200522779 玖、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 於有機電激發光有機材料純化之真空傳輸純化裝置。 【先前技術】 10 15 般市面上之有機電激發光物質，由於含有合成中之 副產物而純度不高，於使用以形成有機電激發光元件之蒸 鍍前，需要再經過進一步之純化。而一般使用之純化方法^ =為蒸發傳輸純化之方& (例如昇華法等），請參考本申 凊人所揭不之前案内容：專利公告第196632號與第 號。目前已經有許多的研究顯示，有機電激發光元件中水分 與氧氣的存在與其含量多寡是導致有㈣激發光元件劣化 的主因’ A目前有機電激發光元件壽命無法達 格的障礙’然十多年來此-障礙之成因並未被找出並; 排除。 另双 而於傳統開放空間收集有機材料粉末過程，在其 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#_ 心健康均具有一定的危害。 、 此類純化過程主要係針對移除有機物200522779 发明 Description of the invention: [Technical field to which the invention belongs] The present invention relates to a vacuum transmission purification device, especially a vacuum transmission purification device suitable for the purification of organic electro-excitation light organic materials. [Previous technology] Organic electroluminescent materials in the general market of 10-15 have low purity because they contain by-products in the synthesis. They need to be further purified before being used to form organic electroluminescent devices by evaporation. For the commonly used purification method ^ = for evaporation transmission purification methods (such as sublimation method, etc.), please refer to the contents of the previous case disclosed by the applicant: Patent Bulletin No. 196632 and No. At present, many studies have shown that the existence and content of moisture and oxygen in organic electroluminescent devices are the main cause of the degradation of tritium excitation optical devices. 'A current obstacle to the life of organic electroluminescent devices cannot reach the standard.' The cause of this obstacle has not been identified and eliminated for years. The other process of collecting organic material powder in the traditional open space will produce dust of organic matter when the purified material condenses on its wall, and these ^ usually have carcinogenic benzene ring structure. 久 之 对 收藏 #_ 心 健康 均Has certain hazards. This type of purification process is mainly aimed at removing organic matter
物與些微的水、氧分之分離。 ^的田U 你π広丄 雕於大軋^ J兄下收集純化物合 使侍原本已用⑧溫昇華趕掉 曰 直允所指娃的气 > 反在閉循^虱氣氛或 —所赴掉的乳乳，又從外界大氣中被剛完成純化的有機 20 200522779 „使得原本耗費周章純化後之目的與功效大打折 :的：Γ經過純化完的有機物，未達到水分、氧氣吸 1的飽和度’具有最高的化學勢驅動力吸收大氣中的水、 乳，且有機粉末的微粒狀態比整批凝結狀態有更 積，更增加與大氣中的水、氧接 ' 錢觸面積與吸附機率，加速 了水分、氧氣污染剛純化完的有機物的速率· =水氧Λ的:Γ會在高真空 ίο 15 出水刀有害物質，直接影響有機發光元件的製进， 造成有機發光元件在亮度、壽命、可靠性的瑕疲。 明差因於此’亟思一種可以解決上 =純化裝置」，幾經研究實驗終至完成此項嘉惠世： 【發明内容】 種真空傳輸純化裝置，俾能 有祛物真空沉積系統進行整 不會釋出有害物質，污染製 之抽氣單元亦能提昇有機物 本發明之目的係在提供一 將有機物純化系統設計與後續 合，以於後續真空鍍膜系統中 程元件與鍍膜腔體，且所配合 純化之傳輸速率。 20 不贫明之另 置，俾能真正的提供無水、氧污 古 七化衣 ^ . '、 回、、、屯度的有機物供萝 造有機電激發光顯示器之用。 、表 本發明之又一目的，Λ於妲# u ,σ 在於棱供純化有機物之收集择作 人貝一安全的工作環境與設備。 、’、 為達成上述目的，本發明直处值 具工傳輸純化裝置至少包含 25 200522779 木箱單元，係至少具有一加熱單元與一收集腔室；其 中收集腔至與加熱單元連接，用於容置一收集内管、一 ϊ載内S以及有機物樣品；—抽氣單元，係與收集腔室連 接’其中’抽氣單it作用在使收集腔室内磨力低於ι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 元/、收木I至的連接方式不限，較佳係透過一閥門，可 使收集箱内產生之真空度不限，較佳為1().121⑽以下的真 空度；本發明中之收集箱單元更可包括一開孔，且開孔較 10 佳係連接一轉接單元。 抽氣單元功能在使收集腔室内壓力低於純化後—有 機材料於一鍍膜腔體内的壓力；抽氣單元可以是任何一種 習用之幫浦，較佳為機械幫浦、魯式幫浦、離子幫浦、低 15 溫幫浦、擴散幫浦與渴輪幫浦等；本發明所使用之抽氣單 凡抽氣方向不限，較佳係將一氣體由加熱單元内之高溫义 化區往其另一端傳送。 门’皿虱 其中收集腔室被加熱單元區隔，較佳係區隔為一基發 ，與-凝結區；且蒸發區往凝結區的方向與收集腔室之二 载i方向一致。 本發明真空傳輸純化裝置所適用之有機物樣品不 限’較佳係用於有機電激發光顯示器的有機材料之純化. 本發明裝置之配合系統不限’較佳更可包含一控制系统: 用於控制電源、溫度、警示、真空度等操作參數；本發明 真空傳輸純化裝置所配合之偵測單元不限，較件係更^八 20 200522779 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 5 熱單元内；加熱單元内之裝置不限，較佳係有一加熱器。 _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。 * 10 本發明真空傳輸純化裝置更可包括一惰性氣體填充 驗’惰性氣體填充搶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驗所使用之搭配單元不限，’ 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 手套或塑膠年m / 較佳為橡踢 I戈塑科套，而本發明裝置之㈣箱單元之箱壁材質 …限制，較佳為至少部分箱壁為透明材質。 、 15 20 【實施方式】 為月b m貝審查委員能更瞭解本發明之技術内 舉一較佳具體實施例說明如下。 特 本發明真空傳輸純化裝置係用以配 130，一承載内昝〗” 叹杲内官 ..^ 及一有機物樣品使用，本妒晋社堪 包括有一收集箱單元10，一 时_ 衣置、，、D構 30，且為方便人η %早12()以及-轉接單元 咬夫去Ϊ 以上裝置均放置於基台上。 Μ參考圖卜收集箱單元_以一 一 之收集腔室，箱壁為透明材質，且 =:雄、閉 手套η，以利操作之進行 1疋有塑膠 利純化後收集之有機物益^ ^括有—開孔12,以 有栻物稭此開孔傳送出收集箱單元1〇;於 25 200522779 本收集箱單元1 〇内包含有一加熱單元i 〇 〇，詳細結構請參考 圖2，為一包括有加熱器11〇之密閉腔室，同時内部包括有 一收集内管U0以及-承載内管12〇，二者為套管形式互相 、’α δ待，，’屯化之有機物樣品係置於加熱單元1 之承载内管 5 I20中進行高溫純化，此時位於加熱器區域之承載内管12〇 -端形成-高溫氣化區Η ’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L,於承载内管12〇中高溫氣化 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130中。 