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WO2003051796A1 - Appareil et procede pour purifier un materiau organique electroluminescent - Google Patents

Appareil et procede pour purifier un materiau organique electroluminescent Download PDF

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Publication number
WO2003051796A1
WO2003051796A1 PCT/KR2002/002344 KR0202344W WO03051796A1 WO 2003051796 A1 WO2003051796 A1 WO 2003051796A1 KR 0202344 W KR0202344 W KR 0202344W WO 03051796 A1 WO03051796 A1 WO 03051796A1
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WO
WIPO (PCT)
Prior art keywords
purified
section
sections
inner tube
sublimation
Prior art date
Application number
PCT/KR2002/002344
Other languages
English (en)
Inventor
Hong Shik Shim
Min Sik Jang
Ki Nam Byun
Sang Hoon Park
Jong Hoon Son
Hyung Mo Kim
Original Assignee
Skc Co., Limited.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Skc Co., Limited. filed Critical Skc Co., Limited.
Priority to AU2002358327A priority Critical patent/AU2002358327A1/en
Priority to JP2003552688A priority patent/JP2005511864A/ja
Publication of WO2003051796A1 publication Critical patent/WO2003051796A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D7/00—Sublimation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B63/00—Purification; Separation; Stabilisation; Use of additives

Definitions

  • the present invention relates to an apparatus and a method for purifying an organic electroluminescent material; and, more particularly, to an apparatus and a method for purifying the organic electroluminescent material, which are capable of reducing a processing time and applicable to a mass production with a high luminous and purification efficiency.
  • a luminescent material for use in an organic electroluminescence device needs to be purified.
  • the purpose of the purification is to separate pure pigment elements from a mixed luminescent material and to use the pure elements for a thin film deposition.
  • a development of a luminescent material purification technique increases a degree of purity and a luminous efficiency of purified materials, thus extending durability of an organic electroluminescence device using such purified materials.
  • the organic electroluminescent material device is conventionally purified by using a sublimation purification method.
  • Sublimation refers to a direct transform from the solid to the gaseous state or from the gaseous to the solid state without becoming a liquid, which occurs under the conditions of a temperature and a pressure below a triple point in a phase equilibrium diagram.
  • a material that may be pyrolyzed at an atmospheric pressure is hardly decomposed at a low pressure below the triple point even by a comparatively higher temperature.
  • a sublimation apparatus capable of controlling a temperature gradient is used for a vacuum sublimation method which applies heat to a mixed material so as to separate impurities having a different sublimation temperature therefrom without decomposing the material.
  • the vacuum sublimation method is a genuinely physical method, any auxiliary reagent or chemical method are not used, and therefore, there is no contamination of the reagent. Further, the vacuum sublimation method having a high separability is very useful for purifying an organic material for use in the organic electroluminescence device.
  • a train sublimation purification method is widely used for purifying the luminescent material for use in the organic electroluminescence device. This method involves mounting a material to be purified in one end of a hollow tube, vacuum-evacuating an inner portion of the tube by using a vacuum pump and heating the tube by using a heater to thereby generate a temperature gradient all over
  • Fig. 1 shows a schematic diagram of a conventional sublimation purifying apparatus for performing the above- described train sublimation purification method.
  • a material to be purified is put into a cell 4, and the cell 4 is prepared at one end of an inner tube 1.
  • Connection members 3 interconnect separate sections of the inner tube 1, and an outer tube 2 covers the inner tube 1.
  • a heater 5 is installed along the circumference of one end of the outer tube 2, wherein the end thereof corresponds to the end of the inner tube 1 where the cell 4 is positioned.
  • a vacuum pump 6 is prepared at the other end of the inner tube 1 to vacuum-evacuate an inner portion thereof.
  • Fig. 2 illustrates a schematic perspective view of the cell 4 to hold therein the material to be purified.
