1228380 狄、發明說明： 【發明所屬之技術領域】 本發明係關於一種真空傳輸純化裝置，尤指一種適用 於有枚電激發光有機材料純化之真空傳輸純化裝置。 【先前技術】 一般市面上之有機電激發光物質，由於含有合成中之 副^物而純度不冑，於使用以形成有機電激發光元件之蒸 鑛前’需要再經過進一步之純化。而一般使用之純化方法、'， 10 2為蒸發傳輸純化之方法（例如昇華法等），請參考本申 請人所^揭示之前案内容：專利公告第196632號與第182193 唬。目丽已經有許多的研究顯示，有機電激發光元件中水分 與氧氣的，在與其含量多寡是導致有機電激發光元件劣二 的主因，疋目前有機電激發光元件壽命無法達到 15格的障礙，然十多年來此-障礙之成因並未被找出並有= ^而於傳統開放空間收集有機材料粉末過程，在到除管 壁凝結之純化物質時會產生有機物之揚塵，而此等有：: 通常都具有致癌性的苯環結構，久之對收集 人 心健康均具有一定的危害。 貝的身 此類純化過程主要係針對移除有機物合成時 =些微的水:氧分之分離。於大氣環境下收集純化物會 直t原t已用高溫昇華趕掉的水分、及密閉循環氮氣氛i —所趕掉的氧氣，又從外界大氣中㈣完成純化的_ 20 1228380 得原本耗費周章純化後之目的與功效大打折 ίο 1::剛經過?ί完的有機物，未達到水分、氧氣吸 1 X *有取面的化學勢驅動力吸收大氣中的水、 二，=有機粉末的微粒狀態比整批凝結狀態有更大的表面 盘〜加與大氣中的水、氧接觸面積與吸附機率，加速 2南了水^氧氣污染剛純化完的有機物的速率；而未 二除水、乳的有機物會在高真空的鑛膜製程時繼續釋放 、/分、氧氣等有害物質，直接影響有機發光元件的製造， k成有機發光元件在亮度、壽命、可靠性的瑕疲。 本發明友因於此，亟思一種可以解決上述問題之「真 空傳輸純化裝置」’幾經研究實驗終至完成此項嘉惠世人 之發明。 【發明内容】 15 纟發明之目的係在提供—種真空傳輸純化裝置，俾能 一夺有機物純化系統设計與後續有機物真空沉積系統進行整 以於後續真空鍍膜系統中不會釋出有害物質，污染製 私几件與鍍膜腔體，且所配合之抽氣單元亦能提昇有機物 純化之傳輸速率。 20 本發明之另一目的，係在提供-種真空傳輸純化裝 置俾月(3真正的提供無水、氧污染、高純度的有機物供製 造有機電激發光顯示器之用。 本發明之又一目的，在於提供純化有機物之收集操作 人員一安全的工作環境與設備。 _5 為達成上述目的，本發明真空傳輸純化裝置至少包含 1228380 收木箱單元，係至少具有一加熱單元與一收集腔室；其 中，收集腔室與加熱單元連接，用於容置一收集内管、二 承載内管以及有機物樣品；一抽氣單元，係與收集腔室連 接，其中，抽氣單元作用在使收集腔室内壓力低於1〇·3 5 本發明之真空傳輸純化裝置中’收集腔室具有中空的 構造，係配置於-具有手套之一箱壁内；所使用之抽氣單 凡’與收集腔室的連接方式不限，較佳係透過一間門，可 使收集箱内產生之真空度不限，較佳為心_以下的直 10 ί度；本發明中之收集箱單元更可包括-開孔，且開孔較 佳係連接一轉接單元。 抽氣單元功能在使收集腔室㈣力低於純化後 機材枓於-鍍膜腔體内的壓力；抽 =之幫浦，較佳為機械幫浦、魯式幫 15 I』方：散幫浦與渦輪幫浦等;本發明所使用之抽氣單 化心=傳;佳係將―㈣加熱單元内之高溫氣 其中收集腔室被加熱單元區 區與-凝結區;且蒸發區往凝結區二=為-蒸發 氣方向一致。 匕的万向與收集腔室之抽 本發明真空傳輸純化裳置所適 限，較佳係用於有機電激發光顯示器的有機勿樣0口不 本發明裝置之配合系統不限，較^才料之純化； 用於控制電源、溫度、逛干、匕3 一控制系統， 真空傳輪純化裝置所配:二、=操作參數， 偵測早几不限，較佳係更包含 20 1228380 一壓力偵測單元。 本發明真空傳輸純化裝置中，收集内管以及承載内管 之結合形式不限，較佳係以套管形式互相結合，且置於加 熱單元内，·加熱單元内之裝置不限，較佳係有一加熱器。 5 本發明裝置之用途不限，較佳係用於有機電激發光顯 示器的有機材料之純化。 本發明真空傳輸純化裝置更可包括一惰性氣體填充 艙；惰性氣體填充艙所使用之惰性氣體不限，較佳為氮氣； 本發明裝置中之惰性氣體填充艙所使用之搭配單元不限， ίο較佳更包含至少一惰性氣體供應單元。 本發明真空傳輸純化裝置中之手套不限，較佳為橡膠 手套或塑膠手而本發明裝置之收集肖單元之箱壁材質 無限制，較佳為至少部分箱壁為透明材質。 15 20 【實施方式】 為能讓貴審查委員能更瞭解本發明之技術内容，： 舉一較佳具體實施例說明如下。 本發明真空傳輸純化裝置係用以配合—收隹内 B0’ -承載内管120以及一有機物樣品使用，本裝二 包括有—收集箱單元10，-抽氣單元20以及—轉接單. 30’且為方便人員操作，以上裝置均放置於基台上。 凊蒼考圖1 ’收集箱單元1〇係以一箱壁圍繞成一糾 之收集腔室’箱壁為透明材f，且於箱壁上還固定有^ 手套U，以作之進行；箱壁上另包括有—開孔12叫 利純化後收集之有機物藉此開孔傳送出收㈣單元m 25 1228380 本收集箱單元10内包含有一加熱單元1〇〇，詳細結構請參考 圖2，為一包括有加熱器110之密閉腔室，同時内部包括有 一收集内官130以及一承載内管12〇，二者為套管形式互相 結合，待純化之有機物樣品係置於加熱單元1〇〇之承載内管 120中進行高溫純化，此時位於加熱器區域之承载内管12〇 一端形成一高溫氣化區H，而另一端收集内管13〇處為溫度 較低之區域，為低溫沈積區乙，於承載内管12〇中高溫氣= 後之有機物係傳輸至收集内管13〇之低溫沈積區域[，而可 以被冷凝沈積於收集内管13〇中。 而本例中所使用之抽氣單元別為一習用之幫浦，此幫 ^作用在使加熱單元_内真空度至少為10_3 t〇rr以下同 %以-閘門21與加熱單元100相連接’以將氣體由加熱單元 100内之高溫氣化區^[往低溫沈積區L傳送。 15 木箱單元10箱壁上之開孔12以一轉接隔離閥31盥 轉接單元30形成密閉之連結；轉接單元3〇為_中空之密閉 ^室’其另—側可視需要選擇性地與—惰性氣體填充^ 連結。惰性氣體填充艙4〇係用以儲放操作所需要之琴且， 或保養維修之用，增加操作彈性與方便。於本較佳例^中， =惰，氣體填充艙40之外’尚包含一氮氣供應單元⑽，以 提供鼠氣於惰性氣體填充㈣或收#箱單元iq，並去除水 氣與氧氣’以形成1性氣體環境，完全隔絕大氣中水八 及氧氣之影響。 刀 發明實施例操作時，係切密閉之收集箱單元1〇中 、入惰性氣體，於本較佳例中為氮氣，以去除大氣中的水 20 1228380 氣與氧氣。而進行純化過程（例如昇華）日寺，係先將待純 化之有機物樣品置入加熱單元1〇〇内之承載内管12〇，同時 :收集内管130組合後，置入加熱單元1〇〇内，而成一完整 岔閉之真空傳輸純化裝置；之後將整個系統内部利用真空 5幫浦20抽真空，並通入氮氣循環後，再抽成真空。純化時，1228380 D. Description of the invention: [Technical field to which the invention belongs] The present invention relates to a vacuum transmission purification device, and more particularly to a vacuum transmission purification device suitable for the purification of organic materials with electro-excitation light. [Prior technology] Generally, organic electro-excitation light substances on the market are not pure because they contain by-products in synthesis. They need further purification before being used to form