10 ⑥本例中所使用之抽氣單元20為-習用之幫浦，此幫 浦作用在使加熱單元⑽内真空度至少為1().3加以下，同 時以1門2!與加熱單元1〇〇相連接，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轉接，-二早兀10相壁上之開孔12以-轉接隔離閥31與 轉接早兀30形成密閉之連結；轉接單元3〇為一中空之宓閉 側可視需要選擇性地與一惰性氣體填充_ 月性虱體填充艙40係用以儲放操作所需要之器具， 3 =之用，增加操作彈性與方便。於本較佳二 :乳體填充搶40之外，尚包含一氮氣供應單元5〇，以 20提供氮氣於惰性氣，埴右於w ^ 氣盘P 4 G或收㈣單元1G，並去除水 及：；/’以形成一惰性氣體環境’完全隔絕大氣中水分 及虱氣之影響。 、T >刀 200522779 5 10 而進行純化過程（例如昇華）日寺’係先將待純 ，樣品置入加熱單元100内之承載内管120,同時 =:13。組合後，置入加熱單元-内，而成-完整 才八二傳輸純化裝置；之後將整個系統内部利用真办 ”，並通入氮氣循環後，再抽成真空。純化二 =將加熱單之承載内管12G部分，即高溫氣化區Η 進仃加熱，使樣品中之純物f轉化成氣態，並藉由抽直空 之方向將氣態物質擴散帶領向收集内管13〇之低溫沉積區 ’：此同時真空幫浦2〇將使封閉之加熱單元1〇〇產生ι〇 3 torr以下的真空度’營造利於轉化之氣態環境以進 行純化。 一待純化完成進行收集時，操作人員將手套入收集箱單 ，10相壁固疋之手套丨丨中，於填充氮氣之收集箱單元中 知：’首先自加熱單元100内卸下收集内管130，並將凝結 15，官壁上之有機物刮下，拆卸過程於之收集箱單元中進 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10上，設置一壓力偵測單元60, 以監視收集箱單元10之麼力狀態，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】 200522779 圖1係本發明—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係本發明真空傳輪純化裝置較佳實施例系統圖 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 【圖號說明】 10收集箱單元 100加熱單元 110加熱器 20抽氣單元 Η 高溫氣化區 30轉接單元 12開孔 12 0承載内管 21閘門 L 低溫沈積區 11手套 130收集内管The substance is separated from a little water and oxygen. ^ 田 U you π 広 丄 carved in the big roll ^ Brother J collected the purified material together, so Shi had already used sublimation to sublimate the qi of the child pointed by Zhiyun > but in a closed cycle ^ atmosphere or-go The milk that has been lost is freshly purified organic from the outside atmosphere. 20 200522779 „The original purpose and effect of the purification after the consumption of weeks are greatly reduced: Γ: The purified organics have not reached the saturation of moisture and oxygen absorption 1. Degree 'has the highest driving force of chemical potential to absorb water and milk in the atmosphere, and the particle state of organic powder has more accumulation than the condensed state of the batch, and increases the contact area with water and oxygen in the atmosphere. Accelerates the rate of pollution of freshly purified organic matter by water and oxygen. = = Hydrogen oxygen Λ: Γ will be a high-vacuum harmful substance, which directly affects the production of organic light-emitting elements, resulting in organic light-emitting elements in brightness, life, The flaw of reliability. The difference is because of this' want to think about a solution that can be solved = purification device ", after several research experiments until the completion of this AirPlus: [Abstract] A vacuum transmission purification device, can not have The material vacuum deposition system does not release harmful substances, and the exhaust system made by pollution can also promote organic matter. The object of the present invention is to provide a design and follow-up of organic matter purification system for the intermediate-range components of the subsequent vacuum coating system and Coated cavity, and the matched transmission rate. 20 It is not necessary to install it separately, and it can truly provide water-free, oxygen-contaminated ancient Qihua clothing ^. ', Hui ,, and Tundu organic materials for the use of organic electroluminescent display. Tables and Tables Another object of the present invention, Λ 于 妲 # u, σ lies in the collection of purified organic matter and is selected as a safe working environment and equipment. In order to achieve the above object, the direct value manual transmission purification device of the present invention includes at least 25 200522779 wooden box unit, which has at least a heating unit and a collection chamber; wherein the collection chamber is connected to the heating unit and used for storage. A collection inner tube, a load of S and organic matter samples are placed; an extraction unit is connected to the collection chamber 'wherein' the extraction single it acts to make the abrasive force in the collection chamber lower than ι 0.35 5 In the vacuum transmission purification device, the collection chamber has a hollow structure, which is arranged in a box wall with gloves; the connection method of the extraction unit / receiver I is not limited, and it is preferably through a The valve can make the degree of vacuum generated in the collection box unlimited, preferably a vacuum degree of 1 (). 