JP2020063476A - Vapor deposition device - Google Patents

Abstract

To provide a vapor deposition device capable of keeping a mass flow controller (MFC) clean from mixture of a thin film forming material, in a room temperature and normal pressure gas flowing system including the MFC at an upstream side of a vapor-containing gas flowing system for securing stability and precision of constant amount supply of the thin film forming material to a film manufacturing chamber.SOLUTION: A vapor deposition device has an evaporation device including a film manufacturing chamber and an evaporation chamber for generating vapor-containing gas containing vapor of a thin film forming material, and supplying the vapor-containing gas to the film manufacturing chamber, and deposits the thin film forming material onto a substrate by blowing the vapor-containing gas. A gas supplying system includes a room temperature and normal pressure gas flowing system only to flow room temperature and normal pressure gas which is gas at room temperature and normal pressure, and a vapor-containing gas flowing system including the evaporation chamber at its downstream side. The room temperature and normal pressure gas flowing system includes the MFC, and at the downstream side of the MFC, comprises a back flow prevention valve automatically closed according to pressure on the further downstream side.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a vapor deposition device. INDUSTRIAL APPLICABILITY The present invention is suitable as, for example, a vapor deposition device used for forming an organic layer forming a functional layer of an organic EL (Electro Luminescence) device.

  In recent years, attention has been paid to organic EL devices as lighting devices that replace fluorescent lamps and LEDs, and much research has been done. In addition, the organic EL method has attracted attention as a method for replacing the liquid crystal method and the plasma method in the display member, and has been commercialized. Here, the organic EL device is one in which an organic EL element is laminated on a substrate such as a glass substrate or a transparent resin film.

  Further, the organic EL element is one in which two electrodes, one or both of which have translucency, are opposed to each other, and a light emitting layer containing an organic compound is laminated between these 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, it can obtain a high-contrast image 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 smaller than that of a fluorescent lamp, there are few restrictions on the installation place, and since it emits light in a planar shape, it is less likely to cause a shadow as compared to an LED having a strong directivity.

  A typical layer structure of the organic EL device is as shown in FIG. The organic EL device 100 shown in FIG. 3 has a configuration called a bottom emission type, in which 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. Further, 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 layers on the glass substrate 110.

  Among the layers described above, the transparent electrode layer 120 is a transparent conductive film of indium tin oxide (ITO) or the like, and is mainly formed by a sputtering method or a CVD method. The functional layer 130 is formed by laminating a plurality of thin films of organic compounds as described above, and each thin film can be formed by a vacuum deposition method. The back electrode layer 140 is generally a metal thin film of aluminum, silver or the like, and can be formed by a vacuum evaporation method.

  As described above, when manufacturing the organic EL device, the vacuum vapor deposition method is often used in the step of forming the thin films forming the respective layers. Here, the vacuum vapor deposition method is a technique for forming a film by using a vapor deposition apparatus as disclosed in Patent Document 1, for example. That is, the vapor deposition apparatus is generally composed of a film forming chamber kept in vacuum and an evaporation apparatus for evaporating a thin film forming material. In the film forming chamber, a base material such as a glass substrate can be installed. A general evaporation device is composed of a heating device using electric resistance and electron beam, and a crucible for containing a thin film forming material.

  Patent Document 1 specifically relates to a vapor deposition apparatus that suppresses material deterioration during deposition of a thin film material and obtains a stable film thickness at a desired vapor deposition rate, in which a base material is installed in a vacuum chamber and a material gas is supplied. A vapor deposition apparatus for depositing a thin film material contained in a material gas supplied from a mechanism on a substrate, wherein the material gas supply mechanism includes a vaporization section to which an aerosol supply mechanism is connected, and the material gas is in the vaporization section. The powder contained in the aerosol supplied from the aerosol supply mechanism contains the vapor of the thin film material obtained by vaporization, and the aerosol supply mechanism separates the powder from the aerosol, the powder separation unit, and the separated and recovered powder. A powder storage unit for storing, and an aerosol forming unit for forming an aerosol from the powder supplied from the powder storage unit, and the entire aerosol supply mechanism is configured to be capable of blocking the inflow of air. Disclose that vapor deposition apparatus. That is, in Patent Document 1, a thin film forming material is quantitatively supplied to an evaporator that is a vaporization unit, and in the evaporator, a part or all of the thin film forming material is evaporated by the heating device or a heated carrier gas, Disclosed is a method for forming a film by transferring the evaporated material to a film forming chamber which is a vacuum chamber. Here, a method in which all the supplied materials are vaporized at once and the non-evaporated material is not retained in the vaporization device is a so-called flash vaporization or a method called flash vaporization.

JP, 2005-101770, A

  The inventors of the present invention have earnestly studied a vapor deposition method for depositing a material vapor transferred from such an evaporator on a substrate in a film forming chamber. As a result, in such a vapor deposition method, even when the film is formed under the same conditions, the film quality and the film forming speed are different depending on the state of the vapor deposition apparatus, and one of the causes is that the vapor gas is contained in the film. I noticed that there was a problem of impurities, so-called contamination.

