JP2019131869A - Vapor deposition apparatus - Google Patents

Abstract

To provide a vapor deposition apparatus capable of securing stability and accuracy in quantitative supply of a material to an evaporation chamber.SOLUTION: A vapor deposition apparatus has a film production chamber and an evaporation device which generate a vapor-containing gas containing vapor of a material for thin film formation. The evaporation device includes a material storage container, a material discharge part, and an evaporation chamber, which comprises a material supply system which supplies the material for thin film formation. The material storage container has; a pressure reduction mechanism for degassing which reduces pressure so as to degas the material for thin film formation being stored; a pressure application mechanism which applies pressure with a gas from a gas supply system; and an agitation mechanism which agitates the material for thin film formation, and the agitation can be performed in a state of pressure reduction for degassing. The material discharge part supplies the material for thin film formation to an evaporation chamber by discharging, and the evaporation chamber vaporizes the discharged material for thin film formation and supplies the vapor-containing gas to the film production chamber.SELECTED DRAWING: Figure 1

Description

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

  In recent years, organic EL devices have attracted attention as illumination devices that replace fluorescent lamps and LEDs, and many studies have been made. In addition, organic EL systems are attracting attention and commercialized as display systems such as televisions, which are replaced with liquid crystal systems or plasma systems.

  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, since the thickness is extremely thin compared to a fluorescent lamp, there are few restrictions on the installation location, and since light is emitted in a planar shape, it is difficult to produce a shadow compared to an LED with strong directivity.

  A typical layer structure of the organic EL device is as shown in FIG. The organic EL device 100 shown in FIG. 7 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 part 150.

  The functional layer 130 is formed by laminating a plurality of thin films of organic compounds. 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.

  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 of organic compounds, and each thin film can be formed by a vacuum deposition method.

  The back electrode layer 140 is 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 in a process of forming a thin film constituting each layer. 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, the vapor deposition apparatus is generally constituted by a film forming chamber kept in a vacuum and an evaporation apparatus for evaporating a thin film forming material. The film forming chamber can be provided with a base material such as a glass substrate.

  A typical 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 Patent Documents 2 and 3, a material for forming a thin film is quantitatively supplied to an evaporation device, and a part or all of the material for forming a thin film is evaporated by a heating device of the evaporation device or a heated carrier gas. Is transferred to a film forming chamber to form a film. Here, a method in which all of the supplied material is evaporated at once and the non-evaporated material is not retained in the evaporation apparatus is a so-called flash vapor deposition or a method called flash evaporation.

JP 2012-52187 A WO 2010/123027 Japanese Patent Laid-Open No. 2006-98417

  The inventors of the present invention diligently studied a vapor deposition method for depositing material vapor transferred from such an evaporation apparatus in a film forming chamber. As a result, in such a vapor deposition method, in order to ensure the stability and accuracy of the quantitative supply, in the storage container, the physical properties of the material itself, for example, the particle size or agglomeration state in the case of powder, liquid If so, the distribution in the container such as viscosity is reduced and the change with time is suppressed, the amount of foreign gas components absorbed or adsorbed by the material is reduced, the distribution in the container is reduced, and It was found that it is important to suppress the change over time.

  Therefore, an object of the present invention is to provide a vapor deposition apparatus that can ensure the stability and accuracy of quantitative supply of materials to an evaporation chamber.

  On the other hand, according to the above-mentioned Patent Document 3, as a method for performing co-evaporation using a plurality of types of thin film forming materials, a plurality of systems of evaporation devices are configured, and individual thin film formation is performed by each evaporation device. A method of controlling the mixing ratio by evaporating a material for use has been proposed.

  However, when such a method is used, it is necessary to configure an evaporation apparatus according to the quantity of thin film forming materials to be used, and there is a problem that the cost of the apparatus becomes expensive.

  Therefore, in addition to the above-mentioned object, the present invention preferably pays attention to the above-mentioned problems of the prior art, and uses a plurality of types of thin-film forming materials even in a single vapor deposition apparatus. It is an object of the present invention to provide a vapor deposition apparatus capable of co-depositing a material accurately controlled and mixed in a mixing ratio.

  In particular, in a vacuum deposition method using flash deposition, a plurality of thin film forming materials are used, and in order to stabilize the physical properties of a thin film formed when performing so-called co-deposition, each vaporized by an evaporator is used. It is necessary to accurately control the mixing ratio of the thin film forming material.

  Various measures for solving the above-described problems have been studied and the present invention has been completed.

That is, the present invention has a film forming chamber provided with a base material holding part capable of holding a base material, an evaporation device that generates a vapor-containing gas containing a vapor of a thin film forming material, a gas supply system, and an exhaust system.
A vapor deposition apparatus for depositing the thin film forming material on the substrate by spraying the vapor-containing gas onto the substrate,
The evaporation device includes a material storage container, a material discharge unit, and an evaporation chamber, and includes a material supply system that supplies the thin film forming material to the evaporation chamber,
The material storage container
A storage space for storing the thin film forming material;
A degassing decompression mechanism for depressurizing the storage space to degas the thin film forming material during storage, a pressurizing mechanism for pressurizing the storage space by injecting gas from the gas supply system, and the thin film A stirring mechanism for stirring the forming material, and
The stirring is possible in the degassed vacuum state;
The material discharge unit supplies the thin film forming material to the evaporation chamber by discharge,
The evaporation chamber relates to a vapor deposition apparatus in which the discharged material for forming a thin film is vaporized and the vapor-containing gas is supplied to the film forming chamber.

