑內進行循環 的熱媒體控制於指定的溫度，以將前述容器內的有機薄膜 材料加熱或是冷卻的方式構成。 如以上所述，因爲有機薄膜材料係隨著環境的氣壓而 變化蒸汽的放出速度，所以根據本發明的有機薄膜製造方 法，將有機薄膜材料配置於有機蒸發源內使放出蒸汽，於 成膜對象物表面形成有機薄膜的場合，控制前述有機薄膜 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）-12 - (請先閲讀背面之注意事項再填寫本頁) Γ 409150 A7 B7 經濟部中央標準局員工消費合作社印裝 五、發明説明（10) 材料被放置處所的環境的壓力，，控制前述蒸汽的放出速 度，其結果可以控制有機薄膜的成長速度。 此外，根據本發明的有機薄膜製造方法，將有機薄膜 材料配置於有機蒸發源內使放出蒸汽，於成膜對象物表面 形成有機薄膜的場合，可以在昇溫前述有機薄膜材料時， 提高前述有機薄膜材料所被放置處的環境的壓力以抑制前 述蒸汽的放出，接著，可以再使前述有機薄膜材料所被放 置處的環境的壓力降低，使前述蒸汽開始放出。. 特別是在昇溫有機薄膜材料時預先升高壓力的話，可 以提高溫度均一性的緣故，將有機薄膜材料昇溫到指定溫 度時所需的加熱時間縮短，此外，因爲從該狀態使壓力降 低的話可以立刻開始放出蒸汽，所以開始有機薄膜的形成 作業所需要的時間會縮短。 如此，根據本發明的有機薄膜製造方法的話，一旦將 有機薄膜材料昇溫之後，僅僅要控制被放置有機薄膜材料 的環境的真空度，就可以使蒸汽開始放出或是結束放出。 藉此，不會浪費昂貴的有機薄膜材料。 因爲有機薄膜材料的反應性很高，隨著壓力的上升， 進行將非活性氣體導入前述有機薄膜材料被置放的環境中 者較佳。此外，壓力降低，可以藉由真空排氣其環境而達 成。 一旦開始放出的前述有機薄膜材料的蒸汽，可以藉由 升高前述有機薄膜材料被置放的環境的壓力而使其停止放 出。 本紙張尺度適用中國國家標準（CNS ) Λ4規格（210X297公釐） (請先閲填背面之注意事項再填寫本頁) -訂-Mr >. This paper size applies to Chinese National Standard (CNS) A4 size (210X297 meals) Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economy 409150 ^ V. Description of the invention (2) (1) Steam pressure comparison of organic thin film materials High, in terms of evaporation source temperature, the metal evaporation source requires 600. 1〇 ~ 2 0 0 t: high temperature, and the evaporation source temperature of organic thin film materials is 0 ° C (sometimes it can reach zero temperature) ~ 4 0 ° C, there are many materials Decomposes in a temperature range of 2 Ot to 400 ° C. In other words, it is better to perform precise temperature control during evaporation. When forming a metal thin film, an electron beam (E / B) evaporation device that irradiates an electron beam to a metal evaporation source is generally used. However, the energy of an organic thin film material is too high. Is broken down. (2) Some organic thin film materials are powdery, but in general, the thermal conductivity of powdery materials is poor. Especially when heating in a vacuum, heating and cooling are not easy due to the thermal insulation effect of the vacuum. , There will be a delay between the control temperature and the actual temperature. 'On the other hand, once the temperature of the evaporation source has risen, it is not easy to cool it down by radiation alone, and even if heating is stopped, evaporation cannot be stopped immediately. However, there is a problem that the so-called "stop" of evaporation is not good. (3) Due to the high vapor pressure of the organic thin film material, the organic thin film material adsorbed on the tank wall of the low temperature vacuum tank will be detached (re-evaporated) due to the temperature rise of the vacuum tank. If the detached particles are mixed into the organic film, It will degrade the characteristics of organic thin films. (4) There are many substances that easily absorb moisture in organic thin film materials. After adsorbing moisture, they will deteriorate and affect the characteristics. In addition, there are multiple layers (please read the notes on the back before filling in this page). P. This paper size applies the Chinese National Standard (CMS) A4 specification (210X297 mm) -5- Ί Ί Staff of the Central Bureau of Standards, Ministry of Economic Affairs Printed by a consumer cooperative 409150 V. Description of the invention (3) When the organic film is taken into the organic film, the interface characteristics may be changed. In particular, when a functional element such as an organic electronic fluorescent element or a piezoelectric / pyroelectric element is made, the final performance defect will occur. (5) The metal evaporation source has directionality during evaporation, and its direction is in accordance with the cosine law ( COS LAW) has almost straight-forward properties starting from the evaporation source, but in the evaporation source of organic thin film materials, there will be a circuitous mixing phenomenon close to the degree of diffusion. (6) When forming a vapor deposition overlap film, it is necessary to make the composition ratio of the two organic thin film materials vapor-deposited at the same time in accordance with the stoichiometric ratio. Where the composition ratio deviates from the stoichiometric ratio, the piezoelectric / pyroelectric element loses its function or reduces its function. In order to make the composition ratio conform to the stoichiometric ratio, the speed of film formation must be precisely controlled. As mentioned above, there are many difficulties in handling organic thin film materials. There are several types of evaporation sources used in the previous vacuum evaporation equipment (Figures 8 (a) ~ (e)). Depending on the nature of the organic thin film materials mentioned above, or the characteristics of the required organic thin film, various Evaporation sources are not suitable. (A) The method of forming an evaporation source container 1 0 1 with metal and heating it directly to evaporate the thin film material (Figure 8 (a): Direct resistance heating) This method has an excellent temperature in the temperature region where the metal is melted. Stability, but the temperature stability and controllability are not good in the temperature region where the organic thin film material is evaporated. That is, the generation rate of organic compound vapors (vapors of organic thin film materials) becomes unstable. This paper size applies to China National Standard (CNS) A4 (210X297 mm) (please read the $ on the back before filling this page) Nail-Μ Printed by the Central Consumers Bureau of the Ministry of Economic Affairs Consumer Cooperatives 409150 A7 B7 V. Invention Explanation (4) In addition, some organic thin film materials may corrode metals and some may react with metals. Therefore, organic thin film materials that are corrosive / reactive to the metal constituting the container cannot be used. (B) A method in which resistance heating elements 1 and 122 are placed around the evaporation source containers 111 and 121, and the film material is evaporated by indirect heating (Figure 8 (b): cone basket form; Figure 8 (c) ): K cell form). This method has excellent temperature stability in the temperature region where the metal is melted, but its temperature stability and controllability are not good in the temperature region where the organic thin film material is evaporated. That is, the generation rate of the organic compound vapor becomes unstable. In addition, the resistance heating body 1 1 2 of this type generally uses a bare metal wire. However, compared with an inorganic thin film material, an organic thin film material is prone to mix back. In the case where the organic thin film material contains a metal clamp compound, there is also a possibility that a short circuit may occur between the resistance heating bodies 1 and 2. In addition, because the evaporation source in the form of "K cells" has a complicated structure, internal sweeping is not easy, and the film material cannot be completely removed. That is, when the thin film materials in the evaporation source containers 1 1 丄 and 1 2 1 are exchanged for different types of thin film materials, the previously left thin film materials may become contaminated. (C) A method of using an evaporation source container 1 3 1 ′ made of a light-transmitting material such as quartz to heat and evaporate a thin film material by infrared radiation 1 3 3 C Figure 8 (d): Light heating type evaporation source ). This method has excellent temperature control at low temperatures, but because the specific heat capacity of the evaporation source container 131 is large, the temperature is controlled and actual (please read the precautions on the back before filling this page) 41 Male 7 29. 