  For example, the organic EL device is very vulnerable to contamination, and the film quality unexpectedly fluctuates due to contamination, which is an adverse effect when a stable high-yield production is attempted. As a result of further detailed investigation of the cause of such fluctuation, it was found that when the gas supply line is contaminated during a power outage or an unexpected trouble, the fluctuation is triggered. In many cases, such troubles take a very long time to recover, so it is important to apply drastic measures to the vapor deposition equipment itself to prevent the contamination of the coating material due to the mixing of impurities from the gas line. It is very important to do.

  In particular, at room temperature and atmospheric pressure, which is a gas at room temperature and atmospheric pressure, such as the heated carrier gas of Patent Document 1, which has a vapor-containing gas flow system for sending a vapor-containing gas containing a thin film forming material vapor at the downstream side. A normal-temperature and normal-pressure gas transfer system intended to transfer only gas, in order to stably and precisely control the supply amount of the thin film forming material vapor to be used for film formation, the vapor-containing gas transfer system It is extremely important to keep the MCF completely clean from the mixing of the thin film forming material itself in the normal temperature and normal pressure gas flow system including the mass flow controller (MFC) upstream of the above.

  Therefore, the present invention is such a room-temperature and normal-pressure gas flow system having such a vapor-containing gas flow system on the downstream side, and the stability and accuracy of the quantitative supply of the thin film forming material to the film forming chamber can be improved. In order to secure the property, in a room temperature and normal pressure gas transfer system including a mass flow controller (MFC) upstream of the steam-containing gas transfer system, it is downstream of the MFC in the room temperature and normal pressure gas transfer system. In addition, by using a vapor deposition apparatus including a specific room temperature and normal pressure gas flow system including a backflow prevention valve upstream of the vapor-containing gas flow system, the MCF can be completely removed from the mixture of the thin film forming material itself. An object of the present invention is to provide a vapor deposition device that can be kept clean.

  On the other hand, in the above-mentioned Patent Document 1, with respect to [FIG. 3] thereof, the description in [0055] “The aerosol supplied to the powder separating section 451 is separated into a powder material and a carrier gas, and the powder material is a powder. Regarding the “mass flow controller 434” described in “The gas is returned to the storage unit 421 and the separated gas is discharged via the mass flow controller 434. It is preferable that the check valve 481 is installed in the above because it can prevent foreign matter from flowing back and mixing into the material gas supply mechanism. ”, The check valve 481 is provided on the downstream side. Although it is "installed," this "backflow prevention valve 481" is installed in the part that discharges the separated carrier gas to the outside of the downstream device, basically to the atmosphere. It has only the function of preventing foreign matter from flowing back into the device from the outside of the device, basically from the atmosphere, and when supplying the vapor-containing gas from the evaporation chamber to the film forming chamber inside the device. The backflow prevention valve according to the present invention having a function of preventing backflow into the MFC for ensuring the stability and accuracy of the constant amount supply of the thin film forming material to the evaporation chamber, and its installation location The functions are also completely different.

  Therefore, although the vapor deposition apparatus of Patent Document 1 is a film deposition apparatus that supplies vapor-containing gas from the evaporation chamber to the film deposition chamber, as in the vapor deposition apparatus of the present invention, the "backflow prevention valve" described in Patent Document 1 is used. Is a component completely different from the check valve according to the present invention, and there is room for improvement in the stable precision controllability of the supply amount of the thin film forming material vapor.

  The present invention has been completed by studying various measures for solving the above problems.

That is, the present invention includes a film forming chamber having a base material holding portion capable of holding a base material, an evaporation chamber for generating a vapor containing gas containing vapor of a thin film forming material, and the vapor containing gas containing the vapor forming gas. An evaporation apparatus that has an evaporator for supplying gas to a chamber, a gas supply system, and an exhaust system, and sprays the vapor-containing gas onto a substrate to deposit the thin film-forming material on the substrate. ,
The gas supply system is a normal-temperature normal-pressure gas transfer system intended to transfer only normal-temperature normal-pressure gas that is a gas at normal temperature and normal pressure, and a vapor-containing gas transfer system including the evaporation chamber downstream thereof. And including a vapor-containing gas flow system for feeding the vapor-containing gas,
The present invention relates to a vapor deposition apparatus in which the normal temperature and normal pressure gas flow system includes a mass flow controller (MFC), and further includes a backflow prevention valve that is automatically closed on the downstream side of the MFC based on the pressure downstream thereof.

According to such a vapor deposition device,
It has a vapor-containing gas flow system for feeding a vapor-containing gas containing vapor obtained by evaporating a thin film-forming material in the downstream, and it is intended to feed only normal-temperature and normal-pressure gas that is a gas at normal-temperature and normal pressure. Gas carrier vapor deposition system, which is a pressurized gas flow system and includes a mass flow controller (MFC) and a normal temperature and atmospheric pressure gas flow system, which is provided with a backflow prevention valve which is automatically closed on the downstream side of the MFC based on the pressure further downstream thereof. Therefore, in the event of a power outage, unexpected trouble, or sudden large amount of evaporation of the thin film forming material, the gas supply line is less likely to be contaminated, so a stable, high quality thin film can be formed. It becomes a possible vapor deposition device.

  In addition, it is preferable that the normal temperature and normal pressure gas flow system further includes a material collecting mechanism that collects the thin film forming material downstream of the MFC, and the entire apparatus including the control of the MFC is more preferable. It becomes possible to control stably.

