WO2007034790A1 - 成膜装置、蒸発治具、及び、測定方法 - Google Patents
成膜装置、蒸発治具、及び、測定方法 Download PDFInfo
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- WO2007034790A1 WO2007034790A1 PCT/JP2006/318530 JP2006318530W WO2007034790A1 WO 2007034790 A1 WO2007034790 A1 WO 2007034790A1 JP 2006318530 W JP2006318530 W JP 2006318530W WO 2007034790 A1 WO2007034790 A1 WO 2007034790A1
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- raw material
- organic
- film forming
- evaporation
- carrier gas
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/246—Replenishment of source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
Definitions
- the present invention relates to a film forming apparatus for forming a layer of a predetermined material, and a jig used in the film forming apparatus.
- the present invention relates to a measurement method using a jig, and more particularly to a film forming apparatus that vaporizes a raw material of a predetermined material to form a predetermined material layer, a jig used in the film forming apparatus, and a measurement method using the jig Is.
- a method of forming a predetermined material layer by vaporizing a raw material of a predetermined material is widely used in the manufacture of semiconductor devices, flat panel display devices, and other electronic devices.
- an organic EL display device will be described below as an example.
- Organic EL display devices with sufficiently bright brightness and a lifetime of more than tens of thousands of hours use organic EL elements that are self-luminous elements, and can be made thin because there are few peripheral parts such as backlights. Ideal as.
- the organic EL elements constituting such an organic EL display device have a long element life while having a large screen, the light emission luminance and the element life in the screen. It is required that there is no variation and that there are no defects typified by dark spots. In order to meet these requirements, organic EL film deposition technology is extremely important.
- Patent Document 1 Japanese Patent Laid-Open No. 2004-79904. It has been.
- the film forming apparatus disclosed in Patent Document 1 distributes the source gas uniformly along with the carrier gas on the substrate by optimally arranging the piping configuration inside the injector installed in the apparatus in a tree shape, thereby forming a film on a large substrate. This is to ensure the uniformity of the thickness.
- the proposed film forming apparatus connects two raw material containers for evaporating and vaporizing the same organic EL raw material, a blowing container for blowing the organic EL raw material on the substrate, and these raw material containers and the blowing container. And a piping system (that is, a distribution channel).
- the piping system including a plurality of valves and orifices is switched before the film formation is started, at the time of film formation, and when the film formation is stopped. At the same time, it controls the temperature of the piping system.
- the gas remaining in the piping system is quickly discharged during a time other than the time of film formation, and the gas is circulated to the other raw material container.
- the film forming apparatus shown in the prior application 1 it is possible to prevent contamination by the gas remaining in the piping system, and to quickly change the state before the start of film formation, at the time of film formation, and at the time of film formation stop. It can be carried out. Since the film forming apparatus according to the prior application 1 can prevent contamination by the organic EL raw material remaining in the piping system, the brightness and life of the organic EL apparatus can be remarkably improved.
- the vaporized organic EL raw material is blown into one raw material container force at the time of film formation.
- the raw material containers are vaporized to the outside and the organic EL raw materials are discharged.
- the organic EL raw material is only effectively used only at the time of film formation, and since it is not used effectively for a time other than at the time of film formation, there is a disadvantage that the utilization efficiency of the organic EL raw material to be used is poor. It was found.
- the organic EL device to be formed is an organic EL device having a long lifetime of 10,000 hours or more and a luminous efficiency of lOOlmZW or more. Further, the structure of the organic EL device according to the present invention can be roughly described.
- the organic EL device is formed by an anode formed of a transparent conductive film on a glass substrate and LiZAg provided so as to face the anode. And a structure in which seven or five organic layers are arranged between the anode and the cathode.
- the organic layer is formed of, for example, an electron injection layer, an electron transport layer, a light emitting layer, a hole transport layer, and a hole injection layer from the cathode side.
- the light-emitting layer, green light-emitting layer, and blue light-emitting layer are composed of a red light-emitting layer, a green light-emitting layer, and a blue light-emitting layer. Can emit light.
- the red light emitting layer, the green light emitting layer, and the blue light emitting layer forming the light emitting layer each have a thickness of about 20 nm, and the electron transport layer and the hole.
- the transport layer is also about 50 nm thick.
