JP2014029844A - Manufacturing method and manufacturing apparatus of light emitting device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a manufacturing method and a manufacturing apparatus of a light emitting device capable of enhancing the utilization efficiency of organic material such as organic EL material.SOLUTION: The manufacturing method includes: a manufacturing step of a light emitting device in which a film of an organic material is formed over a substrate positioned in a deposition chamber; a separation step in which the light emitting device and a part other than the light emitting device in the deposition chamber are separated from each other; a cleaning step in which the organic material deposited on the part other than the light emitting device in the deposition chamber is cleaned by heating in a state where oxygen and water are removed; and a recovery step in which the organic material separated from the part other than the light emitting device in the cleaning step is restored in the state where oxygen and water are removed. The restored organic material is returned to the light emitting device manufacturing step to reuse the same.

Description

  The present invention relates to a manufacturing method and a manufacturing apparatus of a light emitting device using a layer containing an organic compound as a light emitting layer.

  In recent years, research on a light-emitting device having an EL (Electro Luminescence) element as a self-luminous element has been activated, and a light-emitting device using an organic material as an organic EL material has attracted attention. This light emitting device is also called an organic EL display or an organic light emitting diode.

  Organic materials are roughly classified into low molecular weight materials and high molecular weight materials. Among these, low molecular weight materials are mainly formed by vapor deposition.

  An organic material used for the organic EL material is easily oxidized and deteriorated by the presence of oxygen or water. Therefore, a photolithography process cannot be performed after the film formation, and in order to form a pattern, it is necessary to form a pattern at the same time as the film formation with a mask having an opening (hereinafter referred to as an evaporation mask). Therefore, vapor deposition is generally used for film formation. The organic EL material is evaporated and sublimated in an inert gas substitution and reduced pressure state or in a vacuum state, and the film is formed on a substrate having a vapor deposition mask.

  In this vapor deposition, most of the sublimated organic EL material is not formed on the substrate, and the inner wall of the film formation chamber or the vapor deposition mask or deposition shield (to prevent the vapor deposition material from adhering to the inner wall of the film formation chamber). Adheres to the protective plate.

  If the film is deposited while the organic EL material is attached to the inner wall of the film formation chamber, or the deposition mask or deposition shield, the attached organic EL material is re-sublimated and deposited on the substrate as an impurity, resulting in a reduction in product quality. Will be invited.

  For this reason, the vapor deposition mask and the deposition shield are cleaned after use. However, in order to remove the organic EL material attached to the deposition mask and the deposition shield, the deposition chamber and the deposition shield are temporarily released from the atmosphere. It was necessary to take out the film, wash it in a separate process, and return it to the film formation chamber again. Once released to the atmosphere, the attached organic EL material deteriorates and must be discarded. In addition, the water or oxygen adsorbed by the vapor deposition mask or deposition shield when released into the atmosphere and released may be released during the film formation of the organic EL material and taken into the film. There was concern that it could cause a decline.

  Therefore, there is a contrivance to perform cleaning so that oxygen and moisture do not adhere to the vapor deposition mask and the deposition shield by performing cleaning under vacuum (for example, see Patent Document 1).

  In Patent Document 1, cleaning is performed by heating a part to which an organic EL material is adhered in the vapor deposition process to sublimate the material and exhaust it. The cleaned part can be used again during film formation.

Japanese Patent No. 4785269

  In such a conventional light emitting device, since the organic EL material removed in the cleaning process is exhausted, there is a problem that the utilization efficiency of the organic EL material is low.

  An object of this invention is to provide the manufacturing method and manufacturing apparatus of a light-emitting device which can improve the utilization efficiency of organic materials, such as organic EL material.

  In order to achieve this object, a light emitting device manufacturing process of a light emitting device made by depositing an organic material on a substrate provided in a film forming chamber, and a light emitting device other than the light emitting device and the light emitting device in the film forming chamber A separation process for separating the parts, a cleaning process for cleaning the organic material adhering to a part other than the light-emitting device in the film formation chamber by heating in a state where oxygen and moisture are removed, and a light-emitting device by the cleaning process A method for manufacturing a light-emitting device, comprising: a recovery step of recovering an organic material separated from a portion other than a portion in a state where oxygen and moisture are removed; the recovered organic material is returned to the light-emitting device manufacturing step and reused In addition, the manufacturing apparatus is used to achieve the intended purpose.

  According to the present invention, a light-emitting device having an effect of increasing the utilization efficiency of an organic material can be recovered without being deteriorated and reused except for an organic material that is formed on a substrate and effectively used as a light-emitting device. A manufacturing method and a manufacturing apparatus can be provided.