  According to such a vapor deposition apparatus, since the specific material supply system for supplying the thin film forming material to the evaporation chamber is provided, the distribution of the physical properties of the thin film forming material itself in the storage container is small, and the change with time is prevented. In addition, the amount of foreign gas components absorbed or adsorbed by the material can be reduced, the distribution in the container can be reduced, and changes over time can be suppressed. In addition, the material for forming a thin film can be stably supplied in a fixed amount, and the film can be formed in a stable and precisely controlled state.

  In addition, according to such a vapor deposition apparatus, when co-deposition is performed using a plurality of thin film forming materials, even a single vapor deposition apparatus is a material that is accurately controlled and mixed to a predetermined mixing ratio. Thus, an inexpensive vapor deposition apparatus capable of stably forming a co-deposited thin film having a certain physical property repeatedly.

  That is, it is possible to introduce one or more types of thin film forming materials into the material storage container according to the present invention, and to introduce two or more types of thin film forming materials weighed to have a predetermined ratio. In this case, since the material storage container according to the present invention includes a stirring mechanism such as a rotary stirrer, it is possible to mix and uniformly disperse the thin film forming materials inside. It is. By using such a material storage container, various thin film forming materials used for co-evaporation are mixed in advance, and further, in the evaporation chamber, a part or all of the mixed thin film forming material is mixed. It can be vaporized and deposited on a substrate. The material storage container according to the present invention is a degassing decompression mechanism for depressurizing the storage space in order to degas the thin film forming material being stored, and pressurizes the storage space by injecting gas from the gas supply system. Since it has a pressurizing mechanism, it can effectively remove air and moisture mixed in the introduced material, the foreign gas component, etc., and it also includes an aerosol containing gas from the gas supply system and material powder. The material can be stably supplied to the evaporation chamber by forming the film, and with the stirring, the deterioration of the deposition stability with time due to the aggregation of the powder particles can be prevented. Since stirring is possible, a high-quality thin film capable of more effectively removing the foreign gas component and the like can be stably formed.

  Further, the evaporation chamber is preferably capable of introducing a carrier gas heated from the gas supply system, and the thin film forming material supplied by the discharge as a powder is flash evaporated by the heated carrier gas. The vaporization is preferably performed in a state where the powder does not stay at the bottom of the evaporation chamber, and the conductance between the material discharge portion and the evaporation chamber is constant by suppressing the adhesion of the powder to the pipe wall surface. And the evaporation rate distribution due to the particle size distribution can be suppressed, so that even when the film is formed at a particularly low speed, the film can be formed at a constant rate, and the stability of the powder evaporation itself is also improved. . That is, by making the temperature and flow rate of the heated carrier gas supplied directly to the evaporation chamber constant, the evaporation amount is always more stable, so that the deposition rate on the substrate is stable, Due to the heated carrier gas, the powder in the aerosol, preferably in the aerosol, is flash-evaporated into a vapor-containing gas containing vapor, thereby suppressing the evaporation rate distribution due to the particle size distribution of the powder. In addition, it is preferable that at least a part of the carrier gas, together with the material for forming the thin film, is preferably flown as an aerosol from the material discharge part to the evaporation chamber, and the high temperature carrier gas flows backward to the material discharge part. Therefore, it is possible to prevent the supplied thin film forming material from being welded at the low temperature part upstream of the evaporation chamber of the material supply system, that is, the powder on the wall surface of the pipe of the low temperature material supply system. By attachment of is suppressed, the conductance between the evaporation chamber material supply system is constant. In other words, even in the case of low-speed film formation, in order to be able to form a film stably at a constant rate, the powder of the thin film-forming material is preferably formed as an aerosol containing the same, stably and constantly. It is necessary to supply it to the evaporation chamber through a material supply system having conductance, and it is vaporized by mixing and transferring heat between gases at once as a high-temperature heated carrier gas and flash evaporation. It is important to use a vapor-containing gas that deposits on the material. Here, in order to achieve a stable and constant conductance, the material supply system is kept at a low temperature where the powder does not evaporate. It is necessary to prevent the thin film forming material from adhering, and this high-temperature heated carrier gas is directly heated to the evaporation chamber in a preheated state separately from the carrier gas constituting the aerosol. In addition, it is important for the flash evaporation, preferably the powder of the thin film forming material in the aerosol to be evaporated instantaneously by mixing and heat transfer with the gas at once. It is.

  Further, the material discharge part is a vacuum chamber capable of maintaining the inside thereof at a reduced pressure by the exhaust system, and is provided with a material supply device therein, and is a hole on the inner surface thereof, and the inside of the evaporation chamber A vacuum chamber including a material lower receiving portion that communicates with the evaporating chamber and has a hole for discharging the material for forming the thin film as a discharge port, and the material supply device includes the thin film from the material storage container. It is preferable to have a material upper receiving part capable of receiving the forming material and a material discharging part capable of discharging the thin film forming material in the material lower receiving part, and between the material discharging part and the discharge port. When the space in the vacuum chamber through which the material for forming a thin film circulates is used as a material transmission / reception path, the cross-sectional area of the material transmission / reception path is more preferably 1/10 or less of the area of the cross section of the vacuum chamber surface.

  In such a vapor deposition apparatus, the material supply apparatus itself is held in a vacuum chamber, and the material dispensing unit of the material supply apparatus is in a released state under a constant atmosphere. A differential pressure does not occur between the discharge portion and the thin film forming material can be transferred in a stable atmosphere. The material dispensing part is an entrance of a material for forming a thin film that is one end of the material sending / receiving path on the material supply device side, and the discharge port that is the other end of the material sending / receiving path is: This is the outlet for the thin film forming material.

Further, the material storage container preferably further has a deaeration heating mechanism for heating in order to degas the thin film forming material being stored, and the removal can be carried out more effectively.
Higher quality thin films can be formed more stably.

