JP2016098417A - Vapor deposition apparatus and method for manufacturing organic el device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vapor deposition apparatus capable of suppressing deterioration of a thin film forming material during its production and capable of obtaining a desired film forming speed.SOLUTION: In an evaporator, a vacuum chamber 401 capable of maintaining an internal atmosphere at a reduced pressure has a material receiving part 511 housing a material supply device 411 therein and including as a discharge port 531 a hole formed in an inner surface of the vacuum chamber 401 and communicating with the inside of an evaporation chamber 441, the material supply device 411 has a material transfer part 541 holding a thin film forming material and supplying the thin film forming material to the material receiving part 511 through a material sending and receiving passage 521, which is a part of the internal atmosphere in the vacuum chamber 401, and the passage cross-sectional area of the material sending and receiving passage 521 is 1/10 or less the cross-sectional area of the inner surface of the vacuum chamber 401.SELECTED DRAWING: Figure 3

Description

  The present invention relates to a vapor deposition apparatus. The present invention is particularly suitable as a vapor deposition apparatus used for manufacturing an organic EL (ElectroLuminescence) apparatus.

  The present invention also relates to a method for manufacturing an organic EL device.

  In recent years, an organic EL device has attracted attention as a lighting device that replaces an incandescent lamp and a fluorescent lamp, and many studies have been made. In addition, an organic EL method is attracting attention as a method for changing to a liquid crystal method or a plasma method in a display member typified by a television.

  Here, the organic EL device is obtained by laminating an organic EL element on a base material such as a glass substrate or a transparent resin film.

  In addition, the organic EL element has two or more light-transmitting electrodes facing each other, and a light emitting layer made of an organic compound is laminated between the electrodes. The organic EL element emits light by the energy of recombination of electrically excited electrons and holes.

  Since the organic EL device is a self-luminous device, a high-contrast image can be obtained when used as a display material. In addition, light of various wavelengths can be emitted by appropriately selecting the material of the light emitting layer. In addition, the thickness is extremely thin compared to incandescent lamps and fluorescent lamps, and light is emitted in a planar shape, so there are few restrictions on the installation location.

  A typical layer structure of the organic EL device is as shown in FIG. The organic EL device 100 shown in FIG. 9 has a configuration called a bottom emission type. A transparent electrode layer 120, a functional layer 130, and a back electrode layer 140 are laminated on a glass substrate 110, and these are sealed. It is sealed by the stopper 150.

  The functional layer 130 is formed by stacking a plurality of thin films containing an organic compound. The representative functional layer 130 includes a hole injection layer 131, a hole transport layer 132, a light emitting layer 133, and an electron transport layer 134.

  In general, the organic EL device 100 is manufactured by sequentially forming the above-described layers on a glass substrate 110.

  Of the above-described layers, the transparent electrode layer 120 is a transparent conductive film such as indium tin oxide (ITO), and is formed mainly by sputtering or CVD.

  As described above, the functional layer 130 is formed by laminating a plurality of thin films containing an organic compound, and each thin film can be formed by a vacuum deposition method.

  The back electrode layer 140 is generally a metal thin film such as aluminum or silver, and can be formed by a vacuum deposition method.

  Thus, the organic EL device has a structure in which the functional layer including the light emitting layer is sandwiched between the first and second electrode layers of the transparent conductive film and the metal thin film.

  Thus, when manufacturing an organic EL device, a vacuum deposition method is frequently used. Here, the vacuum evaporation method is a technique for forming a film using an evaporation apparatus as disclosed in Patent Document 1, for example.

  That is, a vapor deposition apparatus is comprised by the vacuum chamber and the evaporation apparatus which evaporates the material for thin film formation. A vacuum chamber can install base materials, such as a glass substrate, for example.

  The evaporation apparatus is constituted by a heating apparatus using electric resistance or an electron beam, and a crucible for storing a thin film forming material.

  In the vacuum deposition method implemented with such an apparatus configuration, it is possible to deposit while measuring the film thickness with a film thickness meter, and precise film thickness control is easy. However, in order to obtain a certain productivity, it is necessary to keep the thin film forming material heated during production, and it has been difficult to suppress deterioration of the thin film forming material due to heating, so-called material deterioration.

Therefore, a method by so-called flash vapor deposition as described in Patent Document 2 is disclosed. That is, a thin film forming material is quantitatively supplied to the evaporation chamber, a part or all of the thin film forming material is evaporated by a heating device of the evaporation chamber or a heated carrier gas, and the evaporated material is transferred to the vacuum chamber to form a film. It is a method to do.
JP 2012-52187 A WO 2010/123027

  In the vacuum deposition method by flash deposition, in order to control the film thickness to be formed, it is necessary to accurately control the transfer amount of the thin film forming material transferred to the evaporation apparatus.