The block diagram of the manufacturing method of the light-emitting device of this invention Schematic cross-sectional view of deposition chamber during deposition Schematic cross-sectional view of film formation chamber during cleaning and recovery process The block diagram of the manufacturing method of the light-emitting device of this invention in case a refinement | purification process is included Schematic cross section of the purification chamber during the purification process Schematic of the device structure using the manufacturing method of the light emitting device of the present invention

  The method for manufacturing a light-emitting device according to claim 1 of the present invention includes a light-emitting device manufacturing process of a light-emitting device made by depositing an organic material on a substrate provided in a film-forming chamber, and light emission in the film-forming chamber. A separation step of separating a portion other than the device and the light emitting device, and a cleaning step of cleaning the organic material attached to the portion other than the light emitting device in the film forming chamber by being heated in a state where oxygen and moisture are removed, The organic material separated from the portion other than the light emitting device by the cleaning process is recovered in a state where oxygen and moisture are removed, and the recovered organic material is returned to the light emitting device manufacturing process and reused. It is a manufacturing method of a light-emitting device.

  As a result, organic materials other than the organic material that is formed on the substrate and effectively used as a light emitting device can be recovered without deterioration, and the reuse efficiency of the organic material can be improved by being reused.

  Further, the recovery part of the organic material recovery step may be equal to or lower than the heating temperature of the cleaning step. As a result, the organic material evaporated in the cleaning process is easily deposited in the recovery unit, and the recovery efficiency is improved.

  Further, in the organic material recovery step, the temperature of the part other than the recovery part may be raised to a temperature equal to or higher than the sublimation temperature of the organic material. Thereby, it becomes possible to deposit an organic material only in a collection | recovery part, and it has an effect of a collection rate improvement.

  In the organic material recovery step, the end of the recovery step may be determined by a film thickness meter. As a result, the recovery process can be completed in the shortest necessary time, and the film formation chamber can be reused as the original light emitting device manufacturing process. Efficiency can be increased.

  Moreover, you may use the manufacturing method of the light-emitting device characterized by consisting of the refinement | purification process which isolate | separates and refine | purifies the collect | recovered organic material after a collection | recovery process. In this case, even when impurities are contained in the organic material or when two or more kinds of organic materials are present, it becomes possible to separate and purify the necessary organic material to obtain a high-purity material for reuse. When it does, it has the effect that a higher quality light-emitting device can be manufactured.

  Moreover, the frequency | count of the washing | cleaning process of parts other than a light-emitting device may be more than the frequency | count of the refinement | purification process of an organic material. As a result, the parts other than the light emitting device that has been cleaned can be used again in the light emitting device manufacturing process without waiting for the completion of the purification process, and the production amount of light emitting devices equal to or higher than before can be secured. Have. Further, by performing the washing step twice or more with respect to one purification step, the purification efficiency is improved when the purification time does not depend on the amount of the organic material to be purified in the purification step. In addition, the material can be reused after the purification step.

  Moreover, it is good also as a light-emitting device manufacturing apparatus which manufactures a light-emitting device using the manufacturing method of the light-emitting device as described in any one of Claims 1-7. Thus, in addition to the effects of claims 1 to 7, the light emitting device can be manufactured in the same device, and parts other than the light emitting device can be cleaned. In addition, impurities and a plurality of types can be contained in the recovered organic material without deterioration. Even if the organic material is present, it can be separated and purified, so that the utilization efficiency of the organic material can be increased. The parts other than the light-emitting device that has been cleaned can be used again in the light-emitting device manufacturing process, regardless of the time required for the purification process. Have.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings.

(Embodiment 1)
FIG. 1 shows a block diagram of a method for manufacturing a light emitting device of the present invention.

  The light emitting device manufactured in the light emitting device manufacturing process is separated from portions other than the light emitting device in the separation process (shown by a solid line).

  The parts other than the light emitting device are separated from the light emitting device in the separation process from the light emitting device manufacturing process, separated from the organic material in the cleaning process by heating in a state in which oxygen and moisture are removed, and washed again. Used in (indicated by dotted line). The state in which oxygen and moisture are removed is, for example, an environment substituted with an inert gas or a vacuum state. A vacuum is desirable, and in the following description, it will be described as a vacuum state.

  The organic material that adheres in the light emitting device manufacturing process and adheres to a portion other than the light emitting device separated from the light emitting device in the separation step is separated from a portion other than the light emitting device in a cleaning process that is heated in a vacuum state. At the same time, it is recovered in the recovery process in a vacuum state and used again in the light emitting device manufacturing process (indicated by a broken line).

  The light emitting device manufacturing process is a process in which an organic material is formed between two electrodes (anode and cathode) on a substrate. This step includes steps for manufacturing a light emitting device such as pretreatment of the substrate, electrodes, film formation of an organic material, sealing, and the like. During film formation, the substrate is covered with a vapor deposition mask having an opening in order to pattern it into an arbitrary shape.

  A light emitting device manufacturing process, that is, a film forming process will be described with reference to FIG.

  FIG. 2 is a schematic cross-sectional view of the film forming chamber during vapor deposition.