  Furthermore, it is preferable that the material storage container has a material introduction mechanism capable of introducing at least one kind of the thin film forming material from the outside, and can continuously supply the material. Film formation can be continued over a period of time, combined with the above-described deaeration heating mechanism, deaeration pressure reduction mechanism, pressurization mechanism, stirring mechanism, and a state grasping mechanism described later according to the present invention, High-quality thin films can be stably formed.

  Further, the vapor deposition apparatus of the present invention may include a plurality of the evaporation apparatuses, and in that case, the inside of each of the material supply systems can be individually and directly exhausted by the exhaust system. Preferably, more preferably, the gas supply system can individually introduce a gas such as an inert gas such as nitrogen gas or argon gas into each of the material supply systems. Since the inside of the evaporation device can be individually cleaned, for example, even if a residue of a thin film forming material is generated after the film forming process is completed, the residue can be immediately removed, so that it is stable. High quality thin film can be formed.

  In the vapor deposition apparatus of the present invention, it is preferable that the base material holding part further has a refrigerant circulation mechanism for circulating a refrigerant inside the base material holding part, and more preferably supplied from the gas supply system. A gas spray mechanism for spraying the spray gas toward the base material, and the spray gas is preferably a cooling gas lower than the temperature of the steam-containing gas. Even when the membrane chamber is in a reduced pressure state, the heat exchange between the base material holding part and the base material is promoted by the convection heat transfer of the blowing gas, and the temperature rise of the base material is suppressed. The temperature distribution can be uniformly controlled, and a high-quality thin film can be formed stably.

  The material storage container preferably further has a state grasping mechanism for grasping the state of stirring. For example, when co-evaporation is performed using a plurality of thin film forming materials having different colors, stirring is being performed. By monitoring the trend of the color of the thin film-forming material, it is possible to estimate the timing at which stirring is completed.

  Since the vapor deposition apparatus of the present invention includes a specific material supply system for supplying a thin film forming material to the evaporation chamber, the thin film forming material can be quantitatively supplied to the evaporation chamber accurately and stably, and is stably controlled precisely. The film can be formed in a state.

  In addition, when the vapor deposition apparatus of the present invention performs co-evaporation using a plurality of thin film forming materials, even a single vapor deposition apparatus is accurately controlled and mixed at a predetermined mixing ratio. Thus, a vapor deposition apparatus capable of co-deposition of the material, and an inexpensive vapor deposition apparatus capable of stably forming a co-deposition thin film having a certain physical property repeatedly. In other words, since it is possible to deposit a plurality of types of thin film forming materials on a substrate at a constant mixing ratio with a single evaporation apparatus, the total number of evaporation apparatuses constituting the evaporation apparatus can be calculated. Since the cost can be reduced, the equipment cost can be reduced and the vapor deposition apparatus can be manufactured at low cost.

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 film forming chamber 201, a gas supply system 6, and an exhaust system 7 of FIG. It is the schematic which shows an example of the base material holding | maintenance part 221 provided with the refrigerant | coolant distribution mechanism 251 and the gas blowing mechanism 271. FIG. 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 sectional drawing which shows the general device structure of an organic electroluminescent apparatus. It is an example of the structure figure of the vapor deposition apparatus 1 of this invention which can form into a film simultaneously on two or more base materials 9. FIG.

  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. In the following description, for the sake of explanation, the present invention is described with reference numerals in FIGS. 1, 2, 3, 4, 5, 6, 7, and 8. The description of this code does not limit the present invention in any way.

(Vapor deposition apparatus 1)
The vapor deposition apparatus 1 of the present invention is an apparatus for depositing a thin film forming material on a base material by spraying a vapor-containing gas onto the base material, and includes a film forming chamber 201, an evaporation device 3, and a gas supply system 6. 1 and a plurality of evaporators 3 may be included, and FIG. 1 shows an example including only one evaporator 3, but the structure and series of each evaporator are shown. The number is not limited, and depending on the type and number of thin film products to be formed and the number of thin films to be formed, these elements can be combined in various combinations. Although there are device thin film products having a complicated structure such as an organic EL device, all types of thin films that require a thin film formed by deposition of a vapor-containing gas even when configured as a vapor deposition apparatus including only one evaporation apparatus 3 Can be used as a device capable of forming a film. There is a case. This is one feature of the present invention.

  However, the vapor deposition apparatus 1 of the present invention preferably includes a plurality of evaporation apparatuses 3 from the viewpoint of enabling a plurality of high-quality thin films to be formed in a short tact time, and more preferably, inside each material supply system. Can be directly evacuated individually by the exhaust system 7, and the material supply system can be individually cleaned, so that high film quality stability can be ensured.

  In addition, since the vapor deposition apparatus of the present invention includes a specific evaporation apparatus 3 to be described later, in a co-deposition film in which a plurality of types of materials are uniformly mixed, the mixing ratio of the materials is always constant. Is expensive. In addition, since a plurality of types of thin film forming materials can be co-deposited with a single evaporator, the number of required evaporators can be reduced and the equipment cost can be reduced.

(Film forming chamber 201)
The film forming chamber 201 according to the present invention has a base material holding part 221 that can hold a base material, and a vapor deposition head 231 that blows a vapor-containing gas onto the held base material, and preferably has airtightness. It is directly or indirectly connected to the exhaust system 7, and more preferably has a gate valve 241 for loading and unloading the base material 9 in the film forming chamber 201, and the exhaust system 7 is directly connected to the gas supply system 6, more preferably directly or indirectly connected to the gas supply system 6, particularly preferably directly connected to the gas supply system 6, ie It is preferable that gas can be introduced and exhausted by the film forming chamber 201 alone.