  • the cell 4 comprising a quartz tube 20 with both ends open and a pair of stainless steel caps 21 to be respectively fitted into each end of the tube 20, each of the caps 21 having a hole 22 formed at a substantially central portion thereof.
  • the vacuum pump 6 vacuum-evacuates the inner portion of the inner tube 1, and the small amount of carrier gas is supplied thereinto, so that a slight pressure gradient is generated. Further, when the heater 5 slowly raises a temperature of the inner tube 1, a temperature gradient is generated. In this case, a temperature distribution shows a normal distribution curve. Once the temperature thereof is higher than a sublimation temperature of the material to be purified therein, the material therein starts to be sublimated. Then, the sublimate material is discharged from the tube 20 through the holes 22 and moved toward the vacuum pump 6 due to the pressure gradient. At this time, impurities of which the sublimation temperature is higher than that of the material to be purified remain in the cell 4.
  • the sublimate material changes its phase into solid and is crystallized on an inner surface of the inner tube 2.
  • the inner tube 1 is slowly cooled down.
  • the inner tube 1 is disassembled and purified materials 25, i.e., materials crystallized on the inner surface of the inner tube 1, are collected and obtained.
  • a material for use in the organic electroluminescence device needs to be highly pure with the extremely small amount of impurities.
  • a purification process should be performed multiple times to obtain high purity of the material. Since the purified materials are scratched from the inner surface of the inner tube 1 in order to be collected, a loss in quantity occurs. Further, whenever the purification process is repeated, the outer tube 2 needs to be disassembled, and therefore, the material to be purified may be contaminated or deteriorated by reacting with oxygen or water vapor. Moreover, a processing time of the purification is increased.
  • an apparatus for purifying an organic electroluminescent material including: one or more inner tubes for mounting material to be purified in one ends of the inner tubes; connection members for separating each of the inner tubes into a plurality of sections; a heat unit for heating the sections of respective inner tubes to more than a sublimation temperature of the material to be purified; and a vacuum pump for vacuum-evacuating the sections of the inner tubes, wherein each of the connection members has a partition for partially closing space between two sections and a hole for making sublimate gas from the material to be purified pass therethrough, the hole being formed at a substantially central portion of the partition.
  • a method for purifying an organic electroluminescent material including the steps of: separating inner portions of one or more inner tubes into a plurality of sections being partially connected; supplying a material to be purified to one end of each inner tube; vacuum-evacuating each inner tube through the other end of each inner tube; and heating each inner tube sequentially from a section holding a material to be purified to neighboring sections to more than a sublimation temperature of the material to be purified.
  • Fig. 1 is a schematic diagram of a conventional apparatus for purifying an organic electroluminescent material
  • Fig. 2 illustrates an exploded perspective view of a conventional cell
  • Fig. 3 shows a schematic diagram of an apparatus for purifying an organic electroluminescent material in accordance with a first embodiment of the present invention
  • Figs. 4A and 4B provide views for explaining a coupling between connection members and an inner tube and a coupling between modified connection members and an inner tube, respectively, in accordance with the first embodiment of the present invention
  • Figs. 5A to 5D depict graphs of temperature distributions in inner sections of the inner tube, respectively;
  • Fig. 6 describes a schematic diagram of an apparatus for purifying an organic electroluminescent material in accordance with a second preferred embodiment of the present invention
  • Figs. 7A and 7B offer views for explaining a coupling between connection members and inner tubes and a coupling between modified connection members and inner tubes, respectively, in accordance with the second embodiment of the present invention
  • Figs. 8A and 8B respectively set forth a front view and a side view of a carrier gas supply unit in accordance with the second preferred embodiment of the present invention
  • Fig. 9 demonstrates a schematic diagram of an organic electroluminescence device
  • Fig. 10 presents a graph for comparing luminous efficiencies of the organic electroluminescence device using organic electroluminescent materials purified by the apparatus in accordance with the first preferred embodiment of the present invention and the conventional apparatus, respectively;
  • Fig. 11 represents a graph for comparing purification efficiencies of the organic electroluminescence device using organic electroluminescent materials purified by the apparatus in accordance with the first preferred embodiment of the present invention and the conventional apparatus, respectively;
  • Fig. 12 provides a graph for comparing processing times of the purification using the apparatus in accordance with the first and the second preferred embodiment of the present invention and the conventional apparatus, respectively.