  Further, it is preferable that the material collecting mechanism collects the material by a cooling member capable of cooling, and the cooling member dissipates the thin film forming material by heating, and maintains the cleanness of the MFC according to the present invention. However, maintenance can be done easily.

  Further, it is preferable that the normal temperature and normal pressure gas flow system further includes a gas heating mechanism for heating the normal temperature pressure gas downstream of the MFC, and an upstream side including the MFC according to the present invention during normal operation. Since the side is not affected by the temperature rise due to the heating by the heating mechanism and is maintained at almost room temperature, a high quality thin film can be stably formed.

  In addition, the normal temperature and normal pressure gas flow system further includes a material collecting mechanism that collects the thin film forming material in order on the downstream side from the MFC, and a gas heating mechanism that heats the normal temperature pressurized gas. , And the above-mentioned check valve are preferably provided, and due to the overall synergistic effect of the installation position, the cleanliness of the MFC according to the present invention becomes more reliable and the entire apparatus can be controlled more stably.

  In addition, the normal temperature and normal pressure gas transfer system, from the downstream side of the backflow prevention valve, that is, in the normal temperature and normal pressure gas transfer system, at least from the upstream side of the evaporation chamber, the vapor-containing gas It is preferable that the gas can be exhausted by the exhaust system without passing through a flow system, and there is a possibility that the thin film forming material is attached. Cleaning of the normal temperature and normal pressure gas flow system regardless of the vapor-containing gas flow system. Therefore, the cleanability of the MFC according to the present invention becomes more reliable, the maintainability of the entire apparatus is improved, and the vapor-containing gas flow system is provided from the downstream side of the evaporation chamber to the film forming chamber. It is preferable that the gas can be exhausted by the exhaust system without going through, and more preferably, the exhaust can be automatically performed according to the pressure of the vapor-containing gas flow system, and the thin film forming material is Vapor-containing gas that may adhere It is desirable that the amount of staying material is as small as possible during non-film-forming, and bypasses the film-forming chamber, which requires a long time for evacuation due to long gas residence time, and preferably vapor of another material, for example. When switching the material vapor to be sent to, the cleaning can be performed quickly and the maintainability of the entire apparatus is improved.

  In addition, it is preferable that the evaporation device further includes a material supply system that supplies the thin film forming material to the evaporation chamber, and the thin film forming material is kept in the evaporation chamber heated to a high temperature for a long time. The amount of the material that needs to be supplied to the film forming chamber at each moment from the material supply system while preventing it from being deteriorated at high temperature by supplying a small part of it to the film forming chamber while holding it By supplying the material to the evaporation chamber, such a high temperature deterioration of the material can be prevented, and a vapor deposition apparatus capable of forming a high quality thin film can be obtained. The material supply system includes a material storage container and a material storage container for forming the thin film. It is preferable to include a material discharge part that receives the material and supplies the thin film forming material to the evaporation chamber by discharging, and since the thin film forming material is supplied to the evaporation chamber by such discharging, the temperature becomes high. Material from the evaporation chamber The heat transfer to the storage container is prevented and the above-mentioned high temperature deterioration and, for example, the fusion of the thin film forming material stored / supplied in a powder in a preferable mode is prevented, and further, the pressure in the evaporation chamber is not affected, It is possible to stably supply a constant amount of material.

  Further, the evaporation chamber can introduce a heated carrier gas from the gas supply system, and the thin film forming material supplied by the discharge as powder is flash-evaporated by the heated carrier gas, The powder is preferably vaporized in a state where it does not stay at the bottom of the evaporation chamber, and a vapor deposition apparatus capable of forming a film stably while preventing the above-mentioned high temperature deterioration is obtained.

  Since the vapor deposition apparatus of the present invention includes a specific gas supply system, the gas supply line is unlikely to be contaminated, that is, the MFC according to the present invention can be prevented from being mixed with the material for forming a thin film and adhering the material from the gas containing vapor. Thus, the vapor deposition apparatus can suppress the inaccuracy and instability of the flow rate, and can form a highly controlled, high-quality thin film that is stable and has few troubles.

It is an example of the block diagram of the vapor deposition apparatus 1 of this invention. It is an example of a partial structural detail view including the film forming chamber 201 of the vapor deposition device 1 of the present invention. It is sectional drawing which shows the general device structure of an organic EL device.

  Embodiments of the present invention will be described below. The present invention is not limited to the following embodiments, and various modifications can be made within the technical common sense of those skilled in the art. Further, in the following description, the present invention is described with reference to the reference numerals in FIGS. 1 to 3, but the present invention is not limited by the description of the reference numerals.

(Evaporation apparatus 1)
The vapor deposition device 1 of the present invention is a device for spraying a vapor-containing gas onto a base material to deposit a thin film forming material on the base material, and includes a film forming chamber 201, an evaporation device 3, and a gas supply system 6. , And an exhaust system 7, and may include one or a plurality of evaporators 3. 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, depending on the type of thin film product to be formed into a film or a thin film to be formed, depending on the number, it is possible to configure various combinations of these elements, as a suitable application example, for example, , A device such as an organic EL device, which is vulnerable to contamination.

  The vapor deposition apparatus 1 of the present invention preferably comprises a plurality of vaporizers 3 from the viewpoint of enabling the formation of a plurality of high-quality thin films in a short tact time, and more preferably the inside of each material supply system, The exhaust system 7 can directly exhaust the gas individually, and the material supply system can be individually cleaned, so that high film quality stability can be secured.