- the organic layer of the organic EL device is extremely thin as compared with the thicknesses of various films of other semiconductor devices. In the future, an attempt to further reduce these organic layers is being attempted. In this case, since the contamination of the organic layer is not allowed for the formation of the organic layer, the ultra-fine technology that forms the raw material of the organic layer in the molecular unit is necessary for depositing and forming an extremely thin organic layer with high accuracy. Is essential.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2004-79904
- organic EL raw materials generally have the property that even when they are in liquid form, their heat conductivity is low and heat is not easily transmitted.
- liquid organic EL raw materials do not have a very low viscosity, but when the temperature is increased for vaporization, the viscosity decreases with increasing temperature, and thermal convection tends to occur.
- the prior application 1 uses an evaporation jig equipped with an evaporating dish. While using the conventional evaporating dish As a result, it was found that there was a limit to the characteristics of the organic EL device that could be achieved, and it was not possible to obtain an organic EL device with the target characteristics described above.
- the temperature of the liquid organic EL raw material varies depending on the position of the liquid raw material in the evaporating dish. This results in temperature distribution or temperature spots. Since the amount of vaporization from the evaporating dish changes sensitively with temperature, this is also considered to be one reason why a uniform concentration (evaporation amount) cannot be maintained.
- An object of the present invention is to provide a film forming apparatus capable of controlling and laminating a film necessary for a display device in a molecular unit, such as a large organic EL device exceeding 20 inches.
- Another object of the present invention is to provide a jig suitable for depositing an organic EL raw material.
- Still another object of the present invention is to provide a measurement method for measuring the concentration of an organic EL raw material in a carrier gas using the above-described jig.
- Another object of the present invention is to provide a measurement method capable of identifying an unknown organic EL raw material.
- the film forming apparatus for vaporizing the raw material by the vaporizing means, supplying the vaporized raw material onto the substrate, and forming a film of the predetermined material on the substrate!
- the vaporization means has a container having an opening and a bottom surface, and the container has a partition member extending in a direction facing the bottom surface from the opening. Is obtained.
- the partition member is provided to continuously or partially cross the opening, and It is configured so that the space is continuous at the bottom or side of the cutting member, A film forming apparatus is obtained.
- the partition member does not cause thermal convection when the raw material is liquid and undergoes a vaporization treatment in the container. It is possible to obtain a film forming apparatus characterized in that the liquid surface is configured so as to have a uniform liquid surface.
- the supply of the carrier gas for transporting the vaporized raw material onto the substrate by V A film forming apparatus is further provided, characterized in that the concentration of the raw material in the carrier gas is constant.
- an evaporation jig used for vaporizing a filled raw material has a bottom surface and a side surface standing from the bottom surface, and the bottom surface and the side surface Therefore, it is provided with vaporization J1 in which the opening and the raw material storage space are defined, and a partition member that is accommodated in the raw material storage space and extends in a direction facing the bottom force and the bottom surface.
- An evaporation jig characterized by the following can be obtained.
- the evaporation jig according to the fifth aspect, wherein the partition member is provided so as to continuously or partially cross the opening, and the partition A vaporizing jig is obtained in which the space is configured to be continuous with the bottom or side of the mounting member.
- a seventh aspect of the present invention in the evaporation jig according to the fifth aspect, at least a part of the bottom of the partition member is in contact with the bottom surface, and communicates with the vicinity of the bottom surface.
- An evaporation jig characterized by having holes is obtained.
- the opening is a rectangle having a long side and a short side
- the raw material storage space is
- the partition member includes a long side direction partition piece extending in the long side direction and a short side direction partition piece extending in the short side direction.
- the organic raw material is accommodated and evaporated in the evaporation jig according to any of the fifth to eighth aspects, and the vaporized organic raw material is transported by the carrier gas.
- a film forming method characterized in that the organic material film is deposited on a substrate.
- the organic raw material is accommodated in the evaporation jig according to any of the fifth to eighth aspects and vaporized, and the vaporized organic raw material is transported by the carrier gas.
- a measurement method for measuring the concentration of the vaporized organic raw material in the carrier gas can be obtained.
- the activation energy obtained by the measurement method according to the eleventh aspect, the measured concentration, and the temperature of the raw material are determined.
- Formula (1) defining the concentration V (%) of the vaporized organic raw material in
- V (Ko / P) X e " Ea / kT
- the thirteenth aspect of the present invention there is obtained a measurement method characterized by estimating the organic raw material from the calculation result of the constant Ko obtained by the measurement method according to the twelfth aspect.
