TW201338854A - Organic-material refining device - Google Patents
Organic-material refining device Download PDFInfo
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- TW201338854A TW201338854A TW102106739A TW102106739A TW201338854A TW 201338854 A TW201338854 A TW 201338854A TW 102106739 A TW102106739 A TW 102106739A TW 102106739 A TW102106739 A TW 102106739A TW 201338854 A TW201338854 A TW 201338854A
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Abstract
Description
本發明係關於有機材料之精製裝置。 The present invention relates to a refining device for organic materials.
以往，作為有機材料之精製方法，管柱層析、再結晶、蒸餾、昇華等是已知的。作為電子材料或光學材料所使用的有機材料，其純度可能會大幅影響性能，因此被高純度地精製。 Conventionally, as a method of purifying an organic material, column chromatography, recrystallization, distillation, sublimation, and the like are known. An organic material used as an electronic material or an optical material may be highly purified in purity, which may greatly affect performance.
作為電子材料的一例，可舉出近年來研究開發的熱門項目之有機電致發光元件(以下稱：有機EL元件)所使用的材料。當有機EL元件所使用的材料(以下稱：有機EL元件用材料)中有雜質混入時，該雜質成為載子(電子、電洞)的陷阱或是消光的原因，而使有機EL元件之發光強度、發光效率及耐久性降低。因此，為了減少雜質，必須將有機EL元件用材料進行高純度地精製。 As an example of the electronic material, a material used in an organic electroluminescence device (hereinafter referred to as an organic EL device) which has been researched and developed in recent years is mentioned. When impurities are mixed in a material used in the organic EL device (hereinafter referred to as a material for an organic EL device), the impurity becomes a trap of a carrier (electron or hole) or a cause of extinction, and the organic EL device emits light. Strength, luminous efficiency and durability are reduced. Therefore, in order to reduce impurities, it is necessary to purify the material for an organic EL element with high purity.
關於用來精製有機EL元件用材料之精製裝置，例如揭示於文獻1(國際公開第01/70364號)。文獻1所記載的昇華精製裝置，是利用電磁感應方式將有機EL元件用材料加熱而使其昇華的裝置，讓筒狀的昇華部內所裝入的材料昇華，利用筒狀的捕集部進行凝結或凝固捕集。 A refining device for purifying a material for an organic EL device is disclosed, for example, in Document 1 (International Publication No. 01/70364). The sublimation refining device described in the document 1 is a device for heating and sublimating a material for an organic EL element by electromagnetic induction, and sublimating a material contained in a cylindrical sublimation portion, and coagulating with a cylindrical collecting portion. Or solidification capture.
文獻1所記載的昇華精製裝置，昇華部和捕集部之內部溫度是藉由熱電偶進行測定。然而，在該昇華精製裝置，由於熱電偶以裸露狀態插入昇華部、捕集部的內部，氣體狀的有機材料會附著於熱電偶，而有無法正確地測定昇華部、捕集部的內部溫度之問題。 In the sublimation refining device described in Document 1, the internal temperature of the sublimation portion and the trap portion was measured by a thermocouple. However, in the sublimation refining device, since the thermocouple is inserted into the sublimation portion and the inside of the trap portion in a bare state, the gaseous organic material adheres to the thermocouple, and the internal temperature of the sublimation portion and the trap portion cannot be accurately measured. The problem.
例如，在文獻1所記載的昇華精製裝置，捕集部被區分成設定溫度不同的溫度區，如果在精製中無法正確地測定內部溫度的話，無法將有機材料在期望的捕集部進行捕集，可能被真空泵吸引後往裝置外部排出。因此，比起原料量，可能使有機材料的捕集量減少而造成精製效率降低。此外，如果在精製中無法適切地控制溫度條件的話，捕集部的溫度會發生變動，可能使有機材料的純度降低。 For example, in the sublimation refining device described in Document 1, the collection unit is divided into temperature zones having different set temperatures, and if the internal temperature cannot be accurately measured during the purification, the organic material cannot be trapped in the desired collection unit. It may be sucked by the vacuum pump and discharged to the outside of the unit. Therefore, it is possible to reduce the amount of trapping of the organic material compared to the amount of the raw material, resulting in a decrease in the purification efficiency. Further, if the temperature condition cannot be appropriately controlled during the purification, the temperature of the trap portion may fluctuate, and the purity of the organic material may be lowered.
本發明的目的是為了提供一種有機材料之精製裝置，可正確地測定精製中的內部溫度而防止有機材料之精製效率及純度降低。 An object of the present invention is to provide a refining device for an organic material which can accurately measure the internal temperature during refining to prevent a reduction in the purification efficiency and purity of the organic material.
本發明的有機材料之精製裝置，其特徵在於，係具備氣化器、捕集器、鞘管、熱電偶、以及溫度調整加熱器控制手段；該氣化器具有：內部被供應有機材料之第一筒體、及配置於該第一筒體的外側而讓被供應的有機材料氣化之加熱器；該捕集器具有：與前述氣化器的前述第一筒體連通之 第二筒體、及配置於該第二筒體的外側而用來調整前述第二筒體的溫度之溫度調整加熱器，藉由前述氣化器氣化後之氣體狀的有機材料是在前述第二筒體的內面進行捕集；該鞘管，是從前述第二筒體的外部朝向前述第二筒體的內部插通；該熱電偶被插入前述鞘管的內部；該溫度調整加熱器控制手段，是根據前述熱電偶所檢測出的溫度來進行前述溫度調整加熱器的溫度控制。 The refining device for an organic material according to the present invention is characterized by comprising a gasifier, a trap, a sheath, a thermocouple, and a temperature adjustment heater control means; the gasifier has: an organic material supplied internally a cylinder and a heater disposed on the outer side of the first cylinder to vaporize the supplied organic material; the trap having: communicating with the first cylinder of the gasifier a second cylindrical body and a temperature-regulating heater disposed on an outer side of the second cylindrical body for adjusting a temperature of the second cylindrical body, wherein the gas-like organic material vaporized by the vaporizer is in the foregoing The inner surface of the second cylinder is captured; the sheath is inserted from the outside of the second cylinder toward the inside of the second cylinder; the thermocouple is inserted into the inside of the sheath; the temperature is adjusted and heated The device control means performs temperature control of the temperature adjustment heater based on the temperature detected by the thermocouple.
依據本發明，熱電偶以插入鞘管內部的狀態配置於第二筒體的內部，因此可防止有機材料直接附著於熱電偶。如此，依據本發明能正確地測定筒體內部的溫度。而且，溫度調整加熱器控制手段，可根據熱電偶的測定溫度而適切地調整溫度調整加熱器之加熱條件。如此，依據本發明，縱使是精製中仍能更正確地測定及控制第二筒體的內部溫度，結果可防止有機材料之精製效率及純度降低。 According to the invention, the thermocouple is disposed inside the second cylindrical body in a state of being inserted into the inside of the sheath tube, so that the organic material can be prevented from directly adhering to the thermocouple. Thus, according to the present invention, the temperature inside the cylinder can be accurately measured. Further, the temperature adjustment heater control means can appropriately adjust the heating condition of the temperature adjustment heater in accordance with the temperature measured by the thermocouple. As described above, according to the present invention, even if the internal temperature of the second cylindrical body can be more accurately measured and controlled during the purification, the purification efficiency and purity of the organic material can be prevented from being lowered.
本發明的有機材料之精製裝置較佳為，在前述鞘管內插入複數個熱電偶。 In the refining device for an organic material of the present invention, it is preferable that a plurality of thermocouples are inserted into the sheath tube.
依據本發明，由於將複數個熱電偶插入鞘管內，能在第二筒體的內部之複數部位進行正確的溫度測定。 According to the present invention, since a plurality of thermocouples are inserted into the sheath tube, accurate temperature measurement can be performed at a plurality of portions inside the second cylindrical body.
本發明的有機材料之精製裝置較佳為，前述鞘管為石英製。 In the refining device for an organic material of the present invention, it is preferable that the sheath tube is made of quartz.
依據本發明，鞘管為石英製，由於石英的熱傳導率低，不容易受到軸向溫度分布的影響，可在配置有熱電偶的部位進行精確的溫度測定。此外，石英的伸縮性低，用來 支承鞘管之支承部等不容易損壞，可進行急速的昇溫及降溫。 According to the present invention, the sheath tube is made of quartz. Since the thermal conductivity of quartz is low, it is not easily affected by the axial temperature distribution, and accurate temperature measurement can be performed at a portion where the thermocouple is disposed. In addition, quartz has low flexibility and is used for The support portion of the support sheath tube or the like is not easily damaged, and rapid temperature rise and temperature drop can be performed.