409150 A7 __ ______. B7 V. Description of the Invention (5) There will be a temperature difference between the temperatures of the thin film materials. On the other hand, when measuring and controlling the temperature of the thin material itself, it is likely to cause overheating of the temperature, which may cause decomposition of the organic thin film material. In addition, in order to make the heat rays (infrared rays) emitted from the infrared lamp 1 3 3 It is necessary for the evaporation source container 1 3 1 to be made of a transparent material such as quartz, and the transparent material is liable to be damaged during sweeping or exchange. Furthermore, due to the long-term use of the evaporation source container 131, the transparent material is fogged, so that the transmission intensity of the infrared rays varies depending on the location. 'In terms of organic thin film materials with poor thermal conductivity, there may be local overheating. Fear. In addition, some organic thin film materials are deteriorated by light with a specific wavelength, and this organic material cannot generate steam in this way. (D) A method of irradiating a thin film material with an electron beam 1 4 5 to evaporate it (Fig. 8 (e): electron beam E / B gun). The organic thin-film material decomposes when irradiated with electron beams 1 4 5 and therefore cannot be applied. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs As explained above, the previous techniques (A) ~ (D) of evaporation of inorganic thin film materials are not completely applicable to organic thin film materials. In particular, the decomposition problem caused by the overheating of the organic thin film material, or the difficulty of heating the organic thin film material, are problems that the inorganic thin film material does not have, and need to be solved. The present invention was invented in order to solve the above-mentioned problems of the prior art, and its purpose is to provide that the main component of the organic thin film material will not be thermally decomposed when the temperature is raised, and the temperature change can reach the desired temperature in a short time. This paper scale applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm). Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs. 40915G _ ^ ___ V. Technology of the invention (6). It is also an object of the present invention to provide a technique for suppressing the generation of steam of an organic thin film material and to effectively utilize the organic thin film material in addition to the vapor deposition. In addition, when the organic thin film material is in a liquid state, it is also intended to provide an evaporation source for an organic material that can be heated to a certain temperature and is easy to handle for such an organic thin film material. According to the invention, the present invention has a vacuum exhaust system, a vacuum tank, and an organic evaporation source. The vacuum exhaust system evacuates the inside of the vacuum tank to control the temperature of the organic thin film material contained in the organic evaporation source. A vapor deposition device that generates steam and forms an organic thin film on the surface of a film-forming object disposed in the vacuum tank. A gas introduction system is connected to the vacuum tank to introduce an inert gas into the vacuum. A vapor deposition device configured as a tank. In this case, after the vacuum chamber is evacuated and inert gas is introduced, the organic thin film material in the organic evaporation source can be placed in an inert gas environment. Then, when the temperature of the organic thin film material is controlled, the organic thin film material is used. Convection of an inert gas is generated around, and as a result, the temperature can be increased or decreased faster than when the organic evaporation material is placed in a vacuum environment. Especially when the organic thin film material is a powder, the inert gas invades the particles and acts as a heat medium between the particles. Since the thermal conductivity between the particles constituting the powder is increased, the temperature controllability of the organic thin film material is improved. In addition, the organic film material is locally overheated or overheated (please read the indentations on the back before filling out this page) —i. This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 parent 297 male) -9-409150 at _ B7 V. Description of the invention (7) The situation becomes less prone to occur, which can prevent the decomposition of the organic thin film material. The vapor deposition device of the present invention includes a container, a gas valve, and a discharge port. The structure is such that when the gas valve is opened, the internal environment of the container is connected to the external environment; when the gas valve is closed, it can be shielded. It is constructed in such a manner that the internal environment of the container is disconnected from the external environment. In the case of this organic evaporation source, after the inert gas is introduced into the vacuum tank, the gas valve is closed, and the organic thin film material can be placed in the inert gas environment. In general, the amount of organic compound vapor generated in the inert gas and marrow environment is less than that in the vacuum environment. Therefore, if the organic thin film material is heated / cooled in the inactive gas environment, since Organic thin film materials can be prevented from generating steam, so invalid steam that cannot be used when forming thin films does not occur, which can improve the use efficiency of organic thin film materials and reduce manufacturing costs. Printed by the Consumer Standards Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the note on the back before filling in this page)->-In a vacuum environment, even if the organic thin film material is heated to the temperature at which steam is generated, it can be used The pressure of the inert gas prevents it from generating steam in the inert gas environment. In other words, after the organic thin film material is heated in an inert gas environment and then evacuated, it is possible to form an organic thin film without emitting ineffective vapor. In this case, the organic evaporation source is configured in advance so that it can be connected to a gas introduction system. When the inert gas is introduced into the container with the gas valve closed, the vacuum tank can be built in a vacuum environment. The organic thin film material is placed in an inert gas environment. This paper size applies the Chinese National Standard (CNS) A4 specification (210X2.97 mm) -10- 409150 a7 ______B7__ 5. Description of the invention (8) In other words, it is not necessary to use inactive gas in order to suppress the release of steam. Introduced into a large vacuum tank. In this case, the vacuum exhaust system can be connected to the organic evaporation source. When the gas valve is closed, the inside of the container can be evacuated, and the introduced inert gas can be evacuated, and then the gas valve can be opened. In other words, in the case where the organic vaporization source of the vacuum exhaust system can be connected, the gas introduction system can be connected, and the gas can be introduced into the container when the gas valve is closed. In addition, the vapor of the organic thin film will be precipitated if it is cooled. Therefore, in the case of the organic evaporation source of the present invention, at least between the container and the discharge port, heating means can be provided to keep the steam until it is released into the vacuum tank. Will not cool down. Printed by the Shellfish Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs On the other hand, when steam is generated from a liquid organic thin film material, a container in which the liquid organic thin film material is arranged inside the organic evaporation source, and a thermal medium Heat medium circulation path of the flow path * If the heat medium circulation path is arranged around the container in advance, the entire container can be uniformly heated or cooled by the heat medium, so the heat uniformity of the organic thin film material can be improved. In this case, a heat medium source for controlling the heat medium to a predetermined temperature is provided, so that the organic thin film material in the container can be heated or cooled, because the liquid organic thin film material and the temperature controlled Because of the heat exchange between the heat media, it is possible to precisely control the temperature rise or cooling of the organic evaporation material. Especially when heating up, 'Because the temperature of the organic film will not be higher than the temperature of the heat medium', the Chinese national standard (CNS) A4 specification (210X297 mm) will not be applied to this paper size. -11-Economy, which central standard Printed by the local shellfish consumer cooperative 40915Q at B7 V. Description of the invention (9) Local overheating of organic thin film. In addition, since the heating is not performed by heat radiation, the organic evaporation material is not heated unevenly due to the fogging of the container. In addition, since the container material is not required to have transparency, it can be made of a ceramic material with high heat conduction efficiency. In other words, manipulating. Becomes easier. In this organic evaporation source, the container is configured as a double structure of an inner container and an outer container, and the space between the inner container and the outer container can be used as the heat medium circulation path. In this case, since the heat exchange is performed between the organic thin film material and the heat medium through the wall surface of the inner container, the heat exchange efficiency is very high, and as a result, the temperature controllability is improved. Further, if a heat insulating material is arranged around the outer container, the thermal efficiency or temperature controllability can be further improved. The container of the organic evaporation source of the present invention has a dual structure of an inner container and an outer container. When the inner container and the outer container are used as the heat medium circulation path, the heat medium source is contacted, and The heat medium source can control the heat medium circulating in the heat medium circulation path to a predetermined temperature, and can be configured to heat or cool the organic thin film material in the container. As described above, since the organic thin film material changes the vapor emission speed according to the atmospheric pressure of the environment, according to the organic thin film manufacturing method of the present invention, the organic thin film material is arranged in an organic evaporation source to release the vapor to the film formation object. When an organic thin film is formed on the surface of an object, the aforementioned organic thin film is controlled. The paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) -12-(Please read the precautions on the back before filling this page) Γ 409150 A7 B7 Economy Printed by the Consumer Standards Cooperative of the Ministry of Standards of the People's Republic of China 5. Description of the invention (10) The pressure of the environment in which the material is placed controls the speed of the aforementioned steam release. As a result, the growth rate of the organic film can be controlled. In addition, according to the organic thin film manufacturing method of the present invention, when an organic thin film material is arranged in an organic evaporation source to emit steam, and an organic thin film is formed on the surface of a film formation object, the organic thin film material can be improved when the organic thin film material is heated. The pressure of the environment where the material is placed to suppress the release of the steam, and then the pressure of the environment where the organic thin film material is placed can be lowered again, so that the steam starts to be emitted. In particular, if the pressure is increased in advance when heating the organic thin film material, the temperature uniformity can be improved, and the heating time required to raise the organic thin film material to a predetermined temperature can be shortened. In addition, because the pressure can be reduced from this state, Since the vapor was immediately released, the time required to start the formation of the organic thin film was shortened. In this way, according to the method for manufacturing an organic thin film of the present invention, once the organic thin film material is heated, it is only necessary to control the vacuum degree of the environment in which the organic thin film material is placed, so that steam can be started or stopped. Thereby, no expensive organic thin film material is wasted. Since the organic thin film material is highly reactive, it is preferable to introduce an inert gas into the environment in which the organic thin film material is placed as the pressure increases. In addition, pressure reduction can be achieved by evacuating the environment by vacuum. Once the vapor of the organic thin film material starts to be released, it can be stopped by increasing the pressure of the environment in which the organic thin film material is placed. This paper size applies to Chinese National Standard (CNS) Λ4 specification (210X297 mm) (Please read the notes on the back before filling this page)
II
經濟部智慧財產局員工消費合作社印製 五、發明說明（11) 在此場合，因爲蒸汽的放出立刻停止的緣故，可以進 行所請良好的「中止」的控制。此外，昂貴的有機薄膜材 料也不會浪費。結束有機薄膜形成作業，冷卻有機薄膜材 料時，也可以藉由將有機薄膜材料置於高壓環境中，使冷 卻速度變快。 根據實驗，在低壓環境即使加熱有機薄膜材料直到放 出蒸汽的溫度爲止，雖然會因爲有機薄膜材料的種類而有 些許不同，但只要周圍的環境壓力上升至1 3.3 P a ( 0.1 Torr)〜2.〇Xl03Pa(15 T o r r ) 程度的話，可以確認蒸汽不再被放出。 但是，壓力升高得太高的話，非活性氣體使用量會增 加，此外，真空排氣使其降低到低壓力爲止的時間也會變 長的緣故，所以在抑制蒸汽放出的場合，以將壓力調整爲 6 6 . 5 P a (0.5 Torr〉程度較佳。 另一方面，如此在高壓力環境將有機薄膜材料昇溫之 後，進行真空排氣降爲低壓力環境，而使放出蒸汽的場合 ，爲了提高有機薄膜的品質，以將壓力降低爲1,3 3 X l〇-4Pa(l.〇xl〇_6 To rr)以下，較佳者爲 降低至 1.33xl〇_5Pa (1.OxlO-7 Torr) 以下的壓力較佳。 因爲有機薄膜材料也會有吸附氣體或是水分的場合， 所以導入前述非活性氣體之前，將前述有機薄膜材料置於 真空環境，進行脫氣者佳。於脫氣時，其將有機薄膜材料 加熱至較其蒸發溫度更低的溫度爲止者較佳。 本紙張尺度適用中國國家標準（_CNS)A4規格（210x297公釐）-14 - (請先随讀背面之注意事項再填寫本頁) -------"•訂----r III11 經濟部中央標準局貝工消費合作衽印製 409150 a7 _____B7__ 五、發明説明（12 ) 升高有機薄膜材料被置放的環.境的壓力時，可以導入 非洁性氣體。 此外，將有機薄膜材料降溫時，也可以在導入非活性 氣體的狀態進行。 實施例 第1圖的符號1 0，係本發明之一例之蒸鍍裝置，具 有真空槽1 1。 於真空槽1 1，接續著真空排氣系1 9 ，及氣體導入 系1 8，其係以當起動被設於真空排氣系1 9的真空幫浦 2 1的話，可以將真空槽1 1內部真空排氣至高真空狀態 的方式構成的。 於真空槽1 1的底壁，設有複數有機蒸發源，此處顯 示有2個有機蒸發源1 、1 22。該有機蒸發源1 2ι 、1 22，分別具有放出口 1 、1 4s，於有機蒸發源 1 、1 22內，將分別被收容於其內的有機薄膜材料加 熱至指定的溫度的話，從放出口 1 、1 42向真空槽 1 1內，放出構成有機薄膜材料的有機化合物的蒸汽的方 式被構成的。 於有機蒸發源1 2i、1 22的上方，設有基板持接件 3 0，於其表面，以將欲形成有機薄膜的表面朝向放出口 14:、14s的狀態，保持成膜對象物13 (此處爲玻璃 基板）。 氣體導入系1 8，具有氣體管2 8，流量控制器2 3 本紙張尺度適用中國國家標準（〇呢）八4祕（2歐297公釐）』 -15 - (請先W洗背面之注意事項再填寫本買) 訂. ;1- ' Μ 409250 A7 B7 五、發明説明（13) ，氣體鋼瓶22，2個閥24】、242。氣體鋼瓶22透 過閥24i，流量控制器23、閥242，藉由氣體管28 與真空槽11的內部環境接續。 於氣體鋼瓶2 2內，以：被充塡著有氮氣或是氬氣等 非活性氣體（此處假設爲氮氣），若打開2個閥2 4i、 2 4 2的話，以流量控制器2 3控制流量的狀態，可以將非 活性氣體導入真空槽11內的方式構成的。 在成膜對象物1 3表面附近，設有可以自由.開閉的遮 板35，另一方面，有機蒸發源12i、122的放出口 1 4 :、1 4 2附近，同樣地設有可自由開閉的蒸發源遮板 33!、332»也就是說，即使是從放出口 14!、142 放出有機薄膜材料的蒸汽的場合，只要將基板遮板3 5或 是蒸發源遮板3 3 i、3 32關閉的話，有機薄膜材料的蒸 汽就不會到達成膜對象物1 3的表面，有機薄膜就不會成 長。 經濟部中央標隼局貝工消費合作社印製 此外，於蒸發源遮板3 3 1、3 3 2的上方位置，以使 不會妨礙從放出口 1 4i、1 42所放出的有機薄膜材料的 蒸汽到達成膜對象物1 3的方式，配置著膜厚監測儀3 6 : 、362，以打開蒸發源遮板3 3:、3 32的話，在膜厚 監測儀3 6 t、3 6 2上分別附著有機薄膜材料的蒸汽，可 以測定成膜對象物13上的有機薄膜形成速度的方式構成 的。 於成膜對象物1 3的周圍與真空槽1 1的底壁，分別 配置著可以導入液態氮的氣密的冷卻壁3 1、3 2，以在 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐) ~ Ί K _ 409150 經濟部中央標準局員工消費合作社印製 A7 B7____ 五、發明説明（14) 使真空槽1 1內成爲真空狀態後’於各冷卻壁3 1、3 2 內導入液態氮的話，真空槽1 1的內.部環境中的水分子有 效率地被吸附於冷卻壁3 1、32，可以從真空槽1 1的 內部環境除去水分子的方式構成的。 於不存在冷卻壁3 1、3 2的場合，在有機薄膜的形 成中，吸附於真空槽1 1壁面的有機薄膜材料的蒸汽再度 脫離，而會混入被形成於成膜對象物1 3表面的有機薄膜 中，冷卻壁3 1、3 2，將朝向真空槽1 1的壁面方向的 有機薄膜材料的蒸汽捕獲，使其不再被放出，而可以獲得 高品質的有機薄膜。 