- the organic raw material is a raw material of an organic electoluminescence device. A measurement method is obtained.
- a raw material for forming a film of a predetermined material is vaporized, and the vaporized raw material is supplied onto a substrate to form the film of the predetermined material on the substrate.
- the vaporization means for vaporizing the raw material has a heat-resistant container having an opening of a predetermined area at one end and containing the liquid raw material therein, and the opening of the container is smaller than the predetermined area Dividing the partial space into a partial space having a plurality of small areas, wherein the dividing means divides the partial space in at least one of a portion that continuously or partially crosses the opening and a bottom surface portion or the opening of the container.
- the evaporation jig used for vaporizing the filled liquid raw material includes a bottom surface and a side surface on which the bottom surface force is also erected, and is opened inside the side surface.
- the partition plate includes the plurality of partial spaces on the bottom side of the vaporizing plate. Hold on the vaporizing dish to communicate!
- An evaporative jig characterized by squeezing is obtained.
- the vaporizing dish defines a rectangular or square opening-shaped raw material storage space having a predetermined length, width, and depth.
- the partition plate includes a partition piece extending in a length direction of the vaporization J1 and a partition piece extending in a width direction of the vaporization J1, and the partition piece is lower than a depth of the raw material storage space.
- An evaporation jig characterized by having a thickness is obtained.
- the side surface has a structure for preventing the liquid raw material from rising and rising at the upper part. An evaporation jig is obtained.
- an evaporation jig according to the sixteenth aspect, wherein the partial space is configured to form a polygon when viewed from the force at the top of the opening.
- the evaporation jig used for vaporizing the filled liquid raw material includes a bottom surface and a side surface on which the bottom force is also erected, and is opened inside the side surface.
- An evaporation jig characterized by being held in the vaporizing dish so that a plurality of partial spaces communicate with each other in the parallel direction is obtained.
- a liquid raw material is accommodated in the evaporation jig according to any of the sixteenth to twentieth aspects and vaporized, and the vaporized raw material is transported by a carrier gas,
- a film forming method characterized in that the film of the raw material is deposited on a substrate.
- the liquid raw material is accommodated in the evaporation jig according to any of the sixteenth to twentieth aspects and evaporated under reduced pressure, and the evaporated raw material is supplied to the evaporation jig. Is deposited on the lower surface of the substrate disposed above the substrate.
- the evaporation jig according to any of the sixteenth to twentieth aspects further comprises means for heating the vaporizing dish. Is obtained.
- the evaporation jig according to any one of the sixteenth to twentieth aspects and the twenty-third aspect further includes means for heating the partition plate. An evaporation jig is obtained.
- the evaporation jig according to the twenty-third or twenty-fourth aspect, wherein the heating means includes a heat pipe.
- the evaporation jig according to any of the sixteenth to twentieth aspects further includes means for supplying a carrier gas to the vaporizing dish. An evaporation jig is obtained.
- the evaporation jig according to the twenty-sixth aspect wherein the carrier gas is supplied through a filter.
- the opening of the evaporation dish (vaporization dish) is preferably 5 mm or less, more preferably 3 mm or less, for example, 2.5 mm ⁇ 2.5 mm, by the partition member (partition plate).
- the bottom of the partition plate is, for example, 1 to 2 mm for a liquid depth of 5 mm, and 0.5 to 1 mm for a liquid depth of 3 mm (in this case, for example, a container depth of 5 mm, (4mm), the liquid level of each divided area (each small opening) becomes uniform. Accordingly, since a uniform liquid level can always be maintained as a whole, the amount of vaporization and thus the concentration in the carrier gas can be made uniform over time.
- the partition plate by making the partition plate with a material having good heat conduction, and by adding a heating means such as a heat pipe or a heater to the inside of the partition plate, an area (small opening) surrounded by the partition plate is provided.
- the temperature of the liquid can be kept constant regardless of location and time. Spots are no longer produced. Therefore, by using the evaporation jig according to the present invention, the evaporation amount and concentration of the liquid raw material can be made constant over time.
- FIG. 1 is a schematic configuration diagram showing a film forming apparatus according to a first embodiment of the present invention.
- FIG. 2 is a schematic configuration diagram showing a film forming apparatus according to a second embodiment of the present invention.