organic electro-excitation light elements. For the commonly used purification method, ', 10 2 is the evaporation transmission purification method (such as the sublimation method, etc.), please refer to the applicant's disclosure of the contents of the previous case: Patent Bulletin Nos. 196632 and 182193. Muli has many studies that show that the amount of water and oxygen in organic electroluminescent devices is the main reason that the amount of organic electroluminescent devices is inferior to their content. At present, the lifetime of organic electroluminescent devices cannot reach 15 grids. However, for more than a decade, the cause of this obstacle has not been identified and has = ^ and the process of collecting organic material powder in the traditional open space will produce dust of organic matter when the purified material condensed on the pipe wall is removed, and so on Have :: It usually has carcinogenic benzene ring structure. Over time, it has certain hazards to human health. Shell's body This type of purification process is mainly aimed at removing organic matter during synthesis = slightly water: oxygen separation. Collecting the purified material in the atmospheric environment will directly reduce the moisture that has been driven off by high temperature sublimation, and a closed loop nitrogen atmosphere i — the oxygen that is driven off, and then purify it from the outside atmosphere. _ 20 1228380 It was originally a costly chapter The purpose and effect of purification are greatly reduced. 1: The organic matter that has just passed through does not reach the absorption of water and oxygen 1 X * There is a driving force for the chemical potential of the surface to absorb water in the atmosphere. Second, = particles of organic powder. The state has a larger surface disk than the entire batch of condensed state. Adding the contact area with the water and oxygen in the atmosphere and the probability of adsorption accelerates the rate of water ^ oxygen pollution of freshly purified organic matter; Organic substances will continue to release harmful substances such as oxygen / min and oxygen during the process of high-vacuum ore film production, which directly affects the manufacturing of organic light-emitting elements, which results in defects in brightness, life, and reliability of organic light-emitting elements. For this reason, the inventors of the present invention are eager to think of a "vacuum transmission purification device" that can solve the above problems. After several research experiments, this invention that has benefited the world has been completed. [Summary of the invention] 15 The purpose of the invention is to provide a kind of vacuum transmission purification device. The design of the organic purification system and the subsequent organic vacuum deposition system can be integrated so that no harmful substances are released in the subsequent vacuum coating system. The contamination system and the coating cavity are contaminated, and the matched extraction unit can also improve the transmission rate of organic purification. 