  According to Patent Document 2, a vapor deposition apparatus for depositing a thin film on a base material by vapor deposition, comprising an evaporation apparatus capable of reducing pressure for supplying a material gas, and a vacuum chamber for depositing a thin film on the substrate, The evaporation apparatus includes a quantification unit that quantifies the material for forming a thin film, and an evaporation chamber that vaporizes the material that has passed through the quantification unit. The quantification unit includes an upwardly convex conical lid, A conical concave body provided in opposition to the upper surface, and a mechanism for relatively rotating the lid and the concave body. For example, a thin film forming material is disposed between the lid and the concave body. And a method in which the transfer speed is controlled by the gap width, the relative rotational speed, and the pressure difference between the material supply side and the discharge side between the lid body and the concave surface body. ing. Here, as a method for controlling the pressure difference between the material supply side and the discharge side, it has been proposed that the material supply side has a mechanism capable of introducing gas.

  However, even if such a method is used, the weight of the material for forming a thin film necessary for obtaining a thin film of about 10 nm, for example, is about 10 mg and is very small, so it is difficult to accurately quantify the material. . In addition, for example, even when the valve that partitions the material gas generation unit and the vacuum chamber is opened and closed, a differential pressure is instantaneously generated on the material supply side and the discharge side, so that it is difficult to control the pressure difference. In addition, there is a problem that the material is unintentionally transferred without its amount being sufficiently controlled.

  Therefore, the present invention pays attention to the above-mentioned problems of the prior art, suppresses material deterioration during the production of thin film forming materials, and achieves a desired film formation speed even at a relatively low film formation speed of about nm / min. It is an object of the present invention to provide a relatively simple vapor deposition apparatus that can obtain a stable film thickness.

  As a measure for solving the above-described problems, the vapor deposition apparatus shown in FIG. 8 was devised and various studies were conducted.

That is, a vapor deposition apparatus 1 that has a vacuum chamber (1) 201 in which a base material can be installed and an evaporation apparatus 4, and deposits a thin film forming material emitted as vapor in the evaporation apparatus 4 on the base material. There,
The evaporation apparatus 4 includes a thin film forming material supply unit 5 and an evaporation chamber 444, and can supply a vapor-containing gas containing the vapor to the vacuum chamber (1) 201.
The evaporation chamber 444 can generate the vapor-containing gas from the thin film forming material supplied from the thin film forming material supply unit 5;
The thin film forming material supply unit 5 includes a material holding unit 415 and a material transfer unit that transfers material from the material holding unit 415 and discharges it from the discharge port. The evaporation chamber 444 is connected to the discharge port of the material transfer unit by piping. The thin film forming material is circulated in the pipe, the pipe is further branched by a pipe path, and the other is connected to the material holding part 415 through a partition valve 715, and the material holding part 415 Various investigations were made on an evaporation apparatus which is an apparatus configuration in which the pressure difference at the discharge port hardly occurs.

  If this evaporation apparatus is used, it is possible to obtain a constant film formation speed because it is difficult for the differential pressure between the material holding part 415 and the discharge port to occur during film formation.

  However, even when using such an evaporation apparatus, for example, by opening and closing a valve that partitions the evaporation chamber 444 and the vacuum chamber (1) 201, the pressure in the vicinity of the discharge port temporarily rises. It is difficult to avoid the occurrence of a differential pressure between the material holding part and the discharge port, and the material transfer amount to the evaporation chamber 444 may fluctuate unintentionally.

  Accordingly, in order to solve such problems, further intensive research was conducted and the present invention was completed.

  In the following description, for the sake of explanation, the reference numerals in FIGS. 1, 2, 3, 4, 4, 5, 6 and 7 relating to the present invention will be added. The present invention is not limited in any way.