- FIG. 3 is a diagram for more specifically explaining a piping system, a switch, and a film forming section of the film forming apparatus shown in FIG. 1 and FIG.
- FIG. 4 is a view showing a part of a film forming apparatus according to a third embodiment of the present invention.
- FIG. 5 is a diagram showing a film forming unit of the film forming apparatus shown in FIG.
- FIG. 6 is a timing chart showing switching timing and the like in the film forming apparatus of FIG.
- FIG. 7 is a perspective view showing an example of an evaporating dish constituting the evaporating jig according to the first embodiment of the present invention.
- FIG. 8 is a perspective view showing a partition plate constituting the evaporation jig according to the first embodiment of the present invention.
- FIG. 9 is a cross-sectional view showing the relationship between the partition plate of the evaporation jig and the evaporation dish according to the first embodiment of the present invention.
- FIG. 10 is a plan view for explaining an evaporation jig according to the first embodiment of the present invention.
- FIG. 11 (a) is a diagram for explaining each part of the evaporation jig according to the second embodiment of the present invention.
- FIG. 11 (b) is a cross-sectional view taken along line AA ′ of FIG. 11 (a).
- FIG. 11 (c) is a cross-sectional view taken along BB ′ of FIG. 11 (a).
- FIG. 11 (d) is a cross-sectional view along CC ′ of FIG. 11 (a).
- FIG. 11 (e) is a cross-sectional view taken along the line DD ′ of FIG. 11 (a).
- FIG. 11 (D) is a diagram for explaining a modification of the upper end portion of the plate member shown in FIG. 11 (b) and FIG. 11 (e).
- FIG. 12 is a cross-sectional view for explaining an evaporation jig according to a third embodiment of the present invention. 13]
- FIG. 13 shows the characteristics when using the evaporation jig according to the first, second, and third embodiments of the present invention.
- the organic EL raw material H material in the carrier gas
- FIG. 14 shows the characteristics when using the evaporation jig according to the first, second, and third examples of the present invention.
- the organic EL raw material H It is a figure which shows the pressure dependence of a material) density
- FIG. 15 is a view for explaining an evaporation jig according to a fourth embodiment of the present invention.
- FIG. 16 is a diagram illustrating an application example of the evaporation jig according to the present invention.
- ⁇ 19] is a diagram showing the pressure dependence of the evaporation behavior of the organic EL raw material (H material) when the evaporation jig according to the present invention is used. Here, the pressure dependence when the temperature is kept constant is shown. Is shown.
- the illustrated film forming apparatus includes an organic EL source unit 20 having a plurality of organic EL sources, first and second film forming units 26 and 27, and vaporized organic EL material from the organic EL source unit 20. choose And a switching unit 29 (switching means) for supplying to the first or second film forming unit 26, 27.
- the switching unit 29 is a pipe, an orifice, a mass controller (flow control system), a plurality of valves, etc. It is constituted by.
- the switching unit 29 is controlled by a valve, an orifice, a flow control system, and a control device (not shown) that controls the valve.
- the illustrated organic EL source section 20 includes a container section (hereinafter referred to as a raw material container section) containing organic EL raw materials corresponding to the number of organic EL films to be deposited.
- a container section hereinafter referred to as a raw material container section
- the organic EL source unit 20 includes three raw material container portions each containing the three types of organic EL raw materials.
- a raw material container section containing organic EL raw materials corresponding to the number of the raw materials is provided.
- the organic EL film to be deposited is composed of six layers: an electron transport layer, a red light-emitting layer, a green light-emitting layer, a blue light-emitting layer, an electron blocking layer, and a hole transport layer
- Six raw material container parts containing raw materials are provided in the organic EL source part 20.
- each raw material container 201 of each organic EL source unit 20 simply contains an organic EL raw material and evaporates an organic EL raw material using an evaporating jig (ie, an evaporating dish).
- a heater for heating the organic EL raw material is provided.
- a carrier gas such as argon, xenon, or krypton is introduced into the evaporation jig of each raw material container unit 201 via a nobleb, a flow control system, and a piping system.
- each raw material container section 201 has a function as a vaporizing means for vaporizing the organic EL raw material.
- the organic EL source section 20 includes other organic EL raw materials.
- Corresponding raw material containers are provided. In this way, each raw material container section operates as a vaporizing means for vaporizing the organic EL raw material.