  The substrate 1 is transferred into the film forming chamber 2 through a gate (not shown) and set above the film forming chamber 2. A deposition mask 3 is disposed on the lower surface of the substrate 1 inside the film forming chamber 2, and an adhesion shield 4 is provided so as to surround the side surface and the lower surface of the film forming chamber. A heating unit 11 is provided in the vicinity of the deposition shield 4.

  The vapor deposition source 5 is a cylindrical container having an open top, and is filled with an organic material 6.

  The heating unit 7 includes a heater 8 therein, and the heating unit 7 can be heated by energizing the heater 8.

  The heating unit 7 has a structure in which a lower part of the vapor deposition source 5 is covered with a concave portion at the center, and the bottom surface and the side surface lower part of the vapor deposition source 5 are in contact with the heating unit 7.

  A detection unit 13 of the film thickness meter 12 is installed in the vicinity of the heating unit 7, and the film thickness meter 12 and the detection unit 13 are connected by a power line and a signal line.

  In such a configuration, the organic material 6 heated by the heating unit 7 inside the vapor deposition source 5 is evaporated and sublimated. Since the evaporation source 5 has a cylindrical shape, the moving direction of the organic material 6 is limited, and the film forming chamber 2 is evaporated and sublimated in the upper direction.

  Since the inside of the film forming chamber 2 is depressurized by a vacuum pump (not shown), the number of gas molecules existing in the space is reduced as compared to the atmospheric pressure state.

  In such a state, the organic material 6 evaporated and sublimated from the vapor deposition source 5 can reach the substrate 1 or the like with almost no collision with gas molecules in the film forming chamber 2.

  The organic material 6 that has reached the substrate 1 is formed as an organic material thin film 9. The organic material 6 reaches not only the substrate 1 but also the vapor deposition mask 3 and the deposition shield 4 and is formed as an organic material thin film 9. A typical movement of the organic material 6 is indicated by a dotted arrow.

  The organic material thin film 9 formed in this way does not contain molecules derived from gas components inside the film, and thus can exhibit uniform characteristics.

  As the method for heating the vapor deposition source 5 by the heating unit 7, the method using the heater 8 has been shown. However, in addition to this method, there are a method of heating by infrared rays, high frequency, etc., a method of heating by providing a nichrome wire, electromagnetic induction, etc. However, it is not particularly limited. Since the powdered organic material 6 is heated in a vacuum, it is preferably a heating means having excellent heat transfer efficiency.

  The vapor deposition mask 3 is installed to form the organic material thin film 9 having an arbitrary pattern on the substrate. The deposition mask 3 may be installed in close contact with the substrate 1 or has a space between the substrate 1 and the deposition mask 3. You may install in the film-forming chamber 2 in the state.

  In addition, the heating temperature by the heating part 7 should just be the temperature more than the temperature which the organic material 6 evaporates and sublimates, and should just be low temperature from the temperature which the organic material 6 decomposes | disassembles.

  In order to confirm in advance the temperature at which the organic material 6 evaporates and sublimates, thermogravimetry (hereinafter referred to as TG), which is a measurement method for examining the change in weight when the target material is heated in a vacuum, is performed. That's fine.

  In this embodiment mode, film formation by vapor deposition is exemplified, but any means can be used as long as a uniform organic material thin film can be formed.

  In the separation step, the organic material 6 deposited on the manufactured light-emitting device is separated from the light-emitting device and the light-emitting device other than the light-emitting device and the light-emitting device, for example, the deposition mask 3 and the deposition shield 4 so that the organic material 6 is not washed in the next cleaning step. It is a process to do.

  For example, the substrate 1 in FIG. 2 is separated by being transferred from a gate (not shown) to the outside of the film formation chamber 2.

  FIG. 3 is a schematic cross-sectional view of the film forming chamber during the cleaning and recovery steps after the substrate 1 is taken out after film formation.

  The cleaning process and recovery process in the configuration of FIG. 3 will be described.

  When the light emitting device manufacturing process is completed, the substrate 1 and the vapor deposition source 5 are taken out of the film forming chamber 2, and the recovery unit 14 is installed so as to fit the recess of the heating unit 7 on the bottom surface of the film forming chamber 2.

  In such a configuration, the cleaning process starts by operating the heating unit 10 and the heating unit 11 and heating the vapor deposition mask 3 in the vicinity of the heating unit 10 and the deposition shield 4 in the vicinity of the heating unit 11.

  The organic material thin film 9 present on the surfaces of the deposition mask 3 and the deposition shield 4 is heated and separated from the deposition mask 3 and the deposition shield 4, whereby the deposition mask 3 and the deposition shield 4 are cleaned. Parts other than the cleaned light emitting device are used again in the light emitting device manufacturing process.

  The recovery process is a process of recovering the evaporated and sublimated organic material 6 by vapor deposition on the recovery unit 14 as indicated by the dotted arrow.

  The heating temperature of the vapor deposition mask 3 by the heating unit 10 and the heating temperature of the deposition shield 4 by the heating unit 11 are the temperatures at which the organic material 6 evaporates and sublimes, similar to the temperature when the vapor deposition source 5 is heated in the light emitting device manufacturing process. The temperature may be any of the above, and may be lower than the temperature at which the organic material 6 is decomposed.