  Further, since the vapor deposition device 1 of the present invention includes the specific gas supply system 6 described later, the gas supply line is less likely to be contaminated and a high quality thin film can be stably formed.

(Gas supply system 6)
The gas supply system 6 according to the present invention is a carrier gas, which is preferably an inert gas such as argon or nitrogen, a vapor-containing gas according to the present invention, a cleaning gas, or a mixture of these in an arbitrary ratio. Gas is a facility that can supply gas to a plurality of devices, and includes a specific room temperature and normal pressure gas transfer system, and a vapor-containing gas transfer system, which will be described later according to the present invention, and at least the present invention, a mass flow controller. (MFC) 373 and backflow prevention valve 395, and in addition to these, partition valves 501, 502, 503, 504, 505, 506, 507, 508, 509, 511, 512, 513 ... Mass flow controllers 371, 372, 374, 375, ..., Heat exchangers 361, 362, 363 ,. By going through the vessel, it can be supplied a heated carrier gas, Additional cooling gas and deaeration gas, as an extrusion gas, various gases can allow supply.

(Normal temperature and pressure gas delivery system 61)
The gas supply system 6 according to the present invention is characterized by including a specific room temperature and normal pressure gas flow system 61. That is, the room temperature and pressure gas delivery system 61 according to the present invention is intended to transfer only a room temperature and pressure gas that is a gas at room temperature and pressure, such as an inert gas represented by argon or nitrogen as described above. In addition, or at least in normal operation, only the normal temperature and normal pressure gas is sent, and a steam-containing gas flow system 62 for sending the steam-containing gas is provided downstream thereof, and a mass flow controller (MFC) 373 is included. That is, the MFC 373 is included upstream of the vapor-containing gas flow system 62 in the room temperature and atmospheric pressure gas flow system 61, and the check valve 395 is included downstream of the MFC 373. A backflow prevention valve 395 is provided downstream of the MFC 373 in the normal pressure gas delivery system 61 and upstream of the vapor-containing gas delivery system 62, and the heated carrier gas is passed through the valve. Possible it is.

  The room-temperature and normal-pressure gas flow system 61 according to the present invention includes the MFC 373 and the backflow prevention valve 395 downstream of the MFC 373 as described above, and other than these, preferably, the gas heating mechanism 362 and the material collecting mechanism. One or more mechanisms selected from the group consisting of 390 can be included, preferably can be exhausted by the exhaust system 7 from the downstream side of the check valve 395, more preferably, the vapor-containing gas flow described below. The gas can be exhausted without going through the feeding system 62.

  The gas heating mechanism 362 is a mechanism for heating the room temperature pressure gas, and is preferably installed downstream of the MFC 373 according to the present invention. During normal operation, the upstream side including the MFC 373 is the heating mechanism. Since the temperature is not affected by the temperature rise due to heating by 362 and the temperature is maintained at about room temperature, the entire apparatus including the control of the MFC 373 can be controlled more stably, and more preferably, the backflow prevention according to the invention is prevented. The backflow prevention valve 395 is installed upstream of the valve 395 to stop the heating of the heating mechanism 362 and lower the temperature of the heating mechanism 362, so that the backflow of the vapor-containing gas to the upstream side including the heating mechanism 362 is prevented. Since it is prevented, the cleanliness of the MFC 373 according to the invention is maintained, and the MFC 373 is caused by the thin film forming material adhered to the heating mechanism 362. The material surplus can be prevented in the film formation initial.

  The material collecting mechanism 390 is a mechanism for collecting the thin film forming material according to the present invention, and is preferably a path of the thin film forming material at room temperature and atmospheric pressure by a cooling member capable of cooling. It is a mechanism that collects by adhering to the inner wall surface, can dissipate the thin film forming material by heating the cooling member, and is preferably installed downstream of the MFC 373 according to the present invention and collects the material. The collection by the mechanism 390 makes it difficult for the film-forming material to flow into the upstream side including the MFC 373, so that the cleanliness of the MFC 373 is more easily maintained, and more preferably, the check valve 395 according to the present invention. Even if the valve 395 is installed upstream of the MFC 373 and the backflow prevention is incomplete, the cleanliness of the upstream side including the MFC 373 can be reliably maintained. By the valve 395, the thin film forming material does not accumulate in the material collecting mechanism even during normal operation, and it is possible to prevent the occurrence of an unexpected material supply amount variation during film formation. More preferably, the gas heating mechanism 362 is provided. Since the film forming material is less likely to flow into the upstream side including the gas heating mechanism 362 installed downstream, the cleanliness of the MFC 373 according to the present invention is more easily maintained.

(Backflow prevention valve 395)
The backflow prevention valve is also called a check valve, check valve, check valve, check, etc., and is generally attached to a pipe for sending a fluid such as gas or liquid, and the pressure difference between the upstream and the downstream of the fluid. It is a valve that is operated by a certain back pressure so as to prevent the fluid from flowing backward from the downstream side to the upstream side when the pressure on the upstream side is lower than the pressure on the downstream side.

  The check valve 395 according to the present invention thus has a function of automatically closing the flow path on the basis of the pressure further downstream thereof.