另一方面，於基板持接件3 0內繞拉·著管路3 7，以 在該管路3 7內，流動著熱媒體的方式被構成。亦即，以 使控制溫度之熱媒體進行循環，將有機薄膜形成中的成膜 對象物1 3有效率地加熱使控制在5 0 °C〜1 0 0 °C的溫 度範圍，如此，以藉由進行成膜對象物1 3的溫度控制， 可以於其表面形成密著性佳的有機薄膜的方式被構成的β 有機蒸發源1 、1 22，如第2圖所示，係以藉由 法蘭5 9與0環5 8被氣密地安裝於真空槽1 1底壁的方 式被構成的’此外’以外殻5 1上部的放出口 1 4ι、 1 42朝向真空槽1 1內的方式構成的。 於外殼5 1內’配置著容器5〇，於該容器5〇的周 圍，配置著有底圓筒狀的均熱板5 5 ^此外，於均熱板 5 5，捲繞著微電熱線5 2。此微電熱線5 2，係鎳鉻線 等電阻發熱體***被充塡無機絕緣物的細不銹鋼管的內部 本紙張尺度適用中國固参標準（CNS ) A4規格（2ϊΟχ297公楚) (請先閲木背面之汰1|^項再填寫本育)Printed by the Employees' Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the Invention (11) In this case, because the steam release immediately stopped, you can perform the good “stop” control requested. In addition, expensive organic film materials are not wasted. When the organic thin film forming operation is finished and the organic thin film material is cooled, the organic thin film material may be placed in a high-pressure environment to increase the cooling speed. According to experiments, even if the organic thin film material is heated to a temperature at which steam is emitted in a low-pressure environment, although it is slightly different depending on the type of the organic thin film material, as long as the surrounding environmental pressure rises to 1 3.3 P a (0.1 Torr) ~ 2. 〇Xl03Pa (15 Torr), it can be confirmed that steam is no longer emitted. However, if the pressure is raised too high, the amount of inert gas used will increase, and the time taken for the vacuum exhaust to reduce it to a low pressure will also be longer. Therefore, in order to suppress the release of steam, The adjustment is preferably 6 6. 5 Pa (0.5 Torr). On the other hand, after the organic thin film material is heated in a high pressure environment, the vacuum exhaust is reduced to a low pressure environment, and the steam is emitted in order to Improve the quality of the organic film to reduce the pressure to 1,3 3 X 10-4 Pa (1.0 x 10-10 Torr), preferably to 1.33 x 10-5 Pa (1.OxlO-7 The pressure below Torr) is better. Because organic thin film materials may also adsorb gas or moisture, it is better to degas the organic thin film material before introducing the inert gas. It is better to degas. It is better to heat the organic thin film material to a temperature lower than its evaporation temperature. This paper size is applicable to China National Standard (_CNS) A4 size (210x297 mm) -14-(Please read the note on the back first Matters refill this Page) ------- " • -------- III III11 Shellfish Consumer Cooperation of the Central Bureau of Standards of the Ministry of Economic Affairs print 409150 a7 _____B7__ V. Description of the Invention (12) Raised organic thin film materials are placed When the ambient pressure is under pressure, a non-clean gas can be introduced. In addition, when the organic thin film material is cooled, it can also be performed in a state where an inert gas is introduced. The reference numeral 10 in the first embodiment is an example of the present invention. The vapor deposition device has a vacuum tank 11 and a vacuum exhaust system 19 followed by a vacuum exhaust system 19 and a gas introduction system 18, which are vacuum pumps provided in the vacuum exhaust system 19 when started. If it is 2, it can be constructed by evacuating the inside of the vacuum tank 11 to a high vacuum state. The bottom wall of the vacuum tank 11 is provided with a plurality of organic evaporation sources. Here, two organic evaporation sources 1 and 1 are displayed. 22. The organic evaporation sources 12 and 12 have discharge ports 1 and 14s respectively, and the organic thin film materials contained in the organic evaporation sources 1 and 1 22 are heated to a specified temperature. The discharge ports 1 and 1 42 discharge the organic thin film material into the vacuum tank 1 1 The organic compound is formed in the form of steam. Above the organic evaporation sources 12i and 1222, a substrate holder 30 is provided on the surface thereof so that the surface to be formed with an organic thin film faces the discharge port 14 :, In the state of 14s, the film-forming object 13 (here, the glass substrate) is maintained. The gas introduction system 1 8 has a gas tube 2 8 and a flow controller 2 3 This paper is in accordance with the Chinese national standard (0?) 2 Euro 297 mm) "-15-(please pay attention to the back of the wash before filling out this purchase) order.; 1-'M 409250 A7 B7 V. Description of the invention (13), gas cylinder 22, 2 valves 24 ], 242. The gas cylinder 22 passes through the valve 24i, the flow controller 23, and the valve 242, and is connected to the internal environment of the vacuum tank 11 through a gas pipe 28. In the gas cylinder 2 2, it is filled with inert gas such as nitrogen or argon (here it is assumed to be nitrogen). If the two valves 2 4i and 2 4 2 are opened, the flow controller 2 3 The state of controlling the flow rate may be configured such that an inert gas is introduced into the vacuum tank 11. A shutter 35 that can be opened and closed freely is provided near the surface of the film-forming object 13, and on the other hand, the openings 1 4: and 1 4 2 of the organic evaporation sources 12i and 122 are similarly opened and closed. Evaporation source shields 33 !, 332 »That is, even when the steam of the organic thin film material is emitted from the discharge ports 14 !, 142, as long as the substrate shield 3 5 or the evaporation source shields 3 3 i, 3 When 32 is closed, the vapor of the organic thin film material will not reach the surface of the film object 1 3, and the organic thin film will not grow. Printed by Shellfish Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. It should be placed above the evaporation source shields 3 3 1 and 3 3 2 so as not to hinder the release of organic thin film materials from the outlets 1 4i and 1 42. A film thickness monitor 3 6:, 362 is provided to reach the film object 1 3 to open the evaporation source shutters 3 3: and 3 32, and the film thickness monitor 3 6 t, 3 6 2 Each of the vapors of the organic thin film material is adhered to each other, and it is possible to measure the formation speed of the organic thin film on the film formation object 13. Around the film-forming object 1 3 and the bottom wall of the vacuum tank 11, air-tight cooling walls 3 1 and 3 2 capable of introducing liquid nitrogen are respectively arranged to apply the Chinese National Standard (CNS) A4 at the paper scale. Specifications (210X297mm) ~ Ί K _ 409150 Printed by the Consumers 'Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7____ V. Description of the invention (14) After the vacuum tank 1 1 has been turned into a vacuum state,' on each cooling wall 3 1, 3 2 When liquid nitrogen is introduced into the inside of the vacuum tank 11, water molecules in the internal environment of the vacuum tank 11 are efficiently adsorbed on the cooling walls 3 1 and 32, and the water molecules can be removed from the internal environment of the vacuum tank 11. When there are no cooling walls 3 1 and 3 2, during the formation of the organic thin film, the vapor of the organic thin film material adsorbed on the wall surface of the vacuum tank 11 is detached again, and will be mixed into the surface of the film forming object 13. Among the organic thin films, the cooling walls 3 1 and 3 2 capture the vapor of the organic thin film material toward the wall surface direction of the vacuum tank 11 so that it is no longer released, and a high-quality organic thin film can be obtained. On the other hand, a pipe 37 is drawn around the substrate holder 30, and a heat medium flows in the pipe 37. That is, the temperature-controlled heat medium is circulated, and the film-forming object 13 during the formation of the organic thin film is efficiently heated to be controlled in a temperature range of 50 ° C to 100 ° C. The β organic evaporation sources 1 and 1 22 are formed by controlling the temperature of the film-forming object 13 to form an organic thin film with excellent adhesion on the surface, as shown in FIG. 2. Blue 5 9 and 0 ring 5 8 are configured to be airtightly mounted on the bottom wall of the vacuum tank 1 1. In addition, they are configured such that the upper part of the casing 5 1 discharge ports 1 4 ι and 1 42 face the inside of the vacuum tank 11. of. A container 50 is disposed inside the casing 51, and a bottomed cylindrical heating plate 5 5 is arranged around the container 50. A micro electric heating wire 5 is wound around the heating plate 5 5 2. This micro electric heating wire 5 2 is a nickel-chromium wire and other resistance heating elements are inserted into the thin stainless steel tube filled with inorganic insulators. The paper size is applicable to the Chinese Solid Standards (CNS) A4 specification (2ϊ〇χ297 公 楚) (Please read first (Tip 1 | ^ items on the back of the wood, fill in this education)