  Although the heating unit 7 has a structure having a recess at the center, it is not limited to this shape, and the heating unit 7 is configured using a flat plate member that is in close contact with the entire bottom surface of the recovery unit 14. Also good.

  Any structure may be used as long as the organic material 6 scattered inside the film formation chamber 2 is fixed to the collection unit 14 by heating the collection unit 14 uniformly. It is possible to recover efficiently.

  In the recovery step, it is preferable to arrange the recovery unit 14 so that the surface of the heating unit 7 is not exposed inside the film forming chamber 2. By preventing the organic material 6 from adhering to the heating unit 7 and being fixed, the recovery efficiency of the organic material 6 can be improved.

  The heating temperature of the recovery unit 14 by the heating unit 7 may be lower than the temperature at which the organic material 6 evaporates and sublimes.

  As a result, the organic material 6 evaporated and sublimated from the vapor deposition mask or the deposition shield is condensed and solidified on the recovery unit 14.

  The detection unit 13 of the film thickness meter 12 is installed in the vicinity of the collection unit 14. The detection unit 13 includes a crystal resonator, and by detecting a change in the resonance frequency of the crystal resonator, the mass of a small amount of substance attached to the detection unit can be detected.

  The detection unit 13 of the film thickness meter 12 is maintained at a temperature equivalent to that of the recovery unit 14, that is, a temperature lower than the temperature at which the organic material 6 evaporates and sublimes.

  In such a configuration, the film formation speed and the thickness of the organic material thin film 9 formed on the surface of the detection unit 13 by grasping the state of the resonance frequency variation due to the organic material 6 attached to the crystal resonator. Can know.

  Therefore, since the evaporation and sublimation of the organic material 6 from the vapor deposition mask 3 and the deposition shield 4 can be determined to stop when the film growth on the surface of the detection unit 13 stops, the heating unit 10 and the heating unit 11 can be determined. It is only necessary to stop the heating by quickly, and the recovery process can be completed in the shortest necessary time.

  In the light emitting device manufacturing process, the organic material 6 is deposited on the substrate as an organic material thin film 9 having a thickness of about several tens of nanometers. Therefore, the same organic material is used for the deposition mask 3 and the deposition shield 4 to be cleaned. It is deposited as a thin film 9.

  It is difficult to visually confirm the presence of a thin film of about several tens of nm, and it is difficult to determine the degree of progress of the cleaning process from the surface state of the object to be cleaned. In addition, the film formation chamber 2 is often made of a metal material such as stainless steel, and is tightly sealed to maintain a vacuum, so that the inside of the film formation chamber 2 can be observed from the outside. Is difficult.

  In the present embodiment, when the growth of the film adhering to the surface of the detection unit 13 is stopped, the organic material 6 evaporated from the vapor deposition mask 3 or the deposition shield 4 is not observed without observing the surface state of the cleaning target. It can be determined that the collection has been completed.

  By completing the collection process in the shortest necessary time, the deposition chamber can be reused as the original light-emitting device manufacturing process, which can improve the production efficiency of products and the efficiency of organic material recovery operations. become.

  The purity of the recovered organic material 6 can be measured by an analytical method such as high performance liquid chromatography. Specifically, a high-performance liquid chromatograph in which a part of the recovered organic material 6 is dissolved in an organic solvent is used as an analysis sample, and separation column conditions, mobile phase conditions, detection means, etc. are appropriately set. The purity can be measured from the chromatogram obtained by the analysis.

  If the collected organic material 6 has a purity necessary for film formation, it is used again in the light emitting device manufacturing process and is formed on the substrate 1.

  In the light-emitting device shown in this embodiment mode, the organic material 6 exhibits a function as an organic material thin film of about several tens of nanometers. Therefore, when impurities are mixed in the organic material thin film, the performance and durability may be greatly impaired. is there. Therefore, it is preferable that the recovered organic material 6 has as high a purity as possible, and a high purity of 99.9% or more may be required.

  It is preferable that the cleaning step and the recovery step are performed in the same space. This is because loss of the washed organic material 6 until it is recovered can be suppressed.

  In the cleaning step of the portion other than the light emitting device, cleaning by evaporating the organic material 6 by heating is preferable. In addition, there are cleaning by physical peeling, cleaning with an organic solvent, etc., but heating is preferable as compared with cleaning with an organic solvent, because facilities such as a cleaning liquid tank and a waste liquid tank are not necessary. Furthermore, the organic material 6 is diluted with the organic solvent, and it takes a long time for the recovery in the subsequent recovery process or requires concentration. Therefore, cleaning by evaporation of the organic substance by heating is preferable.

  However, if the above equipment can be introduced or the dilution can be controlled, there is no problem even with washing with an organic solvent.