本發明的有機材料之精製裝置較佳為，前述第二筒體為石英製或不鏽鋼製。 In the refining device for an organic material of the present invention, it is preferable that the second cylindrical body is made of quartz or stainless steel.
依據本發明，鞘管和第二筒體同樣是石英製的，因此能更正確地測定作為溫度測定對象之第二筒體的內面溫度。只要第二筒體內為高真空狀態，由於來自溫度調整加熱器的傳熱是利用輻射熱，藉由使用高輻射率的石英可更正確地測定與有機材料接觸之第二筒體的內面溫度。 According to the invention, since the sheath tube and the second cylinder are made of quartz, the inner surface temperature of the second cylinder which is the temperature measurement target can be more accurately measured. As long as the second cylinder is in a high vacuum state, since the heat transfer from the temperature-regulating heater utilizes radiant heat, the inner surface temperature of the second cylinder in contact with the organic material can be more accurately determined by using quartz having a high emissivity.
此外，依據本發明，由於第二筒體為不鏽鋼製，能使第二筒體的加工性和強度提高。 Further, according to the present invention, since the second cylindrical body is made of stainless steel, the workability and strength of the second cylindrical body can be improved.
本發明的有機材料之精製裝置較佳為，前述捕集器的第二筒體是由複數個捕集室所構成，前述溫度調整加熱器分別設置於前述複數個捕集室中的各個捕集室，前述鞘管貫通前述複數個捕集室內部，在前述鞘管的內部插入複數個前述熱電偶，前述複數個熱電偶是對應於前述捕集室的位置而分別配置，前述溫度調整加熱器控制手段，根據各個熱電偶所檢測出的溫度，獨立地進行各個溫度調整加熱器的溫度控制。 Preferably, in the refining device for organic material of the present invention, the second cylinder of the trap is composed of a plurality of collection chambers, and each of the temperature adjustment heaters is disposed in each of the plurality of collection chambers. a plurality of the thermocouples are inserted into the sheath tube through the sheath chamber, and the plurality of thermocouples are disposed corresponding to positions of the collection chamber, and the temperature adjustment heater is disposed The control means independently controls the temperature of each of the temperature adjustment heaters based on the temperature detected by each of the thermocouples.
依據本發明，捕集器被區分成複數個捕集室。因此，氣化後的有機材料是被各捕集室進行捕集，能將高純度材 料和低純度材料分開而進行精製。此外，對應於捕集室個別的位置而配置之熱電偶，都處於插入鞘管內的狀態。因此，可正確地測定各捕集室的內部溫度。而且，溫度調整加熱器控制手段，根據各熱電偶的測定溫度可對各捕集室適切地調整捕集溫度條件。 According to the invention, the trap is divided into a plurality of trap chambers. Therefore, the vaporized organic material is captured by each collection chamber, and the high-purity material can be The material is refined separately from the low purity material. Further, the thermocouples arranged corresponding to the individual positions of the collection chamber are in a state of being inserted into the sheath tube. Therefore, the internal temperature of each collection chamber can be accurately measured. Further, the temperature adjustment heater control means can appropriately adjust the collection temperature conditions for each collection chamber based on the measured temperatures of the respective thermocouples.
因此，依據本發明，可更正確地測定及控制各捕集室的內部溫度，而在捕集室內部高效率地捕集高純度的有機材料。 Therefore, according to the present invention, the internal temperature of each of the collection chambers can be more accurately measured and controlled, and the high-purity organic material can be efficiently collected in the collection chamber.
本發明的有機材料之精製裝置較佳為，係具備：從前述第一筒體的外部朝向前述第一筒體的內部插通之第一筒體用鞘管、被插入前述第一筒體用鞘管的內部之熱電偶、以及根據前述熱電偶所檢測出的溫度進行前述加熱器的溫度控制之加熱器控制手段。 In the refining device for an organic material according to the present invention, the first tubular body sheath that is inserted from the outside of the first cylindrical body toward the inside of the first cylindrical body is preferably inserted into the first cylindrical body. A thermocouple inside the sheath and a heater control means for controlling the temperature of the heater based on the temperature detected by the thermocouple.
依據本發明，在內部被供應有機材料之第一筒體內部也讓第一筒體用鞘管插通，在第一筒體用鞘管內部也讓第一筒體用的熱電偶插入，而測定第一筒體內部溫度。因此，利用該熱電偶可正確地測定第一筒體的內部溫度。此外，加熱器控制手段，根據第一筒體用鞘管內的熱電偶的檢測溫度，可適切地調整加熱器加熱條件。因此，依據本發明，縱使是在精製中，仍能更正確地測定及控制第一筒體的內部溫度，而能以適切的溫度及速度進行有機材料的氣化。 According to the present invention, the first cylindrical body is inserted through the sheath inside the first cylindrical body to which the organic material is supplied, and the thermocouple for the first cylindrical body is also inserted into the first cylindrical sheath tube. The internal temperature of the first cylinder was measured. Therefore, the internal temperature of the first cylinder can be accurately measured by the thermocouple. Further, the heater control means can appropriately adjust the heater heating condition based on the detected temperature of the thermocouple in the sheath tube for the first cylinder. Therefore, according to the present invention, even in the refining, the internal temperature of the first cylinder can be more accurately measured and controlled, and the vaporization of the organic material can be performed at an appropriate temperature and speed.
本發明的有機材料之精製裝置較佳為，前述第一筒體 用鞘管為石英製。 Preferably, the refining device for organic material of the present invention is the first cylinder The sheath tube is made of quartz.
依據本發明，第一筒體用鞘管為石英製，由於石英的熱傳導率低，不容易受到軸向溫度分布的影響，可在配置有熱電偶的部位進行精確的溫度測定。此外，石英的伸縮性低，用來支承鞘管之支承部等不容易損壞，可進行急速的昇溫及降溫。 According to the present invention, the sheath for the first cylinder is made of quartz, and since the thermal conductivity of the quartz is low, it is not easily affected by the axial temperature distribution, and accurate temperature measurement can be performed at a portion where the thermocouple is disposed. Further, quartz has low stretchability, and the support portion for supporting the sheath tube is not easily damaged, and rapid temperature rise and temperature drop can be performed.
本發明的有機材料之精製裝置較佳為，前述第一筒體為石英製、或不鏽鋼製。 In the refining device for an organic material of the present invention, it is preferable that the first cylindrical body is made of quartz or stainless steel.
依據本發明，第一筒體用鞘管和第一筒體同樣是石英製的，因此能更正確地測定作為溫度測定對象之第一筒體的內面溫度。只要第一筒體內為高真空狀態，由於來自溫度調整加熱器的傳熱是利用輻射熱，藉由使用高輻射率的石英可更正確地測定與有機材料接觸之第一筒體的內面溫度。 According to the invention, since the first tubular sheath tube and the first tubular body are made of quartz, the inner surface temperature of the first cylindrical body to be temperature-measured can be more accurately measured. As long as the first cylinder is in a high vacuum state, since the heat transfer from the temperature-regulating heater utilizes radiant heat, the inner surface temperature of the first cylinder in contact with the organic material can be more accurately determined by using quartz having a high emissivity.
此外，依據本發明，第一筒體為不鏽鋼製，能使第一筒體的加工性和強度提高。 Further, according to the present invention, the first cylinder is made of stainless steel, and the workability and strength of the first cylinder can be improved.
本發明的有機材料之精製裝置較佳為，在前述第一筒體內部配置石英製的收容部，該收容部是用來收容前述有機材料。 In the refining device for an organic material according to the present invention, it is preferable that a accommodating portion made of quartz is disposed inside the first cylindrical body, and the accommodating portion is for accommodating the organic material.
依據本發明，第一筒體用鞘管和收容部同樣是石英製的，可正確地測定作為溫度測定對象之收容部的溫度。只要第一筒體內為高真空狀態，由於來自溫度調整加熱器的傳熱是利用輻射熱，藉由使用高輻射率的石英，能更正確地測定用來收容有機材料之收容部的溫度。 According to the invention, the first tubular sheath tube and the accommodating portion are made of quartz, and the temperature of the accommodating portion which is the temperature measurement target can be accurately measured. As long as the first cylinder is in a high vacuum state, since the heat transfer from the temperature-regulating heater uses radiant heat, by using quartz having a high emissivity, the temperature of the accommodating portion for accommodating the organic material can be more accurately measured.