That is, the present invention has a vacuum chamber (1) 201 in which the base material 9 can be installed, and the evaporation device 4, and deposits the thin film forming material emitted as vapor in the evaporation device 4 on the base material 9. A vapor deposition apparatus 1 for causing
The evaporation apparatus 4 includes a thin film forming material supply unit 5 and evaporation chambers 441 and 442, and can supply a vapor-containing gas containing the vapor to the vacuum chamber (1) 201.
The evaporation chambers 441 and 442 can generate the vapor-containing gas from the thin film forming material supplied from the thin film forming material supply unit 5;
The thin film forming material supply unit 5 includes vacuum chambers (2) 401 and 402 that can maintain the internal atmosphere at a reduced pressure, and include vacuum chambers (2) 401 and 402 that accommodate the material supply devices 411 and 412. And a material receiving portion (1) 511 including a hole on the inner surface of the vacuum chamber (2) 401, 402 and a hole communicating with the inside of the evaporation chamber 441, 442 as a discharge port,
The material supply devices 411 and 412 hold the thin film forming material, and the thin film forming material is supplied to the material receiving portion (1) 511 via a material transmission / reception path 521 which is a part of the internal atmosphere. A material holding unit 551 to be supplied, having a material holding unit 551 supported on the inner surfaces of the vacuum chambers (2) 401 and 402 via support units 421 and 422,
Furthermore, the present invention relates to a vapor deposition apparatus characterized in that the cross-sectional area of the material transmission / reception path 521 is 1/10 or less of the area of the cross section of the inner surface of the vacuum chamber (2) 401, 402.

  According to the vapor deposition apparatus 1, the material supply apparatuses 411 and 412 themselves are held in the vacuum chamber, and the material discharge ports 531 of the material supply apparatuses 411 and 412 are released in a constant atmosphere. Therefore, there is no differential pressure between the material holding portion 551 and the material discharge port 531, and the thin film forming material can be transferred in a stable atmosphere. The material discharge port 531 is an entrance of a material for forming a thin film, which is one end of the material sending / receiving path 521 on the material holding portion 551 side, and the other end of the material sending / receiving path 521. The material receiving portion (1) 511 is an outlet for the material for forming a thin film.

  Further, the support parts 421 and 422 may have a weighing mechanism capable of measuring the weight of the thin film forming material held by the material holding part 551.

  By using such a weighing mechanism, it is possible to always grasp the remaining amount of the thin film forming material in the material holding portion 551, so that the transfer amount of the thin film forming material can be controlled more accurately. This makes it possible to easily perform precise control of the amount of film deposited on the substrate.

  Furthermore, as the thin film forming material, not only a solid but also a liquid material can be applied as long as it is a material that can be divided and transferred, but from the viewpoint of more effectively achieving the effects of the present invention. Is preferably a powder, more preferably a powder having a weight average particle diameter of 0.1 μm or more and 10 mm or less, and further preferably a powder having a weight average particle diameter of 1 μm or more and 1 mm or less. Is the body. That is, by using the vapor deposition apparatus of the present invention, regardless of the shape of the thin film forming material, even in the case of powder, for example, the material can be stably transferred without problems.

  Furthermore, in the present invention, the evaporation apparatus 1 further includes a carrier gas supply unit 6 capable of supplying a carrier gas to at least the internal atmosphere, and the vapor-containing gas includes the carrier gas. In this way, a part of the carrier gas is circulated in the vacuum chambers (2) 401 and 402 and then sent to the evaporation chambers 441 and 442, whereby the vacuum chambers (2) 401 and 402 and the evaporation chamber 441 are transferred. , 442 is prevented from adhering to the material for forming a thin film in the material transfer pipe (1) 501, and the vapor-containing gas is prevented from flowing back into the vacuum chambers (2) 401, 402. Can do.

Furthermore, the material supply devices 411 and 412 according to the present invention can move the thin film forming material held by the material holding portion 551 in the horizontal direction and send it to the material sending / receiving path 521. A moving mechanism, and
The material horizontal movement mechanism includes a power mechanism arranged outside the vacuum chamber (2) 401, 402, and a shaft driven by the power mechanism,
The shaft is preferably introduced into the vacuum chamber (2) while maintaining hermeticity so that power can be transmitted in the horizontal direction, so that at least when power is stopped. Because the weight of the power supply mechanism and the shaft driven by the power supply mechanism is not applied to the material supply devices 411 and 412, the weight of the material supply devices 411 and 412 can be accurately measured. The remaining amount of material in the material supply apparatus can be grasped. For example, a mechanism capable of generating power in a vacuum apparatus may be used without using such a power transmission mechanism.

  Furthermore, it can have a material transfer pipe (1) 501 in which the material receiving portion (1) 511 has an opening at one end and a hole on the inner surface of the evaporation chambers 441 and 442 has an opening at the other end.

  Furthermore, in the present invention, the vacuum chambers (2) 401 and 402 are arranged outside the vacuum chambers (2) 401 and 402, and have material storage containers 431 and 432 for storing the thin film forming material. A material receiving portion capable of replenishing the thin film forming material from the material storage container 431, 432 through the internal atmosphere of the vacuum chamber (2) 401, 402 while maintaining the airtightness of the vacuum chamber (2) 401, 402 (2) A supply port can be provided as 561.