- the switching unit 29 is provided corresponding to the illustrated raw material container unit 201, and a similar switching unit is also provided in the other raw material container unit. Omitted for Has been.
- the switching unit 29 is connected to a carrier gas piping system 31 (piping, valves, flow control system, orifice, etc.) that supplies the same type of gas as the carrier gas such as argon, xenon, krypton, etc. to the switching device 29.
- the carrier gas piping system 31 is connected to each of the first and second film forming units 26 and 27 one by one.
- This carrier gas piping system 31 is a carrier gas supply means for supplying the carrier gas to the gas discharge means via the vaporization means.
- the illustrated switching unit 29 includes a piping system including piping, valves, orifices, a flow control system, and the like inside thereof, and selectively selects the first and second carrier gas and vaporized organic EL raw material. Supplied to deposition units 26 and 27.
- the first and second film forming units 26 and 27 have the same configuration, and, as will be described later, the piping systems 331 and 332 having portions having the same piping path length. It is connected to the switch 29 via The illustrated first and second film forming units 26 and 27 will be described assuming that the organic EL material vaporized in the illustrated material container unit 201 is blown out and deposited. However, when depositing a plurality of organic EL raw materials in the first and second film forming units 26 and 27, respectively, between the plurality of raw material container units and the first and second film forming units 26 and 27, respectively. It is necessary to provide a plurality of switches and install a piping system (gas flow path) for connecting the plurality of raw material container parts to the first and second film forming parts 26 and 27 via these switches. is there.
- Each of the first and second film forming units 26 and 27 has a fixed temperature and a blowing container configured to uniformly blow the carrier gas containing the vaporized organic EL material onto the glass substrate.
- a transport device that transports the glass substrate on the stage held in a stage, and discharges the carrier gas containing the evaporated organic EL material onto the glass substrate and deposits the organic EL film. Therefore, the blowing container can be called a gas releasing means.
- the illustrated film forming apparatus includes a plurality of gas releasing means for one vaporizing means.
- the blowout container has a supply port arranged so that the organic EL raw materials from the piping systems 331 and 332 are uniformly dispersed, and a filter that leads to a glass substrate or the like from the supply port. ⁇ .
- the filter may be replaced with a shower plate in which fine holes are formed in a ceramic or metal plate.
- the organic EL raw material from the raw material container unit 201 is vaporized together with the carrier gas through the piping system of the switching unit 29.
- it is supplied to the first film forming unit 26 via the piping system 331.
- the organic EL raw material is being supplied to the first film forming unit 26
- the piping system 332 connected to the second film forming unit 27 is closed.
- film formation is being performed in the first film formation unit 26
- a glass substrate is supplied to the entrance of the second film formation unit 27, and a film formation standby state is entered.
- the switching of the piping system by the switch 29 causes the organic EL material from the material container unit 201 to pass through the piping system 332 for the second time. Supplied to the film forming section 27. While film formation is being performed in the second film formation unit 27, the glass substrate after film formation in the first film formation unit 26 is used to form another organic EL raw material by the transfer device. Guided to another blowing container provided in the first film forming section 26, another organic EL raw material is formed. In other words, different substrates are supplied at different timings to the plurality of gas releasing means corresponding to one vaporization means.
- the first and second film forming units 26 and 27 are controlled to be switched with each other at the timing determined by the switch 29, and the deposited organic EL materials are sequentially switched.
- the organic EL film required for the organic EL device is deposited on a glass substrate that flows in parallel.
- the piping system 332 between the switch 29 and the second film forming unit 27 has a length equal to that of the piping system 331 between the switch 29 and the first film forming unit 26.
- the piping tree is configured so that film formation is performed under the same conditions.
- the piping systems 331 and 332 are controlled so that the organic EL raw material is supplied to the first and second film forming units 26 and 27 at the same flow rate. As a result, in the first and second film forming units 26 and 27, the same organic EL raw material is selectively formed under the same conditions.
- the film forming apparatus shown in FIG. 1 can simultaneously form organic EL raw material films on a plurality of glass substrates simultaneously and in parallel, and can use as much as 201 organic EL raw material materials without waste, Use efficiency of OLED raw materials can be greatly improved.
- FIG. 2 there is shown a conceptual diagram of a film forming apparatus according to the second aspect of the present invention.