  In the present embodiment, the base material 9 is introduced into the film forming chamber 201 through the gate valve 241 and placed on the base material holding part 221. Next, the vapor-containing gas is blown out toward the base material 9 through the vapor deposition head 231, so that film formation is performed. It is preferable that the blowing part of the vapor deposition head 231 has a proper opening pattern and has a mechanism for blowing the vapor-containing gas uniformly to the film forming surface side of the substrate 9.

(Base material holding part 221)
The base material holding part 221 has a function of holding the base material in the film forming chamber 201 as described above, but preferably further suppresses an increase in the base material temperature due to the radiant heat of the heated vapor deposition head 231 or the like. Therefore, as a structure (251) capable of cooling the substrate, it has a refrigerant distribution mechanism for distributing the refrigerant therein, and more preferably a structure having a substrate mounting surface capable of efficiently cooling the substrate. More preferably, the refrigerant circulates.

  The base material holding part 221 preferably has a gas spray mechanism 271 for spraying the spray gas (261) supplied from the gas supply system in the direction of the base material. It is preferable to have an appropriate opening pattern on the surface, and by blowing the blowing gas (261) on the non-film-forming surface side of the base material 9, the base material holding part 221 and the base material 9 are formed by convection heat transfer or the like. Heat exchange is promoted, cooling efficiency can be improved, heat uniformity over the entire surface of the substrate is enhanced, and in some cases, deposition efficiency can be improved by confining the vapor-containing gas in the vicinity of the substrate.

  Thus, by using the base material holding part 221 having the refrigerant circulation mechanism and / or the gas blowing mechanism, it is possible to suppress the temperature rise of the base material and keep the in-plane temperature constant. As a result, good film properties can be obtained, and quality stability can be improved.

  FIG. 3 is a schematic diagram illustrating an example of the base material holding unit 221 including the refrigerant circulation mechanism 251 and the gas blowing mechanism 271.

(Substrate 9)
The substrate 9 according to the present invention 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.

(Thin film forming materials)
The material for forming a thin film according to the present invention can be used as long as the material is vaporized by heating and the vapor can be deposited on the substrate 9 by cooling. A material that can be introduced into the vapor deposition apparatus of the invention is preferable from the viewpoint of sufficiently exerting the effects of the present invention, and examples thereof include an organic EL material constituting an organic EL element.

  In the present invention, such a material for forming a thin film according to the present invention is supplied to the material holding portion 471 from the material storage container 311 through the partition valve 508 and the upper material transfer pipe 401 as shown in FIG. The material for forming a thin film in the holding unit 471 is driven by driving the drive unit 491, so that the driving power is transmitted to the material transfer unit 461 through the power transmission mechanism 481, and the material transfer unit 461 is driven by the power. It is transferred to the evaporation chamber 351 through the transfer portion 461, the material discharge portion 451, the material receiving path 441 which is the atmosphere inside the vacuum chamber 301, the material lower receiving portion 431, and the lower material transfer pipe 411, and is vaporized, and then a thin film is formed. The vapor-containing gas containing the material vapor is supplied to the film forming chamber 201 and deposited on the substrate 9.

  Here, among the introduced thin film forming materials, the ratio of the material that contributes to the film deposition is generally called film deposition efficiency, and various values can be obtained depending on the calculation criteria. The ratio of the amount of film deposited as a steady state when the substrate 9 is deposited and stabilized for a long time and the substrate 9 having the same area as the stage on which the substrate 9 is placed to the amount of consumed material is absolutely It can be defined as a typical deposition efficiency and can be one of the performance evaluation scales of the vapor deposition apparatus.

(Evaporation device 3)
The evaporation apparatus 3 according to the present invention is an apparatus that generates a vapor-containing gas containing the vapor of the thin film forming material and supplies the generated vapor-containing gas to the film forming chamber, and the thin film forming material is supplied to the evaporation chamber 351. The material supply system 4 includes an evaporation chamber 351 that is a place where the thin film forming material is actually evaporated. The material supply system 4 includes a material storage container 311, a material discharge unit 5, and an evaporation chamber 351.

(Material storage container 311)
The material storage container 311 according to the present invention is a container for temporarily storing a thin film forming material, and includes a storage space for storing the thin film forming material.

  Such a material storage container 311 according to the present invention has a function of degassing the thin film forming material being stored in the storage space, and a function of stirring the degassing decompression state. This is one of the features of the present invention.

  That is, the material storage container 311 according to the present invention includes a degassing decompression mechanism that decompresses the storage space by the exhaust system 7, and a press-fitting that introduces a degassing gas, preferably a carrier gas, from the gas supply system 6 into the interior. It has a pressurizing mechanism that pressurizes the storage space, a stirring mechanism 321 that stirs the thin film forming material, preferably a degassing heating mechanism that heats to degas the thin film forming material being stored, preferably Has a state grasping mechanism to be described later, and preferably has a material introduction mechanism 381 capable of introducing at least one kind of thin film forming material. Preferably, the material storage container 311 can be evacuated independently by an exhaust system 7 directly connected to the material storage container 311 via a pipe or a valve.

  The stirring mechanism 321 is, for example, a stirring bar disposed in the storage space, and is preferably used for stirring and mixing two or more kinds of thin film forming materials.

  The degassing heating mechanism is a mechanism for heating the material storage container 311 from the outside, preferably while adjusting the temperature, for example, by a jacket heater or the like.