本發明的有機材料之精製裝置較佳為，前述溫度調整加熱器為面狀發熱體。 In the refining device for an organic material of the present invention, it is preferable that the temperature adjustment heater is a planar heating element.
依據本發明，由於溫度調整加熱器是面狀發熱體，能均等地進行加熱。因此，沿著第二筒體的軸向以包覆第二筒體的周圍的方式配置複數個面狀發熱體，能正確地形成第二筒體內部的溫度梯度。 According to the invention, since the temperature adjustment heater is a planar heating element, heating can be performed uniformly. Therefore, a plurality of planar heat generating bodies are disposed so as to cover the periphery of the second cylindrical body in the axial direction of the second cylindrical body, and the temperature gradient inside the second cylindrical body can be accurately formed.
本發明的有機材料之精製裝置較佳為，具備：將前述第一筒體及前述第二筒體收容於內部之外筒體，前述加熱器配置於前述第一筒體及前述外筒體的外側，前述溫度調整加熱器配置於前述第二筒體及前述外筒體的外側。 Preferably, the organic material refining device of the present invention includes: the first cylindrical body and the second cylindrical body are housed inside the outer cylindrical body, and the heater is disposed in the first cylindrical body and the outer cylindrical body The temperature adjustment heater is disposed outside the second cylinder and the outer cylinder.
依據本發明，精製裝置成為在外筒體內部收容有第一筒體及第二筒體之雙重管式構造，縱使這種雙重管式構造的精製裝置在精製中，仍能更正確地測定及控制第二筒體的內部溫度，結果可防止有機材料之精製效率及純度降低。 According to the present invention, the refining device has a double tubular structure in which the first tubular body and the second cylindrical body are housed inside the outer cylindrical body, and the refining device of the double tubular structure can be more accurately measured and controlled even during refining. The internal temperature of the second cylinder prevents the purification efficiency and purity of the organic material from being lowered.
此外，藉由使精製裝置成為雙重管構造，在將第一筒體及第二筒體朝裝置外部卸下而進行清掃的期間，能將其他的第一筒體及第二筒體配置於外筒體內部而開始進行精製。因此能使精製裝置的運轉率提高。 Further, by making the refining device into a double pipe structure, the other first cylindrical body and the second cylindrical body can be disposed outside while the first cylindrical body and the second cylindrical body are detached from the outside of the device and cleaned. The inside of the cylinder was started and purification was started. Therefore, the operation rate of the refining device can be improved.
1、1A‧‧‧有機材料之精製裝置 1, 1A‧‧‧ refining device for organic materials
2‧‧‧裝置主體 2‧‧‧Device body
3‧‧‧真空泵 3‧‧‧vacuum pump
3a‧‧‧閥 3a‧‧‧Valves
4‧‧‧溫度控制器 4‧‧‧ Temperature Controller
5‧‧‧氣化器 5‧‧‧ gasifier
6‧‧‧捕集器 6‧‧‧Trappers
21‧‧‧內筒體 21‧‧‧Inner cylinder
22‧‧‧外筒體 22‧‧‧Outer cylinder
23、24‧‧‧蓋部 23, 24‧‧ ‧ cover
41、43‧‧‧溫度感測器 41, 43‧‧‧ Temperature Sensor
42、44‧‧‧控制部 42. 44‧‧‧Control Department
51‧‧‧第一內筒體 51‧‧‧First inner cylinder
52‧‧‧第一外筒體 52‧‧‧First outer cylinder
53‧‧‧加熱器 53‧‧‧heater
54‧‧‧收容部 54‧‧‧ Housing Department
61‧‧‧第二內筒體 61‧‧‧Second inner cylinder
61A‧‧‧第一捕集筒體 61A‧‧‧First capture cylinder
61B‧‧‧第二捕集筒體 61B‧‧‧Second trapping cylinder
61C‧‧‧第三捕集筒體 61C‧‧‧The third trapping cylinder
62‧‧‧第二外筒體 62‧‧‧Second outer cylinder
63‧‧‧溫度調整加熱器 63‧‧‧temperature adjustment heater
63A‧‧‧第一溫度調整加熱器 63A‧‧‧First temperature adjustment heater
63B‧‧‧第二溫度調整加熱器 63B‧‧‧Second temperature adjustment heater
63C‧‧‧第三溫度調整加熱器 63C‧‧‧third temperature adjustment heater
411、416、431‧‧‧鞘管 411, 416, 431‧‧ ‧ sheath
412、432A、432B、432C‧‧‧熱電偶 412, 432A, 432B, 432C‧‧‧ thermocouples
R1‧‧‧第一捕集室 R1‧‧‧First Capture Room
R2‧‧‧第二捕集室 R2‧‧‧Second collection room
R3‧‧‧第三捕集室 R3‧‧‧ third capture room
第1圖係本發明的第一實施方式之有機材料之精製裝置的剖面概略圖。 Fig. 1 is a schematic cross-sectional view showing a refining device for an organic material according to a first embodiment of the present invention.
第2圖係本發明的第二實施方式之有機材料之精製裝置的剖面概略圖。 Fig. 2 is a schematic cross-sectional view showing a refining device for an organic material according to a second embodiment of the present invention.
以下，參照圖式說明本發明的實施方式。 Hereinafter, embodiments of the present invention will be described with reference to the drawings.
第1圖顯示本實施方式的有機材料之精製裝置1之沿著長邊方向的剖面概略圖。 Fig. 1 is a schematic cross-sectional view showing the organic material refining device 1 of the present embodiment along the longitudinal direction.
精製裝置1係具備：用來精製有機材料之裝置主體2、作為將裝置主體2內部施以減壓的排氣裝置之真空泵3、以及控制裝置主體2的溫度之溫度控制器4。以下是舉例說明，將作為有機材料之有機EL元件用材料實施精製的情況。 The refining device 1 includes a device main body 2 for purifying an organic material, a vacuum pump 3 as an exhaust device for decompressing the inside of the device main body 2, and a temperature controller 4 for controlling the temperature of the device main body 2. The following is an example of the case where the material for an organic EL device as an organic material is purified.
裝置主體2係具備：圓筒狀的內筒體21、配置於該內筒體21的外側而將內筒體21收容於內部之圓筒狀的外筒體22，外筒體22的兩端藉由蓋部23,24封閉而成為雙重管構造。 The apparatus main body 2 includes a cylindrical inner cylinder 21, a cylindrical outer cylinder 22 disposed outside the inner cylinder 21 and housing the inner cylinder 21 therein, and both ends of the outer cylinder 22 The lid portions 23, 24 are closed to form a double tube structure.
在裝置主體2，於內筒體21及外筒體22之一側設有 氣化器5，於內筒體21及外筒體22之另一側設有捕集器6，氣化器5和捕集器6是沿著裝置主體2的水平方向呈連續地設置。 In the apparatus main body 2, one side of the inner cylinder 21 and the outer cylinder 22 is provided The gasifier 5 is provided with a trap 6 on the other side of the inner cylinder 21 and the outer cylinder 22, and the vaporizer 5 and the trap 6 are continuously provided in the horizontal direction of the apparatus main body 2.
此外，如第1圖所示般，在設置於裝置主體2之捕集器6側的端部之蓋部24，連接真空泵3。在該真空泵3，透過閥3a設有配管構件，配管構件以與裝置主體2內部連通的方式連接於蓋部24。因此，真空泵3能將裝置主體2的內部施以排氣。在本實施方式，將裝置主體2內的壓力設定為10-1Pa以下。宜在裝置主體2和真空泵3之間介設捕集(trap)裝置(未圖示)。 Further, as shown in Fig. 1, the vacuum pump 3 is connected to the lid portion 24 provided at the end portion of the apparatus main body 2 on the side of the trap 6. In the vacuum pump 3, a pipe member is provided in the transmission valve 3a, and the pipe member is connected to the lid portion 24 so as to communicate with the inside of the apparatus body 2. Therefore, the vacuum pump 3 can apply the exhaust gas to the inside of the apparatus main body 2. In the present embodiment, the pressure in the apparatus main body 2 is set to 10 -1 Pa or less. A trap device (not shown) is preferably interposed between the apparatus main body 2 and the vacuum pump 3.