  In the cleaning by physical peeling, the organic material thin film 9 attached to the surfaces of the vapor deposition mask 3 and the deposition shield 4 can be peeled using a member harder than the organic material thin film 9.

  However, a member harder than the vapor deposition mask 3 and the deposition shield 4 cannot be used as a member used for peeling, and care must be taken in selecting an appropriate material.

  Further, there is a possibility that the vapor deposition mask 3 and the deposition shield 4 are deformed by the peeling operation. In particular, when the vapor deposition mask 3 is deformed, an accurate pattern of the organic material thin film 9 cannot be formed on the substrate 1 in the light emitting device manufacturing process. Therefore, cleaning by evaporation of organic substances by heating is preferable.

  The recovery step is preferably recovery by vapor deposition. Other recovery methods include physical collection, suction recovery, adsorption recovery, and the like, but vapor deposition which is a method that easily suppresses deterioration of materials is preferable. However, other methods may be used as long as deterioration of the material can be suppressed.

  The collecting unit 14 is preferably made of a material that can be deposited. For example, a material that is not denatured by the temperature at the time of vapor deposition, such as metal, glass, ceramics, and fluororesin, is preferable.

  Moreover, the surface area of the adhesion part of the collection | recovery part 14 of the organic material 6 is smaller than the area which combined the surface area of the vapor deposition mask 3, and the effective surface area which shields the organic material 6 of the deposition shield 4. As a result, the organic material 6 adhering to the collection part 14 is vapor deposited thicker than the state adhering to the vapor deposition mask 3 and the deposition shield 4.

  Therefore, in the light emitting device manufacturing process or the purification process, when the organic material 6 is separated from the recovery unit 14 and then only the organic material 6 is transferred to another container and heated, the surface of the recovery unit 14 is relatively thick. Since the organic material 6 is attached in a thick state, it can be easily peeled off by a physical peeling means such as a scraper.

  In the light emitting device manufacturing process or the refining process, the organic material 6 is heated while attached to the recovery unit 14. However, since the recovery unit 14 has a relatively small shape, the light emitting device manufacturing process or Heating can be efficiently performed with less input energy in the purification process.

  At the time of recovery, the recovery unit 14 is lower than the temperature heated at the time of washing, preferably the temperature other than the recovery unit 14 and the detection unit 13 is raised to a temperature higher than the sublimation temperature of the organic material 6, and the recovery unit 14 and the detection unit 13 are It is desirable that the temperature be lower.

  This temperature is adjusted by the heating unit 7, the heating unit 10, and the heating unit 11.

  Examples of temperature control such as heating include a method of heating from the outside with a heater, infrared rays, high frequency, etc., a method of heating by providing a nichrome wire or the like in the heating portion, a method of heating by electromagnetic induction, and the like.

  In this embodiment, the heating units 7, 9, and 10 are provided in the vicinity of the vapor deposition source 5, the vapor deposition mask 3, and the deposition shield 4, but heating is performed inside the vapor deposition source 5, the vapor deposition mask 3, and the deposition shield 4. It is good also as a structure which provides a part. For example, in the case of a method of embedding a nichrome wire or heating by electromagnetic induction, the same effect can be obtained without providing the heating unit 10 in the vicinity.

  Although the heating unit 7 has a structure having a recess at the center, it is not limited to this shape, and the heating unit 7 is configured using a flat plate member that is in close contact with the entire bottom surface of the recovery unit 14. Also good.

  In FIG. 3, the detection unit 13 is installed adjacent to the recovery unit 14. However, the detection unit 13 is not limited to this arrangement, and the adhesion rate of the organic material 6 to the recovery unit 14 can be estimated in the cleaning process. The same effect can be obtained at any position. In order to accurately estimate the amount of the organic material 6 recovered in the recovery unit 14, the attachment site of the organic material 6 in the detection unit 13 is set toward the vapor deposition mask 3 and the deposition shield 4 in the same manner as the recovery unit 14. It is desirable to do.

  By performing cleaning and recovery in a vacuum state, deterioration of the organic material 6 can be suppressed.

  This is because, like the light emitting device manufacturing process, oxygen and moisture are removed in a vacuum, and deterioration of the material can be suppressed. In addition, the evaporation of the organic substance by heating in a vacuum state may be a temperature lower than the temperature necessary for peeling and evaporating in the atmospheric pressure, so that the probability of detaching the intramolecular bond in the organic substance is reduced or separated. Separation and evaporation are possible from parts other than the light emitting device.

  For example, Alq3 (tris (8-quinolinolato) aluminum), which is often used as an organic EL material, has a melting point of 413.5-414.5 ° C. at atmospheric pressure in the catalog of jilin OLED Material tech. No. 4208492 describes that it is 202 ° C. in a vacuum.

  Therefore, in the cleaning process, heating to 202 ° C. or higher in vacuum is performed by sublimation and cleaning while suppressing deterioration of the material, and the recovery portion can be deposited and recovered at a temperature lower than 202 ° C. Compared to vapor deposition in the air, it has an energy saving effect.