  The state grasping mechanism is an observation facility such as a CCD camera, and is used to grasp the stirring state, preferably the mixed state. For example, the state grasping mechanism monitors the color change of one or more kinds of mixed thin film forming materials. By doing so, mixing can be completed at an appropriate timing, and the mixed state of the thin film forming material can be managed.

(Material discharge part 5)
The material discharge unit 5 includes at least a material supply device 331 that receives a material for forming a thin film from the material storage container 311 and a discharge port. The material discharge unit 5 supplies the thin film formation material to the evaporation chamber 351 by discharge from the discharge port. From the viewpoint of shutting off heat from the evaporation chamber 351, the vacuum chamber 301 is preferably capable of holding the inside under reduced pressure.

  That is, it is preferable that the material supply device 331 is stored inside the vacuum chamber 301 which is the material discharge unit 5, and the discharge port is preferably a hole on the inner surface of the vacuum chamber 301, preferably on the bottom surface. In this case, the discharge port is included in the lower material receiving portion 431 of the vacuum chamber 301. By using such a material discharge portion 5, a thin film held in a material holding portion 471, both of which will be described later. Since the forming material can be transferred by the material transfer unit 461 in a state where the material holding unit 471 and the material discharging unit 451 are at an equal pressure, the supply speed of the thin film forming material supplied to the evaporation chamber 351 is stabilized. Can be made.

  In this case, when the space in the vacuum chamber 301 in which the material for forming a thin film between the material discharge part and the discharge port flows is defined as a material transmission / reception path 441, the path cross-sectional area of the material delivery path 441 is a vacuum. If it is 1/10 or less of the area of the cross section of the inner surface of the chamber 301, it is easy and easy to maintain the material holding part 471 and the material discharging part 451 at equal pressure.

  The discharge port communicates with the inside of the evaporation chamber 351 through the lower material transfer pipe 411, and discharges the material for forming a thin film into the evaporation chamber 351, preferably as a powder.

  From the viewpoint of efficiently receiving the material for forming a thin film discharged from the material supply device 331, the material lower receiving portion 431 preferably has a funnel shape with a large opening inside the vacuum chamber 301 and a small discharge opening. The discharge port is an entrance on the material discharge part 5 side of the lower material transfer pipe 411. In this case, the thin film forming material is discharged toward the material lower receiving part 431 through the internal atmosphere of the vacuum chamber 301. Is done.

  More preferably, the structure capable of supplying a part of the carrier gas from the gas supply system 6 to the vacuum chamber 301 can suppress the adhesion of the material for forming a thin film in the material transfer pipe 411 and can evaporate. The vapor-containing gas generated in the chamber 351 can be prevented from flowing back into the vacuum chamber 301, and contamination of the vacuum chamber 301 can be prevented, so that the quality of the formed thin film can be easily maintained at a high level.

  More preferably, if the vacuum system 301 can be individually evacuated by the exhaust system 7, it becomes easy to exhaust impurity gas such as moisture desorbed from the thin film forming material stored inside. .

(Material supply device 331)
The material supply device 331 according to the present invention is a device that quantitatively supplies a material for forming a thin film to the evaporation chamber 351, and is preferably housed in the vacuum chamber 301. In this case, preferably, the material supply is performed in the vacuum chamber 301. It is supported by the device support part 341.

  When the material supply device 331 is supported by the material supply device support part 341, the material supply device support part 341 preferably has a weighing mechanism, and the material supply device 331 has a vacuum chamber only via the material supply device support part 341. It is more preferable if the mechanism is held in 301. Since the weight of the thin film forming material held in the material supply device 331 can be measured, the transfer amount of the thin film forming material can be controlled more accurately. The film thickness obtained on the substrate 9 can be easily controlled.

  Such a material supply device 331 is configured so that the material supply device 331 can receive the material for forming a thin film through the upper material transfer pipe 401 from the material storage container 311, preferably further through the internal atmosphere of the vacuum chamber 301. The receiving part 421, the material holding part 471 that temporarily holds the received thin film forming material, and the material transfer part 461 that quantitatively transfers the thin film forming material held in the material holding part 471 to a material dispensing part described later. The material delivery unit 451 is capable of delivering the transferred thin film forming material as it is to the discharge port.

  When the material discharge unit 5 is the vacuum chamber 301, the material upper receiving unit 421 maintains the confidentiality of the vacuum chamber 301 in order from the material storage container 311 in order of the upper material transfer pipe 401 and the vacuum chamber 301. The material for forming a thin film is preferably received via the internal atmosphere, and the material lower receiving portion 431 is supplied from the material dispensing portion 451 via the internal atmosphere of the vacuum chamber 301 while maintaining the confidentiality of the vacuum chamber 301. Thus, it is preferable to accept a thin film forming material.

  The material supply device 331 further includes a drive unit 491 for driving the material transfer unit 461 and a power transmission mechanism 481 that transmits power from the drive unit 491 to the material transfer unit 461.

  For example, as shown in FIGS. 4 and 5, the power transmission mechanism 481 includes a driving side shaft 601 and a driven side shaft 611, and the driving side shaft 601 uses the wall surface of the vacuum chamber 301 as the confidentiality of the vacuum chamber 301. As shown in FIG. 6, it is connected to the driven side shaft 611 and the drive unit 491 is operated by moving up and down to connect with the external drive unit 491 and moving up and down. Power can be transmitted to the transfer unit 461, and the thin film forming material in the material holding unit 471 can be horizontally transferred to the material dispensing unit 451.

(Evaporation chamber 351)
The evaporation chamber 351 according to the present invention vaporizes the thin film forming material discharged and supplied from the discharge port, preferably as a powder, and produces the generated vapor-containing gas via the vapor-containing gas transfer unit. Supply to the membrane chamber 201.

