WO2020054974A1

WO2020054974A1 - Sublimation purification apparatus and sublimation purification method

Info

Publication number: WO2020054974A1
Application number: PCT/KR2019/009812
Authority: WO
Inventors: 홍석광; 김형석; 이헌영; 정광진; 신영환
Original assignee: 주식회사 엘지화학
Priority date: 2018-09-12
Filing date: 2019-08-06
Publication date: 2020-03-19

Abstract

A sublimation purification apparatus, according to one embodiment of the present invention, comprises: a vacuum chamber; a tube housing disposed within the vacuum chamber; a boat in close contact with the tube housing; and a heating unit positioned adjacent to an outer surface of the boat and an outer surface of the tube housing, wherein the boat contains a material subject to sublimation purification, and at least one of the boat and the tube housing is formed of a metal.

Description

Sublimation purification device and sublimation purification method

Cross-citation with relevant application (s)

This application claims the benefit of priority based on Korean Patent Application No. 10-2018-0109089 dated September 12, 2018 and Korean Patent Application No. 10-2019-0066109 dated June 4, 2019, and documents of the Korean patent application All content disclosed in is included as part of this specification.

The present invention relates to a sublimation purification apparatus and a sublimation purification method, and more particularly, to a sublimation purification apparatus and a sublimation purification method capable of realizing a high-purity purification efficiency and improving yield due to a continuous process and reducing production time.

The electroluminescent device is a self-luminous device that emits phosphors by recombination of electrons and holes, and may have a purity of a light-emitting layer material as a factor affecting the luminescence properties of the electroluminescent device. In particular, in the case of an organic electroluminescent device, organic The purity of the material greatly affects the luminescence properties of the device. When impurities are mixed in the organic material, it is necessary to purify the organic material in order to remove these impurities because the impurities become a trap of carriers or cause quenching, which significantly decreases the luminous intensity and luminous efficiency of the device. have.

As a method for purifying the organic material, a recrystallization method using a solvent or recrystallization using a solvent is generally used. Since the recrystallization method by sublimation has an organic substance sublimation and recrystallization under vacuum, it has a property that impurities do not enter, and thus, a conventional train-sublimation method may be used for purification of an organic material for an organic EL device. This method, as can be seen in the principle diagram shown in Figure 1, the first heating zone (1) by heating and vaporizing the organic material (6) containing the purified material and impurities, the gases through the quartz tube (5) Molecular movement is performed in the direction of pumping, and at this time, the phase changes while liquefying or solidifying while meeting the second heating zone 2 and the third heating zone 3 having different temperature regions, thereby purifying the purified material 7 and impurities 8 It can be collected separately.

As shown in FIG. 2, the conventional sublimation purification apparatus is provided with several second quartz tubes 20 inside the first quartz tube 10 for vacuum, but outside the first quartz tube 10 It can be made by installing a heater cover 30 is provided with a ceramic heater (31). When the organic material 51 is introduced into the sublimation purification device, and the heater cover 30 is closed and the ceramic heater 31 is heated, the purification material 52 and impurities 53 due to the temperature gradient inside the sublimation device Separation is achieved.

In this sublimation purification device, the first quartz tube 10 is used for airtightness with a vacuum atmosphere or the atmosphere, and the second quartz tube 20 is separated into a plurality of sections and controlled at different temperatures to control the organic material 51. Purification material 52 is obtained by removing impurities. However, the internal material of the sublimation purification device has the disadvantage that the yield is lowered and the manpower is increased due to the limitations of mass production due to the disadvantages of the material and the difficulty of having the process continuity.

The problem to be solved by the present invention is to improve the process continuous automation through metallization of the internal material, high purity purification efficiency, yield improvement due to the continuous process, and metallization of the internal material to compensate for the limitations of the design process limitation and the durability of the quartz, which is the material of the refiner, and It is to provide a sublimation purification apparatus and a sublimation purification method that realizes a reduction in production time and the like.

However, the problems to be solved by the embodiments of the present invention are not limited to the above-described problems and can be variously extended within the scope of the technical spirit included in the present invention.

An apparatus for sublimation purification according to an embodiment of the present invention includes a vacuum chamber, a tube housing positioned in the vacuum chamber, a boat in close contact with the tube housing, and a heating positioned adjacent to the outer surface of the tube and the outer surface of the tube housing It includes a portion, and the sublimation target material is contained in the boat, and at least one of the boat and the tube housing is formed of metal.