  By using such a material holding part, it is preferable to replenish the material for forming a thin film from the outside while keeping the inside of the vacuum chamber (2) in a vacuum, and the material can be replenished in a sealed state, so continuous production is possible. It becomes. The material storage containers 431 and 432 preferably further have a heating mechanism, and the material holding unit 551 can be replenished after the thin film forming material is sufficiently heated and degassed.

  Furthermore, in the present invention, a gas pipe capable of supplying the carrier gas directly from the carrier gas supply unit 6 to the evaporation chambers 441 and 442 can be provided.

  Furthermore, the present invention manufactures an organic EL device by sequentially laminating a functional layer including at least a first electrode layer, a thin film including an organic compound and including a light emitting layer, and a second electrode layer on a substrate. An organic EL device comprising a step of depositing at least one organic compound of a thin film containing the organic compound on the substrate using the vapor deposition apparatus of the present invention as the thin film forming material With respect to this manufacturing method, it is possible to perform vapor deposition with precisely controlled film deposition amount, so that an organic EL device having excellent characteristics can be manufactured.

  Further, in such a manufacturing method of the present invention, a plurality of thin film forming materials can be sequentially or simultaneously evaporated by one vapor deposition apparatus, and even a device having a complicated structure can be manufactured.

  If the vapor deposition apparatus of the present invention as described above is used, the thin film-forming material can be maintained at room temperature, so that a thin film with little material deterioration and high quality stability can be obtained. Further, the material for forming a thin film can be evaporated at a constant rate, a desired film formation rate can be easily obtained, and the quality stability is high. Furthermore, it is possible to form a film sequentially or simultaneously using a plurality of thin film forming materials with a simple apparatus configuration, and the apparatus cost is low.

  The same applies to the manufacturing method of the organic EL device of the present invention, and even a device having a complicated structure can be manufactured by one vapor deposition device.

  In the vapor deposition apparatus of the present invention, since the thin film forming material can be stably supplied from the thin film forming material supply unit into the evaporation chamber, it is easy to obtain a desired film forming speed and a stable film thickness can be obtained. Therefore, quality stability is high.

It is an example of the block diagram of the vapor deposition apparatus 1 of this invention. FIG. 2 is an example of a detailed configuration diagram of a vacuum chamber (1) 201 and an exhaust unit 211 in FIG. 1. FIG. 2 is an example of a detailed configuration diagram of the evaporator 1 of FIG. 1. It is an example of the structure detailed front view of the material supply apparatus power transmission part of FIG. It is an example of the structure detailed side view of the material supply apparatus power transmission part of FIG. It is an example of the structure detailed figure at the time of the material supply apparatus power transmission part connection of FIG. It is an example of the block diagram of the vapor deposition apparatus 1 of this invention which can form into a film on two or more base materials 9 simultaneously. It is a reference drawing of the vapor deposition apparatus of the examination stage of this invention. It is sectional drawing which shows the general device structure of an organic electroluminescent apparatus.

  Examples of embodiments of the present invention will be further described below. In addition, this invention is not limited to the following embodiment, A various change is possible within the technical common sense of those skilled in the art.

  The vapor deposition apparatus 1 of the present invention includes a vacuum chamber (1) 201 and an evaporation device 4, and an exhaust part 211 is connected to the vacuum chamber (1) 201 as a downstream side thereof. Therefore, as an example, the vapor deposition apparatus 1 includes, for example, as shown in FIG. 1, the vacuum chamber (1), the exhaust system 2, the gas mixing unit 3, the evaporation device 4, and the heating carrier gas flow unit 7.

  In addition, each device, piping, valve, etc. that come into contact with the heated carrier gas is heated by an appropriate ribbon heater, jacket heater, etc. as necessary to prevent the evaporation material from sticking and material deterioration, and the temperature of each part is controlled by an appropriate control method. It is a structure that can be controlled.

  As shown in FIG. 2, the vacuum chamber (1) and the exhaust unit system 2 include a vacuum chamber (1) 201, an exhaust unit 211 that is a vacuum exhaust pump, and an exhaust valve 221.

  The vacuum chamber (1) 201 is airtight, preferably has a substrate holding mechanism 231 and a vapor deposition head 24120 in the vacuum chamber, and preferably has a gate valve 251 for loading and unloading the substrate 9.

  In the present embodiment, the base material 9 is introduced into the vacuum chamber 201 through the gate valve 251 and placed on the base material holding mechanism 231. The base material 9 is made of a transparent material such as glass. The transparent electrode layer 120 on the substrate is preferably made of a transparent conductive material such as ITO (Indium Tin Oxide). The transparent electrode layer 120 is formed by, for example, a sputtering method.