- the organic EL raw material from the organic EL source unit 20 is switched to 29, it is supplied to only three film forming units 26 and 27 in that it is individually supplied to three film forming units, that is, the first to third film forming units 26 to 28.
- the third film forming unit is connected to the switch 29 via the piping system 333, and the piping system 333 is controlled in the same manner as the other piping systems 331 and 332.
- the vaporized organic EL raw material from each raw material container part 201 is selectively supplied via the switch 29 to the first to third. Supplied to deposition units 26-28.
- FIG. 3 a part of the film forming apparatus shown in FIGS. 1 and 2 is shown.
- the organic EL source unit 20, the switch 29, and a single component are shown.
- a connection relationship with the film part 26 is shown together with a partial configuration in the film formation part 26.
- the film forming unit 26 shown in FIG. 3 includes a blowing container 261 that blows out a carrier gas containing organic EL raw materials (molecules) into the film forming unit 26 and a stage 262 that supports the glass substrate 30.
- 262 is assumed to be movable in a direction perpendicular to the paper surface of FIG. 3, for example, with the glass substrate 30 mounted.
- the blowout container 261 In the blowout container 261, six gas dispersion plates 263 are provided in this example, and a filter 264 made of metal or ceramic is installed at a position facing the glass substrate 30.
- the supply ports are provided in correspondence with the gas distribution plates, and both are arranged in a line in the same direction (the vertical direction on the paper surface in Fig. 3).
- the filter (or shower plate) has a shape extending in the arrangement direction of the supply port and the gas dispersion plate.
- the illustrated film forming unit 26 is maintained at a pressure of about 5 to 30 mTorr, and the stage 262 is maintained at room temperature.
- the filter 264 is preferably composed of porous ceramic.
- gas or liquid A fluid that also has a force can be uniformly supplied at a predetermined angle onto a large-area substrate.
- the illustrated organic EL source 20 is characterized by a single raw material container 201, and the illustrated raw material container 201 is connected to an upstream pipe and a downstream pipe.
- the upstream pipe is a pipe for introducing the carrier gas into the raw material container section 201.
- FCS1 flow control system
- V3 and V4 the flow control system
- the downstream piping constitutes part of the switch 29.
- the raw material container section 201 is divided into an upstream area and a downstream area by a partition wall 202 extending vertically, and an evaporation section 203 filled with an organic EL material is provided below the partition wall 202. ing. Further, as described above, the raw material container 201 is provided with a heater (not shown).
- the carrier gas introduced through the upstream pipe is led from the upstream region of the raw material container 201 into the evaporation unit 203, and is vaporized in the evaporation unit 203 by the heating by the heater ( Molecule) is led to the downstream piping through the downstream region of the raw material container 201 together with the carrier gas.
- a switch 29 is connected to the raw material container unit 201.
- the switch 29 shown in FIG. 3 includes a piping system for connecting a plurality of film forming units 26, 27, etc. and the organic EL source 20 (that is, the raw material container unit 201), and a carrier gas to the film forming unit 26. And a piping system to supply to
- the piping system of the switch 29 that connects the raw material container unit 201 and the blowing container 261 of the film forming unit 26 includes valves V5 and V6, and an orifice ORF1, and includes a blowing container 261.
- a carrier gas source (not shown) such as xenon, argon, etc. provided outside is directly blown out
- Two containers 261 A second piping system leading to the gas dispersion plate 263 is provided.
- the second piping system reaches the supply port corresponding to the gas distribution plate 263 of the blowing container 261 via the valve VI, the flow control system FCS2, and the orifice ORF2.
- a third piping system for introducing the same kind of gas as the carrier gas from the outside is connected between the orifice ORF1 of the first piping system and the valve V6.
- the third piping system is connected to the valve V2, F Includes low control system FCS3 and valve V7.
- a fourth piping system for supplying vaporized organic EL raw material to other film forming units for example, 27 in FIG. 1).
- the fourth piping system contains valve V8.
- an orifice ORF indicates a gas pressure adjusting unit for adjusting and controlling the gas pressure including the orifice and the knob. Therefore, a gas pressure adjusting part is provided between the vaporizing means and the blowing container, and the gas pressure adjusting part and the supply port of the blowing container are connected by a pipe.