  Since the melting point and the sublimation temperature differ depending on the material to be handled, the temperature elevation temperature in the above washing and recovery process is an example.

  The organic material 6 to be used is not limited to a low molecule or a high molecule, but a material having sublimation property is desirable. Examples thereof include materials used for organic electronics materials, organic semiconductor materials, organic solar cell materials, organic EL materials, pharmaceutical organic materials, fragrances, and the like. By having sublimation properties, it is possible to form a film only by changing from solid to gas and from gas to solid, and it is easy to form a film in an arbitrary shape.

  The recovered organic material 6 can be reused as it is in the light emitting device manufacturing process as long as the purity is necessary for film formation. Specifically, as an alternative to the vapor deposition source 5, the organic material 6 can be reused by installing the recovery unit 14 on which the organic material 6 is vapor deposited on the heating unit 7.

  In the present embodiment, the evaporation source 5 is a container having a cylindrical shape with an open top, and the movement direction during evaporation and sublimation of the organic material 6 is limited to the upper direction. Therefore, when the collection unit 14 is used as an alternative to the vapor deposition source 5, the movement direction during evaporation and sublimation of the organic material 6 cannot be limited to the upper direction. Therefore, a large amount of the organic material 6 adheres to the deposition shield 4 other than the substrate 1, which may reduce the work efficiency of the light emitting device manufacturing process.

  However, if it is expected that the operation efficiency of the recovery process is greatly improved by omitting the work of peeling the organic material 6 from the recovery unit 14, the recovery unit 14 is used as an alternative to the vapor deposition source 5. May be.

  When the organic material 6 is reused, it is not necessary to newly add the organic material 6 depending on the recovered amount.

  The light emitting device manufacturing process is preferably a vapor deposition method. Vapor deposition is often performed in a vacuum. In vacuum vapor deposition, it is possible to remove components that alter the organic material 6 such as moisture adhering to the substrate 1 or the like. There are other application processes, but in the application process, when a liquid material is formed, the material needs to be dried and takes time. In addition, when the organic material 6 is laminated, the material deposited below may be dissolved again. Therefore, the vapor deposition process which is a dry process is preferable. However, when the drying time and re-dissolution of the material are not a problem, there is no problem even in the coating process if control is possible.

  In the light emitting device manufacturing process or the refining process, the organic material 6 is heated inside the recovery unit 14, and the recovery unit 14 has a dish-like shape whose peripheral part is relatively higher than the central part. Therefore, even if the organic material 6 heated in the light emitting device manufacturing process or the purification process is liquefied, the organic material 6 can be prevented from flowing out from the recovery unit 14.

  As described above, by using the method of the present invention, it is possible to efficiently recover the organic material 6 attached to a portion other than the light emitting device at the time of manufacturing the light emitting device, and deterioration of the recovered organic material 6 is suppressed. Therefore, it can be used again in the light emitting device manufacturing process, and the use efficiency of the organic material 6 can be increased. Compared to the case where it has been disposed of up to now, material costs and disposal costs can be reduced.

(Embodiment 2)
FIG. 4 shows a block diagram of a method for manufacturing a light emitting device of the present invention including a purification step. The same components as those in FIGS. 1 to 3 are denoted by the same reference numerals, and detailed description thereof is omitted.

  The light emitting device manufactured in the light emitting device manufacturing process is separated from portions other than the light emitting device in the separation process (shown by a solid line).

  The parts other than the light emitting device are separated from the light emitting device in the separation process from the light emitting device manufacturing process, separated from the organic material in the cleaning process by heating in a vacuum, washed, and used again in the light emitting device manufacturing process (dotted line) ).

  The organic material that adheres in the light emitting device manufacturing process and adheres to a portion other than the light emitting device separated from the light emitting device in the separation step is separated from a portion other than the light emitting device in a cleaning process that is heated in a vacuum state. At the same time, it is recovered in the recovery step in a vacuum state, separated and purified in the purification step, and used again in the light emitting device manufacturing step (indicated by a broken line).

  FIG. 5 is a schematic cross-sectional view of the purification chamber during the purification process.

  The recovery unit 14 to which the organic material 6 is attached is carried into the purification unit 21, and a plurality of heating units 22 are provided along the purification unit 21 outside. An inert gas is introduced from the entrance, and the pressure is reduced from the exit.

  The plurality of heating units 22 can be set at different temperatures, and can give a temperature gradient to the inner wall surface of the purification unit 21.

  In such a configuration, the organic material 6 collected from the collection unit 14 is first heated and sublimated in the purification unit 21 (dotted line arrow). In addition to the flow of the inert gas introduced and reduced pressure in the purification unit 21, a temperature gradient is generated by the plurality of heating units 22. Therefore, the sublimated organic material 6 moves in the purification unit 21 along with the gas flow, and sublimates (solidifies) in a region where the material has a sublimation temperature unique to the material. Since the sublimation temperature is unique to the material, it can be separated from impurities and multiple materials and purified simultaneously.