(Steam-containing gas flow system 62)
The gas supply system 6 according to the present invention sends the vapor-containing gas according to the present invention downstream of the room-temperature and normal-pressure gas delivery system 61, and also includes a vaporization chamber 351 to be described later. A system 62 is included. That is, the vapor-containing gas flow system 62 according to the present invention feeds the vapor-containing gas generated in the evaporation chamber 351 to the film-forming chamber 201 at least when the vapor-containing gas is supplied to the film-forming chamber 201.

  The vapor-containing gas flow system 62 according to the present invention can be preferably exhausted from the downstream side of the evaporation chamber 351 by the exhaust system 7, and more preferably can be exhausted without the film forming chamber 201 described later. is there.

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

  In FIG. 1, the heating 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, and the vapor-containing gas is generated therein.

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

  In order to maintain the temperature of each device, pipes, valves, etc. that come into contact with the heated carrier gas, it is important to heat them with a ribbon heater, jacket heater, etc., as necessary, 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 fed or flows backward, in order to prevent the vaporized material from sticking and the material from deteriorating.

(Film forming chamber 201)
The film forming chamber 201 according to the present invention has a base material holding portion 221 capable of holding a base material, and a vapor deposition head 231 that blows a vapor-containing gas onto the held base material, and is preferably airtight. It has, and is directly or indirectly connected to the exhaust system 7, and more preferably has a gate valve 241 for loading and unloading the substrate 9 in the film forming chamber 201. 7 directly, more preferably directly or indirectly connected to the gas supply system 6, and 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 via the gate valve 241 and placed on the base material holding portion 221. Next, the vapor-containing gas is blown out toward the substrate 9 via the vapor deposition head 231, so that the film formation is performed. It is preferable that the blowing portion of the vapor deposition head 231 has a proper opening pattern and that the vapor-containing gas is blown out uniformly to the film forming surface side of the base material 9.

(Base material holding part 221)
The base material holding section 221 has a function of holding the base material in the film forming chamber 201 as described above.

(Base material 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 base material 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.

(Material for thin film formation)
As the thin film forming material according to the present invention, various materials can be used as long as they can be vaporized by heating and the vapor can be deposited on the substrate 9 by cooling, but they are solid at room temperature and are formed as powder. 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 that constitutes an organic EL element.

  In the present invention, such a thin film forming material according to the present invention is preferably replenished to the material holding unit 471 through the partition valve 508 and the upper material transfer pipe 401 from the material storage container 311 as shown in FIG. The driving force of the thin film forming material in the material holding unit 471 is transmitted to the material transfer unit 461 through the power transmission mechanism 481 by driving the driving unit 491, and the material transfer unit 461 is driven by the power. The material transfer section 461, the material delivery section 451, the material receiving path 441 which is the internal atmosphere of the vacuum chamber 301, the lower material receiving section 431, and the lower material transfer pipe 411 are transferred to the evaporation chamber 351 and vaporized, and thereafter, The vapor-containing gas containing the vapor of the thin film forming material is supplied to the film forming chamber 201 and is deposited on the substrate 9.

(Evaporator 3)
The evaporation device 3 according to the present invention is a device for generating a vapor-containing gas containing vapor of a thin film forming material and supplying the generated vapor-containing gas to a film forming chamber, and for forming a thin film of at least solid or liquid. The material is evaporated to generate a vapor-containing gas containing the vapor of the thin film forming material, that is, an evaporation chamber 351 which is a place for vaporizing the thin film forming material is included, and the thin film forming material is preferably contained in the evaporation chamber 351. Preferably contains a material supply system 4 to be supplied as a powder.

(Evaporation chamber 351)
The evaporation chamber 351 according to the present invention supplies the vapor-containing gas generated by vaporizing the thin film forming material to the film forming chamber 201 via the vapor-containing gas transfer unit.

  The evaporation chamber 351 is preferably capable of introducing the above-mentioned heated carrier gas from the gas supply system 6, and the thin film forming material supplied as powder is more preferably powder as the evaporation chamber. While not staying at the bottom of the 351, it is flash-evaporated by heat transfer from the heating carrier gas.

  Here, from the viewpoint of efficiently exchanging heat between the heating carrier gas and the thin film forming material, the evaporation chamber 351 is preferably configured by a spiral pipe, and the spiral pipe has an inner circumference thereof. It is more preferable that the system is configured so that the heat is uniformly heated from the outer circumference.

  Further, it is preferable that the evaporation chamber 351 can be independently evacuated by the exhaust system 7 directly connected to the evaporation chamber 351 through a pipe or a valve. By doing so, for example, the inside of the evaporation chamber 351 can be heated with a heating carrier gas. Since individual cleaning is possible, the amount of impurities in the formed film is kept low, and 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 an exhaust valve 215.

  Furthermore, the pressure in the evaporation chamber 351 is preferably controllable from the viewpoint of maintaining sufficient material evaporation efficiency. In order to enable this control, the pressure in the vapor-containing gas transfer section is arranged. It is preferable that the partition valve 514 shown in FIG. 1 has an adjustable opening degree.

(Material supply system 4)
The material supply system 4 receives the thin film forming material from the material storing container 311 having a storage space for storing the thin film forming material and the material storing container 311, and discharges the thin film forming material into the evaporation chamber. The material discharge part 5 to supply is included.