  Next, the evaporation material is discharged toward the substrate 9 through the vapor deposition head 241, thereby forming a film. It is preferable that the discharge part of the vapor deposition head 241 has an appropriate aperture pattern and has a structure that uniformly discharges the evaporation material onto the base film forming surface. In addition, the base material holding mechanism 231 preferably has a structure (261) in which, for example, a coolant or the like can be circulated to cool the substrate in order to suppress an increase in the base material temperature due to the radiant heat of the heated vapor deposition head 241 or the like. .

  The vacuum chamber (1) 201 is evacuated using an evacuation unit 211 constituted by an evacuation pump such as a dry pump connected to the outside. Furthermore, if the inside of the vacuum chamber (1) 201 can be evacuated to high vacuum using a TMP (turbo molecular pump) or CP (cryopump), for example, residual moisture in the vacuum chamber or the evaporation device can be removed. Therefore, it is preferable from the viewpoint of quality improvement. Furthermore, it is preferable that the exhaust valve 221 is a valve whose opening degree can be controlled because the film formation rate and the like can be controlled by adjusting the pressure in the vacuum chamber.

  The gas mixing unit 3 includes a gas mixer 311 and valves 321 and 331 for switching the flow destination to the vapor deposition head 241 or the exhaust unit 211 of the vacuum chamber (1) 201. The carrier gas containing the vapor of the thin film forming material fed from the evaporator 4 and the heated carrier gas feed unit 7 is uniformly mixed by the gas mixer 311 and fed to the vapor deposition head 241 or the exhaust unit 211 in the vacuum chamber. Is done. As the gas mixer 311, for example, a static mixer or the like is used, and the vapor of the thin film forming material is uniformly dispersed in the carrier gas. By adopting such an apparatus configuration, for example, while the evaporation of the thin film forming material is unstable, the material can be sent to the exhaust part 211 and then sent to the vapor deposition head 241 after the evaporation is stabilized.

  For example, as shown in FIG. 3, the evaporation apparatus 4 includes an evaporation chamber 441 where the thin film forming material is actually evaporated, a heat exchanger 451 for heating the carrier gas to a predetermined temperature, and the thin film forming material as the evaporation chamber 441. A thin film forming material supply unit 5 for supplying the carrier gas to the thin film forming material supply unit 5 and the heat exchanger 451, valves 701, 711, 721, 731, 741 for partitioning each part, 751 and 761.

  The evaporation chamber 441 is connected to the heat exchanger 451, the material transfer pipe (1) 501 connected to the thin film forming material supply unit, and the vapor-containing gas discharge unit (path from the evaporation chamber 441 to the gas mixing unit 3 through the valve 701). Is done. The carrier gas and the thin film forming material heated through the heat exchanger 451 and the material transfer pipe (1) 501 are supplied to the inside of the evaporation chamber 441, where a vapor-containing gas containing the vapor of the thin film forming material is generated.

  Here, the evaporation chamber 441 is preferably formed of a spiral pipe, and the spiral pipe is heated in the spiral pipe as long as the structure is heated from the inner periphery and the outer periphery appropriately and uniformly. In addition, heat exchange between the carrier gas and the thin film forming material is efficiently performed.

  Furthermore, it is preferable that the valve 701 disposed in the path of the vapor-containing gas discharge unit can be adjusted in opening degree in order to improve the material evaporation efficiency by controlling the pressure in the evaporation chamber 411.

  The heat exchanger 451 is configured, for example, by winding an electric heater around the gas pipe, and can heat the carrier gas flowing through the gas pipe to a desired temperature.

  Here, the heat exchanger 451 uses, for example, a static mixer type gas pipe, and is heated in contact with an element inside the pipe, so that the heat exchange efficiency can be improved.

  The thin film forming material supply unit 5 includes a vacuum chamber (2) 401 capable of holding the inside under reduced pressure, a material supply device 411 housed in the vacuum chamber (2) 401, and a material supply device 411 in the vacuum chamber (2). A material supply device support 421 for supporting is included.

  The inner surface of the vacuum chamber (2) 401 has a material receiving portion (1) 511 including a hole communicating with the evaporation chamber 441 through the material transfer pipe (1) 501 as a discharge port.

  The inside of the vacuum chamber (2) 401 is maintained outside the vacuum chamber (2) 401 in a state where the thin film forming material is supplied and stored from the outside and the airtightness of the vacuum chamber (2) 401 is maintained. It is preferable to dispose a material storage container 431 capable of replenishing the material supply device 411 with the thin film forming material.