phn Μ: ^ :| Λ:>w -17- 409150 A7 B7 ________五、發明説明（彳5 ) 者。 於均熱板5 5的底部，設有熱電.偶5 6 ’藉由熱電偶 5 6以使均熱板5 5的溫度成爲指定的溫度的方式監視之 ，同時由被配置在真空槽11外部的電源通電至微電熱線 5 2使其發熱，以可以將被容納於容器5 0內的有機薄膜 材料54，維持於150 °C〜400 °C的溫度範圍內的所 要溫度的方式構成的。 微電熱線5 2的周圍，配置著有反射板5 3，反射由 微電熱線5 2朝向外殼5 1放射的熱輻射，以抑制外殼 5 1的溫度上昇，同時可將容器5 0有效率地加熱的方式 構成的。 又，微電熱線52的捲繞密度，在放出口 1 、 1 4 2側較密集，而在容器5 0的底面側較稀疏，以使放出 口 1 、1 42的溫度較容器5 0或是有機物5 4的溫度 更高的方式構成的，其結果使得所產生的有機薄膜材料的 蒸汽不會附著於放出口 1 、1 42附近。 如此的有機蒸發源之1 2:、1 2s，於一方的有機蒸 發源1 2:內，將具有下圖所示的化學式的化合物A 1 q3 〔Tris ( 8-hydroxy quinoline ) aluminium ’ sublimed]( 三（8 —基）鋁，已昇華的）’ _phn Μ: ^: | Λ: > w -17- 409150 A7 B7 ________ 5. The description of the invention (5). At the bottom of the soaking plate 5 5 is provided a thermocouple. The thermocouple 5 6 ′ monitors the temperature of the soaking plate 5 5 to a predetermined temperature by means of the thermocouple 5 6 and is arranged outside the vacuum tank 11. The electric power source is supplied to the micro electric heating line 52 to generate heat, and is configured so that the organic thin film material 54 contained in the container 50 can be maintained at a desired temperature within a temperature range of 150 ° C to 400 ° C. Around the micro electric heating wire 5 2, a reflecting plate 5 3 is arranged to reflect the heat radiation radiated from the micro electric heating wire 5 2 toward the casing 51 to suppress the temperature rise of the casing 51 and at the same time, the container 50 can be efficiently Constructed by heating. In addition, the winding density of the micro-electric heating wire 52 is denser on the sides of the discharge ports 1 and 1 2 and sparse on the bottom side of the container 50 so that the temperatures of the discharge ports 1 and 1 42 are higher than those of the container 50 or 50. The temperature of the organic substance 54 is higher, and as a result, the generated vapor of the organic thin film material does not adhere to the vicinity of the discharge ports 1 and 1 42. In such an organic evaporation source 1 2: 1 and 12 s, in one of the organic evaporation sources 1 2 :, a compound A 1 q3 having the chemical formula shown in the figure below [Tris (8-hydroxy quinoline) aluminium 'sublimed] ( Three (8-based) aluminum, sublimated) '_
40915C A7 ______B7_ 五、發明説明（16 ) 配置作爲有機薄膜材料。此A 1 q 3係粉體狀之具有昇 華性的有機薄膜材料。 首先，起動前述的真空幫浦2 1，將真空槽1 1內抽 成真空環境，在該狀態將成膜對象物1 3搬入。將真空槽 11內進而抽至更低的真空，將成膜對象物13，與有機 蒸發源121內的八1(13置於1.〇\1〇-6 T 〇 r r 的真空環境（第4圓的步驟Sd 。 在該狀態對有機蒸發源1 2 :內的微電熱線5. 2通電， 將Alq3加熱至l〇〇°C〜200°C。在此溫度，由 A 1 q3所產生的蒸汽產生量很少，吸附氣體被放出。 進行2 0〜3 0分鐘的脫氣（S2)，接著將真空槽 1 1內真空排氣同時由氣體導入口 2 9將氮氣導入作爲非 活性氣體（S 3 )。' 真空槽1 1內與有機蒸發源1 在壓力1 3.340915C A7 ______B7_ V. Description of the invention (16) Configured as an organic thin film material. This A 1 q 3 series powder is a sublimable organic thin film material. First, the above-mentioned vacuum pump 21 is started, the inside of the vacuum tank 11 is evacuated, and the film-forming object 13 is carried in this state. The vacuum chamber 11 is further evacuated to a lower vacuum, and the film-forming object 13 and the 8-1 (13 in the organic evaporation source 121 are placed in a vacuum environment of 1.〇 \ 1〇-6 T 〇rr (No. 4 Round step Sd. In this state, the micro-heating wire 5.2 inside the organic evaporation source 12: is energized, and the Alq3 is heated to 100 ° C to 200 ° C. At this temperature, the amount produced by A1q3 The amount of steam generated is very small, and the adsorbed gas is released. After degassing for 20 to 30 minutes (S2), the vacuum in the vacuum tank 11 is evacuated at the same time and the nitrogen is introduced as an inert gas through the gas introduction port 29 ( S 3). 'Vacuum chamber 1 1 and organic evaporation source 1 at pressure 1 3.3
Pa (〇.1 Torr)的非活性氣體環境下安定之後， 經濟部中央標準局員工消费合作社印製 (請先聞衆背面之ί£意事項再填寫本頁) 增加對微電熱線5 2的通電量，將蒸發源1 2^內的 A 1 q3昇溫到蒸發溫度（在此A 1 q3爲3 0 0°C程度） (S4) »在此昇溫之時，因爲A1q3係被置於非活性氣 體環境‘中的緣故，A I q3粒子間可以有效率地傳熱，不會 發生溫度的過熱，此外A 1 q3蒸汽的產生也未被觀察到。 A丨d 3安定處於該蒸發溫度之後，停止非活性氣體的 導入，將真空槽1 1內再度抽真空成爲1.3 3 X 1 0—4 Pa (1.0xl0_6Torr) ( S 5 )。 真空槽1 1內安定於該壓力時，保持在關閉基板遮板 本紙張尺度適用中國國家標準（CNS ) Α4规格（210X297公釐） -19- 經濟部t央標準局貝工消費合作社印製 40915G Α7 Β7 五、發明説明（彳7) 3的狀態下，打開蒸發源遮板33:，從放出口 14^將 A 1 Q 3蒸汽放出。 . A i q 3蒸汽到達膜厚監測儀3 6 i ,，因爲於其表面 被形成有機薄膜的緣故，測定其成長速度，在成長速度安 定時打開基板遮板3 5，對成膜對象物1 3表面開始形成 有機薄膜（AlQ3薄膜）（S6)。 進行5分鐘的有機薄膜的形成，到達指定膜厚時關閉 基板遮板3 5與蒸發源遮板3 3:，停止對微電.熱線5 2 之通電，結束蒸鍍（S 7)。. 其次，從氣體導入口 2 9將非活性氣體導入真空槽 11內，將有機蒸發源12!內的Alq3置於壓力 1 3 . 3 P a (0.1 Tor r)的非活性氣體環境，使停 止產生A1Q3蒸汽。此時，非活性氣體成爲熱媒體，此 外因爲產生對流的綠故，’所以A 1 q 3的冷卻變快。 第5圖顯示上述有機薄膜形成工程中，在非活性氣體 環境下從A 1 Q3的昇溫開始直到蒸鍍結束冷卻爲止的 A 1 q 3的溫度變化與蒸發速度的變化。又，第6圖顯示 在真空氣氛下的A 1 Q3與下述化學式Pa (〇.1 Torr) after stabilization in an inert gas environment, printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please listen to the matter on the back of the public before filling out this page) Add the micro electric hotline 5 2 The amount of electricity is used to heat up A 1 q3 in the evaporation source 1 2 ^ to the evaporation temperature (here A 1 q3 is about 3 0 0 ° C) (S4) »At this time, because the A1q3 system is placed in inactive In the gas environment ', AI q3 particles can efficiently transfer heat without overheating of the temperature, and the generation of A 1 q3 steam has not been observed. After A 3 d is stable at this evaporation temperature, the introduction of the inert gas is stopped, and the inside of the vacuum tank 11 is evacuated again to 1.3 3 X 1 0-4 Pa (1.0xl0_6Torr) (S 5). When the pressure in the vacuum tank 11 is settled, the substrate is kept closed when the pressure is closed. The paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm). Α7 Β7 5. In the state of the invention (彳 7) 3, open the evaporation source shield 33: and release A 1 Q 3 steam from the discharge port 14 ^. A iq 3 reaches the film thickness monitor 3 6 i, and because the organic thin film is formed on the surface, the growth rate is measured, and the substrate shield 3 5 is opened at a constant growth rate, and the film formation object 1 3 An organic thin film (AlQ3 thin film) begins to form on the surface (S6). The formation of the organic thin film is performed for 5 minutes, and the substrate shield 35 and the evaporation source shield 3 3: are closed when the predetermined film thickness is reached, and the energization of the micro-electricity and hotline 5 2 is stopped, and the evaporation is terminated (S 7). Next, the inert gas is introduced into the vacuum tank 11 from the gas introduction port 29, and the Alq3 in the organic evaporation source 12! Is placed in an inert gas environment with a pressure of 13.3 Pa (0.1 Tor r) to stop A1Q3 steam is produced. At this time, the inert gas becomes a heat medium, and since convection green is generated, the cooling of A 1 q 3 becomes faster. Fig. 5 shows the temperature change and evaporation rate change of A1q3 in the above-mentioned organic thin film formation process from the temperature rise of A1Q3 to the cooling completion of vapor deposition in an inert gas environment. Fig. 6 shows A 1 Q3 and the following chemical formula in a vacuum atmosphere.