(Material storage container 311)
The material storage container 311 is a container for temporarily storing the thin film forming material, has a storage space for storing the thin film forming material, and preferably has a material introducing mechanism 381 capable of introducing the thin film forming material. The exhaust system 7 directly connected through the pipes and the valves enables the individual exhaust.

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

  That is, the material supply device 331 is preferably housed inside the vacuum chamber 301 which is the material discharge unit 5, and the discharge port communicates with the inside of the evaporation chamber 351 to form a thin film in the evaporation chamber 351. Materials for. It is preferably a hole for discharging as powder, preferably on the inner surface of the vacuum chamber 301, more preferably on the bottom surface thereof, and in this case, the discharge port is included in the lower material receiving portion 431 of the vacuum chamber 301. By using the material discharge unit 5 as described above, the thin film forming material held in the material holding unit 471, which will be described later, is transferred to the material holding unit 471 and the material dispensing unit 451 by the material transfer unit 461. Since the material can be transferred under pressure, the supply rate of the thin film forming material supplied to the evaporation chamber 351 can be stabilized.

(Material supply device 331)
The material supply device 331 is a device that is preferably incorporated in the vapor deposition device of the present invention for the purpose of quantitatively supplying the thin film forming material to the evaporation chamber 351, and as described above, is preferably housed in the vacuum chamber 301. In that case, more preferably, it is supported by the material supply device supporting portion 341 in the vacuum chamber 301.

  When the material supply device 331 is supported by the material supply device support part 341, it is preferable that the material supply device support part 341 has a weighing mechanism, and the material supply device 331 is a vacuum chamber only via the material supply device support part 341. It is more preferable if the mechanism is held in 301, and since the weight of the thin film forming material held in the material supply device 331 can be measured, it is possible to more accurately control the transfer amount of the thin film forming material. Therefore, it becomes easy to control the film thickness obtained on the base material 9.

  Such a material supply device 331 has at least a material upper receiving portion 421 capable of receiving a thin film forming material via the upper material transfer pipe 401 from the material storage container 311 and preferably further via the internal atmosphere of the vacuum chamber 301. And a material dispensing unit 451 capable of dispensing the thin film forming material to the discharge port, and preferably, the material holding unit 471 that temporarily holds the received thin film forming material and the material holding unit 471 hold the material. A material transfer unit 461 that quantitatively transfers the thin film forming material to the material delivery unit 451 is included.

  When the material discharge part 5 is the vacuum chamber 301, the material upper part receiving part 421 keeps the airtightness of the vacuum chamber 301, and sequentially from the material storage container 311 to the upper material transfer pipe 401 and the vacuum chamber 301. It is preferable to receive the material for forming a thin film through the internal atmosphere, and the material lower part receiving portion 431 can maintain the airtightness of the vacuum chamber 301, and then the material discharging portion 451 through the internal atmosphere of the vacuum chamber 301. Therefore, it is preferable to receive the thin film forming material.

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

  In this case, when the space in the vacuum chamber 301 through which the material for forming a thin film flows between the material dispensing part and the discharge port is the material transfer path 441, the path cross-sectional area of the material transfer 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 preferable to maintain the pressure equalization between the material holding portion 471 and the material dispensing portion 451.

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

  From the viewpoint of efficiently receiving the thin film forming material dispensed from the material supply device 331, the lower material receiving portion 431 preferably has a large opening inside the vacuum chamber 301 and a discharge opening having a small opening. The discharge port is an inlet of the lower material transfer pipe 411 on the material discharge unit 5 side, and in this case, the thin film forming material is discharged toward the lower material receiving unit 431 through the internal atmosphere of the vacuum chamber 301. To be done.

  More preferably, a structure capable of supplying a part of the carrier gas from the gas supply system 6 to the vacuum chamber 301 can prevent the thin film forming material from adhering to the inside of the material transfer pipe 411 and evaporate. The vapor-containing gas generated in the chamber 351 can be prevented from flowing back to the vacuum chamber 301, and the vacuum chamber 301 can be prevented from being contaminated. Therefore, 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 exhausted by the exhaust system 7, it becomes easy to exhaust the impurity gas such as moisture desorbed from the thin film forming material stored inside. .

(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 to the film forming chamber 201, the evaporator 3, the gas supply system 6 and the like, and the connected equipment. It is necessary to select an appropriate vacuum exhaust pump according to the application of (3), and it is preferable that each equipment has an individual exhaust system 7.

  As valves related to such an exhaust system 7, exhaust valves 213, 214, and 215 are illustrated in FIG. 1, and the material storage container 311, the material discharge part 5, and the evaporation chamber 351 are individually provided through each of them. Exhaust valves 211 and 212 are also illustrated, and the film forming chamber 201 and the vapor-containing gas supply system can be individually exhausted through these exhaust valves, respectively. Such an exhaust system 7 may be switched by one pump to exhaust a plurality of pumps, or may be exhausted by an individual pump. Such an exhaust valve allows pump performance to be sufficiently exerted and the ultimate vacuum degree to be achieved. From the viewpoint of forming a high quality thin film, it is preferable that the conductance is larger than that of the partition valve.