  • Fig. 3 schematically shows an apparatus for purifying an organic electroluminescent material in accordance with a first preferred embodiment of the present invention.
  • the apparatus in accordance with the first preferred embodiment of the present invention includes an inner tube 31 made of quartz, an outer tube 32 covering the inner tube 31 and a first to a fourth heater 34a to 34d installed along the circumference of the outer tube 32.
  • the inner tube 31 has therein a cell
  • a plurality of, e.g., four connection members 33 separates an inner portion of the inner tube 31 into multiple, e.g., five sections of a first to a fifth section A to E, and interconnects the separate sections of the inner tube 31.
  • Each of the heaters 34a to 34d corresponds to each of the sections A to D, respectively, and thus may heat its corresponding section at a certain temperature independently. If one of the heaters 34a to 34d heats its corresponding section, a temperature of sections adjacent thereto also increases. Since each heater corresponds to each section in the present invention, each section can be consecutively heated. Heating process of at least two sections of the tube may also be carried out by a sliding device for moving a heater against the tube or the tube against the heater.
  • a vacuum pump 37 installed at one end of the inner tube 31 can vacuum-evacuate the inner portion thereof. Further, a carrier gas supply unit 38 installed at the other end thereof can supply nitrogen or inert gas into the inner tube 31.
  • connection members 33 a coupling between connection members 33 and the inner tube 31 in accordance with the first preferred embodiment of the present invention.
  • Each of the connection members 33 is inserted into a portion of the inner tube 31 located between two sections of the inner tube 31.
  • Each connection member 33 has a partition 42 for partially closing a space between two sections and a hole 41 formed at a substantially central portion of the partition 42.
  • Fig. 4B describes a coupling between modified connection members 33a and the inner tube 31.
  • a configuration of the modified connection members 33a is similar to that of the connection members 33 illustrated in Fig. 4A. That is to say, each of the modified connection members 33a also has a partition 45 and a hole 46 formed at a central portion of the partition 45, except for a net 43 prepared at the hole 46.
  • connection members 33 and 33a and the net 43 may be made of any material selected from quartz, stainless steel, aluminum, gold, silver, platinum, nickel, teflon, urethane and glass or a mixture of such materials.
  • a diameter of the holes 41 and 46 is approximately more than 3mm but less than 10mm.
  • Each graduation of the net 43 ranges from about 0.1mm x 0.1mm to about 5mm x 5mm.
  • the to-be-purified material containing impurities is inserted into the cell 35, and the cell 35 is arranged in the first section A of the inner tube 31. If the heater 34a is heated to more than a sublimation temperature of pure materials included in the to-be-purified material, primarily purified materials are moved to the second section B. At this time, as can be seen from Fig. 5A, a temperature of the inner tube 31 is highest in the first section A and becomes lower in following sections B to D. When the material to be purified is sublimated and changes its phase into gas, the sublimate gas is discharged through a hole of the cell 35 and then moved to the second section B by a flow of carrier gas supplied by the carrier gas supply unit 38.
  • the gas passes through the hole 41 of the partition 42 of the connection members 33 as illustrated in Fig. 4A or through the net 43 as shown in Fig. 4B.
  • the holes 41 and 46 of the partition 42 and 45 and the net 43 are used for preventing impurities from moving to another section.
  • a temperature of the heater 34a and a flow rate of the carrier gas it is possible to control a crystallized location of the sublimate gas on an inner surface of the second section B. It is most preferable that the purified materials are crystallized at a central portion of the second section B.