依據該裝置主體2，有機EL元件用材料是在氣化器5的內部進行氣化，氣化後之氣體狀的有機EL元件用材料，被真空泵3吸引而流入捕集器6，在捕集器6的內部固化而被捕集。如此，要精製的有機EL元件用材料，是從氣化器5側流向捕集器6側。以下，沿著有機EL元件用材料的流動方向，會有將裝置主體2之配置有氣化器5的一側稱為上游側、將裝置主體2之配置有捕集器6的另一側稱為下游側的情況。 According to the apparatus main body 2, the material for the organic EL element is vaporized inside the vaporizer 5, and the gas-formed material for the organic EL element is sucked by the vacuum pump 3 and flows into the trap 6 to be trapped. The interior of the device 6 is solidified and trapped. In this way, the material for the organic EL device to be purified flows from the vaporizer 5 side to the trap 6 side. Hereinafter, along the flow direction of the material for the organic EL element, the side where the vaporizer 5 is disposed in the apparatus main body 2 is referred to as the upstream side, and the other side of the apparatus main body 2 in which the trap 6 is disposed is referred to as the other side. For the downstream side of the situation.
裝置主體2的材質較佳為，由對有機EL元件用材料為惰性的材質所構成。這是為了防止，在精製時的條件(溫度、壓力等)下使有機EL元件用材料分解、或是發生聚合等的變質。 The material of the apparatus main body 2 is preferably made of a material that is inert to the material for the organic EL element. This is to prevent deterioration of the material for the organic EL element or deterioration of polymerization or the like under conditions (temperature, pressure, and the like) at the time of purification.
氣化器5配置於裝置主體2的上游側。氣化器5係具備：作為構成內筒體21的上游側之第一筒體、即第一內筒體51、構成外筒體22的上游側而配置於第一內筒體51的外側之第一外筒體52、配置於第一外筒體52的外側之加熱器53、以及作為配置於第一內筒體51內部的原料容器、即收容部54。 The vaporizer 5 is disposed on the upstream side of the apparatus main body 2. The gasifier 5 is disposed on the outer side of the first inner cylindrical body 51 as the first cylindrical body that constitutes the upstream side of the inner cylindrical body 21, that is, the first inner cylindrical body 51 and the upstream side of the outer cylindrical body 22. The first outer cylinder 52, the heater 53 disposed outside the first outer cylinder 52, and the storage portion 54 as a raw material container disposed inside the first inner cylinder 51.
第一內筒體51及第一外筒體52形成為圓筒狀。第一內筒體51可直接載置於第一外筒體52的內面；亦可在第一內筒體51的底面側配置支承構件(圖示省略)，透過該支承構件來載置第一內筒體51。 The first inner cylinder 51 and the first outer cylinder 52 are formed in a cylindrical shape. The first inner cylinder 51 can be placed directly on the inner surface of the first outer cylinder 52. A support member (not shown) can be disposed on the bottom surface side of the first inner cylinder 51, and the support member can be placed through the support member. An inner cylinder 51.
加熱器53是由紅外線加熱器等所構成，呈環狀地配置於第一外筒體52的外側。 The heater 53 is constituted by an infrared heater or the like and is disposed in an annular shape outside the first outer cylinder 52.
收容部54配置於第一內筒體51的內部。收容部54例如形成為盤狀，用來收容粉末狀等固體的有機EL元件用材料；該盤狀係具備：四角形板狀的底面、從該底面的周緣朝面外方向豎起之側面。 The accommodating portion 54 is disposed inside the first inner cylinder 51. The accommodating portion 54 is formed, for example, in a disk shape for accommodating a solid organic EL element material such as a powder, and the disk shape includes a bottom surface having a quadrangular plate shape and a side surface rising from the peripheral edge of the bottom surface in the out-of-plane direction.
第一內筒體51、第一外筒體52及收容部54的材質較佳為，由對有機EL元件用材料為惰性的材質所構成，在本實施方式是石英玻璃所構成。 The material of the first inner cylinder 51, the first outer cylinder 52, and the accommodating portion 54 is preferably made of a material that is inert to the material for the organic EL element, and is configured by quartz glass in the present embodiment.
捕集器6配置於裝置主體2的下游側。捕集器6係具備：作為構成內筒體21的下游側之第二筒體、即第二內筒體61、構成外筒體22的下游側而配置於第二內筒體61 的外側之第二外筒體62、以及配置於第二外筒體62的外側之溫度調整加熱器63。 The trap 6 is disposed on the downstream side of the apparatus main body 2. The trap 6 is provided on the downstream side of the second cylindrical body 21 that constitutes the downstream side of the inner cylindrical body 21, that is, the second inner cylindrical body 61, and is disposed on the downstream side of the outer cylindrical body 22, and is disposed in the second inner cylindrical body 61. The second outer cylinder 62 on the outer side and the temperature adjustment heater 63 disposed on the outer side of the second outer cylinder 62.
第二內筒體61及第二外筒體62形成為圓筒狀。第二內筒體61可直接載置於第二外筒體62的內面，亦可在第二內筒體61的底面側配置支承構件(圖示省略)，透過該支承構件來載置第二內筒體61。 The second inner cylinder 61 and the second outer cylinder 62 are formed in a cylindrical shape. The second inner cylinder 61 may be directly placed on the inner surface of the second outer cylinder 62, or a support member (not shown) may be disposed on the bottom surface side of the second inner cylinder 61, and the support member may be placed through the support member. Two inner cylinders 61.
在本實施方式，第一外筒體52和第二外筒體62成為一體的圓筒狀，第一內筒體51和第二內筒體61則是由不同構件所形成。再者，第二內筒體61，在本實施方式是將三個圓筒狀的捕集筒體，具體而言從上游側依序將第一捕集筒體61A、第二捕集筒體61B及第三捕集筒體61C可分割地連結而構成。第一捕集筒體61A和第一內筒體51連接。第一捕集筒體61A的內部成為第一捕集室R1，第二捕集筒體61B的內部成為第二捕集室R2，第三捕集筒體61C的內部成為第三捕集室R3，捕集室R1,R2,R3是朝向下游側沿水平方向連續地形成，而互相連通。 In the present embodiment, the first outer cylinder 52 and the second outer cylinder 62 are formed in a cylindrical shape, and the first inner cylinder 51 and the second inner cylinder 61 are formed of different members. In the second embodiment, the second inner cylindrical body 61 has three cylindrical collecting cylinders, specifically, the first collecting cylinder 61A and the second collecting cylinder from the upstream side. The 61B and the third collecting cylinder 61C are connected to each other in a divided manner. The first collecting cylinder 61A is connected to the first inner cylinder 51. The inside of the first collecting cylinder 61A is the first collecting chamber R1, the inside of the second collecting cylinder 61B is the second collecting chamber R2, and the inside of the third collecting cylinder 61C is the third collecting chamber R3. The trap chambers R1, R2, and R3 are continuously formed in the horizontal direction toward the downstream side, and communicate with each other.
溫度調整加熱器63是由紅外線加熱器等所構成，呈環狀地配置於第二外筒體62的外側。在本實施方式，溫度調整加熱器63是由面狀發熱體所構成。 The temperature adjustment heater 63 is constituted by an infrared heater or the like and is disposed in an annular shape outside the second outer cylinder 62. In the present embodiment, the temperature adjustment heater 63 is constituted by a planar heat generating body.
溫度調整加熱器63係具備：調整第一捕集室R1的溫度之第一溫度調整加熱器63A、調整第二捕集室R2的溫度之第二溫度調整加熱器63B、以及調整第三捕集室R3的溫度之第三溫度調整加熱器63C。該等溫度調整加熱器63A,63B,63C各個，能藉由作為後述溫度調整加熱器控制 手段之控制部44而將各捕集室R1,R2,R3內部的溫度予以獨立地調整。 The temperature adjustment heater 63 includes a first temperature adjustment heater 63A that adjusts the temperature of the first collection chamber R1, a second temperature adjustment heater 63B that adjusts the temperature of the second collection chamber R2, and a third capture adjustment. The third temperature of the chamber R3 is adjusted to the heater 63C. Each of the temperature adjustment heaters 63A, 63B, and 63C can be controlled by a temperature adjustment heater which will be described later. The control unit 44 of the means independently adjusts the temperature inside each of the collection chambers R1, R2, and R3.
第二內筒體61及第二外筒體62的材質較佳為，由對有機EL元件用材料為惰性的材質所構成。在本實施方式，第二內筒體61及第二外筒體62是石英玻璃所構成。 The material of the second inner cylinder 61 and the second outer cylinder 62 is preferably made of a material that is inert to the material for the organic EL element. In the present embodiment, the second inner cylinder 61 and the second outer cylinder 62 are made of quartz glass.