121⑽ or less; the collection box unit in the present invention may further include an opening, and the opening is better than 10 Transfer unit. The function of the pumping unit is to make the pressure in the collection chamber lower than that after purification—the pressure of the organic material in a coating chamber; the pumping unit can be any conventional pump, preferably mechanical pump, Lupu pump, Ion pump, low-temperature pump, diffusion pump, thirsty pump, etc. The pumping direction used in the present invention is not limited, and it is preferred to move a gas from the high-temperature unscented zone in the heating unit to it. Send at the other end. Door 'dish lice. The collection chamber is partitioned by a heating unit, preferably the base is divided into a condensation zone and a -condensation zone; and the direction of the evaporation zone toward the condensation zone is the same as the direction of the load chamber i. The organic material sample applicable to the vacuum transmission purification device of the present invention is not limited to 'preferably the purification of organic materials for organic electroluminescent display. The matching system of the device of the present invention is not limited.' It may further include a control system: Control operating parameters such as power supply, temperature, warning, vacuum degree, etc .; the detection unit that the vacuum transmission purification device of the present invention is equipped with is not limited, and it is a pressure detection unit. In the vacuum transmission purification device of the present invention, the combined form of the collecting inner tube and the bearing inner tube is not limited, and it is preferably combined with each other in the form of a sleeve and placed in a heating unit; the device in the heating unit is not limited. A heater is attached. The use of the device of the present invention is not limited, and it is preferably purification of organic materials used in organic electroluminescent display. * 10 The vacuum transmission purification device of the present invention may further include an inert gas filling test. The inert gas used for the inert gas filling test is not limited, preferably nitrogen. The matching unit used for the inert gas filling test in the device of the present invention is not limited. ′ ′ Preferably further includes at least one inert gas supply unit. In the vacuum transmission purification device of the present invention, the glove or plastic year m / is preferably a rubber kick, and the material of the box wall of the box unit of the device of the present invention is limited. Preferably, at least part of the box wall is transparent material. 15 20 [Embodiment] A review of the technical aspects of the present invention for a better understanding of the present invention will be given below. The vacuum transmission purification device of the present invention is specially equipped with 130, a load-bearing internal container. "" Sigh internal officials .. ^ and an organic sample for use, the Envy Jinshe can include a collection box unit 10, _ clothes set ,, , D structure 30, and for the convenience of people η% early 12 () and-the transfer unit bite to remove the above devices are placed on the abutment. ΜRefer to the figure collection box unit _ one by one collection chamber, box The wall is transparent material, and =: male, closed gloves η, to facilitate the operation of 1 organic plastics collected after purification and plastic benefits ^ ^ included-open hole 12, the open hole to send out the collection Box unit 10; in 25 200522779 This collection box unit 10 includes a heating unit i 00. For the detailed structure, please refer to FIG. 2. It is a closed chamber including a heater 11 and also includes a collection inner tube. U0 and-bearing inner tube 120, both of which are in the form of sleeves, 'α δ to be treated,' and the organic samples are placed in the bearing inner tube 5 I20 of the heating unit 1 for high-temperature purification, at this time in the heating 120-end formation of the bearing inner tube in the vessel area-high temperature gasification zone Η '' At the other end of the collection tube 130, the lower temperature region is the low-temperature deposition area L, and the organic matter after the middle-temperature gasification of the load-bearing tube 120 is transferred to the low-temperature deposition area of the collection tube 130, and It can be condensed and deposited in the collection inner tube 130. 