The boat includes a first boat and a second boat, and the first boat and the second boat are located together in the vacuum chamber, and the tube housing becomes a movement path, whereby the sublimation purification material contained in the first boat is After being heated, it can be allowed to be captured in the second boat.

The heating unit located adjacent to the outer surface of the tube housing is a first heating zone located in a portion corresponding to the first boat, a second heating zone located between the first boat and the second boat, and the second boat It includes a third heating zone located in the portion corresponding to, the first heating zone is the sublimation purification target material activated by the gas contained in the first boat to control the temperature to maintain the gas state, the second heating The zone is to sublimate the substance to be purified sublimation activated by the gas, and the third heating zone is to control the temperature to maintain the solution status of the substance to be sublimated purification to sublimate purification in the solution state to the second boat. You can make the target material fall.

The tube housing may have a tilted structure along the movement path of the sublimation purification target material.

The metal may include titanium or tantalum.

The sublimation purification device further includes a sealing gasket formed at an end of the tube housing, and the sealing gasket may be interposed between the tube housing and the boat.

The sealing gasket may include at least one of titanium (Ti), silver (Ag), copper (Cu), and ceramic.

The sublimation purification apparatus according to another embodiment of the present invention includes a chamber moving part, a plurality of chambers located adjacent to the chamber moving part, a tube housing located in the chamber, and located between the chamber moving part and the chambers A gate, a boat moving inside the chamber moving part by a transfer robot or loading or unloading from the chamber moving part into the chamber, and a heating part surrounding the outer surface of the boat and the outer surface of the tube housing, The boat includes a first boat and a second boat connected to each other with the tube housing.

The sublimation purification device may further include an up-and-down transfer device that moves at least one of the first and second boats to the tube housing by moving the boat passing through the gate in the chamber.

At least one of the boat and the tube housing may be formed of metal.

The sublimation purification apparatus further includes a sealing gasket formed at an end of the tube housing, and when the boat is loaded into the chamber and engaged with the tube housing, the sealing gasket is interposed between the tube and the tube housing. You can.

The plurality of chambers includes a first chamber and a second chamber adjacent to each other, and the tube housing positioned in the first chamber is removed by heating a sublimation purification target material contained in the first boat loaded in the first chamber Sublimation purification targets contained in the first boat loaded into the second chamber, where impurities are captured in the second boat, the first boat unloaded from the first chamber is loaded into the second chamber through the chamber moving part, and The material can be melted and activated with gas.

The sublimation purification device may further include a sublimation purification amount measurement member fixed inside the chamber, and the sublimation purification amount measurement member may be located below the boat.

The boat may be spaced apart from the tube housing by the transfer device to reach the sublimation purification amount measurement member to measure the sublimation purification amount.

The sublimation purification method according to another embodiment of the present invention comprises loading a first boat containing a sublimation purification target material in a first chamber, and impurities removed by heating the sublimation purification target material contained in the loaded first boat Capturing to the second boat through the tube housing, unloading the first boat from the first chamber and loading the first boat into the second chamber through a transfer robot, loaded into the second chamber Melting the sublimation purification target material contained in the first boat and activating it with gas, liquefying the gas-activated material, and transporting the solution through the tube housing included in the second chamber; Capturing to a second boat located in the second chamber, the second boat located in the second chamber to the cooling chamber using the transfer robot And cooling the liquefied material contained in the second boat loaded in the cooling chamber, wherein at least one of the first boat, the second boat and the tube housing is formed of metal. .

The sublimation purification method may further include cleaning a chemical solution of parts formed of a metal in the first boat, the second boat, and the tube housing.

The sublimation purification method may further include baking after the washing step.

The material for an organic light emitting device according to another embodiment of the present invention is purified by the sublimation purification method described above.

The organic light emitting device according to another embodiment of the present invention includes a material for an organic light emitting device described above.

According to embodiments, it is possible to improve the yield according to the continuity of the production and purification of the purified material with a large capacity, which is difficult due to the disadvantages of the quartz material, by replacing the existing quartz refiner with a metal.