溫度控制器4係具備：測定氣化器5內部的溫度之溫度感測器41、作為根據溫度感測器41所測定的溫度資訊來控制加熱器53的加熱器控制手段、即控制部42、測定捕集器6內部的溫度之溫度感測器43、以及根據溫度感測器43所測定的溫度資訊來控制溫度調整加熱器63之控制部44。 The temperature controller 4 includes a temperature sensor 41 that measures the temperature inside the vaporizer 5, and a heater control means that controls the heater 53 based on the temperature information measured by the temperature sensor 41, that is, the control unit 42, The temperature sensor 43 that measures the temperature inside the trap 6 and the temperature control information measured by the temperature sensor 43 control the control unit 44 of the temperature adjustment heater 63.
溫度感測器41係具備：從內筒體21的上游側端部插通於第一內筒體51之鞘管411(第一筒體用鞘管)、及插入鞘管411的內部之第一筒體用的熱電偶412。熱電偶412與配置於裝置主體2外部之控制部42連接。熱電偶412所測定的溫度資訊被送往控制部42。 The temperature sensor 41 includes a sheath 411 (a first cylindrical sheath) that is inserted into the first inner cylinder 51 from the upstream end of the inner cylinder 21, and a first insertion into the sheath 411. A thermocouple 412 for the barrel. The thermocouple 412 is connected to a control unit 42 disposed outside the apparatus main body 2. The temperature information measured by the thermocouple 412 is sent to the control unit 42.
鞘管411較佳為，由對有機EL元件用材料為惰性的材質所構成，在本實施方式為石英製。配置於第一內筒體51內部之鞘管411的前端部是封閉的。鞘管411如第1圖所示般，插通於第一內筒體51內部的上部。 The sheath tube 411 is preferably made of a material that is inert to the material for the organic EL element, and is made of quartz in the present embodiment. The front end portion of the sheath tube 411 disposed inside the first inner cylindrical body 51 is closed. The sheath tube 411 is inserted into the upper portion of the inside of the first inner cylindrical body 51 as shown in Fig. 1 .
控制部42連接於加熱器53，根據從溫度感測器41輸入的溫度資訊來控制加熱器53所進行的加熱。 The control unit 42 is connected to the heater 53, and controls the heating by the heater 53 based on the temperature information input from the temperature sensor 41.
溫度感測器43係具備：從內筒體21的下游側端部插通於第二內筒體61之鞘管431(第二筒體用鞘管)、插入鞘管431的內部之第二筒體用的三根熱電偶432A,432B,432C。熱電偶432A,432B,432C與作為配置在裝置主體2外部的溫度調整加熱器控制手段之控制部44連接。溫度感測器43所測定的溫度資訊被送往控制部44。 The temperature sensor 43 includes a sheath 431 (a second cylindrical sheath) that is inserted into the second inner cylinder 61 from the downstream end of the inner cylinder 21, and a second inside of the sheath 431. Three thermocouples 432A, 432B, 432C for the barrel. The thermocouples 432A, 432B, and 432C are connected to a control unit 44 as a temperature adjustment heater control means disposed outside the apparatus main body 2. The temperature information measured by the temperature sensor 43 is sent to the control unit 44.
鞘管431較佳為，由對有機EL元件用材料為惰性的材質所構成，在本實施方式為石英製。第二內筒體61內部之鞘管431的前端部是封閉的。鞘管431如第1圖所示般，插通於第二內筒體61內部的上部。 The sheath tube 431 is preferably made of a material that is inert to the material for the organic EL element, and is made of quartz in the present embodiment. The front end portion of the sheath tube 431 inside the second inner cylinder 61 is closed. The sheath tube 431 is inserted into the upper portion of the inside of the second inner cylinder 61 as shown in Fig. 1 .
熱電偶432A配置於第一捕集室R1的內部，熱電偶432B配置於第二捕集室R2的內部，熱電偶432C配置於第三捕集室R3的內部。 The thermocouple 432A is disposed inside the first collection chamber R1, the thermocouple 432B is disposed inside the second collection chamber R2, and the thermocouple 432C is disposed inside the third collection chamber R3.
控制部44連接於溫度調整加熱器63，根據從溫度感測器43輸入的溫度資訊，控制溫度調整加熱器63所進行的加熱。在本實施方式，控制部44將捕集室R1,R2,R3個別的溫度調整加熱器63A,63B,63C予以獨立地控制。例如，控制部44以溫度從第一捕集室R1側朝向第三捕集室R3側連續或逐步改變的方式控制溫度調整加熱器63A,63B,63C。 The control unit 44 is connected to the temperature adjustment heater 63, and controls the heating by the temperature adjustment heater 63 based on the temperature information input from the temperature sensor 43. In the present embodiment, the control unit 44 independently controls the temperature adjustment heaters 63A, 63B, and 63C of the collection chambers R1, R2, and R3. For example, the control unit 44 controls the temperature adjustment heaters 63A, 63B, 63C in such a manner that the temperature changes continuously or stepwise from the first collection chamber R1 side toward the third collection chamber R3 side.
作為精製對象之有機EL元件用材料，只要是有機EL 元件所使用的材料即可，沒有特別的限定。 As the material for the organic EL element to be purified, as long as it is an organic EL The material used for the element is not particularly limited.
針對使用精製裝置1將有機EL元件用材料進行精製的方法作說明。 A method of purifying a material for an organic EL device using the refining device 1 will be described.
首先，在收容部54收容固體粉末狀之昇華性的有機EL元件用材料。 First, a material for sublimating organic EL elements in a solid powder form is accommodated in the accommodating portion 54.
接著，安裝蓋部23,24，使氣化器5及捕集器6內部成為密閉。 Next, the lid portions 23, 24 are attached to seal the inside of the vaporizer 5 and the trap 6.
接著，從氣化器5的上游側端部，將插入熱電偶412後的鞘管411插通於第一內筒體51內部。另一方面，從捕集器6的下游側端部，將鞘管431插通於第二內筒體61內部。 Next, the sheath tube 411 into which the thermocouple 412 is inserted is inserted from the upstream end portion of the vaporizer 5 into the inside of the first inner cylinder 51. On the other hand, the sheath tube 431 is inserted into the inside of the second inner cylinder 61 from the downstream end portion of the trap 6.
接著，利用真空泵3將裝置主體2內部減壓至10-1Pa以下。 Next, the inside of the apparatus main body 2 is pressure-reduced to 10 -1 Pa or less by the vacuum pump 3.
減壓後，藉由加熱器53將第一內筒體51加熱，藉由溫度調整加熱器63將第二內筒體61加熱，而進行溫度調整。這時，溫度控制器4，根據溫度感測器41、溫度感測器43之測定溫度資訊而控制加熱器53及溫度調整加熱器63所進行的加熱。具體而言，加熱器53將第一內筒體51加熱至使固體粉末狀的有機EL元件用材料昇華(從固體變化成氣體)的溫度(昇華溫度)，並保持該溫度。溫度調整加熱器63A,63B,63C互相獨立地加熱至既定溫度，而調整第一捕集室R1、第二捕集室R2及第三捕集室R3的 溫度。在本實施方式，相對於使作為精製對象之有機EL元件用材料從氣體變化成固體的溫度，將第一捕集室R1調整至稍高的溫度，將第二捕集室R2調整至比該溫度低的溫度，將第三捕集室R3調整至比第二捕集室R2更低的溫度。 After the pressure reduction, the first inner cylinder 51 is heated by the heater 53, and the second inner cylinder 61 is heated by the temperature adjustment heater 63 to perform temperature adjustment. At this time, the temperature controller 4 controls the heating by the heater 53 and the temperature adjustment heater 63 based on the temperature information measured by the temperature sensor 41 and the temperature sensor 43. Specifically, the heater 53 heats the first inner cylinder 51 to a temperature (sublimation temperature) at which the material for the organic EL element in the form of a solid powder is sublimated (changed from a solid to a gas), and the temperature is maintained. The temperature adjustment heaters 63A, 63B, 63C are independently heated to a predetermined temperature, and the first trap chamber R1, the second trap chamber R2, and the third trap chamber R3 are adjusted. temperature. In the present embodiment, the first collection chamber R1 is adjusted to a slightly higher temperature, and the second collection chamber R2 is adjusted to a temperature at which the material for the organic EL element to be purified is changed from a gas to a solid. The temperature at a low temperature adjusts the third trap chamber R3 to a lower temperature than the second trap chamber R2.