所示的T D P的溫度與蒸發速度的關係。 從第6圖來看’可知在真空環境下，A 1 q3在 本紙張尺度適用中國國家標準（CNS ) A4規格（21〇χ297公釐） (請先聞资背面之·注意事項再填寫本頁)The relationship between the temperature of T D P and the evaporation rate is shown. Looking at Figure 6, it can be seen that in a vacuum environment, A 1 q3 applies the Chinese National Standard (CNS) A4 specification (21〇 × 297 mm) in this paper standard. (Please read the notes on the back of the asset before filling in this page. )
20 409150 A7 B7 五、發明説明（彳8 ) 3 0 0 t：前後的溫度，T D P則在2 .3 0 °C的溫度前後產 生有機薄膜材料的蒸發。另一方面’由第5圖可知’在真 空環境下即使將Alq3昇溫至產生有機薄膜材料的蒸汽 的溫度爲止，在非活性氣體中不會產生A 1 q 3蒸汽。也 就是說，可知有機薄膜材料的蒸汽的產生，可以藉由非活 性氣體環境的壓力抑制之。 又，從第5圖可知，在非活性氣體環境中昇溫有機薄 膜材料的場合，未觀察到溫度過熱。 第7圖顯示與以上之有機薄膜製造方法比較，如從前 技術般的，不使用.非活性氣體而形成有機薄膜的場合之 A 1 q 3的溫度變化與蒸發速度的變化<在昇溫時，因爲 A 1 Q3是被真空絕熱的，產生部分過熱，可觀察到溫度 過熱的現象。此外在昇溫時與冷卻時，產生A1Q3蒸汽 ，可知會產生多量對於有機薄膜的形成並無貢獻的A 1 Q 3 蒸汽。 其次’說明適於液體狀的有機薄膜材料的加熱、冷卻 的有機蒸發源。 經濟部中央標準局負工消費合作社印製 (請先聞请背面之注意事項再填寫本頁) 參照第3圖’符號4 2係藉由液體狀的熱媒體進行有 機薄膜材料的溫度控制（加熱、冷卻）之油浴方式的有機 蒸發源’也可以改換爲第1圖所記載的有機蒸發源1 21、 1 2 2.設於真空槽]_ 1。 此有機蒸發源42，特別是適於在_2〇°C〜180 °C的溫度範圍，維持有機材料的溫度於一定，使產生有機 薄膜材料的蒸汽的場合’具有外殼7 1、容器7 〇與熱媒 本&張尺度適用中國國家標準（CNS ) A4&格（2T〇^297i^-：-' 409150 A7 B7 五、發明説明（19 ) 體源6 0。 容器7 0，被鑲入外殼7 1內，外殼7 1成爲外側容 器，而容器7 0成爲內側容器之雙重構造，其間被當成熱 媒體的循環路徑7 8。熱媒體源6 0具有油浴6 3，及電 熱器6 5，及投入式冷卻器6 4，以使被貯藏於油浴6 3 內的矽油可以加熱或冷卻熱媒體6 1的方式構成的。 於熱媒體61內被浸漬著供給管66:的先端，而且 係以若使被設於供給管6 6 i的途中的循環幫浦6.2動作的 話，油浴63內的熱媒體61被吸起，通過供給管6 6 l 被供給到循環路徑7 8內，透過容器7 0與有機薄膜材料 74熱交換之後，通過排出管662而回到油浴63的方 式構成的。 於容器7 0的上端，氣密地接續著蒸汽放出管7 5的 一端，從另一端的放出口 4 4，係以可以將容器7 0內所 產生的有機薄膜材料的蒸汽，放出至第3圖所未顯示出的 真空槽內的方式構成的。 經濟部中央標準局員工消費合作社印製 (請先閲赛背面之洼$項再填寫本莧) 於蒸汽放出管7 5的途中，設有可以控制氣體的通過 之開閉閥4 5，於被設於開閉閥4 5與容器7 0之間的蒸 汽放出管7 5，被接續著氣體管4 3的一端。氣體管4 3 的另一端，設有被充塡著氮氣或氬氣等非活性氣體的氣體 鋼瓶46，於氣體管43的途中，設有氣體閥48i、 482。氣體管43，在氣體閥48:、482之間分歧， 於分歧部分的途中，設有氣體閥4 8 3，其先端被接續著真 空幫浦4 7。 本紙張尺度適用中國國家標準（CNS〉A4規格（210X297公釐） -22- 409150 A7 _ .__B7_五、發明説明（2〇 ) 外殼7 1內的容器7 0中，例如容納著有以下列化學 式.20 409150 A7 B7 V. Description of the invention (彳 8) 3 0 0 t: temperature before and after, T D P evaporation of organic thin film material occurs at a temperature around 2.3 ° C. On the other hand, as can be seen from Fig. 5, A 1 q 3 vapor is not generated in an inert gas even if Alq 3 is heated to a temperature at which the vapor of the organic thin film material is generated in a vacuum environment. That is to say, it can be seen that the generation of vapor of the organic thin film material can be suppressed by the pressure of the inert gas environment. In addition, it can be seen from Fig. 5 that when the organic thin film material is heated in an inert gas environment, no overheating of the temperature is observed. Fig. 7 shows the temperature change of A 1 q 3 and the change of evaporation rate in the case of forming an organic thin film without using an inert gas, as in the prior art, as compared with the above organic thin film manufacturing method. Because A 1 Q3 is insulated by vacuum, partial overheating occurs, and the phenomenon of overheating of temperature can be observed. In addition, A1Q3 steam was generated during the temperature rise and cooling, and it was found that a large amount of A1Q3 steam that did not contribute to the formation of the organic thin film was generated. Next, an organic evaporation source suitable for heating and cooling a liquid organic thin film material will be described. Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives (please read the notes on the back before filling out this page) Refer to Figure 3 'Symbol 4 2 Series for temperature control of organic thin film materials (heating by liquid heat medium) , Cooling) oil bath type organic evaporation source 'can also be replaced with the organic evaporation source 1 21, 1 2 described in Figure 1 2. Installed in a vacuum tank] _ 1. This organic evaporation source 42 is particularly suitable for the case where the temperature of the organic material is maintained at a temperature range of -20 ° C to 180 ° C so that the vapor of the organic thin film material is generated. 'It has a casing 7 1 and a container 7 〇 And the heat medium book & Zhang scale is applicable to Chinese National Standard (CNS) A4 & grid (2T〇 ^ 297i ^-:-'409150 A7 B7 V. Description of the invention (19) Volume source 6 0. Container 70, is inserted into Inside the casing 71, the casing 71 becomes the outer container, and the container 70 becomes the double structure of the inner container, which is used as a circulation path for the heat medium 78. The heat medium source 60 has an oil bath 6 3, and an electric heater 6 5 And the input cooler 6 4 is configured so that the silicone oil stored in the oil bath 6 3 can heat or cool the heat medium 61. The heat medium 61 is impregnated with the tip of the supply pipe 66 :, and When the circulation pump 6.2 provided in the middle of the supply pipe 6 6 i is operated, the heat medium 61 in the oil bath 63 is sucked up, is supplied into the circulation path 78 through the supply pipe 6 6 l, and passes through After the container 70 is heat-exchanged with the organic thin film material 74, it returns to the side of the oil bath 63 through the discharge pipe 662 The upper end of the container 70 is airtightly connected to one end of the steam discharge pipe 75 and the discharge port 4 4 from the other end is for the steam of the organic thin film material generated in the container 70. Released into a vacuum tank not shown in Figure 3. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the $ item on the back of the competition before filling in this note) on the steam release tube 7 5 On the way, an on-off valve 45, which can control the passage of gas, is provided, and a steam release pipe 75, which is provided between the on-off valve 45 and the container 70, is connected to one end of the gas pipe 4 3. The gas pipe 4 3 On the other end, a gas cylinder 46 filled with inert gas such as nitrogen or argon is provided, and gas valves 48i and 482 are provided on the way of the gas pipe 43. The gas pipe 43 is provided between the gas valves 48: and 482. There is a divergence between them. On the way of the divergence part, there is a gas valve 4 8 3, whose tip is followed by a vacuum pump 4 7. This paper size applies to the Chinese national standard (CNS> A4 specification (210X297 mm) -22-409150 A7 _ .__ B7_ V. Description of the invention (20) In the container 70 in the casing 71, The houses have the following chemical formula.