- the length of the piping between the orifice ORF1 and the supply port of the blowing container 261 is set as follows. If all are the same, the organic EL raw material (molecular gas) can be supplied to reach the glass substrate 30 evenly and simultaneously.
- the number of the organic EL molecular gas supply ports in the blowing container 261 is 2 n , and these supply ports and the orifice 1 are connected to each other by 2 n piping. (N is a natural number).
- the same organic EL raw material film is uniformly formed under the same conditions in the plurality of film forming units. It can be formed into a film.
- the temperature of the first piping system from the raw material container section 201 to the blowing container 261 is set so that the organic EL raw material (molecules) does not precipitate and adsorb on the wall of the pipe forming the piping system.
- the temperature is set higher than the temperature of the raw material container 201 during supply.
- the operation of the film forming apparatus will be described with reference to FIG. 1 and FIG.
- the operation of the illustrated film forming apparatus can be divided into operations before the start of film formation, at the time of film formation, and at the time of film formation stop for each of the film forming units 26 and 27.
- the operations at the time of film formation and at the time of film formation stop are described as mode 1, mode 2, and mode 3, respectively.
- the valves VI, V2, V3, V4, and V7 are in the open state, the valve V6 is in the closed state, and the valves V5 and V8 are in the open state. . Therefore, in mode 1, the flow control system FCS1 and orifice ORF are controlled from the valve VI.
- the carrier gas is supplied to the blowout container 261 through the valve 2, while the carrier gas is supplied from the valve V 2 to the blowout container 261 through the flow control system FCS 3, the valve V 7, and the orifice ORF 1.
- the pressure in the blowing container 261 and the pressure on the glass substrate 30 are controlled to predetermined pressures. In this case, for example, the pressure in the blowing container 261 is controlled to lOTorr, and the pressure on the glass substrate is controlled to lmTorr.
- the carrier gas introduced into the raw material container 201 that supplies the organic EL molecules is the valve V3, the flow control system FCS1, and the valve
- the organic EL raw material is not supplied to the film forming unit 26 and is passed through the valves V5 and V8 in the open state, because the valve V6 is led to the raw material container 201 via the path V4 and the valve V6 is closed.
- Part (eg 27) Of course, in the mode before the start of film formation of the entire film forming apparatus, the nozzles V5 and V8 are also closed, and no organic EL raw material is given to either film forming part 26 or 27 from the raw material container part 201. Only the same type of carrier gas is provided by the piping system provided in both film forming sections.
- valves V2, V7, and V8 are closed, and valves VI, V3, V4, V5, and V6 are opened.
- the carrier gas is supplied to the upper and lower supply ports of the blowing container 261 via VI, the flow control system FCS2 and the orifice ORF2, and the organic EL molecular gas vaporized in the raw material container section 201 is supplied to the valve V3 and the flow control.
- the carrier gas introduced through the system FCS1 and valve V4, V5, V6, and the orifice ORF1 are supplied to the four supply ports of the discharge vessel 261.
- the same type of gas (flow rate fl) as the carrier gas supplied via the valve V2, the flow control system FCS3, the valve V7, and the orifice ORF1 is stopped.
- the carrier gas flow rate from the raw material container section 201 that supplies the organic EL molecules to the blowout container 261 is basically matched with the above flow rate fl. It is desirable.
- the transport gas flow rate in the path of the valves V5, V6, and the orifice ORF1 is supplied in the path of the valve V2, the flow control system FCS3, the solenoid V7, and the orifice ORF1 in mode 1. It is desirable to be equal to the flow rate fl of the same type of gas as the carrier gas! /
- mode 3 when the film formation is stopped will be described with respect to the first film formation unit 26.
- valve V6 is closed, valves V5 and V8 are opened, and at the same time, valves V2 and V7 are opened. That is, in mode 3, the NOROBE VI, V2, V3, V4, V5, V7, and V8 forces are opened, while the NOROBE V6 force is closed, and the organic EL raw material from the raw material container portion 201 is subjected to another film formation. Part (eg 27).
- FIG. 4 is a perspective view of a main part of a film forming apparatus system according to the third embodiment of the present invention.
- each of the film forming units 26 and 27 having two film forming units is provided with six blowing containers.
- FIG. 4 portions corresponding to the embodiment of FIGS. 1 and 3 are given the same reference numerals.
- the film forming unit will be described in detail in FIG.