  Since an appropriate sublimation temperature and vacuum degree differ depending on the organic material 6, it is presented as an example. Alq3 (tris (8-quinolinolato) aluminum), which is often used as an organic EL material, is atmospheric pressure in the catalog of jilin OLED Material tech. Among them, the melting point was 413.5-414.5 ° C., but Japanese Patent No. 4208492 describes that it is 202 ° C. in a vacuum. Therefore, purification is performed by sublimation by heating to 202 ° C. or higher in vacuum.

  The purification step is desirably performed when the organic material 6 recovered in the recovery step contains impurities or a plurality of types of organic materials 6. That is, when the purification process described in the first embodiment is not performed, one type of organic material 6 is used inside the film formation chamber 2, and the deposition mask 3 and the deposition shield 4 are used in the cleaning process. This is a case where no substances other than the organic material 6 to be collected are generated.

  Examples of cases that require a purification step include co-evaporation in which two types of organic materials are simultaneously deposited at different deposition rates, and cases in which two or more types of organic materials are continuously deposited in the same film formation chamber 2. The When the organic material thin film 9 to be collected has two or more types of components, the organic material 6 attached to the collection unit 14 is likely to contain two or more types of components, so the purification process is performed. Thus, it is necessary to separate and purify into a single component.

  In the purification process, impurities are separated, recovered or discarded, but the definition of impurities is arbitrary and is left to the user's discretion. In addition, the purification process includes separation, purification, recovery, and disposal of a plurality of types of organic materials 6, but the determination of the organic material 6 that is to be purified and recovered is optional, and it is not necessary to purify and recover all of them, and they are discarded. It doesn't matter.

  The number of washing steps and purification steps are not necessarily the same. That is, it is not necessary to carry out a single purification step after a single washing step, and it is desirable that the number of washing steps is larger than the number of purification steps. The fact that the number of washing steps is larger than the number of purification steps means that the organic material 6 is accumulated through several washing steps in the recovery step and is collectively purified in the purification step. In this case, since the cleaning can be performed regardless of the time required for the purification process, the light emitting device manufacturing process can be performed without delay and the light emitting device can be manufactured. In other words, the use efficiency of the organic material 6 can be increased by securing the same amount of light emitting device production as before and allowing the organic material 6 to be reused.

  The method used in the purification step is preferably the sublimation purification method described above. Other methods include chromatography and recrystallization.

  Examples of the inert gas include nitrogen, helium, argon, and the like and gases having low reactivity with the organic material 6.

  As described above, by using the method of the present invention, it is possible to efficiently recover the organic material 6 attached to a portion other than the light emitting device at the time of manufacturing the light emitting device without deteriorating, and the recovered organic material 6 is subjected to a purification process. By passing, it becomes possible to reduce impurities and to separate and purify a plurality of types of organic materials 6, and to increase the use efficiency of the organic materials 6 by reusing the organic materials 6 purified in the light emitting device manufacturing process. I can do it. It can also be used when a plurality of types of organic materials 6 are formed and laminated in the light emitting device manufacturing process. Moreover, compared with the case where the organic material 6 has been disposed of up to now, the material cost and the disposal cost can be suppressed.

  Since a series of steps can be performed in a vacuum, it has become possible to reduce the cost and labor for releasing to the atmosphere and re-depressurization.

  By using different numbers of washing and refining processes, it is possible to secure the same amount of light emitting device production as before, and to increase the efficiency of use of organic material 6 by enabling reuse of organic material 6. It became.

(Embodiment 3)
FIG. 6 shows a schematic diagram of a structure of a manufacturing apparatus using the method for manufacturing a light emitting device of the present invention. Detailed descriptions of the same components as those in FIGS. 1 to 5 are omitted.

  FIG. 6 shows an example of a cluster-type light emitting device manufacturing apparatus, but this embodiment does not depend on the light emitting device manufacturing method of the present invention.

  In FIG. 6, the preparation chamber 31, the pretreatment chamber 34, the film formation chamber A 35, the film formation chamber B 36, the film formation chamber C 37, and the sealing chamber 38 are connected through the gate 39 with the transfer chamber 32 as the center. The purification chamber 40 is connected to each film forming chamber through a gate 39 at a portion different from the portion connected to the transfer chamber 32.

  The separation, washing, recovery, and purification steps from the manufacturing of the light emitting device will be described.

  The preparation chamber 31 is a chamber for preparing the substrate 1. In the preparation chamber 31, the substrate 1 is set from the outside. Next, the substrate 1 is transferred from the preparation chamber 31 to the pretreatment chamber 34 via the transfer chamber 32 by the transfer mechanism 33, and pretreatment for film formation, such as cleaning the surface of the substrate 1, is performed. And it is carried to film-forming chamber A35, and the electrode and the organic material 6 are formed into a film. When multiple layers are formed, the film is transferred from the film formation chamber A35 to the film formation chamber B36 and from the film formation chamber B36 to the film formation chamber C37 for each material and layer. The deposited substrate 1 is sealed in the sealing chamber 38 to complete the light emitting device. Finally, the completed light emitting device is carried out from the preparation chamber 31.