  The evaporation chamber 351 is preferably capable of introducing a carrier gas heated from the gas supply system 6, and more preferably, the thin film forming material supplied as a powder is supplied to the bottom of the evaporation chamber 351 as a powder. The liquid is flash-evaporated by the heated carrier gas without staying.

  Here, the evaporation chamber 351 is preferably formed of a spiral pipe from the viewpoint of efficiently performing heat exchange between the heated carrier gas and the thin film forming material, and the spiral pipe has an inner circumference. It is more preferable that the system is configured to be heated uniformly from the outer periphery.

  Furthermore, it is preferable that the evaporation chamber 351 can be evacuated independently by an exhaust system 7 directly connected to the evaporation chamber 351 via a pipe or a valve. By doing so, for example, the inside of the evaporation chamber 351 can be heated with a heated carrier gas. Since individual cleaning is possible, the amount of impurities in the formed film is kept low, which is preferable from the viewpoint that the film quality is stably maintained at a high level. For example, in FIG. 1, the evaporation chamber 351 is directly connected to the exhaust system 7 via the exhaust valve 215.

  Furthermore, the pressure in the evaporation chamber 351 is preferably controllable from the viewpoint of maintaining a sufficient material evaporation efficiency. In order to enable this control, the pressure in the vapor-containing gas transfer unit is arranged. In FIG. 1, it is preferable that the partition valve 514 is capable of adjusting the opening degree.

(Gas supply system 6)
The gas supply system 6 according to the present invention is a facility capable of supplying an inert gas such as argon or nitrogen, a cleaning gas, or a mixed gas obtained by mixing them at an arbitrary ratio to a plurality of apparatuses, Valves 501, 502, 503, 504, 505, 506, 507, 508, 509, 511, 512, 513, etc., mass flow controllers 371, 372, 373, 374, 375, etc., heat exchangers 361, 362 , 363... Can be supplied, for example, heated carrier gas can be supplied through a heat exchanger, and in addition, blowing gas (cooling gas), degassing gas, for extrusion Various gases can be supplied as the gas.

  For example, the vapor deposition apparatus 1 of FIG. 1 which is a preferred embodiment of the present invention includes a bypass carrier gas flow section 8, and this gas supply system 6 includes a heat exchanger 374, and the flow from the bypass carrier gas flow section 8. The heated carrier gas sent is separate from the heated carrier gas supplied from the heated carrier gas flow system of the evaporation system 30 including the evaporator 3 and the vapor-containing gas containing the vapor of the thin film forming material. In addition, it is preferable that it can be supplied to the film forming chamber 201 together with this, and it is more preferable that the heated carrier gas alone can be supplied to the film forming chamber 201 from the bypass carrier gas flow section 8.

(Heating carrier gas)
The heated carrier gas according to the present invention is the heated carrier gas that vaporizes the material for forming a thin film in the evaporation chamber 351, specifically, for example, heated to about 100 ° C. to 700 ° C. Nitrogen gas, argon gas, etc., preferably inert gas, more preferably nitrogen gas.

  In FIG. 1, the heated carrier gas and the thin film forming material are supplied to the evaporation chamber 351 through the heat exchanger 362 and the lower material transfer pipe 411, where a vapor-containing gas is generated.

  As the heat exchanger, it is preferable to use a static mixer type gas pipe, and since the element inside the pipe and the carrier gas are heated in contact with each other, the heat exchange efficiency can be improved.

  In order to maintain the temperature of each device, piping, valve, etc. in contact with the heated carrier gas, it is important to heat them with the necessary ribbon heater, jacket heater, etc., and adjust the temperature with an appropriate control method. In particular, such temperature control is important for the portion where the vapor-containing gas is flowed or the portion where the vapor flows back in order to suppress the sticking of the evaporated material and the material deterioration.

(Exhaust system 7)
The exhaust system 7 according to the present invention includes a vacuum exhaust pump such as a dry pump, and pipes and valves that connect the vacuum exhaust pump and the film forming chamber 201, the evaporation device 3, the gas supply system 6 and the like, and are connected to the equipment. Depending on the application, it is necessary to select an appropriate evacuation pump, and it is preferable that each facility has a separate evacuation system 7.

  FIG. 1 illustrates exhaust valves 213, 214, and 215 as such valves related to the exhaust system 7, and the material storage container 311, the material discharge unit 5, and the evaporation chamber 351 are individually connected through these valves. Exhaust valves 211 and 212 are also illustrated as examples that can be evacuated, and the film forming chamber 201 and the vapor-containing gas supply system can be individually evacuated through these, respectively. Such an exhaust system 7 may be switched by a single pump and exhausted by a plurality of pumps, or may be exhausted by individual pumps. Such an exhaust valve exhibits sufficient pump performance and achieves ultimate vacuum. From the viewpoint of forming a high-quality thin film, the conductance is preferably larger than that of the partition valve.

  Furthermore, it is preferable to connect a single exhaust system 7 to each of the film forming chamber 201 and the evaporation apparatus 3 because the film forming chamber 201 and the evaporation apparatus 3 can be individually exhausted. With such an apparatus configuration, for example, while the evaporation of the thin film forming material is unstable, it is sent to the exhaust system 7 through the partition valve 212, and after the evaporation is stabilized, the vapor deposition head 231 is passed through the partition valve 514. Can be streamed to.

  Furthermore, it is preferable that the exhaust valve 211 connecting the film forming chamber 201 and the exhaust system 7 is a valve whose opening degree can be controlled because the film forming speed can be controlled by adjusting the pressure in the film forming chamber.