  • connection members 33 or through the net 43 prepared at the hole 46 of the connection members 33a.
  • impurities from the comparatively purified material remain in the second section B and more purified materials in the third section C.
  • the third heater 34a and the fourth heater 34d are operated, and the to-be-purified material is more and more purified in the third section C and the fourth section D. Consequently, the most purified materials remain in the fifth section E.
  • the purifying apparatus in accordance with the first preferred embodiment of the present invention is applied to an experiment for purifying tris (8-hydroxyquinolinato) aluminum (Alq 3 ) that is a luminescent material used for manufacturing an organic electroluminescence device, wherein a manufacturer of Alq 3 guarantees more than 95% of purity of the Alq 3 involved.
  • a temperature of the first heater 34a is raised up to 340°C for three hours at room temperature, which is high enough to sublimate the organic electroluminescent material, and the raised temperature is maintained for six hours.
  • a temperature of the second section B reaches approximately 220°C due to the high temperature of the first heater 34a.
  • the temperature of the second heater 34b is raised from 220°C to 340°C five hours later when the temperature of the first heater 34a reaches 340°C.
  • the first heater 34a is naturally cooled down.
  • the temperature of the second heater 34b is maintained at 340°C for six hours. Five hours later, the third heater 34c starts to be heated.
  • the above-mentioned processes can be equally applied to the third and the fourth heater 34c and 34d. Further, in another case, at least two sections can be heated by moving a single heater against a single inner tube or the single inner tube against the single heater.
  • the carrier gas may not be uniformly supplied into the inner tube.
  • an apparatus for purifying an organic electroluminescent material in accordance with the second preferred embodiment of the present invention has a plurality of inner tubes and multiple connection members.
  • FIG. 6 describes a schematic diagram of an apparatus for purifying an organic electroluminescent material in accordance with a second preferred embodiment of the present invention.
  • Figs. 7A and 7B illustrate connection members 53 and 53a used in the purifying apparatus in accordance with the second embodiment of the present invention.
  • Figs. 8A and 8B schematically show a carrier gas supply unit used in the purifying apparatus.
  • the purifying apparatus in accordance with the second preferred embodiment of the present invention includes a plurality of, e.g., seven inner tubes 51 made of quartz, an outer tube 52 covering the inner tubes 51 and a first to a fourth heater 54a to 54d prepared along the circumference of the outer tube 52. Since each of the inner tubes 51 has a same configuration and function, a description thereof will be based on one inner tube.
  • the inner tube 51 has therein a cell 55 holding a material to be purified. Since a configuration of the cell 55 is same as that of the cell described with reference to Fig. 2, a detailed description thereon will be omitted.
  • a plurality of, e.g., four connection members separate an inner portion of the inner tube 51 into multiple, e.g., five sections of a first to a fifth section A to E, and interconnect the separate sections of the inner tube 51.
  • the first to the fourth heater 54a to 54d correspond to the first to the fourth section of the inner tube 51, respectively, and thus, each heater can heat its corresponding section at a certain temperature. If one of the heaters 54a to 54d heats its corresponding section, a temperature of sections adjacent thereto is also increased.
  • each section can be consecutively heated in the present invention.
  • Heating process of at least two sections of the tube may also be carried out by a sliding device for moving a heater against the tube or the tube against the heater.
  • a vacuum pump 56 installed at one end of the outer tube 52 can vacuum-evacuate the inner tube 51.
  • a carrier gas supply unit 57 installed at the other end of the outer tube 52 can supply nitrogen or inert gas into the inner tube 51.
  • Figs. 7A and 7B offer views for explaining a coupling between the connection members 53 and the inner tubes 51 and a coupling between the modified connection members 53a and the inner tubes 51, respectively, in accordance with the second embodiment of the present invention.