收容部54所收容的固體粉末狀的有機EL元件用材料，當收容部54被加熱保持至昇華溫度時，會發生氣化。氣體狀的有機EL元件用材料，朝捕集器6側移動，在與各捕集室R1,R2,R3對應之第二內筒體61的內面使其固化而進行捕集。 The material for the solid powdery organic EL element contained in the accommodating portion 54 is vaporized when the accommodating portion 54 is heated and held to the sublimation temperature. The material for the gaseous organic EL element moves toward the trap 6 and is solidified by the inner surface of the second inner cylinder 61 corresponding to each of the collection chambers R1, R2, and R3, and is collected.
在本實施方式，相對於作為精製對象之有機EL元件用材料的氣化(昇華)溫度，各捕集室R1,R2,R3以上述般的關係被實施加熱保持。因此，在被加熱保持成相對於該氣化(昇華)溫度為適切的溫度之第二捕集室R2，作為精製對象之有機EL元件用材料能以高純度進行捕集。在第一捕集室R1及第三捕集室R3，供應給收容部54之有機EL元件用材料所含的雜質成分被濃縮而進行捕集。 In the present embodiment, each of the collection chambers R1, R2, and R3 is heated and held in the above-described relationship with respect to the vaporization (sublimation) temperature of the material for the organic EL element to be purified. Therefore, in the second collection chamber R2 which is heated and maintained at a temperature suitable for the vaporization (sublimation) temperature, the material for the organic EL element to be purified can be collected with high purity. In the first collection chamber R1 and the third collection chamber R3, the impurity components contained in the material for the organic EL element supplied to the accommodating portion 54 are concentrated and collected.
依據本實施方式之精製裝置1及使用精製裝置1之精製方法，可發揮以下效果。 According to the refining device 1 of the present embodiment and the purification method using the refining device 1, the following effects can be exhibited.
依據精製裝置1，熱電偶432A,432B,432C以插入鞘管431內部的狀態配置於第二內筒體61的內部，因此可防止有機EL元件用材料直接附著於熱電偶 432A,432B,432C。 According to the refining device 1, the thermocouples 432A, 432B, and 432C are disposed inside the second inner cylinder 61 in a state of being inserted into the inside of the sheath tube 431, so that the material for the organic EL element can be prevented from directly adhering to the thermocouple. 432A, 432B, 432C.
如此，依據精製裝置1，縱使是精製中仍能正確地測定第二內筒體61內部的溫度。而且，作為溫度調整加熱器控制手段之控制部44，根據熱電偶432A,432B,432C之測定溫度，能適切地調整溫度調整加熱器63A,63B,63C的加熱條件。如此，依據精製裝置1，能更正確地測定及控制第二內筒體61的內部溫度，結果能防止有機EL元件用材料之精製效率及純度降低。 As described above, according to the refining device 1, the temperature inside the second inner cylinder 61 can be accurately measured even during the refining. Further, the control unit 44 as the temperature adjustment heater control means can appropriately adjust the heating conditions of the temperature adjustment heaters 63A, 63B, and 63C based on the measured temperatures of the thermocouples 432A, 432B, and 432C. In this way, according to the refining device 1, the internal temperature of the second inner cylinder 61 can be more accurately measured and controlled, and as a result, the purification efficiency and purity of the material for the organic EL element can be prevented from being lowered.
依據精製裝置1，捕集器6被區分成複數個捕集室R1,R2,R3。因此，氣化後的有機EL元件用材料，被各個捕集室R1,R2,R3進行捕集，因此可將高純度的材料和低純度的材料分開而進行精製。此外，對應於捕集室R1,R2,R3個別的位置而配置之熱電偶432A,432B,432C，都處於插入鞘管431內的狀態。因此，能正確地測定各捕集室R1,R2,R3的內部溫度。而且，作為溫度調整加熱器控制手段之控制部44，根據各熱電偶432A,432B,432C的測定溫度，能對各捕集室R1,R2,R3適切地調整捕集溫度條件。 According to the refining device 1, the trap 6 is divided into a plurality of trap chambers R1, R2, R3. Therefore, since the material for the organic EL element after vaporization is collected by the respective collection chambers R1, R2, and R3, the high-purity material and the low-purity material can be separately purified. Further, the thermocouples 432A, 432B, and 432C disposed corresponding to the respective positions of the collection chambers R1, R2, and R3 are all inserted into the sheath tube 431. Therefore, the internal temperature of each of the collection chambers R1, R2, and R3 can be accurately measured. Further, the control unit 44 as the temperature adjustment heater control means can appropriately adjust the collection temperature conditions for the respective collection chambers R1, R2, and R3 based on the measured temperatures of the respective thermocouples 432A, 432B, and 432C.
因此依據精製裝置1，可更正確地測定及控制各個捕集室R1,R2,R3的內部溫度，能將高純度的有機EL元件用材料在捕集室內部進行高效率地捕集。 Therefore, according to the refining device 1, the internal temperature of each of the collection chambers R1, R2, and R3 can be more accurately measured and controlled, and the material for the high-purity organic EL element can be efficiently collected in the inside of the collection chamber.
依據精製裝置1，鞘管411及鞘管431為石英製，由於石英的熱傳導率低，不容易受到軸向溫度分布的影響，可在配置有熱電偶的部位進行精確的溫度測定。此外，石 英的伸縮性低，用來支承鞘管之支承部等不容易損壞，可進行急速的昇溫及降溫。 According to the refining device 1, the sheath tube 411 and the sheath tube 431 are made of quartz, and since the thermal conductivity of quartz is low, it is not easily affected by the axial temperature distribution, and accurate temperature measurement can be performed at a portion where the thermocouple is disposed. In addition, stone The British has a low stretchability, and the support portion for supporting the sheath tube is not easily damaged, and rapid temperature rise and temperature drop can be performed.
此外，依據精製裝置1，第一內筒體51、第二內筒體61及收容部54是和鞘管同樣是石英製的。只要第一內筒體51及第二內筒體61內部為高真空狀態，由於來自溫度調整加熱器的傳熱是利用輻射熱，藉由使用高輻射率的石英，能更正確地測定與有機EL元件用材料接觸之第一內筒體51及第二內筒體61的內面溫度、以及收容有機EL元件用材料之收容部54的溫度。 Further, according to the refining device 1, the first inner cylinder 51, the second inner cylinder 61, and the accommodating portion 54 are made of quartz like the sheath. As long as the inside of the first inner cylinder 51 and the second inner cylinder 61 is in a high vacuum state, since the heat transfer from the temperature-regulating heater utilizes radiant heat, by using a high emissivity quartz, the organic EL can be more accurately measured. The temperature of the inner surface of the first inner cylinder 51 and the second inner cylinder 61 which are in contact with the material for the element, and the temperature of the accommodating portion 54 for accommodating the material for the organic EL element.
依據精製裝置1，由於鞘管411及鞘管431的前端部都是封閉的，可防止有機EL元件用材料進入鞘管411,431內部。結果，可確實地防止有機EL元件用材料附著於熱電偶412,432A,432B,432C。 According to the refining device 1, since the tip end portions of the sheath tube 411 and the sheath tube 431 are closed, the material for the organic EL element can be prevented from entering the inside of the sheath tubes 411 and 431. As a result, the material for the organic EL element can be surely prevented from adhering to the thermocouples 412, 432A, 432B, and 432C.
依據精製裝置1，在第一內筒體51內部也讓鞘管411插通，在其內部也讓熱電偶412插入，藉由該熱電偶412，可正確地測定第一內筒體51之內部溫度。此外，作為加熱器控制手段之控制部42，根據鞘管411內的熱電偶412之檢測溫度，可適切地調整加熱器53之加熱條件。如此，依據精製裝置1，能更正確地測定及控制第一內筒體51的內部溫度，讓有機EL元件用材料之氣化在適切的溫度及速度下進行。 According to the refining device 1, the sheath tube 411 is inserted into the first inner cylinder 51, and the thermocouple 412 is also inserted therein. The thermocouple 412 can accurately measure the inside of the first inner cylinder 51. temperature. Further, the control unit 42 as the heater control means can appropriately adjust the heating conditions of the heater 53 based on the detected temperature of the thermocouple 412 in the sheath tube 411. As described above, according to the refining device 1, the internal temperature of the first inner cylinder 51 can be more accurately measured and controlled, and the vaporization of the material for the organic EL element can be performed at an appropriate temperature and speed.