  The film forming chamber 201 is preferably capable of evacuating the film forming chamber 201 using a dry pump, TMP (turbo molecular pump) or CP (cryo pump), for example, removing residual moisture in the film forming chamber. Therefore, it is preferable from the viewpoint of improving the quality of the thin film.

(Film forming method)
Hereinafter, specific examples of the film forming method using the vapor deposition apparatus of the present invention will be described.

  First, the material storage container 311 is filled with an appropriate amount of a thin film forming material via the material introduction mechanism 381 and sealed. When co-evaporation is performed, it is preferable to adjust the weight ratio between the thin film forming materials used in advance. Next, the exhaust valve (1) 213 is opened, the material storage device 311 is evacuated by using the exhaust system 7, and the material is deaerated. The exhaust valve (1) 213 is capable of adjusting the opening degree and controlling the pressure reduction speed in order to prevent the internal thin film forming material from flying up due to sudden pressure fluctuation in the material storage container 311 during exhaust. It is preferable to be able to.

  The vacuum evacuation is preferably performed by high vacuum evacuation using a dry pump, a turbo molecular pump, or a cryopump to remove as much as possible residual moisture or the like that leads to deterioration in characteristics of the organic EL device or the like. In the material degassing, the time required for degassing can be shortened by heating the material storage container 311 using a heating mechanism in a range that does not affect the degradation of the thin film forming material. Moreover, it is possible to improve the degassing efficiency of the thin film forming material and to further reduce the time required for degassing, preferably by using the stirring mechanism 321 together during heating. Even when the thin film forming materials are filled, the thin film forming materials can be mixed in the material storage container 311.

  When a plurality of types of thin film forming materials are mixed using the stirring mechanism 321, the mixing state is monitored by an observation facility provided in the material storage container 311, for example, based on the degree of color change of the mixed thin film forming materials. Can do.

  Next, each part is heated to a predetermined temperature by a heater installed in each part. The set temperature may be appropriately set in accordance with the operation method and characteristics of the apparatus. However, if the temperature is set as low as possible within a range not lowering the boiling point of the thin film forming material, it is possible to fix the evaporated material and prevent material deterioration. To preferred.

  Next, the material for forming a thin film is transferred from the material storage container 311 to the material supply device 331 through the partition valve 508 and the upper material transfer pipe 401. In addition, when the pressure in the vacuum chamber 301 is set to the same level as the material storage container 311 by the exhaust system 7 via the exhaust valve (1) 214 in advance, It is preferable because the thin film forming material can be prevented from rising due to the pressure difference in the vacuum chamber 301 and contaminating the vacuum chamber 301.

  In this case, when material clogging occurs in the upper material transfer pipe 401, the extrusion gas can be supplied from the gas supply system 6 through the partition valves 503 and 511, and can be pumped. If the material supply device support 341 is a weighing mechanism, the supply amount of the thin film forming material supplied to the material supply device 331 can be controlled.

  Next, the base material 9 is put into the film forming chamber 201 through the gate valve 241 and placed on the base material support mechanism 221. Further, the coolant is circulated in the base material holding part 221 (251), and the base material 9 is cooled. For example, ethylene glycol or the like is used as the refrigerant. Furthermore, through the partition valves 501 and 502 and the mass flow controller (1) 375, a structure in which a cooling gas controlled at a predetermined flow rate can be directly sprayed from the base material holding part 221 toward the non-film-forming surface side of the base material 9 ( 271) is preferable because more effective cooling of the base material 9 can be expected by convective heat transfer between the base material holding part 221 and the base material 9. As the kind of the cooling gas, in order to improve the convective heat transfer property, for example, a gas having a high thermal conductivity such as helium is preferable.

  Next, with the mass flow controller (1) 373, the heat exchanger (1) 362, and the like, the carrier gas is controlled to a predetermined flow rate and temperature and supplied to the evaporation chamber 351 and the like. Further, the carrier gas is controlled to a predetermined flow rate by the mass flow controller (1) 372 and supplied to the evaporation chamber 351 through the partition valves 505 and 509. In this case, the carrier gas flow rate controlled by the mass flow controller (1) 372 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 351.

  Next, a material for forming a thin film is supplied from the material supply device 331 to the evaporation chamber 351 through the material transfer path 441 and the lower material transfer pipe 411 at a predetermined supply rate. In this case, the partition valve 509 is preferably a ball valve, for example, because the thin film forming material passing through the lower material transfer pipe 411 can be supplied to the evaporation chamber 351 without being clogged in the transfer pipe.

  In this case, for example, by making 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 device 351, the production 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 331. However, preferably, the material supply apparatus support section 341 having a weighing mechanism is used to achieve a more accurate predetermined supply speed. Can be controlled.

  Further, the internal pressure of the evaporation chamber 351 or the like can be efficiently evaporated by adjusting the opening of the partition valve 514 or the like to about 10000 Pa, for example.

  In this manner, the vapor-containing gas containing the vapor of the thin film forming material generated in the evaporation apparatus 3 is discharged from the vapor deposition head 231 together with the carrier gas, and is deposited on the substrate 9 by being cooled and deposited.

  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 231.

  When the flow rate and temperature of the carrier gas discharged from the vapor deposition head 231 are constant regardless of the process conditions of the evaporation apparatus 3, the mass flow controller 374 and the heat exchanger 363 from the bypass carrier gas flow unit 8 This can be carried out by appropriately controlling the flow rate and temperature of the carrier gas and feeding it to the film forming chamber 201.

  When the amount of film deposited on the substrate 9 is precisely controlled, first, the vapor-containing gas of the thin film forming material is sent to the exhaust system 7 through the exhaust valve 212 to evaporate the thin film forming material. A method of feeding to the vapor deposition head 231 after stabilization is preferable.