  The material storage container 431 is preferably capable of supplying a carrier gas from the carrier gas supply unit 6. Moreover, it is preferable that the material storage container 431 can be heated by attaching a jacket heater, for example.

  The material supply device 411 includes a material receiving unit 561 that receives a thin film forming material from the material storage container 431 via the internal atmosphere of the vacuum chamber (2) 401, a material holding unit 551 that stores the thin film forming material, and a material holding unit 551. From the material transfer unit 541 for quantitatively transferring the thin film forming material held in the chamber, the material transfer unit 541 sends the thin film forming material to the material receiving unit (1) 511 via the internal atmosphere of the vacuum chamber (2) 401. A material discharge port 531, a drive unit 591 for driving the material transfer unit 541, and a power transmission mechanism 581 for transmitting power from the drive unit 591 to the material transfer unit 541.

  That is, the thin film forming material is supplied from the material storage container 431 to the material holding unit 551 through the partition valve 761 and the material transfer pipe (2) 571, and the thin film forming material in the material holding unit 551 drives the driving unit 591. As a result, the driving power is transmitted to the material transfer unit 541 through the power transmission mechanism 581, and the material transfer unit 541 is driven by the power, whereby the material transfer unit 541, the material discharge port 531, and the vacuum chamber (2) 401. The material is transferred to the evaporation chamber 441 through the material transmission / reception path (1) 521, the material receiving part (1) 511, and the material transfer pipe (1) 501.

  By using such a thin film forming material supply unit 5, the thin film forming material held in the material holding unit 551 passes through the material transfer unit 541 and the material holding unit 551 and the material discharge port 531 are in an equal pressure state. Therefore, the supply speed of the thin film forming material supplied to the evaporation chamber 441 can be stabilized.

  In this case, if the path cross-sectional area of the material transmission / reception path is 1/10 or less of the area of the cross section of the inner surface of the vacuum chamber (2) 401, the material holding part 551 and the material discharge port 531 are maintained at a uniform pressure. Is easy and preferable.

  More preferably, if the carrier gas supply unit 6 can supply a part of the carrier gas to the vacuum chamber (2) 401, the material for forming a thin film adheres in the material transfer pipe (1) 501. In addition, the vapor-containing gas containing the vapor of the thin film forming material generated in the evaporation chamber 441 can be prevented from flowing back into the vacuum chamber (2) 401.

  More preferably, if the material supply device support 421 has a weighing mechanism and the material supply device 411 is a mechanism that is held in the vacuum chamber only through the material supply device support 421, the material supply device 411 is held by the material supply device 411. Since the weight of the thin film forming material can be measured, the transfer amount of the thin film forming material can be controlled more accurately, and the film thickness obtained on the substrate can be easily controlled.

  As shown in FIGS. 4 and 5, for example, the power transmission mechanism 581 includes a drive side shaft 801 and a driven side shaft 811. The drive side shaft 801 forms a wall of the vacuum chamber (2) 401 with a vacuum chamber (2). 2) By passing through a mechanism capable of maintaining the airtightness of 401 to connect with the external drive unit 591 and move up and down, the drive unit 591 is connected with the driven shaft 811 as shown in FIG. By driving, it is possible to transmit power to the material transfer unit 541 and horizontally transfer the thin film forming material in the material holding unit 551 to the material discharge port 531.

  The vapor deposition apparatus 1 according to the present invention includes one or a plurality of evaporation apparatuses 4. Although FIG. 1 shows an example of two evaporators 4, the structure and the number of series of each evaporator are not limited.

  The carrier gas supply unit 6 includes mass flow controllers 461 and 471, partition valves 741 and 751 with each unit, and the like. The carrier gas is supplied through a gas valve 771, and is branched into a heated carrier gas supplied to the evaporation chamber 441 through heat exchangers 451 and 451, and a carrier gas supplied to the vacuum chamber (2) 401 or the material storage container 431, respectively. It is preferable that it can be sent quantitatively.

  The heated carrier gas flow unit 7 includes a gas heater 453, a mass flow controller 473, and partition valves 703 and 753 with each unit. The heated carrier gas fed from the heated carrier gas feed unit 7 is preferably supplied to the gas mixing unit 3 together with the heated carrier gas containing the vapor of the thin film forming material supplied from the evaporator 4.

  Hereinafter, a specific example of a film forming method using the vapor deposition apparatus of the present invention will be described.

  First, the material storage container 431 is filled with an appropriate amount of a thin film forming material and sealed. Next, the inside of the vacuum chamber (1) 201 is evacuated using the exhaust part 211. Further, the entire process from the gas valve 771 to the vacuum chamber (1) 201 is evacuated and material degassing is performed.