依據精製裝置1，從裝置主體2的上游側端部讓鞘管411插通，從下游側端部讓鞘管431插通。因此，比起從裝置主體2之長邊方向一端部讓單獨一根長形的鞘管插通 的情況，可縮短每一根的長度。因此，將鞘管411及鞘管431插拔時的操作性提高。此外，比起讓單獨一根長形的石英製鞘管插通的情況，石英製的鞘管411及鞘管431的長度變短，不容易發生破損。 According to the refining device 1, the sheath tube 411 is inserted from the upstream side end portion of the apparatus main body 2, and the sheath tube 431 is inserted from the downstream side end portion. Therefore, a single elongated sheath is inserted through one end portion from the longitudinal direction of the apparatus main body 2. In case of, the length of each root can be shortened. Therefore, the operability at the time of inserting and removing the sheath tube 411 and the sheath tube 431 is improved. Further, the length of the sheath tube 411 and the sheath tube 431 made of quartz is shortened compared to the case where a single elongated quartz sheath tube is inserted, and damage is unlikely to occur.
依據精製裝置1，鞘管411插通於第一內筒體51內部的上部，鞘管431插通於第二內筒體61內部的上部。因此，能防止有機EL元件用材料附著於鞘管411,431，能正確地進行內部溫度的溫度測定。 According to the refining device 1, the sheath tube 411 is inserted into the upper portion of the inside of the first inner cylinder 51, and the sheath tube 431 is inserted into the upper portion of the inside of the second inner cylinder 61. Therefore, it is possible to prevent the material for the organic EL element from adhering to the sheath tubes 411 and 431, and it is possible to accurately measure the temperature of the internal temperature.
接下來，針對本發明的第二實施方式之有機EL元件用材料之精製裝置作說明。又在以下的說明，對於與已經說明的部分相同的部分，是賦予同一符號而將其說明予以省略或簡略。 Next, a refining device for a material for an organic EL device according to a second embodiment of the present invention will be described. In the following description, the same reference numerals are given to the same parts as those already described, and the description thereof will be omitted or simplified.
第2圖顯示本實施方式的有機EL元件用材料之精製裝置1A的剖面概略圖。 Fig. 2 is a schematic cross-sectional view showing a refining device 1A for a material for an organic EL device of the present embodiment.
在精製裝置1A，從捕集器6的下游側端部讓長形的一根鞘管416插通，其前端到達第一內筒體51內部。在鞘管416內部，在對應於第一內筒體51內部及各捕集室R1,R2,R3的位置分別配置熱電偶412,432A,432B,432C。 In the refining device 1A, an elongated sheath tube 416 is inserted from the downstream end portion of the trap 6, and the tip end thereof reaches the inside of the first inner cylinder 51. Inside the sheath tube 416, thermocouples 412, 432A, 432B, and 432C are disposed at positions corresponding to the inside of the first inner cylinder 51 and the respective collection chambers R1, R2, and R3, respectively.
鞘管416也是較佳為，由對有機EL元件用材料為惰性的材質所構成，在本實施方式是石英玻璃所構成。此外，第一內筒體51、第一外筒體52、收容部54、第二內筒體61及第二外筒體62，在本實施方式也是石英玻璃所構 成。 The sheath tube 416 is also preferably made of a material that is inert to the material for the organic EL element, and is configured by quartz glass in the present embodiment. Further, the first inner cylinder 51, the first outer cylinder 52, the accommodating portion 54, the second inner cylinder 61, and the second outer cylinder 62 are also made of quartz glass in the present embodiment. to make.
依據第二實施方式之精製裝置1A，除了以下所示的效果以外，可發揮與第一實施方式的精製裝置1同樣的效果。 According to the refining device 1A of the second embodiment, in addition to the effects described below, the same effects as those of the refining device 1 of the first embodiment can be exhibited.
依據精製裝置1A，只要讓一根鞘管416插通於裝置主體2內部即可，比起在上游側及下游側分別讓一根鞘管插通的情況，能使鞘管416之插拔過程變簡單。 According to the refining device 1A, as long as one sheath tube 416 is inserted into the inside of the apparatus main body 2, the insertion and removal process of the sheath tube 416 can be performed by inserting a sheath tube on the upstream side and the downstream side, respectively. It becomes simple.
此外，依據精製裝置1A，能更正確地測定及控制第二內筒體61的內部溫度，結果能防止有機EL元件用材料之精製效率及純度降低。再者，依據精製裝置1A，能更正確地測定及控制第一內筒體51的內部溫度，而讓有機EL元件用材料的氣化在適切的溫度及速度下進行。 Further, according to the refining device 1A, the internal temperature of the second inner cylinder 61 can be more accurately measured and controlled, and as a result, the purification efficiency and purity of the material for the organic EL element can be prevented from being lowered. Further, according to the refining device 1A, the internal temperature of the first inner cylinder 51 can be more accurately measured and controlled, and the vaporization of the material for the organic EL element can be performed at an appropriate temperature and speed.
此外，依據精製裝置1A，能更正確地測定及控制各個捕集室R1,R2,R3的內部溫度，在上述精製方法之溫度條件下，能將高純度的有機EL元件用材料在捕集室內部進行高效率地捕集。 Further, according to the refining device 1A, the internal temperature of each of the collection chambers R1, R2, and R3 can be more accurately measured and controlled, and the material for the high-purity organic EL element can be placed in the collection chamber under the temperature conditions of the purification method. The department conducts efficient collection.
又本發明並不限定於上述實施方式，在可達成本發明目的的範圍內，也包含以下所示的變形等。 Further, the present invention is not limited to the above-described embodiment, and includes the following modifications and the like within the scope of the object of the invention.
鞘管411,431並不限定於從氣化器5及捕集器6的軸向端部插通的情況，亦可為從與外筒體22的軸向交叉的方向插通而到達內筒體21內部的態樣。在此情況，在第二內筒體61，可在對應於各捕集室R1,R2,R3的位置讓個 別的鞘管插通。如此般，設置複數個讓鞘管插通的部位，可按照目的而適宜地改變內溫的測定部位，能謀求有機材料的附著防止及加熱器輸出控制的提昇。 The sheaths 411 and 431 are not limited to being inserted from the axial end portions of the vaporizer 5 and the trap 6, and may be inserted into the inner cylinder 21 from a direction intersecting the axial direction of the outer cylinder 22. Internal aspect. In this case, in the second inner cylinder 61, a position corresponding to each of the collection chambers R1, R2, and R3 can be given. The other sheath is inserted. In this manner, a plurality of portions for inserting the sheath tube are provided, and the measurement portion of the internal temperature can be appropriately changed according to the purpose, and adhesion prevention of the organic material and improvement of the heater output control can be achieved.
此外，在上述第一實施方式，是從捕集器6的下游側端部讓鞘管431插通，在其內部插入三個熱電偶432A,432B,432C，但並不限定於這種態樣。例如，可對一根鞘管將一個熱電偶插入，在上述第一實施方式的情況下，是將熱電偶432A,432B,432C分別插入個別的鞘管，讓該等鞘管從捕集器6的下游側端部插通到與各捕集室對應的位置。 Further, in the first embodiment described above, the sheath tube 431 is inserted from the downstream end portion of the trap 6, and three thermocouples 432A, 432B, and 432C are inserted therein, but the present invention is not limited to this aspect. . For example, a thermocouple can be inserted into a sheath. In the case of the first embodiment described above, thermocouples 432A, 432B, and 432C are respectively inserted into individual sheaths, and the sheaths are removed from the trap 6. The downstream side end portion is inserted into a position corresponding to each of the collection chambers.
此外，與上述第二實施方式之精製裝置1A的情況不同，不是從捕集器6之下游側端部，而是從氣化器5之上游側端部讓長形的鞘管416插通亦可。 Further, unlike the case of the refining device 1A of the second embodiment described above, the elongated sheath tube 416 is not inserted from the downstream side end portion of the trap 6, but also from the upstream side end portion of the vaporizer 5. can.
在上述實施方式，是在第一內筒體51及第二內筒體61的內部讓鞘管411,431插通，但本發明並不限定於這種態樣。 In the above embodiment, the sheath tubes 411 and 431 are inserted into the first inner cylindrical body 51 and the second inner cylindrical body 61. However, the present invention is not limited to this.