In addition, since impurities are purified in a plurality of chambers and the boat is moved by a gate and a robot, the boundary in each purification step is clear, so that high-purity purification efficiency can be improved.

In addition, it is possible to reduce the risk of stable accidents that may occur due to the damage of the internal material quartz and the strength of durability in the purification operation made of high vacuum.

1 shows a principle diagram of purification of an organic material.

2 is a cross-sectional view showing a conventional purification device.

Figure 3 is a schematic diagram showing a sublimation purification apparatus according to an embodiment of the present invention.

FIG. 4 is an enlarged view showing a form in which the tube housing and the boat located in one chamber are closely attached in the sublimation purification apparatus of FIG. 3.

FIG. 5 is a view showing a modified embodiment in which a part of the tube housing has a tilted structure in the sublimation purification device of FIG. 4.

FIG. 6 is a view showing a state in which the boat is loaded into the chamber in the sublimation purification apparatus of FIG. 3.

7 is a perspective view showing a state in which the tube housing and the boat are in close contact in FIG. 4.

8 is a perspective view showing a heating unit according to an embodiment of the present invention.

9 is a view showing a state in which the boat is in close contact with the tube housing in one chamber of the sublimation purification apparatus according to another embodiment of the present invention.

10 is a perspective view showing a vertical transfer device and a sublimation purification amount measuring member in part A of FIG. 9.

11 is a front view showing the sublimation purification amount measuring member of FIG. 10.

Hereinafter, various embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art to which the present invention pertains can easily practice. The present invention can be implemented in many different forms and is not limited to the embodiments described herein.

Also, in the specification, when a part “includes” a certain component, it means that the component may further include other components, not to exclude other components, unless otherwise stated.

In addition, throughout the specification, when referred to as "planar", this means when the object portion is viewed from above, and when it is referred to as "cross-sectional", it means when the cross section of the object portion vertically cut is viewed from the side.

Referring to FIG. 3, the sublimation purification apparatus 1000 according to the present embodiment includes a chamber moving part 600, a plurality of

chambers

110, 120, 130, 140, and a chamber moving part 600 and

chambers

110, 120 , 130, 140. The tube housing 200 is located in each

chamber

110, 120, 130, 140, and two boats 300 can be connected to each other by the tube housing 200. The bow 300 may be in close contact with the tube housing 200 to perform a sublimation purification process. Each of the plurality of

chambers

110, 120, 130, and 140 may be a vacuum chamber. It is preferable that the chamber moving part 600 also maintains a vacuum state.

The sublimation purification apparatus 1000 includes a heating unit 400 and a cooling unit covering the heating unit 400 located adjacent to the outer surface of the tube housing 200 located inside the

chambers

110, 120, 130, and 140. 500. The heating part 400 is also formed in a portion adjacent to the outer surface of the boat 300.

The sublimation purification apparatus 1000 according to the present embodiment further includes a cooling chamber 150 in addition to the plurality of

chambers

110, 120, 130 and 140 in order to recover the material for the organic light emitting device in the final step of the sublimation purification process It can contain. Inside the cooling chamber 150, there is no tube housing 200 located inside the

other chambers

110, 120, 130, 140, and only the cooling unit 500 may be included. Cooling chamber 150, after the purification process, when the boat 300 containing the material purified by the transfer robot 650 passes through the gate 700 and is loaded into the cooling chamber 150, the purified material in solution state After cooling, the material for an organic light emitting device for use as a product can be recovered.

The transfer robot 650 is located in the chamber moving unit 600, and the bow 300 moves the inside of the chamber moving unit 600 by the transfer robot 650 or the

chambers

110 and 120 are moved in the chamber moving unit 600. , 130, 140, 150). When the bow 300 is loaded or unloaded from the chamber moving part 600 to each

chamber

110, 120, 130, 140, 150, the chamber moving part 600 and each

chamber

110, 120, 130, 140 , 150, the boat 300 positioned between the gates 300 may pass through. The boat 300 loaded through the gate 700 and loaded inside the

chambers

110, 120, 130, and 140 may be in close contact with the tube housing 200 by the vertical transfer device 800.