20 Another object of the present invention is to provide a vacuum transmission purification device (3) to truly provide water-free, oxygen-contaminated, high-purity organic matter for the manufacture of organic electroluminescent display. Another object of the present invention, It is to provide a safe working environment and equipment for the collection operator of purified organic matter. _5 In order to achieve the above purpose, the vacuum transmission purification device of the present invention includes at least a 1228380 wooden box unit, which has at least a heating unit and a collection chamber; among them, The collection chamber is connected to the heating unit and is used for containing one collection inner tube, two bearing inner tubes and organic samples. An extraction unit is connected to the collection chamber. The extraction unit acts to make the pressure in the collection chamber low. In the 10.5-35 vacuum transfer purification device of the present invention, the 'collection chamber has a hollow structure, and is arranged in a box wall with one glove; the extraction pump used is unique' and the collection chamber. No limit, preferably through a door, the degree of vacuum generated in the collection box can be unlimited, preferably 10 degrees below the heart _; the collection in the present invention The unit may further include an opening, and the opening is preferably connected to an adapter unit. The function of the suction unit is to make the pressure of the collection chamber lower than the pressure of the purified material on the coating chamber; pumping = help Pumps, preferably mechanical pumps, Lu pumps 15 I "square: scattered pumps and turbine pumps; etc .; the pumping unit used in the present invention = transmission; the best will be-high temperature gas in the heating unit The collection chamber is heated by the heating unit zone and the -condensation zone; and the evaporation zone is in the same direction as the condensing zone. The direction of the dagger and the pumping of the collection chamber are limited. The best organic organic light emitting diode used in organic electroluminescent display is not limited to the system of the device of the present invention, which is more purified than expected; it is used to control power, temperature, drying, and control. Vacuum control system The round purification device is equipped with: two, = operating parameters, the detection is not limited as early as possible, and preferably includes a pressure detection unit of 20 1228380. In the vacuum transmission purification device of the present invention, a combination of a collection inner tube and a bearing inner tube No limitation, it is preferably combined with each other in the form of sleeves, and In the heating unit, the device in the heating unit is not limited, preferably a heater. 5 The device of the present invention is not limited in use, and is preferably used for the purification of organic materials used in organic electroluminescent display. The vacuum transmission purification of the present invention The device may further include an inert gas filled tank; the inert gas used in the inert gas filled tank is not limited, preferably nitrogen; the matching unit used in the inert gas filled tank in the device of the present invention is not limited, and preferably includes at least An inert gas supply unit. The gloves in the vacuum transmission purification device of the present invention are not limited, preferably rubber gloves or plastic hands, and the material of the box wall of the collecting unit of the device of the present invention is not limited, preferably at least part of the box wall is transparent Material 15 20 [Embodiment] In order to make your reviewing committee better understand the technical content of the present invention, a preferred embodiment will be described below. The vacuum transmission purification device of the present invention is used to cooperate with the collection tube B0'-bearing inner tube 120 and an organic sample. The second package includes a collection box unit 10, an extraction unit 20 and a transfer order. 