  The vacuum evacuation is preferably performed by high vacuum evacuation using a turbo molecular pump or a cryopump to remove residual moisture or the like that leads to deterioration of the characteristics of the organic EL device as much as possible. In material degassing, the time required for degassing can be shortened by heating the material storage container 431 within a range not affecting the decomposition and degradation of the material.

  Next, each part is heated to a predetermined temperature by a heater installed in each part. The set temperature may be appropriately set according to the operation method and characteristics of the apparatus, but if it is set as low as possible within the range not lowering the boiling point of the thin film forming material, from the viewpoint of fixation of the evaporation material and prevention of material deterioration. preferable.

  Next, the material for forming a thin film is transferred from the material storage container 431 to the material supply device 411 through the partition valve 761 and the material transfer pipe (2) 571. In this case, when material clogging occurs in the material transfer pipe (2) 571, it can be pumped with a small amount of carrier gas through the partition valve 711. In this case, if the material supply device support 421 is a weighing mechanism, the supply amount of the thin film forming material supplied to the material supply device 411 can be controlled.

  Next, the base material 9 is put into the vacuum chamber (1) 201 through the gate valve 251 and placed on the base material holding mechanism 231. In addition, a coolant is circulated in the base material holding mechanism 231 (261) to perform substrate cooling. For example, ethylene glycol or the like is used as the refrigerant.

  Next, the carrier gas is controlled to a predetermined flow rate and temperature by the mass flow controller 471 and the heat exchanger 451, and supplied to the evaporation chamber 441 and the like. The mass flow controller 461 controls the carrier gas to a predetermined flow rate and supplies the carrier gas to the evaporation chamber 441 through the partition valve 721 and the vacuum chamber (2) 401. In this case, the carrier gas flow rate controlled by the mass flow controller 461 may be small enough to suppress the backflow of the vapor-containing gas including the vapor of the thin film forming material evaporated in the evaporation chamber 441.

  Next, a material for forming a thin film is supplied from the material supply device 411 to the evaporation chamber 441 through the material transfer path 521 and the material transfer pipe (1) 501 at a predetermined supply speed.

  In this case, for example, by setting various conditions such as the flow rate and temperature of the carrier gas capable of evaporating the entire amount of the thin film forming material supplied to the evaporation chamber 441, the formation rate can be increased at the supply speed of the thin film forming material. The membrane speed can be controlled. The supply speed of the material for forming a thin film can be controlled by the mechanism of the material supply apparatus 411. However, it is preferable to use the material supply apparatus support section 421 having a weighing mechanism so that the supply speed is more accurately set to a predetermined supply speed. Can be controlled.

  Further, the internal pressure of the evaporation chamber 441 or the like can be efficiently evaporated by adjusting the opening of the partition valve 701 or the like to about 10000 Pa, for example.

  In this way, the vapor-containing gas containing the vapor of the evaporated thin film forming material is discharged from the vapor deposition head 241 through the gas mixing unit 3 together with the carrier gas, and is cooled and deposited on the base material 9 to form a film. To do.

  In this case, the deposition efficiency and deposition distribution on the base material 9 vary depending on the flow rate and temperature of the carrier gas discharged from the vapor deposition head 241.

  When the flow rate and temperature of the carrier gas discharged from the vapor deposition head 241 are kept constant regardless of the process conditions of the evaporation apparatus 4, the mass flow controller 473 and the heat exchanger 453 This can be carried out by appropriately controlling the flow rate and temperature of the carrier gas and feeding it to the gas mixing unit 3.

  Further, in the case of precisely controlling the amount of film deposited on the substrate 9, first, the vapor-containing gas of the thin film forming material is sent to the exhaust unit 211, and after the evaporation speed of the thin film forming material is stabilized, the vapor deposition head 241 is used. The method of flowing to is preferable.

  After the film formation is completed, the material supply device 411 may be stopped and the valve may be closed as appropriate.

  For example, when two layers are laminated using two kinds of thin film forming materials or when co-evaporation is performed, a plurality of evaporators 4 may be configured and the above-described deposition method may be used. As described above, if an appropriate number of evaporation apparatuses are installed, it is possible to perform multilayer deposition or co-evaporation with multiple materials using a plurality of materials. For example, the functional layer 130 of FIG. 95 is configured. All the layers can be formed by one vapor deposition apparatus of the present invention.

  Further, as shown in FIG. 7, a plurality of substrates can be obtained by appropriately combining a plurality of vacuum chambers (1) and exhaust system 2 with a gas mixing unit 3, an evaporator 4 and a heated carrier gas flow unit 7. At the same time, film formation can be advanced to improve productivity.