MDA 所表示之 MDA(4，4’ — diamino-diphenyl methan ; 4，4’ -二胺基二苯基甲烷）或是以下列化學式MDA (4,4 ’— diamino-diphenyl methan; 4,4’ -diaminodiphenylmethane) represented by MDA or the following chemical formula
MDI (請先閲资背面^注意事項再填寫本頁) ii 41 經濟部中央標準局貝工消費合作社印袋 所表示之 M D I ( 4 ，4 ’ — diphenyl- methan- diisocyanate ; 4，4’ 一二苯基甲烷異氰酸酯）等的液體 狀有機薄膜材料7 4，關閉被設於蒸汽放·出管7 5的開閉 閥45與氣體鋼瓶46之前的氣體閥482 ，使真空幫浦 47動作，打開其他氣體閥48〗、483的話容器70內 被真空排氣，有機薄膜材料7 4被置於真空環境。 在該狀態使循環幫浦動作，將有機薄膜材料7 4在真 空環境中昇溫至不產生有機薄膜材料的蒸汽的溫度進行脫 氣。 接著，關閉真空幫浦47之前的開閉閥483，而打開 氣體鋼瓶46之前的氣體閥482的話，氣體鋼瓶46內 的非活性氣體流過氣體管4 3，被導入容器7 0內，有機 薄膜材料7 4被置於非活性氣體環境。 容器7 ◦內成爲13.3Pa〜2.0xi03Pa ( 0.1 T〇rr〜15 To rr)程度的壓力的非活性氣 體環境之後，關閉非活性氣體流動路徑上的2個氣體閥 本紙張尺度適用中國國家標準（C.NS ) A4規格.（210X297公釐） -X, -23- 經濟部中央標準局員工消費合作社印製 409150 at ___ B7 五、發明説明（21 ) 48ι、482 ’接著，使熱媒體6 1的溫度上升，被導入 循環路徑7 8內的話，該熱媒體6 1.，與容器7 0的周圍 以及底面接續同時流動，容器7 〇全體被均一地加熱，結 果，有機薄膜材料被均勻地加熱。 在該狀態將熱媒體以指定的昇溫速度提高溫度的話， 有機薄膜的溫度也跟著上升。 此時’有機薄膜材料7 4被置於指定壓力的非活性氣 體環境’有機薄膜材料7 4，在低壓力（真空環境）下即 使上升到產生蒸汽的蒸發溫度，也因爲環境壓力而成爲不 會產生有機薄膜材料74的蒸汽。 有機薄膜材料7 4，在該蒸發溫度安定之後，以關閉 氣體鋼瓶4 6之前的氣體閥4 82的狀態，打開氣體閥 、482 ’藉由真空幫浦47將蒸發容器70內真空 排氣的話有機薄膜材料7 4的周圍環境的壓力降低，結果 ，開始產生有機薄膜材料7 4的蒸汽。 在容器7 0內安定於指定的壓力時打開開閉閥4 5的 話，有機薄膜材料7 4的蒸汽通過蒸汽放出管7 5從放出 口44向真空槽內放出。 於蒸汽放出管7 5捲繞著微電熱線7 2，係以可以另 外進行不同於熱媒體6 1的溫度控制的方式構成的。從有 機薄膜材料7 4放出蒸汽時，預先對微電熱線7 2通電， 以使蒸汽放出管7 5的溫度成爲較有機薄膜材料7 4的溫 度更高的方式預先加熱。 如此，預先將蒸汽的通路加熱的話，有機薄膜材料 本紙張尺度逋用中國國家標準（CNS ) A4规格（210X297公釐） (請先閲#背面^'注意事項再填窝本頁) .tr X-. -24- 409150 A7 ___B7_ 五、發明説明（22) 7 4的蒸汽就不會被冷卻，也就是說，有機薄膜材料7 4 的蒸汽不會在蒸汽放出管7 5的途中析出，成爲不會·塞住 開閉閥4 5 ^ 真空槽內安定於1.33x10 4 Pa (1·〇χ1〇 -6 To I· r )的壓力後，與第1圖的蒸鍍裝置1 〇的場合相 同，打開被設於放出口 4 4上部的蒸發源遮板，以被Μ 於放出口 4 4上部的膜厚監測儀確認有機薄膜材料7 4的 蒸汽被安定放出之後，打開基板遮板，開始對成，.膜對象牧f 表面形成有機薄膜。 有機薄膜被形成至指定厚度後，關閉開閉閥4 5，結 束對真空槽內的有機薄膜材料7 4的蒸汽·放出。接著，將: 非活性氣體導入容器7 0內，使冷卻器6 4動作把熱媒體 6 3降溫。此時，非活性氣體被導入容器7 0內，医|爲壓 力變高的緣故，抑制有機薄膜材料7 4的蒸汽的產生，以 不產生無效浪費的蒸汽的狀態進行有機薄膜材料7 4的冷 卻。 另一方面，結束蒸鍍之後，在真空槽內，被形成有機 薄膜的成膜對象物與未處理的成膜對象物交換，開始下一 個蒸鍍作業。 以上所述，僅說明形成一層有機薄膜的場合，但是使 用複數有機蒸發源，形成多成有機薄膜的場合，也只要將 各有機蒸發源內的有機薄膜材料在昇溫降溫時置於非活性 氣體環境即可。 有機薄膜材料可以是液體也可以是固體，特別是針對 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 經濟部中央標準局員工消費合作社印製 409150 A7 B7__ 五、發明説明（23 ) 粉體狀者，因爲非活性氣體侵入粉體粒子間’成爲熱媒體 的緣故所以昇溫、冷卻速度變快’有機薄膜材料的均熱性 也可以提高。 另一方面，液體狀的有機薄膜材料的場合，因爲藉由 熱媒體進行昇溫以及降溫，所以熱交換的效率很高。特別 是在昇溫時，有機薄膜材料的溫度不會較熱媒體的溫度更 高，所以不會產生突沸。熱媒體除了砂油等液體之外’也 可以是氣體。 又，於上述實施例使用氮氣氣體作爲非活性氣體，只 要是不與有機薄膜材料起反應的氣體，也可以使用其他氣 Μ曲 體。 如此，根據本發明，在冷卻、昇溫時不產生無效浪費 的有機薄膜材料的蒸汽，此外，有機薄膜材料的昇溫速度 、冷卻速度也變快。 進而，溫度控制性提高，不會產生溫度過高的緣故， 所以發生有機薄膜材料的突沸。 此外，因爲提高有機薄膜材料的均熱性，所以直到有 機薄膜材料的蒸汽產生速度安定下來爲止所需要的時間變 短。 圖面之簡單說明 第1圖係本發明的蒸鍍裝置之一例。 第2圖係使用於本發明的蒸鍍裝置之有機蒸發源之一 例。 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐} (請先閎.背面ti£意事項再填寫本頁)MDI (please read the back of the fund ^ Note before filling in this page) ii 41 MDI (4, 4 '— diphenyl-methan- diisocyanate; 4, 4' 12) Liquid organic thin film material 74 such as phenylmethane isocyanate), and closed the on-off valve 45 and the gas valve 482 before the gas cylinder 46 in the steam discharge and discharge pipe 75, and the vacuum pump 47 is operated to open other gases When the valves 48 and 483 are evacuated, the inside of the container 70 is evacuated, and the organic thin film material 74 is placed in a vacuum environment. The circulation pump is operated in this state, and the organic thin film material 74 is heated in a vacuum environment to a temperature at which no vapor of the organic thin film material is generated, and degassed. Next, when the on-off valve 483 before the vacuum pump 47 is closed and the gas valve 482 before the gas cylinder 46 is opened, the inert gas in the gas cylinder 46 flows through the gas pipe 43 and is introduced into the container 70. The organic thin film material 7 4 is placed in an inert gas environment. Container 7 ◦ After the inert gas environment at a pressure of 13.3Pa ~ 2.0xi03Pa (0.1 Torr ~ 15 To rr), close the 2 gas valves on the flow path of the inert gas. This paper applies Chinese national standards ( C.NS) A4 specifications. (210X297mm) -X, -23- Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 409150 at ___ B7 V. Invention Description (21) 48ι, 482 'Next, make the hot media 6 1 If the temperature rises and is introduced into the circulation path 78, the heat medium 61 will flow simultaneously with the surrounding and bottom surface of the container 70, and the entire container 70 will be uniformly heated. As a result, the organic thin film material will be uniformly heated. . When the temperature of the heat medium is increased at a predetermined temperature increase rate in this state, the temperature of the organic thin film also increases. At this time, the 'organic thin film material 7 4 is placed in a non-reactive gas environment at a specified pressure'. The organic thin film material 7 4 will not rise under the low pressure (vacuum environment) to the evaporation temperature at which the steam is generated. The vapor of the organic thin film material 74 is generated. After the organic thin film material 7 4 is stabilized, the gas valve 4 82 before the gas cylinder 4 6 is closed, the gas valve is opened, and 482 ′ is vacuum-evacuated in the evaporation container 70 by a vacuum pump 47. The pressure of the surrounding environment of the thin film material 74 is reduced, and as a result, steam of the organic thin film material 74 is started to be generated. When the on-off valve 45 is opened when the pressure in the container 70 is stabilized at a predetermined pressure, the vapor of the organic thin film material 74 is discharged from the discharge port 44 into the vacuum tank through the steam discharge pipe 75. A micro electric heating wire 72 is wound around the steam release pipe 75, and is configured so that it can perform temperature control different from that of the heat medium 61. When steam is emitted from the organic thin film material 74, electricity is applied to the micro electric heating wire 72 in advance so that the temperature of the steam discharge pipe 75 is higher than that of the organic thin film material 74. In this way, if the steam path is heated in advance, the organic thin film material will use the Chinese National Standard (CNS) A4 specification (210X297 mm) (please read the # back ^ 's precautions before filling this page) .tr X -. -24- 409150 A7 ___B7_ V. Description of the invention (22) The steam of 7 4 will not be cooled, that is, the steam of the organic thin film material 7 4 will not precipitate on the way of the steam discharge pipe 7 5 and will not After closing the on-off valve 4 5 ^, the pressure in the vacuum tank was set to 1.33 × 10 4 Pa (1.0 × 10-6 To I · r), and then opened