10 ⑥ The suction unit 20 used in this example is a customary pump, which acts to make the vacuum degree in the heating unit 至少 at least 1 (). 3 plus In the following, 1 door 2! Is connected to the heating unit 100 at the same time to transfer the gas from the high-temperature gasification zone within the heating unit 100] ^ to the low-temperature deposition zone L. 15 transfers, -Early stage 10 phase wall The upper opening 12 is a closed connection with the transfer isolation valve 31 and the transfer early 30. The transfer unit 30 is a hollow closed side and can be optionally filled with an inert gas as required. Filling tank 40 is used to store the equipment needed for operation. 3 = It is used to increase the flexibility and convenience of operation. In addition to the second preferred embodiment: in addition to the milk filling grab 40, it also contains a nitrogen supply unit 50, with 20 Provide nitrogen to the inert gas, and then to the gas tray P 4 G or the receiving unit 1G, and remove the water and :; Into an inert gas environment 'to completely isolate the effects of moisture and lice in the atmosphere. T > Knife 200522779 5 10 For purification process (such as sublimation), Risi's first puts the sample to be purified and the sample is placed in the heating unit 100. Inner tube 120, at the same time =: 13. After the combination, put it into the heating unit-into the complete-82 transmission and purification device; after that, the entire system is used inside, and after passing through the nitrogen cycle, it is pumped into vacuum. Purification 2 = heating the 12G part of the inner tube of the heating sheet, that is, the high-temperature gasification zone, to heat the pure substance f in the sample into a gaseous state, and diffuse the gaseous substance into the collection through the direction of evacuation The low temperature deposition zone of the tube 130: At the same time, the vacuum pump 20 will cause the closed heating unit 100 to generate a vacuum degree below ι3 torr to create a gaseous environment conducive to conversion for purification. Once the purification is completed and the collection is completed, the operator puts the gloves into the collection box, 10-phase wall-fixed gloves, and knows in the nitrogen-filled collection box unit: 'First remove the collection inner tube from the heating unit 100 130, and condensed 15, the organic matter on the official wall is scraped off, and the disassembly process is performed in the collection box unit, which can 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 force state of the collection box unit 10, so that the entire purification and operation process 20 can be obtained according to the pressure condition detected by the pressure detection unit 60. control. The above embodiments are merely examples for the convenience of description. 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] 200522779 FIG. 1 shows the structure of a collecting box unit according to the present invention—the preferred embodiment. FIG. 2 shows the structure of a heating unit according to a preferred embodiment of the present invention. Fig. 3 is a system of a preferred embodiment of the vacuum transfer wheel purification device of the present invention. Fig. 31 Transfer isolation valve 40 Inert gas filling compartment 50 Nitrogen supply unit 60 Pressure detection unit [Illustration of drawing number] 10 Collection tank unit 100 Heating unit 110 Heater 20 Extraction unit Η High-temperature gasification zone 30 Transfer unit 12 Opening hole 12 0 Bearing inner pipe 21 Gate L Low temperature deposition zone 11 Gloves 130 Collecting inner pipe
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