  • connection members 53 and 53a in Figs. 7A and 7B connect seven inner tubes 51 at one time, and therefore, seven purification processes can be simultaneously executed.
  • Fig. 7A there are illustrated the connection members 53 separating an inner portion of each inner tube 51 of quartz into multiple sections.
  • the connection members 53 have seven partitions 47a for partially closing a space between two sections and seven holes 46a formed at substantially central portions of the partitions 47a.
  • Each of the connection members 53 connects two sections prepared on a left and a right side thereof, and, further, forms the inner tube 51.
  • connection members 53a shown in Fig. 7B is similar to that of the connection members 53 illustrated in Fig. 7A. That is to say, the connection members 53a also have a plurality of partitions 47b and holes 46b formed at substantially central portions of the partitions 47b, except for a net 48 prepared at each of the holes 46b.
  • the carrier gas supply unit 57 illustrated in Figs. 8A and 8B has a space 81 for containing the carrier gas and a plurality of holes 82 for making the carrier gas uniformly flow during multiple purification processes.
  • the carrier gas supply unit 57 may be manufactured by using any material selected from quartz, stainless steel, aluminum, gold, silver, platinum, nickel, teflon, urethane, glass or a mixture of such materials.
  • a diameter of each hole 82 ranges from about 0.1 mm to about 5 mm.
  • a method for purifying the material to be purified by using the above-described purifying apparatus in accordance with the second preferred ' embodiment of the present invention is equal to that by using the apparatus in accordance with the first preferred embodiment of the present invention.
  • the difference is in that multiple purification processes are simultaneously performed through a plurality of. inner tubes 51 in the second preferred embodiment of the present invention.
  • a cross section of the inner tube 51 may be of a rectangular shape.
  • a purification process may be performed in such a manner that an inner tube having a rectangular cross- section is prepared, and a material to be purified is uniformly distributed in a bottom portion of the inner tube, wherein a cross-sectional area of the rectangular inner tube is approximately equal to the total cross-sectional area of the aforementioned circular inner tubes.
  • the purifying apparatus in accordance with the second preferred embodiment of the present invention is applied to an experiment for purifying tris (8-hydroxyquinolinato) aluminum (Alq 3 ) that is a luminescent material used for manufacturing an organic electroluminescence device, wherein a manufacturer of Alq 3 guarantees more than 95% of purity of the Alq 3 involved.
  • Seven cells 55 holding 3g of Alq 3 are arranged in the first section A of each inner tube 51.
  • the vacuum pump 56 vacuum- evacuates each inner tube 51, and then, the carrier gas supply unit 57 supplies thereinto nitrogen of 50 cm 3 per minute.
  • the first heater 54a is heated and raised up to 340°C for three hours at room temperature, and the raised temperature, which is high enough to sublimate the aforementioned organic electroluminescent material, is maintained for four hours. At this time, a temperature of the section B reaches 220°C due to the high temperature of the first heater 54a.
  • the temperature of the second heater 34b is raised from 220°C to 340°C three hours later when the temperature of the first heater 34a reaches 340°C.
  • the first heater 54a starts to be naturally cooled down.
  • the temperature of the second heater 54b is maintained for four hours at 340°C.
  • the third heater 54c starts to be heated.
  • Heating process of at least two sections of the tube may also be carried out by a sliding device for moving a heater against the tube or the tube against the heater. In this experiment, after an operation of the fourth heater 54d is completed, materials remaining in the fifth section E are collected. When the heating is completed, the inner tubes 51 are naturally cooled down for three hours until its temperature reaches the room temperature.
  • the cell 4 holds 20g of Alq 3 to be purified and then is prepared at one end of an inner tube 1, wherein the end thereof corresponds to one end of an outer tube 2 where the heater 5 is installed. Further, conditions used in the apparatus of the present invention are equally applied to the- conventional apparatus. That is to say, the cell 4 is vacuum-evacuated by the vacuum pump 6 and the carrier gas is supplied therein. The heater 5 is heated for three hours at room temperature until its temperature reaches 340°C, and the raised temperature is maintained for six hours. For the next three hours, the cell 4 is cooled down until its temperature reaches the room temperature. Subsequently, a vacuum state of the cell 4 is released and purified Alq 3 are collected.