30 'And for the convenience of personnel operation, the above devices are placed on the abutment.凊 苍 考 Figure 1 'The collection box unit 10 is a collection chamber surrounded by a box wall' The box wall is made of transparent material f, and ^ gloves U are also fixed on the box wall for this purpose; There are also included on it—openings 12 are used to collect the organic matter collected after purification. The openings are used to convey the collection unit m 25 1228380. The collection box unit 10 contains a heating unit 100. For detailed structure, please refer to FIG. A sealed chamber including a heater 110, and a collection inner tube 130 and a bearing inner tube 120, both of which are combined with each other in the form of a sleeve. The organic matter sample to be purified is placed in the bearing of the heating unit 100. High-temperature purification is performed in the inner tube 120. At this time, a high-temperature gasification zone H is formed at one end of the carrying inner tube 120 located in the heater area, and the lower end of the inner tube collection 130 is a lower-temperature area and a low-temperature deposition area. B. After the medium temperature of the inner tube 120 is loaded, the organic matter is transferred to the low-temperature deposition area of the collecting inner tube 130, and can be condensed and deposited in the collecting inner tube 130. The pumping unit used in this example is a customary pump. This pump is used to make the internal vacuum of the heating unit at least 10_3 t0rr and the same%. The gate 21 is connected to the heating unit 100 ' The gas is transferred from the high-temperature gasification zone ^ [in the heating unit 100 to the low-temperature deposition zone L. 15 Wooden box unit 10 The opening 12 in the wall of the box is a closed connection with a transfer isolation valve 31 and the transfer unit 30 forms a closed connection; the transfer unit 30 is a _hollow closed chamber ^ and the other side can be selected as required Ground is connected to-inert gas filling ^. The inert gas-filled compartment 40 is used for storing organs required for operation, or for maintenance and repair, increasing operation flexibility and convenience. In the preferred embodiment, the inert gas tank 40 includes a nitrogen supply unit ⑽ to provide rat gas in the inert gas fill ㈣ or to close the box unit iq and remove water and oxygen. Form a uni-gas environment, completely isolate the effects of water and oxygen in the atmosphere. In the operation of the embodiment of the knife, the closed collection box unit 10 is cut into an inert gas, and in this preferred embodiment, nitrogen is used to remove water and oxygen from the atmosphere. For the purification process (such as sublimation), the Risi Temple first puts the organic matter sample to be purified into the bearing inner tube 120 in the heating unit 100, and at the same time: After collecting the inner tube 130 combination, it is placed in the heating unit 100. Inside, it becomes a complete closed vacuum transmission purification device; after that, the entire system is evacuated with a vacuum of 5 pumps and 20, and after passing through a nitrogen cycle, it is evacuated. During purification,