At least one of the boat 300 and the tube housing 200 according to the present embodiment may be formed of metal. The bow 300 and the tube housing 200 are parts made of the inner material of the sublimation purification apparatus 1000, and the part made of the inner material is a part of the bow 300 and the tube housing 200 that comes into contact with the substance to be purified. Can be Here, the metal may include titanium, tantalum, alumina, stainless steel, tungsten, silver, copper, invar, aluminum, and the like. It may be preferably titanium or tantalum. Quartz, which has been used in the related art, is a kind of general glass, and is made of only silicon dioxide, which is a main component, and has a very low impurity content, and is used for semiconductors, laboratory equipment, and optical components. Quartz has advantages in that it has a material of light transmittance, thermal stability, chemical resistance and high purity, but it is vulnerable to durability, has limitations in processing parts, and has a disadvantage of low thermal conductivity. Therefore, if a sublimation purification device is manufactured of quartz material, there is a limitation in size processing, and if the size of the thickness is large due to low thermal conductivity, it takes a long time to heat the sublimation purification, and the irrationality of work during disassembly / assembly It is difficult to mass-produce purified substances due to the like.

As an example of the metal material of the boat, titanium can be used, and titanium is light and hard with a small specific gravity of the metal, and is excellent in corrosion resistance and excellent in deformation and corrosion. Therefore, it is possible to effectively control the phase change of a material to be melted using a high-strength material component, and there is little limitation in size processing. As an example of the metal material of the boat, tantalum can be used, and tantalum is excellent in ductility, easy to process, and has very good thermal conductivity and electrical conductivity.

As an example of the metal material of the tube housing, titanium can also be used, and since titanium has the characteristics described above, it is easy to clean and heat transfer is stable, so it is easy to change the phase by accurately controlling the heating conditions, and each phase-changed material It may be easy to move between the chambers corresponding to the purification zone. As an example of the metallic material of the tube housing, tantalum can also be used.

In the first chamber 110 and the third chamber 130 included in the sublimation purification apparatus 1000 according to the present embodiment, outgassing and other impurities mixed in a substance to be sublimated contained in the boat 300 are removed. The process can be performed. Here, the outgassing and other impurities may be organic impurities mixed in a sublimation purification target material. Outgassing is a solvent used in a synthesis process, which is a step prior to the sublimation process, and is a solvent such as ethanol, water, and hexane, and other impurities may be monomolecular compounds smaller than a good molecular weight.

The first chamber 110 and the third chamber 130 shown in FIG. 3 contain the substance to be sublimed in the left side 300, and the right side 300 after heating in the tube housing 200. Cooled outgassing and other impurities are captured. Therefore, the primary sublimation purified material remains on the left side of the boat 300, and the primary sublimation purified material containing the boat 300 can be moved to the second chamber 120 and the fourth chamber 140. .

The first sublimation purified material is contained in the bow 300 of each of the second chamber 120 and the fourth chamber 140, and the material is melted and gasified while passing through the heating unit 400, The liquefied material is liquefied, and the liquefied material can be captured as a sublimation purified material on the right side boat 300. Sublimation purified material captured on the right boat 300 of the second chamber 120 and the fourth chamber 140 may be transferred to the cooling chamber 150 to be recovered as a material for an organic light emitting device through a cooling process.

In other words, the tube housing 200 located in the first chamber 110 heats the sublimation purification material contained in the first boat loaded in the first chamber 110 to remove impurities removed from the second boat. , The first boat unloaded from the first chamber 110 is loaded into the second chamber 120 through the chamber moving part 600, and the sublimation purification target contained in the first boat loaded in the second chamber 120 The material is melted and activated with gas, the gasified material is in solution, and the solution can be captured as a sublimated purified material in the second boat.

After the purification process is sequentially performed in the first chamber 110 and the second chamber 120 described above, the right boat 300 of the second chamber 120 is directly moved to the cooling chamber 150, or additional sublimation When a purification process is required, the purification process sequentially performed in the first chamber 110 and the second chamber 120 may be repeated once again in the third chamber 130 and the fourth chamber 140.

Hereinafter, referring to FIGS. 4 to 7, the tube housing 200, the boat 300, the heating unit 400, and the cooling unit associated with the sublimation purification path are located inside each

chamber

110, 120, 130, and 140. (500) will be described in detail.