  • the purified Alq 3 are inserted into the cell 4 again, and same purification processes are performed four times. In each purification process, a quantity of collected Alq 3 and the processing time thereof are checked.
  • Fig. 9 provides a schematic diagram of an organic electroluminescence device using organic electroluminescent materials purified by the first preferred embodiment of the present invention.
  • a voltage is applied between the transparent electrode layer 62 and the metal electron layer 65.
  • Fig. 10 presents a graph for comparing luminous efficiencies of the organic electroluminescence device using organic electroluminescent materials purified by the conventional apparatus and the apparatus in accordance with the first preferred embodiment of the present invention, respectively.
  • a data point 71 indicates the luminous efficiency of the organic electroluminescence device using materials purified by the conventional apparatus described with reference to Fig. 1. In this case, the more frequently the purification process is performed, the higher the luminous efficiency becomes.
  • a data point 73 represents the luminous efficiency of the organic electroluminescence device using materials purified by the apparatus in accordance with the first preferred embodiment of the present invention. At this time, only a first and a second heater 34a and 34b are operated and purified materials in a third section C are collected.
  • a data point 74 depicts the luminous efficiency of the organic electroluminescence device using materials purified by the apparatus in accordance with the first preferred embodiment of the present invention.
  • the materials purified by the apparatus in accordance with the first preferred embodiment of the present invention provide a higher luminous efficiency.
  • Fig. 11 represents a graph for comparing purification efficiencies of the organic electroluminescence device using organic electroluminescent materials purified by the apparatus in accordance with the first preferred embodiment of the present invention and the conventional apparatus, respectively.
  • a data point 91 indicates the amount of materials collected by using the conventional apparatus illustrated in Fig. 1.
  • Data points 92 and 93 represent the amount of materials collected in a third and a firth section C and E, respectively, of the apparatus of the present invention as shown in Fig. 3.
  • the purification process ' is performed four times in the conventional method thereby collecting 17.2g (86% of the input) thereof.
  • approximately 18.6g (93% of the input) thereof are collected, which provides a higher purification efficiency than the conventional method.
  • Considering 95% of purity guaranteed by a manufacturer of an organic electroluminescent material to be purified almost the total quantity of purified materials can be collected in a new purification method.
  • Fig. 12 provides a graph for comparing processing times of the purification using the apparatus in accordance with the first and the second preferred embodiment of the present invention and the conventional apparatus, respectively.
  • the conventional apparatus requires approximately 14 hours in order to perform a purification process once: input time of materials to be purified (one hour) , heating time (three hours) , heating maintenance (six hours) , cooling time (three hours) , collecting and cleaning time (one hour) and re-input of materials to be purified. Accordingly, it takes 56 hours to carry out such process four times.
  • the apparatus in accordance with the first preferred embodiment of the present invention needs 32 hours to perform the purification process: input time of materials to be purified (one hour), heating time (three hours) , heating maintenance (24 hours, i.e., six hours x four times), cooling time (three hours) and collecting and cleaning time (one hour) .