係將加熱單元100内之承載内管120部分，即高溫氣化區H 進行加熱，使樣品中之純物質轉化成氣態，並藉由抽真空 之方向將氣態物質擴散帶領向收集内管130之低溫沉積區 L，於此同時真空幫浦2〇將使封閉之加熱單元1〇〇產生 10至10·12 t〇rr以下的真空度，營造利於轉化之氣態環境以進 行純化。 待純化完成進行收集時，操作人員將手套入收集箱單 7〇1〇鈿壁固定之手套丨丨中，於填充氮氣之收集箱單元中 操作，首先自加熱單元100内卸下收集内管130,並將凝結 15於官壁上之有機物刮下，拆卸過程於之收集箱單元丨〇中進 行’可避免純化後的有機物接觸到水氣與氧氣。此一密閉 收集箱單元10亦可避免操作人員吸入或接觸到有機物之粉 塵。本較佳例於收集箱單元1 〇上，設置一壓力偵測單元6 〇， 以監視收集箱單元1 〇之壓力狀態，使整個純化與操作過程 20 可依壓力偵測單元60偵測壓力狀況而得控制。 上述實施例僅係為了方便說明而舉例而已，本發明所 主張之權利範圍自應以申請專利範圍所述為準，而非僅限 於上述實施例。 25 【圖式簡單說明】 1228380 圖1係本發明一較佳實施例之收集箱單元結構。 圖2係本發明一較佳實施例之加熱單元結構。 圖3係本發明真空傳輸純化裝置較佳實施例系統圖。 5 【圖號說明】 10 收集箱單元 12 開孔 11手套 100 加熱單元 120 承載内管 130收集内管 110 加熱器 20 抽氣單元 21 閘門 Η 向溫氣化區 L 低溫沈積區 30 轉接單元 31 轉接隔離閥 40 惰性氣體填充艙 50 氮氣供應單元 60 壓力偵測單元The heating inner tube 120 in the heating unit 100, that is, the high-temperature gasification zone H, is heated to convert the pure substance in the sample into a gaseous state, and the gaseous substance is diffused to the collection inner pipe 130 by the direction of the vacuum. The low-temperature deposition zone L, at the same time, the vacuum pump 20 will cause the closed heating unit 100 to generate a vacuum of 10 to 10 · 12 t0rr or less, and create a gaseous environment conducive to conversion for purification. When the purification is completed and the collection is performed, the operator puts the gloves into the collection box list 7101, the gloves fixed on the wall, and operates in the collection box unit filled with nitrogen. First, the collection inner tube 130 is removed from the heating unit 100 And the condensate 15 is scraped off the organic matter on the official wall, and the disassembling process is performed in the collection box unit 丨 0 to prevent the purified organic matter from contacting water and oxygen. The closed collection box unit 10 can also prevent the operator from inhaling or coming into contact with organic dust. In this preferred example, a pressure detection unit 60 is provided on the collection box unit 10 to monitor the pressure state of the collection box unit 10, so that the entire purification and operation process 20 can detect the pressure condition according to the pressure detection unit 60. Get control. The above embodiments are merely examples for the convenience of description. The scope of the rights claimed in the present invention should be based on the scope of the patent application, rather than being limited to the above embodiments. 25 [Brief description of the drawings] 1228380 FIG. 1 is a structure of a collecting box unit according to a preferred embodiment of the present invention. FIG. 2 shows the structure of a heating unit according to a preferred embodiment of the present invention. FIG. 3 is a system diagram of a preferred embodiment of the vacuum transmission purification device of the present invention. 5 [Illustration of drawing number] 10 Collecting box unit 12 Opening hole 11 Gloves 100 Heating unit 120 Carrying inner tube 130 Collecting inner tube 110 Heater 20 Extraction unit 21 Gate Η To warm gasification zone L Low temperature deposition zone 30 Transfer unit 31 Transfer isolation valve 40 Inert gas filling tank 50 Nitrogen supply unit 60 Pressure detection unit
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