例如，以配置於內筒體21和外筒體22之間的方式，讓鞘管411,431插通亦可。能將鞘管411,431的表面上所附著的有機材料量減少，而使第二內筒體61的捕集效率提高。此外，精製結束後之鞘管411,431的洗淨變容易。 For example, the sheath tubes 411 and 431 may be inserted so as to be disposed between the inner cylinder 21 and the outer cylinder 22. The amount of organic material adhering to the surfaces of the sheaths 411, 431 can be reduced, and the collection efficiency of the second inner cylinder 61 can be improved. Further, the cleaning of the sheath tubes 411, 431 after the completion of the purification becomes easy.
在上述實施方式，內筒體21及外筒體22是舉圓筒狀的情況為例來作說明，但本發明並不限定於這種態樣。例如可採用箱狀、筒狀、槽型、立方體型等的任意形狀。此外，作為內筒體21及外筒體22的剖面形狀，可列舉圓形 、多角形、半圓形等的形狀。此外，其剖面形狀可為一定，又局部的剖面形狀為不同亦可。此外，內筒體21和外筒體22不是相同剖面形狀亦可。 In the above embodiment, the case where the inner cylinder 21 and the outer cylinder 22 are cylindrical is described as an example, but the present invention is not limited to this. For example, any shape such as a box shape, a cylindrical shape, a groove shape, or a cubic shape may be employed. Moreover, as a cross-sectional shape of the inner cylinder 21 and the outer cylinder 22, a circular shape is mentioned. , polygonal, semi-circular, etc. shapes. In addition, the cross-sectional shape may be constant, and the partial cross-sectional shape may be different. Further, the inner cylinder 21 and the outer cylinder 22 may not have the same cross-sectional shape.
此外，在上述實施方式，是舉第二內筒體61由三個捕集筒體所構成的態樣為例作說明，但並不限定於這種態樣。例如，可使用一體地形成之第二內筒體。 Further, in the above-described embodiment, the second inner cylinder 61 is exemplified by the three collecting cylinders, but the invention is not limited thereto. For example, a second inner cylinder integrally formed may be used.
此外，在上述實施方式，是舉裝置主體2為雙重管構造的情況為例來作說明，但並不限定於這種態樣，不設置外筒體而成為單重管構造亦可。 Further, in the above-described embodiment, the case where the apparatus main body 2 has a double pipe structure will be described as an example. However, the present invention is not limited to such a configuration, and the outer tubular body may not be provided and may be a single pipe structure.
對於捕集器6之各捕集室R1,R2,R3之加熱溫度的設定，並不限定於上述實施方式所說明者。 The setting of the heating temperature of each of the collection chambers R1, R2, and R3 of the trap 6 is not limited to the one described in the above embodiment.
此外，捕集室的數目並不限定於上述實施方式之三個。 Further, the number of collection chambers is not limited to three of the above embodiments.
在上述實施方式，是在收容部54收容粉末狀的有機EL元件用材料，讓其氣化而進行精製，但亦可在收容部54收容液體狀的材料，讓其氣化而進行精製。 In the above-described embodiment, the material for the organic EL element is stored in the accommodating portion 54 and is vaporized and purified. However, the liquid material may be stored in the accommodating portion 54 and vaporized and purified.
使用本發明的精製裝置所精製的有機材料，並不限定於有機EL元件用材料。 The organic material purified by using the refining device of the present invention is not limited to the material for an organic EL device.
此外，使用本發明的精製裝置所精製的有機材料，可反覆進行精製而使純度進一步提高。 Further, the organic material purified by using the refining device of the present invention can be repeatedly purified to further improve the purity.
1‧‧‧有機材料之精製裝置 1‧‧‧Refining device for organic materials
2‧‧‧裝置主體 2‧‧‧Device body
3‧‧‧真空泵 3‧‧‧vacuum pump
3a‧‧‧閥 3a‧‧‧Valves
4‧‧‧溫度控制器 4‧‧‧ Temperature Controller
5‧‧‧氣化器 5‧‧‧ gasifier
6‧‧‧捕集器 6‧‧‧Trappers
21‧‧‧內筒體 21‧‧‧Inner cylinder
22‧‧‧外筒體 22‧‧‧Outer cylinder
23、24‧‧‧蓋部 23, 24‧‧ ‧ cover
41、43‧‧‧溫度感測器 41, 43‧‧‧ Temperature Sensor
42、44‧‧‧控制部 42. 44‧‧‧Control Department
51‧‧‧第一內筒體 51‧‧‧First inner cylinder
52‧‧‧第一外筒體 52‧‧‧First outer cylinder
53‧‧‧加熱器 53‧‧‧heater
54‧‧‧收容部 54‧‧‧ Housing Department
61‧‧‧第二內筒體 61‧‧‧Second inner cylinder
61A‧‧‧第一捕集筒體 61A‧‧‧First capture cylinder
61B‧‧‧第二捕集筒體 61B‧‧‧Second trapping cylinder
61C‧‧‧第三捕集筒體 61C‧‧‧The third trapping cylinder
62‧‧‧第二外筒體 62‧‧‧Second outer cylinder
63‧‧‧溫度調整加熱器 63‧‧‧temperature adjustment heater
63A‧‧‧第一溫度調整加熱器 63A‧‧‧First temperature adjustment heater
63B‧‧‧第二溫度調整加熱器 63B‧‧‧Second temperature adjustment heater
63C‧‧‧第三溫度調整加熱器 63C‧‧‧third temperature adjustment heater
411、431‧‧‧鞘管 411, 431‧‧ ‧ sheath
412、432A、432B、432C‧‧‧熱電偶 412, 432A, 432B, 432C‧‧‧ thermocouples
R1‧‧‧第一捕集室 R1‧‧‧First Capture Room
R2‧‧‧第二捕集室 R2‧‧‧Second collection room
R3‧‧‧第三捕集室 R3‧‧‧ third capture room
Claims (11)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012081397A JP2013208590A (en) | 2012-03-30 | 2012-03-30 | Organic-material refining device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| TW201338854A true TW201338854A (en) | 2013-10-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW102106739A TW201338854A (en) | 2012-03-30 | 2013-02-26 | Organic-material refining device |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP2013208590A (en) |
| KR (1) | KR20150002700A (en) |
| TW (1) | TW201338854A (en) |
| WO (1) | WO2013145832A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI754459B (en) * | 2019-12-16 | 2022-02-01 | 日商富士金股份有限公司 | Gasification supply method and gasification supply device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6096144B2 (en) * | 2014-03-26 | 2017-03-15 | 出光興産株式会社 | Conveying jig, loading method, and purification method |
| KR102297249B1 (en) | 2018-09-12 | 2021-09-03 | 주식회사 엘지화학 | Sublimation purifying apparatus and sublimation purifying method |
| CN112090106B (en) * | 2020-09-15 | 2021-07-27 | 中国地质大学（武汉） | Reagent purification device and method for purifying ammonium bifluoride or ammonium fluoride by using same |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4123498A (en) * | 1977-02-17 | 1978-10-31 | General Electric Company | Process for separating fission product molybdenum from an irradiated target material |
| KR100212132B1 (en) * | 1996-04-24 | 1999-08-02 | 윤종용 | Profile thermocouple of horizontal furnace |
| JP3740587B2 (en) * | 1996-11-25 | 2006-02-01 | 山里産業株式会社 | thermocouple |
| JP4795502B2 (en) * | 1998-09-25 | 2011-10-19 | 新日鐵化学株式会社 | Sublimation purification method and apparatus |
| AU2002358327A1 (en) * | 2001-12-15 | 2003-06-30 | Skc Co., Limited. | Apparatus and method for purifying an organic electroluminescent material |
| JP2005106512A (en) * | 2003-09-29 | 2005-04-21 | Shin Etsu Handotai Co Ltd | Protection tube for thermocouple, and temperature measuring instrument using the same |
-
2012
- 2012-03-30 JP JP2012081397A patent/JP2013208590A/en active Pending
-
2013
- 2013-01-28 KR KR20147030057A patent/KR20150002700A/en not_active Application Discontinuation
- 2013-01-28 WO PCT/JP2013/051712 patent/WO2013145832A1/en active Application Filing
- 2013-02-26 TW TW102106739A patent/TW201338854A/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI754459B (en) * | 2019-12-16 | 2022-02-01 | 日商富士金股份有限公司 | Gasification supply method and gasification supply device |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2013145832A1 (en) | 2013-10-03 |
| KR20150002700A (en) | 2015-01-07 |
| JP2013208590A (en) | 2013-10-10 |
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