  Furthermore, it is preferable to connect a separate exhaust system 7 to the film forming chamber 201 and the evaporator 3, because the film forming chamber 201 and the evaporator 3 can be separately exhausted. With such a device 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 evaporation head 231 is supplied through the partition valve 514. Can be sent 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 can be controlled because the film forming speed and the like can be controlled by adjusting the pressure inside the film forming chamber.

  In the film forming chamber 201, it is preferable that the film forming chamber 201 can be evacuated to a high vacuum by using a dry pump, a TMP (turbo molecular pump) or a CP (cryo pump). For example, residual moisture in the film forming chamber can be removed. Therefore, it is preferable from the viewpoint of improving the quality of the thin film.

(Film forming method)
A specific example of a film forming method using the vapor deposition device of the present invention will be described below.

  First, the material storage container 311 is filled with an appropriate amount of the thin film forming material via the material introduction mechanism 381 and sealed. When co-deposition is performed, it is preferable to adjust the weight ratio of the thin film forming materials to be used in advance. Next, the exhaust valve 213 is opened, the material storage device 311 is evacuated using the exhaust system 7, and the material is degassed. The exhaust valve 213 is capable of adjusting the opening and controlling the depressurization rate in order to prevent the internal thin film forming material from soaring due to a sudden pressure change in the material storage container 311 during exhaust. I like it.

  For vacuum evacuation, it is preferable to perform high vacuum evacuation by using a dry pump, a turbo molecular pump, or a cryopump to remove residual water and the like that lead to deterioration of characteristics of the organic EL device and the like as much as possible. For the material degassing, the time required for degassing can be shortened by heating the material storage container 311 within a range that does not affect the decomposition and deterioration of the thin film forming material using a heating mechanism.

  Next, each part is heated to a predetermined temperature with a heater installed in each part. The set temperature may be appropriately set according to the operation method and characteristics of the device.

  Next, the thin film forming material 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. Note that the pressure of the vacuum chamber 301 is made approximately equal to that of the material storage container 311 by the exhaust system 7 via the exhaust valve 214 in advance, so that the material storage container 311 and the vacuum chamber 301 can be transferred when the thin film forming material is transferred. This is preferable because it is possible to suppress the thin film forming material from flying up due to the pressure difference and contaminating the inside of 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 pressure-fed, and in this case, If the material supply device support portion 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 substrate 9 is put into the film forming chamber 201 via the gate valve 241 and placed on the substrate support mechanism 221. Further, the coolant is circulated in the base material holding portion 221 (251) to cool the base material 9. 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 MFC 373 and the heat exchanger 362 and supplied to the evaporation chamber 351 and the like, and the carrier gas heated by the heat exchanger 362 causes the thin film in the evaporation chamber 351. The forming material is heated and vaporized. Further, by controlling the carrier gas at a predetermined flow rate by the MFC 372 and supplying it to the evaporation chamber 351 through the partition valves 505 and 509, the thin film forming material is transferred from the material discharge part 5 to the evaporation chamber 351 along with the carrier gas. Will be supplied. In this case, the carrier gas flow rate controlled by the MFC 372 may be small enough to suppress the backflow of the vapor-containing gas containing the vapor of the thin film forming material vaporized in the vaporization chamber 351.

  At this time, in the present invention, the thin film system forming material is temporarily supplied in a large amount due to pulsation, is unexpectedly stayed and bumps, and the carrier gas supply amount from the material discharge part 5 is unexpected. Even if the pressure of the vapor-containing gas flow system 62 on the downstream side including the evaporation chamber 351 becomes higher than the pressure of the normal-temperature / normal-pressure gas flow system 6 on the upstream side due to excess, the backflow prevention valve The presence of 395 prevents the MFC 373 from being contaminated by the thin film forming material.

  In supplying the heated carrier gas to the evaporation chamber 351 and the like by the MFC 373 and the heat exchanger 362 and the like, the heat exchanger 390 is provided as a material collecting mechanism between the MFC 373 and the heat exchanger 362, and the carrier It is preferable that the gas is once cooled to room temperature or lower and then heated in the heat exchanger 362. By doing so, impurities such as water in the carrier gas are prevented from flowing into the evaporation chamber 351 on the downstream side, and the MFC 373 on the upstream side is prevented from backflowing the thin film forming material or the like from the downstream side. It The material trapped by the material collecting mechanism 390 can be discharged to the outside of the system by heating in the material collecting mechanism 390 during maintenance and moving in the exhaust system 7.

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

  In this case, for example, by setting various conditions such as the flow rate and temperature of the carrier gas that can completely evaporate the thin film forming material supplied to the evaporation device 351, the thin film forming material can be manufactured at the supply speed of the thin film forming material. The membrane speed can be controlled. The supply speed of the thin film forming material can be controlled by the mechanism of the material supply device 331, but preferably, by using the material supply device supporting portion 341 having a weighing mechanism, the supply speed can be more accurately adjusted to a predetermined supply speed. You can control.

  Further, the pressure inside the evaporation chamber 351 and the like can be efficiently evaporated by adjusting the opening of the partition valve 514 and the like to about 10,000 Pa.

  In this way, the vapor-containing gas containing the vapor of the thin film forming material generated in the evaporation device 3 is discharged from the vapor deposition head 231 together with the carrier gas, cooled on the base material 9 and deposited to form a film.