  • the apparatus in accordance with the second preferred embodiment of the present invention requires 24 hours to carry out the purification process: input time of materials to be purified
  • An apparatus and method for purifying an organic electroluminescent material in accordance with the present invention provides a higher luminous and purification efficiency than a conventional apparatus and method. Further, when the same amount of materials needs to be purified, a processing time is reduced. In other words, a large amount of materials can be purified during the predetermined processing time. Since the present invention performs a plurality of processes at the predetermined time, materials in a cell can be distributed and a heat transfer becomes efficient. Consequently, an organic electroluminescence device using organic electroluminescent materials purified by the apparatus and method of the present invention is advantageous to a mass production and also provides a high quality.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Electroluminescent Light Sources (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un appareil pour purifier un matériau organique électroluminescent, cet appareil comprenant un ou plusieurs tubes internes, dont une extrémité est destinée à recevoir le matériau à purifier, des éléments de raccordement séparant chacun des tubes internes en une pluralité de segments, une unité de chauffage pour chauffer les segments des tubes internes respectifs à une température dépassant la température de sublimation du matériau à purifier, et une pompe à vide pour faire le vide dans les segments des tubes internes. Chaque élément de raccordement est subdivisé pour renfermer des espaces partiels entre deux segments et un orifice pour permettre le passage à un gaz de sublimation émanant du matériau à purifier, cet orifice étant situé dans une partie sensiblement centrale de la subdivision.
PCT/KR2002/002344 2001-12-15 2002-12-13 Appareil et procede pour purifier un materiau organique electroluminescent WO2003051796A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2002358327A AU2002358327A1 (en) 2001-12-15 2002-12-13 Apparatus and method for purifying an organic electroluminescent material
JP2003552688A JP2005511864A (ja) 2001-12-15 2002-12-13 有機電界発光材料の精製装置及び精製方法

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Application Number Priority Date Filing Date Title
KR20010079725 2001-12-15
KR2001/79725 2001-12-15

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WO2003051796A1 true WO2003051796A1 (fr) 2003-06-26

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JP (1) JP2005511864A (fr)
KR (1) KR100959824B1 (fr)
CN (1) CN1714061A (fr)
AU (1) AU2002358327A1 (fr)
WO (1) WO2003051796A1 (fr)

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WO2006112225A1 (fr) * 2005-03-31 2006-10-26 Nippon Steel Chemical Co., Ltd. Materiau organique el, element organique el l’utilisant, et procede de production de l'element organique el
WO2007001840A2 (fr) * 2005-06-23 2007-01-04 Lucent Technologies Inc. Purification de compositions organiques par sublimation
CN1313183C (zh) * 2005-03-15 2007-05-02 友达光电股份有限公司 用于有机发光材料的纯化系统
CN101865611A (zh) * 2010-06-22 2010-10-20 沈阳慧宇真空技术有限公司 一种有机发光材料升华提纯装置的视窗结构
CN102961890A (zh) * 2012-12-12 2013-03-13 中国科学院长春应用化学研究所 有机小分子材料真空升华提纯的设备及工艺
WO2013176443A1 (fr) * 2012-05-21 2013-11-28 Rohm And Haas Electronic Materials Korea Ltd. Appareil et procédé de purification par sublimation
US20140191422A1 (en) * 2011-08-13 2014-07-10 Beijing Aglaia Technology Development Co., Ltd. Sublimation method for the purification of organic small molecules
US9937438B2 (en) 2013-08-13 2018-04-10 Merck Patent Gmbh Method for vacuum purification
JP6432874B1 (ja) * 2018-06-26 2018-12-05 株式会社奥本研究所 精製装置
CN110538482A (zh) * 2019-09-12 2019-12-06 深圳普瑞材料技术有限公司 一种升华提纯设备
JP2021023868A (ja) * 2019-08-02 2021-02-22 株式会社奥本研究所 精製装置
US11426678B2 (en) 2018-09-12 2022-08-30 Lg Chem, Ltd. Sublimation purification apparatus and sublimation purification method

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KR100754902B1 (ko) * 2005-12-09 2007-09-04 (주) 디오브이 유기전계 발광재료의 정제방법
JP2007246424A (ja) * 2006-03-15 2007-09-27 National Institute Of Advanced Industrial & Technology 有機材料の精製方法
JP5525677B2 (ja) * 2006-07-07 2014-06-18 株式会社半導体エネルギー研究所 精製装置
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