FIG. 4 is an enlarged view of a tube housing and a boat positioned in one chamber in a sublimation purification apparatus of FIG. 3 in close contact. FIG. 5 is a view showing a modified embodiment in which a part of the tube housing has a tilted structure in the sublimation purification device of FIG. 4. FIG. 6 is a view showing a state in which the boat is loaded into the chamber in the sublimation purification apparatus of FIG. 3. 7 is a perspective view showing a state in which the tube housing and the boat are in close contact in FIG. 4.

Referring to FIG. 4, in this embodiment, the tube housing 200 has a movement path of a sublimation purification target material to be captured in the second boat 300b after the sublimation purification target material contained in the first boat 300a is heated. Can be. Substances subject to sublimation purification may be mixed materials in which organic substances and impurities are mixed.

The heating part 400 positioned adjacent to the outer surface of the tube housing 200 according to the present embodiment includes a first heating zone 410 and a first boat 300a located in a portion corresponding to the first boat 300a. And a second heating zone 420 positioned between the second boat 300b and a third heating zone 430 positioned at a portion corresponding to the second boat 300b. Sublimation purification target material contained in the first boat 300a is heated and liquefied by the lower heating unit 440 located under the first boat 300a, and the temperature of the sublimation purification target is further increased by gas. Activated, the gas-activated sublimation material reaches the first first heating zone 410 of the tube housing 200 and then moves to the second heating zone 420 having a low temperature. At this time, the first heating zone 410 maintains a gas state by maintaining a temperature condition equivalent to that of the first boat 300a, and allows the sublimation material in the gas state to fly to the second heating zone 420.

The second heating zone 420 may lower the temperature to phase change the sublimation purification target material activated with the gas into a liquid state. At this time, the second heating zone 420 may also have a cooling function in order to control phase changes between materials due to excessive heat interference of the first heating zone 410. The material liquefied in the second heating zone 420 enters the third heating zone 430, and the third heating zone 430 controls the temperature to maintain the temperature of the solution state of the sublimated purification target material. Make it possible. Substances subject to sublimation purification through the third heating zone 430 are dropped into a solution state in the second boat 300b. At this time, as a modified embodiment, as shown in FIG. 5, the tube housing 200 may have a tilted structure along a movement path of a sublimation purification target material. Due to the tilted structure, the material can be smoothly moved from the first boat 300a to the second boat 300b. The structure of the tilt is to allow the material to be purified to be sublimated to flow well to the second boat 300b. The tilted degree may be approximately 5 degrees.

Referring to FIG. 6, the boat 300 loaded through the gate 700 in FIG. 3 and loaded inside the chamber 120 may be in close contact with the tube housing 200 by the vertical transfer device 800. The vertical transfer device 800 moves the boat 300 in the chamber 120 so that the loaded boat 300 is in close contact with the tube housing 200 located in the chamber 120 so that a sublimation purification process can be performed. Can play a role.

The vertical transfer device 800 may be a pneumatic sealer. The transfer robot 650 described in FIG. 3 moves the first boat 300a while the

lower heating units

440 and 450 mounted below the first boat 300a are lowered by the vertical transfer device 800. It can be mounted on the second chamber 120. Subsequently, by closing the gate and creating a vacuum atmosphere, the

lower heating units

440 and 450 are raised toward the tube housing 200 by using the up-and-down transfer device 800, so that the first mounted in the second chamber 120 is mounted. The boat 300a may be tightly coupled to the tube housing 200 by physical force. Since the first boat 300a and the tube housing 200 are in close contact / combination, it is possible to prevent external contamination that may occur due to the gasified material being lost into the gap between the first boat 300a and the tube housing 200.

On the other hand, the second boat 300b exists in a separate state from the tube housing 200, so that the sublimation is performed while the first boat 300a and the tube housing 200 are kept in close contact with each other. In the state separated from the housing 200, the second boat 300b collects the liquefied material. Specifically, the material liquefied by the inclined angle according to the tilt structure of the tube housing 200 may be collected in the second boat 300b through the phenomenon of falling from top to bottom. In addition, because the tube housing 200 and the second boat 300b are separated, the internal pressure of the second chamber 120 and the internal pressure of the tube housing 200 may be maintained the same.