in the same manner as in the case of the vapor deposition device 1 in FIG. 1 and opened. The evaporation source shield provided on the upper part of the discharge port 4 4 is confirmed by the film thickness monitor on the upper part of the discharge port 4 4 to release the steam of the organic thin film material 7 4. Then, the substrate shield is opened and the pairing is started. An organic thin film is formed on the surface of the film object. After the organic thin film is formed to a predetermined thickness, the on-off valve 45 is closed, and the steam and the organic thin film material 7 4 in the vacuum chamber are released. Next, the inert gas is introduced into the container 70, and the cooler 64 is operated to cool the heat medium 63. At this time, the inert gas is introduced into the container 70, so that the organic film material 74 is suppressed from generating steam because the pressure becomes high, and the organic film material 74 is cooled without generating inefficient waste steam. . On the other hand, after the vapor deposition is completed, the film-forming object on which the organic thin film is formed is exchanged with the unprocessed film-forming object in the vacuum chamber, and the next vapor deposition operation is started. The above description only describes the case of forming one layer of organic thin film, but when multiple organic evaporation sources are used to form multiple organic thin films, the organic thin film materials in each organic evaporation source need only be placed in an inactive gas environment during temperature rise and temperature reduction. Just fine. Organic thin film materials can be liquid or solid, especially for this paper size. Chinese National Standard (CNS) A4 specification (210X297 mm) applies. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economy. 409150 A7 B7__ V. Description of the invention (23 ) In the case of powder, the infiltration of inert gas between the powder particles becomes a heat medium, so that the temperature rises and the cooling rate becomes faster. The thermal uniformity of the organic thin film material can also be improved. On the other hand, in the case of a liquid organic thin film material, the heat exchange efficiency is high because the temperature is raised and lowered by a heat medium. Especially when the temperature is raised, the temperature of the organic thin film material is not higher than that of the heat medium, so bumping does not occur. The heat medium may be a gas other than a liquid such as sand oil. Also, in the above embodiment, a nitrogen gas is used as the inert gas, and other gases may be used as long as they do not react with the organic thin film material. As described above, according to the present invention, the vapor of the organic thin film material is not generated inefficiently during cooling and heating, and the heating rate and cooling rate of the organic thin film material are also increased. Furthermore, since the temperature controllability is improved and the temperature is not excessively high, bumping of the organic thin film material occurs. In addition, since the soaking property of the organic thin film material is improved, the time required until the vapor generation rate of the organic thin film material is stabilized is shortened. Brief Description of Drawings Fig. 1 is an example of a vapor deposition apparatus according to the present invention. Fig. 2 is an example of an organic evaporation source used in the vapor deposition apparatus of the present invention. This paper size applies to China National Standard (CNS) Α4 specification (210X297 mm) (please note first. Please note on the back and fill in this page)
-26- 409150 A7 B7 經濟部中央標準局貝工消費合作社印裂 五、發明説明（24 ) 第3圖係本發明的有機蒸發源之一例。 第4圖係供說明本發明的方法的流程圖。 第5圖係供說明藉本發明的方法形成有機薄膜的場合 之有機薄膜材料的溫度變化與蒸發速度的變化之圖。 第6圖係供說明A 1 q 3及TPD的溫度與蒸發速度的 關係之圖。 第7圖係供說明以先行技術形成有機薄膜的場合之有 機薄膜材料的溫度變化與蒸發速度的變化之圖。.. 第8圖（a )〜（e ):供說明先行技術之蒸發源的 圖。. 符號說明 10 蒸鍍裝置 11 真空槽 12i' 1 2 2 ' 4 2 有機蒸發源 13 成膜對象物 2 9 氣體導入口 50、70 蒸發源容器 5 4、7 4 有機薄膜材料 本紙張尺度適用中國固家標準（CNS ) A4规格U10X297公釐） / ! (請先閲填背面1注意事項再填寫本頁) .-s>—-26- 409150 A7 B7 Printed by the Shellfish Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the Invention (24) Figure 3 is an example of the organic evaporation source of the present invention. Fig. 4 is a flowchart for explaining the method of the present invention. Fig. 5 is a diagram for explaining a change in temperature of an organic thin film material and a change in evaporation rate when an organic thin film is formed by the method of the present invention. Fig. 6 is a graph for explaining the relationship between the temperature and evaporation rate of A 1 q 3 and TPD. Fig. 7 is a diagram for explaining a change in temperature of an organic thin film material and a change in evaporation rate in a case where an organic thin film is formed by a prior art technique. .. Figures 8 (a) ~ (e): diagrams for explaining evaporation sources of prior art. DESCRIPTION OF SYMBOLS 10 Evaporation device 11 Vacuum tank 12i '1 2 2' 4 2 Organic evaporation source 13 Film-forming object 2 9 Gas inlet 50, 70 Evaporation source container 5 4, 7 4 Organic thin film material This paper is applicable to China Gujia Standard (CNS) A4 specification U10X297 mm) /! (Please read the notes on the back 1 before filling this page) .-s > —
27-27-
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34264996A JP3788835B2 (en) | 1996-12-06 | 1996-12-06 | Organic thin film manufacturing method |
| JP34265296A JP3691615B2 (en) | 1996-12-06 | 1996-12-06 | Evaporation source for organic materials |
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| Publication Number | Publication Date |
|---|---|
| TW409150B true TW409150B (en) | 2000-10-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| TW87108447A TW409150B (en) | 1996-12-06 | 1998-05-29 | Evaporation apparatus, organic material evaporation source and method of manufacturing thin organic film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112095078A (en) * | 2020-09-24 | 2020-12-18 | 福建华佳彩有限公司 | Cooling buffer chamber for surface evaporation source and driving method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112095078A (en) * | 2020-09-24 | 2020-12-18 | 福建华佳彩有限公司 | Cooling buffer chamber for surface evaporation source and driving method |
| CN112095078B (en) * | 2020-09-24 | 2023-12-05 | 福建华佳彩有限公司 | Cooling buffer chamber for surface evaporation source and driving method |
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