  The above is the part corresponding to the light emitting device manufacturing process and the separation process.

  Next, cleaning, recovery, and purification steps will be described.

  In the film formation chamber, the organic material 6 that has not been formed on the light emitting device adheres to parts other than the light emitting device, such as the vapor deposition mask 3, the deposition shield 4, and the shutter (not shown) of the vapor deposition source 5. Therefore, the organic material 6 separated from the portion other than the light emitting device is recovered without being deteriorated by performing the cleaning in a vacuum state. Here, the parts other than the light emitting device that has been cleaned are used again in the light emitting device manufacturing process. The recovered organic material 6 is sent to the purification chamber 40, where it is separated and purified. The purified material can be used again in the light emitting device manufacturing process.

  In this description, three film forming chambers A35, B36, and C37 are provided as an example, but the number is not limited. When one layer may be formed, one chamber may be used, and when multiple layers are formed, chambers may be provided for the number of times of stacking. Further, even when a plurality of layers are formed, the films can be formed in one room if only the materials are changed.

  As long as the recovered organic material can be used in the light emitting device manufacturing process, the purification process may not be performed.

  The transfer chamber 32, the pretreatment chamber 34, the film formation chamber, the sealing chamber 38, and the purification chamber 40 are preferably replaced with an inert gas and are in a reduced pressure state or a vacuum state. The inert gas includes nitrogen, helium, argon, etc., and a gas having low reactivity with the organic material 6.

  In this description, since the space can be saved, the cleaning / recovery process is performed in the film forming chamber. However, the cleaning / recovering process may be performed in different places, or the cleaning process and the recovery process may be performed separately.

  As described above, by using the apparatus of the present invention, in addition to the effects described in Embodiments 1 and 2, it is possible to perform film formation, cleaning, and recovery in one chamber, and the light emitting device can be installed in the same apparatus. It is possible to manufacture, and parts other than the light-emitting device can be washed, and even if impurities or a plurality of types of organic materials are present in the collected organic material 6, separation and purification are possible. It is possible to increase the effect.

  The method for manufacturing a light emitting device according to the present invention is capable of increasing the utilization efficiency of organic materials, reduces the amount of newly added organic materials, and discards organic materials that have been discarded so far. This is useful for reducing processing costs for disposal and reducing environmental impact. In addition, organic materials targeted by the present invention include organic electronics materials, organic semiconductor materials, organic solar cell materials, organic EL materials, pharmaceutical organic materials, and the like, and are useful in various fields.

DESCRIPTION OF SYMBOLS 1 Substrate 2 Deposition chamber 3 Deposition mask 4 Deposition shield 5 Deposition source 6 Organic material 7 Heating part 8 Heater 9 Organic material thin film 10 Heating part 11 Heating part 12 Film thickness meter 13 Detection part 14 Collection part 21 Purification part 22 Heating part 31 Preparation chamber 32 Transfer chamber 33 Transfer mechanism 34 Pretreatment chamber 35 Film formation chamber A
36 Deposition chamber B
37 Deposition chamber C
38 Sealing chamber 39 Gate 40 Purification chamber

Claims (8)

A light emitting device manufacturing process of a light emitting device made by depositing an organic material on a substrate provided in a film forming chamber;
A separation step of separating a portion other than the light emitting device and the light emitting device in the film forming chamber;
A cleaning step of cleaning the organic material attached to a part other than the light emitting device in the film forming chamber by being heated in a state where oxygen and moisture are removed;
It consists of a recovery process that recovers organic materials separated from parts other than the light emitting device by a cleaning process in a state where oxygen and moisture are removed,
A method of manufacturing a light emitting device, wherein the recovered organic material is returned to the light emitting device manufacturing process and reused. 2. The method for manufacturing a light emitting device according to claim 1, wherein in the recovery step, the organic material that has been washed away and removed from the portion other than the light emitting device in the cleaning step is deposited on the surface of the recovery portion and recovered. The method for manufacturing a light emitting device according to claim 2, wherein the surface temperature of the recovery unit is set to be equal to or lower than the heating temperature in the cleaning process. 4. The method for manufacturing a light emitting device according to claim 2, wherein the temperature of the portion other than the recovery portion is raised to a temperature higher than a sublimation temperature of the organic material. 5. The method for manufacturing a light emitting device according to claim 2, wherein the end of the collecting step is determined by a film thickness meter. After the recovery process,
The method for manufacturing a light emitting device according to claim 1, wherein a purification step of separating and purifying the recovered organic material is performed. The method for manufacturing a light emitting device according to claim 6, wherein the number of cleaning steps other than the light emitting device is greater than the number of organic material purification steps. The light-emitting device manufacturing apparatus using the manufacturing method of the light-emitting device as described in any one of Claim 1 to 7.

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