Referring to FIG. 7, in the sublimation purification apparatus according to the present embodiment, when the bow 300 and the tube housing 200 are in close contact, the sealing gasket 250 is interposed between the bow 300 and the tube housing 200. It may further include. The sealing gasket 250 is formed at the end of the tube housing 200, and the sealing gasket 250 fills a narrow gap occurring in a portion where the end of the tube housing 200 is bent. The sealing gasket 250 may include at least one of titanium (Ti), silver (Ag), copper (Cu), and ceramic.

The sealing gasket 250 becomes a fluid when the solid is heated in the chamber 120, and this fluid can be prevented from leaking out of the tube housing.

Hereinafter, the heating unit will be described in detail with reference to FIG. 8. 8 is a perspective view showing a heating unit according to an embodiment of the present invention.

Referring to FIG. 8, the tube housing 200 may have a tub shape, and the tub may have an inverted structure. The first boat 300a and the second boat 300b are in close contact with both edges of the tube housing 200, respectively.

The heating unit according to the present embodiment includes an upper heating unit positioned adjacent to the outer surface of the tube housing 200 and a lower heating unit positioned adjacent to the outer surfaces of the first and

second boats

300a and 300b. The upper heating part includes a first heating zone 410 positioned in a portion corresponding to the first boat 300a, a second heating zone 420 positioned between the first boat 300a and the second boat 300b, and It includes a third heating zone 430 located in the portion corresponding to the second boat (300b). The lower heating part includes a fourth heating zone 440 surrounding the side surface of the first boat 300a and a fifth heating zone 450 surrounding the side surface of the second boat 300b.

The heating unit according to the present embodiment may be formed of tantalum. Since tantalum is excellent in ductility, easy to process, and has good thermal conductivity and electrical conductivity, independent heat transfer is possible in the heating zone to be heated, and heat transfer control can be very stable. Alternatively, the heating portion may be formed of Inconel. Inconel has good heat resistance and does not oxidize even in an oxidizing condition of about 900 degrees Celsius or higher, and may have excellent properties such as elongation, tensile strength, and yield point that do not change up to 600 degrees Celsius.

9 is a view showing a state in which the boat is in close contact with the tube housing in one chamber of the sublimation purification apparatus according to another embodiment of the present invention. 10 is a perspective view showing a vertical transfer device and a sublimation purification amount measuring member in part A of FIG. 9. 11 is a front view showing the sublimation purification amount measuring member of FIG. 10.

9 and 10, the sublimation purification apparatus according to the present embodiment further includes a sublimation purification amount measuring member 850 fixed inside the chamber 120. The sublimation purification amount measuring member 850 may be located under the boat 300. As such, the sublimation purification amount measurement member 850 is located at the bottom of the boat 300, so that the sublimation purification amount can be checked in real time during the sublimation purification process. The sublimation purification amount measuring member 850 is a transducer for measuring force or load as a load sensor, and is a device capable of outputting an output as an electrical signal.

Specifically, referring to FIG. 11, the heating part 440, which is a heating part located at the bottom of the bow 300, surrounds the bow 300, but the sublimation purification amount measuring member 850 according to this embodiment has a heating part 440. ) In the lower center portion, a tripod-shaped pin 860 protrudes from a portion that does not interfere with the heating portion 440. The heating unit 440 may be a wire-type heating wire, and the heating wire is formed in a plurality while having a gap, thereby enclosing the tube housing 200 as shown in FIG. 9. In other words, between the plurality of heating wires, the tripod-shaped pin 860 protrudes upward, so that the boat 300 and the sublimation purification amount measuring member 850 can be assembled without interference from the heating unit 440.

When the boat 300 moves downward by the vertical transfer device 800 supporting the boat 300, the boat 300 reaches the pin 860 of the sublimation purification amount measuring member 850. At this time, the purification amount of the sublimation purification material in the boat 300 can be measured.

In the past, if the sublimation purification amount was simply visually confirmed, and the process conditions and the process termination time could be determined from a subjective viewpoint based on experience, the sublimation purification device according to the present embodiment uses a sublimation purification amount measurement member 850 Therefore, it is possible to check the material movement amount and material consumption in real time during the process, thereby minimizing the deviation between processes and problems that may occur in the process.

Hereinafter, a method of sublimation purification according to another embodiment of the present invention will be described with reference to FIGS. 3 to 8 again.