  In this case, the film deposition efficiency and the film deposition distribution on the substrate 9 change 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 evaporator 3, the bypass carrier gas flow section 8 allows the mass flow controller 374 and the heat exchanger 363 to This can be performed by appropriately controlling the flow rate and temperature of the carrier gas and sending the carrier gas to the film forming chamber 201.

  Further, in the case of precisely controlling the film deposition amount on the base material 9, 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 sending to the vapor deposition head 231 after stabilizing is preferable.

  After the film formation is completed, the material supply device 331 may be stopped and the valve may be closed appropriately.

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

  Using the apparatus shown in FIG. 1 as the vapor deposition apparatus of the present invention, the temperature of the heating carrier gas is 450 ° C., the concentration of the thin film forming material contained in the heating carrier gas is about 200 μg / sccm, and the film forming chamber is When a thin film was formed under the condition that the pressure inside 201 was 200 Pa and the surface temperature of the substrate 9 was 70 ° C., the absolute film deposition efficiency could be calculated as 0.6. It is possible to repeatedly form a film, and it is possible to form a film at the same film forming speed under the same conditions even before and after the maintenance of the evaporation device. The MFC according to the present invention is an evaporation device including a vapor-containing gas flow system. However, it was confirmed that it could be kept clean.

1. Evaporation device 3. Evaporator 4. Material supply system 5. Material discharge part 6. Gas supply system 61. Room temperature and pressure gas delivery system 62. Steam-containing gas flow system 7. Exhaust system 9. Substrate 101. Organic EL device 111. Glass substrate 121. Transparent electrode layer 131. Functional layer 141. Back electrode layer 151. Sealing portion 201. Film forming chamber 211. Exhaust valve 221. Base material holding portion 231. Vapor deposition head 241. Gate valve 301. Vacuum chamber 311. Material storage container 331. Material cooperative supply device 341. (Material Supply Device) Support Unit 351. Evaporation chamber 361. Heat exchanger 372. Gas heating mechanism 371. MFC
373. Mass flow controller (MFC) according to the present invention
381. Material introduction mechanism 390. Material collection mechanism 395. Backflow prevention valve 401. Upper material transfer pipe 411. Lower material transfer pipe 421. Upper material receiving portion 431. Lower material receiving portion 441. Material transfer route 451. Material discharging unit 461. Material transfer unit 471. Material holding unit 481. Power transmission mechanism 491. Drive unit 501. Partition valve 511. Partition valve 521. Partition valve 601. Drive shaft 611. Driven shaft 701. Exhaust valve 711. Mass flow controller 721. Heat exchanger

Claims (8)

A vapor deposition chamber including a substrate holding unit capable of holding a substrate, an evaporation chamber for generating a vapor-containing gas containing a vapor of a thin film forming material, and vaporization for supplying the vapor-containing gas to the film-forming chamber A vapor deposition apparatus having a device, a gas supply system, and an exhaust system, and spraying the vapor-containing gas onto a substrate to deposit the thin film forming material on the substrate,
The gas supply system is a normal-temperature normal-pressure gas transfer system intended to transfer only normal-temperature normal-pressure gas that is a gas at normal temperature and normal pressure, and a vapor-containing gas transfer system including the evaporation chamber downstream thereof. And including a vapor-containing gas flow system for feeding the vapor-containing gas,
A vapor deposition apparatus in which the room-temperature and normal-pressure gas flow system includes a mass flow controller (MFC), and further includes a backflow prevention valve that is automatically closed downstream of the MFC based on the pressure downstream thereof.   The vapor deposition apparatus according to claim 1, wherein the room temperature and normal pressure gas flow system further includes a material collecting mechanism that collects the thin film forming material downstream of the MFC. The vapor deposition apparatus according to claim 2, wherein the material collecting mechanism collects the material by a cooling member that can be cooled, and the cooling member diffuses the thin film forming material by heating.   The vapor deposition apparatus according to any one of claims 1 to 3, wherein the normal temperature and normal pressure gas flow system further includes a gas heating mechanism downstream of the MFC for heating the normal temperature pressure gas.   In order to heat the room temperature and pressure gas, the room temperature and normal pressure gas delivery system further sequentially collects the thin film forming material in the downstream side from the MFC (373). The vapor deposition apparatus according to claim 4, further comprising a gas heating mechanism (362) according to claim 4 and the backflow prevention valve (395). The normal temperature and normal pressure gas flow system, from the downstream side of the backflow prevention valve, without passing through the vapor-containing gas flow system, can be exhausted by the exhaust system, and
The vapor deposition apparatus according to any one of claims 1 to 5, wherein the vapor-containing gas flow system can be exhausted from the downstream side of the vaporization chamber by the exhaust system without going through the film forming chamber. The evaporation device further includes a material supply system for supplying the thin film forming material to the evaporation chamber,
The material supply system includes a material storage container, and a material discharge unit that receives the thin film formation material from the material storage container and supplies the thin film formation material to the evaporation chamber by discharging. The vapor deposition device according to any one of to 6.   The evaporation chamber is capable of introducing a heated carrier gas from the gas supply system, and the thin film forming material supplied as a powder by the discharge is flash-evaporated by the heated carrier gas to produce a powder. The vapor deposition apparatus according to claim 7, wherein the vaporization is performed in a state where the vapor does not stay as a body on the bottom of the evaporation chamber.

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