  After film formation, the material supply device 331 may be stopped and the valve may be closed as appropriate.

  By using the vapor deposition apparatus 1 of the present invention and the vapor deposition method described above, a single vapor deposition apparatus 3 can form a co-deposition film using a plurality of types of thin film forming materials. For example, even in the case of a multilayer laminated film such as the functional layer 130 shown in FIG. 7, if the number of evaporation apparatuses 3 corresponding to the type of layers forming the functional layer 130 is installed, the vapor deposition apparatus 1 of the present invention. All layers can be formed on a table.

  In addition, as shown in FIG. 8, a plurality of film forming chambers, gas supply systems, and exhaust systems 7 are appropriately combined with an evaporation device 3 and a bypass carrier gas flow section 8 to simultaneously manufacture a plurality of substrates. The film can be advanced to improve productivity.

  As the vapor deposition apparatus of the present invention, using the apparatus shown in FIG. 8, the temperature of the heated carrier gas is 450 ° C., the concentration of the thin film forming material contained in the heated carrier gas is about 200 μg / sccm, and the film forming chamber When a thin film was formed under the conditions that the pressure inside 201 was 200 Pa and the surface temperature of the substrate 9 was 70 ° C., vapor deposition with an absolute film formation efficiency of 0.6 was possible. Compared with conventional vacuum vapor deposition using resistance heating or chemical vapor deposition using plasma discharge or the like, the film could be formed with extremely high efficiency.

1. Vapor deposition apparatus 2. Film forming chamber, gas supply system, and exhaust system Evaporator 4 4. Material supply system Material discharge part 6. 6. Gas supply system Exhaust system 8. 8. Heated carrier gas flow section Base material 30. Evaporation system 101 including the evaporation apparatus 3. Organic EL device 111. Glass substrate 121. Transparent electrode layer 131. Functional layer 141. Back electrode layer 151. Sealing part 201. Film forming chamber 211. Exhaust valve (1)
221. Substrate holding part 231. Deposition head 241. Gate valve 251. Refrigerant distribution mechanism 261. Blowing (cooling) gas 271. Gas spray mechanism 301. Vacuum chamber 311. Material storage container 321. Stirring mechanism 331. Material cooperative supply device 341. (Material supply device) Support portion 351. Evaporation chamber 361. Heat exchanger (1)
371. Mass flow controller (1)
381. Material introduction mechanism 401. Upper material transfer pipe 411. Lower material transfer pipe 421. Material upper receiving portion 431. Material lower receiving portion 441. Material transmission / reception path 451. Material discharge unit 461. Material transfer unit 471. Material holding part 481. Power transmission mechanism 491. Drive unit 501. Partition valve (1)
511. Partition valve (2)
521. Partition valve (3)
601. Drive side shaft 611. Driven shaft 701. Exhaust valve (2)
711. Mass flow controller (2)
721. Heat exchanger (2)

Claims (7)

A film forming chamber having a substrate holding portion capable of holding a substrate, an evaporation device that generates a vapor-containing gas containing vapor of a thin film forming material, a gas supply system, and an exhaust system, and based on the vapor-containing gas A vapor deposition apparatus for depositing the thin film forming material on the substrate by spraying on the material,
The evaporation device includes a material storage container, a material discharge unit, and an evaporation chamber, and includes a material supply system that supplies the thin film forming material to the evaporation chamber,
From the gas supply system, the material storage container stores a storage space for storing the thin film forming material, a degassing decompression mechanism for depressurizing the storage space to degas the thin film forming material being stored. A pressurizing mechanism for pressurizing the storage space by injecting the gas, and an agitating mechanism for agitating the thin film forming material, and the agitation can be performed in the degassing reduced pressure state.
The material discharge unit supplies the thin film forming material to the evaporation chamber by discharge,
The evaporation apparatus, wherein the evaporation chamber vaporizes the discharged thin film forming material and supplies the vapor-containing gas to the film forming chamber.   The evaporation chamber is capable of introducing a carrier gas heated from the gas supply system, and the thin film forming material supplied by discharge as powder is flash-evaporated by the heated carrier gas, and the powder The vapor deposition apparatus according to claim 1, wherein the vaporization is performed in a state where the vapor does not stay in a bottom of the evaporation chamber as a body. The material discharge unit is a vacuum chamber capable of maintaining the inside thereof at a reduced pressure by the exhaust system, and is provided with a material supply device therein, and is a hole on an inner surface thereof, and communicates with the inside of the evaporation chamber. A vacuum chamber including a material lower receiving portion provided with, as a discharge port, the hole for discharging the thin film forming material in the evaporation chamber, and
The material supply device has a material upper receiving portion capable of receiving the thin film forming material from the material storage container, and a material discharging capable of discharging the thin film forming material to the material lower receiving portion. Or the vapor deposition apparatus according to 2.   The material storage container further introduces a degassing heating mechanism that heats the thin film forming material being stored to deaerate, and at least one kind of the thin film forming material can be introduced from the outside. The vapor deposition apparatus in any one of Claims 1-3 which has a mechanism.   The vapor deposition apparatus according to any one of claims 1 to 4, further comprising a plurality of the evaporation apparatuses and capable of directly exhausting the inside of each of the material supply systems individually by the exhaust system.   The base material holding part further includes a refrigerant circulation mechanism that circulates a refrigerant inside the base material holding part, and a gas blowing mechanism that blows a blowing gas supplied from the gas supply system toward the base material. The vapor deposition apparatus in any one of 1-5. The vapor deposition apparatus according to claim 1, wherein the material storage container further includes a state grasping mechanism for grasping the state of the stirring.