3 to 8, in the sublimation purification method according to the present embodiment, the first chamber 300 loaded with the sublimation purification target material in the first chamber 110 is loaded and heated to be mixed with the sublimation purification target material Outgassing and other impurities are removed first. At this time, in addition to the purified material, residual solvent and monomolecular impurities are first sublimed and trapped in the second boat 300b. Thereafter, the temperature is not sublimated, that is, cooled to a temperature in a range that is not gasified.

Subsequently, the first boat 300a containing the first purified material in the first chamber 110 is unloaded from the first chamber 110, and the first boat is transferred to the second chamber 120 through the transfer robot 650 ( 300a). The sublimation purification target material contained in the first boat 300a loaded in the second chamber 120 is heated to a fourth heating zone 440 to be solutiond, and the temperature is further increased to activate the gas. The sublimation material activated by gas moves to the first heating zone 410, and the sublimation material activated by gas maintains the same temperature as the first boat 300a in the first heating zone 410 so that the sublimation material activated by gas is the second heating zone ( 420). By lowering the temperature in the second heating zone 420, the sublimation purification target material activated with the gas is solutiond. The substance liquefied in the second heating zone 420 enters the third heating zone 430, and controls the third heating zone 430 to maintain the temperature of the solution state of the solution-sublimed purification target material. 2 Drop to the boat (300b) in a solution state and capture. After the process is completed in the second chamber 120, the second boat 300b is moved to the cooling chamber 150 using the transfer robot 650, and the second boat 300b loaded in the cooling chamber 150 The solution material contained in can be cooled.

During the sublimation purification process, in order to obtain a high-purity purification material before loading the second boat 300b into the cooling chamber 150, a process sequentially performed in the first chamber 110 and the second chamber 120 is performed. , It may be repeatedly performed in the third chamber 130 and the fourth chamber 140.

The first boat 300a, the second boat 300b, and the tube housing 200 are formed of metal, and the sublimation purification method according to the present embodiment may further include cleaning a chemical solution of parts formed of the metal. have. Through such a cleaning process, metal impurities eluted from the metal component material constituting the heating part, the boat, and the tube housing during high vacuum are mixed in the sublimation purification target material, thereby preventing problems such as an increase in voltage and a shortened lifespan when filing an organic light emitting device. have.

Additionally, the sublimation purification method according to the present embodiment may further include baking after the washing step. Baking may be performed at a temperature of about 200 degrees Celsius or higher, and may be performed at least twice.

The preferred embodiments of the present invention have been described in detail above, but the scope of the present invention is not limited to this, and various modifications and improvements of those skilled in the art using the basic concept of the present invention defined in the following claims are also provided. It belongs to the scope of rights.

[Description of codes]

1000: sublimation purification device

110, 120, 130, 140: chamber

150: cooling chamber

200: tube housing

250: sealing gasket

300: boat

400: heating section

410, 420, 430, 440, 450: heating zone

500: cooling unit

600: chamber moving part

650: transfer robot

700: gate

800: up and down transfer device

850: no sublimation purification amount measurement

Claims

Vacuum Chamber,

A tube housing located in the vacuum chamber,

A bolt in close contact with the tube housing and

And a heating portion located adjacent to the outer surface of the boat and the outer surface of the tube housing,

The sublimation purification target material is contained in the boat, and at least one of the boat and the tube housing is formed of a metal.
In claim 1,

The boat includes a first boat and a second boat, and the first boat and the second boat are located together in the vacuum chamber, and the tube housing becomes a movement path, whereby the sublimation purification material contained in the first boat is Sublimation purification device to be trapped in the second boat after being heated.
In claim 2,

The heating unit located adjacent to the outer surface of the tube housing is a first heating zone positioned at a portion corresponding to the first boat, a second heating zone located between the first boat and the second boat, and the second boat It includes a third heating zone located in the portion corresponding to,

The first heating zone controls the temperature so that the sublimation purification target material activated by the gas contained in the first boat maintains a gas state, and the second heating zone liquefies the sublimation purification target material activated by the gas. , The third heating zone is a sublimation purification apparatus that controls the temperature to maintain the solution state of the solution sublimation purification target substance so that the sublimation purification target substance in solution state falls to the second boat.
In claim 3,

The tube housing is a sublimation purification device having a tilted structure along a movement path of the sublimation purification target material.
In claim 1,