DESCRIPTION OF SYMBOLS 1 Deposition apparatus 2 Vacuum chamber (1) and exhaust part system 3 Gas mixing part 4 Evaporating apparatus 5 Thin film formation material supply part 6 Carrier gas supply part 7 Heating carrier gas flow part 9 Base material 100 Organic EL apparatus 110 Glass substrate 120 Transparent electrode layer 130 Functional layer 140 Back electrode layer 150 Sealing portion 201 Vacuum chamber (1)
211 Exhaust part 221 Exhaust valve 231 Substrate holding mechanism 241 Deposition head 251 Gate valve 261 Refrigerant flow part 311 Gas mixer 401, 402 Vacuum chamber (2)
411, 412 Material supply device 421, 422 (Material supply device) support part 431, 432 Material storage container 441, 442 Evaporation chamber 451, 452, 453 Heat exchanger 461, 462, 471, 472, 473 Mass flow controller 501 Material transfer piping (1)
511 Material receiving part (1)
521 Material delivery path 531 Material discharge port 541 Material transfer part 551 Material holding part 561 Material receiving part (2)
571 Material transfer piping (2)
581 Power transmission mechanism 591 Drive unit

Claims (9)

A vacuum chamber (1) in which a substrate can be placed, and an evaporation apparatus, and a deposition apparatus for depositing a thin film forming material emitted as vapor in the evaporation apparatus on the substrate,
The evaporation apparatus includes a thin film forming material supply unit and an evaporation chamber, and can supply a vapor-containing gas containing the vapor to the vacuum chamber (1).
The evaporation chamber can generate the vapor-containing gas from the thin film forming material supplied from the thin film forming material supply unit;
The thin film forming material supply unit includes a vacuum chamber (2) capable of maintaining the internal atmosphere at a reduced pressure, the vacuum chamber (2) accommodating the material supply device, and the vacuum chamber (2) A material receiving portion (1) which is a hole on the inner surface and includes a hole communicating with the inside of the evaporation chamber as a discharge port;
The material supply device holds the thin film forming material and supplies the thin film forming material to the material receiving portion (1) via a material transmission / reception path that is a part of the internal atmosphere. And having a material holding part supported on the inner surface of the vacuum chamber (2) via a support part,
Further, the vapor deposition apparatus characterized in that the cross-sectional area of the material transmission / reception path is 1/10 or less of the cross-sectional area of the inner surface of the vacuum chamber (2).   The evaporation apparatus according to claim 1, wherein the support unit has a weighing mechanism capable of measuring a weight of the thin film forming material held by the material holding unit.   The vapor deposition apparatus according to claim 1, wherein the thin film forming material is powder.   The said evaporation apparatus further has a carrier gas supply part which can supply a carrier gas to the said internal atmosphere at least, and the said vapor | steam containing gas contains this carrier gas, The 1-3 characterized by the above-mentioned. The vapor deposition apparatus in any one of. The material supply device further has a material horizontal transfer mechanism capable of moving the thin film forming material held by the material holding part in the horizontal direction and sending it to the material sending / receiving path, and
The material horizontal transfer mechanism includes a power mechanism disposed outside the vacuum chamber (2), and a shaft driven by the power mechanism,
5. The vapor deposition according to claim 1, wherein the shaft is introduced into the vacuum chamber (2) while maintaining airtightness and can transmit power in the horizontal direction. apparatus.   The vapor deposition according to any one of claims 1 to 5, further comprising a material transfer pipe (1) having the discharge port as an opening at one end and the hole at the inner surface of the evaporation chamber as an opening at the other end. apparatus. The vapor deposition apparatus according to any one of claims 1 to 6, further comprising a material storage container that is disposed outside the vacuum chamber (2) and stores the thin film forming material.
A material receiving portion (2) capable of replenishing the material for forming a thin film from the material storage container through the internal atmosphere of the vacuum chamber (2) while the material holding portion maintains the airtightness of the vacuum chamber (2). The vapor deposition apparatus according to claim 1, further comprising a supply port.   The vapor deposition apparatus according to claim 1, further comprising a gas pipe capable of supplying the carrier gas directly from the carrier gas supply unit to the evaporation chamber. A method of manufacturing an organic EL device by sequentially laminating a functional layer including a light emitting layer and a second electrode layer, including at least a first electrode layer, a thin film containing an organic compound, and a second electrode layer on a substrate, An organic process comprising a step of depositing a film on the substrate using at least one organic compound of the thin film containing the organic compound as the thin film forming material using the vapor deposition apparatus according to claim 1. Manufacturing method of EL device.