The metal sublimation purification apparatus comprising titanium or tantalum.
In claim 1,

A sublimation purification device further comprising a sealing gasket formed at an end of the tube housing, wherein the sealing gasket is interposed between the tube housing and the boat.
In claim 6,

The sealing gasket is a sublimation purification apparatus including at least one of titanium (Ti), silver (Ag), copper (Cu), and ceramic.
Chamber moving part,

A plurality of chambers located adjacent to the chamber moving portion,

A tube housing located within the chamber,

A gate located between the chamber moving part and the chambers,

A boat that moves inside the chamber moving part by a transfer robot or is loaded or unloaded from the chamber moving part into the chamber and

And a heating part surrounding the outer surface of the boat and the outer surface of the tube housing,

The boat is a sublimation purification apparatus including a first boat and a second boat connected to each other with the tube housing.
In claim 8,

The heating unit located adjacent to the outer surface of the tube housing is a first heating zone positioned at a portion corresponding to the first boat, a second heating zone located between the first boat and the second boat, and the second boat It includes a third heating zone located in the portion corresponding to,

The first heating zone controls the temperature so that the sublimation purification target material activated by the gas contained in the first boat maintains a gas state, and the second heating zone liquefies the sublimation purification target material activated by the gas. , The third heating zone is a sublimation purification apparatus that controls the temperature to maintain the solution state of the solution sublimation purification target substance so that the sublimation purification target substance in solution state falls to the second boat.
In claim 9,

The tube housing is a sublimation purification device having a tilted structure along a movement path of the sublimation purification target material.
In claim 10,

At least one of the first boat and the second boat further comprises a vertical transfer device that moves the boat passing through the gate in the chamber to be in close contact with the tube housing.
In claim 8,

At least one of the boat and the tube housing is a sublimation purification device formed of a metal.
In claim 12,

The metal sublimation purification apparatus comprising titanium or tantalum.
In claim 8,

A sublimation purification device further comprising a sealing gasket formed at an end of the tube housing, wherein the sealing gasket is interposed between the boat and the tube housing when the boat is loaded into the chamber and engaged with the tube housing.
In claim 8,

The plurality of chambers include a first chamber and a second chamber adjacent to each other,

In the tube housing positioned in the first chamber, impurities removed by heating a sublimation purification material contained in the first boat loaded in the first chamber are trapped in the second boat, and unloaded from the first chamber. A sublimation purification apparatus in which one boat is loaded into the second chamber through the chamber moving part, and a sublimation purification target material contained in the first boat loaded in the second chamber is melted and activated with gas.
Loading the first boat containing the sublimation purification target material in the first chamber,

Capturing impurities removed by heating the sublimation purification target material contained in the loaded first boat through a tube housing to a second boat,

Unloading the first boat from the first chamber and loading the first boat into the second chamber through a transfer robot,

Melting the sublimation purification target material contained in the first boat loaded in the second chamber to activate it with a gas,

Solution of the substance activated with the gas,

Capturing the liquefied material through a tube housing included in the second chamber to a second boat located in the second chamber,

Moving the second boat located in the second chamber to a cooling chamber using the transfer robot; and

Cooling the liquefied material contained in the second boat loaded in the cooling chamber,

At least one of the first boat, the second boat and the tube housing is a sublimation purification method formed of a metal.
In claim 16,

And substituting a chemical solution of parts formed of metal in the first boat, the second boat, and the tube housing.
In claim 16,

And a step of baking after the washing step.
A material for an organic light-emitting device purified by the sublimation purification method of claim 16.
An organic light-emitting device comprising the material for an organic light-emitting device of claim 19.
In claim 1,

Further comprising a sublimation purification amount measuring member fixed in the chamber,

The sublimation purification amount measuring member is a sublimation purification device located at the bottom of the boat.
In claim 8,

Further comprising a sublimation purification amount measuring member fixed in the chamber,

The sublimation purification amount measuring member is a sublimation purification device located at the bottom of the boat.
In claim 22,

At least one of the first boat and the second boat further comprises a vertical transfer device that moves the boat passing through the gate in the chamber to be in close contact with the tube housing.
In claim 23,

A sublimation purification device for measuring the amount of sublimation purification by reaching the sublimation purification amount measurement member by the boat spaced apart from the tube housing by the transfer device.