- in the first film formation unit array (chamber CHM1) six blowing containers each extend so as to have a length equivalent to the width of the glass substrate, and the length direction thereof.
- the second film formation unit array (chamber CHM2) is configured in the same manner, and another glass substrate 30 is supplied onto the second film formation unit array (chamber CHM2) at a timing different from that on the first array, and the balloons arranged in the two arrays.
- the containers form a pair, and the same raw material container part is supplied with carrier gas containing raw materials at different timings.
- the carrier gas containing the raw material When the carrier gas containing the raw material is selectively supplied to one of the pair of blowing containers, a glass substrate exists on the carrier gas, and at that time, the carrier gas containing the raw material is supplied to the other blowing container of the pair. There is no glass substrate on it. Glass substrate supply and movement The carrier gas containing the raw material is always supplied to one of the pair, and a substrate is present on the pair of blowing container pairs. The timing is determined as follows.
- FIG. 5 a single film forming unit array (channel) of the film forming apparatus system according to the embodiment of FIG. 4 will be described.
- a single deposition unit array is shown that is used to produce an organic EL device by forming an organic EL film.
- six layers of films are deposited on the substrate.
- substrates of sizes from 730 X 920 (mm) force to 3000 X 5000 (mm) can be used.
- the illustrated film forming unit array includes six blowing containers 26-1 to 26-6 divided by partition walls 1 to 7, and the carrier gas containing the organic EL raw material is placed on the upper glass in the order of lamination. Blow out to the substrate.
- These six blowing containers 26-1 to 26-6 are arranged so that the extending directions of the internal filters or shower plates are parallel to each other.
- the glass substrates 30-1 and 30-2 are spaced at regular intervals, and the left force in the figure also advances to the right in the upper part of the six blowout containers.
- Each blowout section on each blowout container 26-1 to 26-6 An organic EL film is formed from the organic EL raw material ejected upward in the force diagram.
- a predetermined distance is maintained between the substrates 30-1, 30-2 and the partition and between the substrates 30-1, 30-2 and the blowing containers 26 1 to 26-6.
- the distance between the substrates 30-1 and 30-2 and the bulkhead is smaller than the distance between the substrates 30-1 and 30-2 and the blowing containers 26-1 to 26-6.
- the gas ejected upward in each blowing container force is exhausted downward as shown by an arrow through a gap between the side wall of the blowing container and the inner surface of the partition wall.
- a piping system as shown in Figs. 3 and 4 is connected to each blowing container. Therefore, the film forming unit array (chamber) shown in FIG. 5 is connected to other film forming unit arrays (chambers) (not shown) by respective piping systems.
- the dimensions of the glass substrates 30-1 and 30-2 are 2,160 mm ⁇ 2,540 mm, and proceed in the longitudinal direction.
- the width of the blowout port in the direction of movement of the glass substrate of the blowout container is 50 mm
- the length of the blowout port in the vertical direction is 2,170 mm.
- the width (thickness) of the side wall of the container is 15 mm
- the distance between the outer surface of the side wall of the blowing container and the inner surface of the partition walls on both sides is 30 mm
- the distance between the inner surfaces of the adjacent partition walls is 140 mm
- the thickness of the partition wall is 15 mm.
- the length of the deposition unit array (chamber) in the substrate traveling direction is 945 mm.
- the distance between the upper surface of the blowing container and the substrate was 20 mm, the distance between the partition wall and the substrate was 2 mm, and the temperatures of the partition wall and the blowing container were 350 to 450 ° C, respectively.
- the film forming atmosphere pressure is 30 mTorr, the blowing speed of the carrier gas containing the raw material blown out from the blowing portion is 3 mZsec, and the carrier gas containing the raw material reaches the substrate in 0.1 second.
- the flow rate of the carrier gas containing the raw material of the blower container is 317 ccZmin in terms of room temperature and atmospheric pressure, and the substrate feed rate is 1. OcmZsec.
- the time required for the substrate to pass through one blower container is 264 seconds.
- the time required for the substrate to pass through the six blowout containers is 341.5 seconds, and the usage efficiency of the organic EL material reaches 90%.
- the upper chart is a timing chart showing a cycle of switching between a pair of blowing containers arranged in two film formation unit arrays (chambers). Yes, the gas supply is switched every 264 seconds.
- the lower timing chart shows the cycle of operation in each chamber. In each chamber, six layers were formed in 341.5 seconds as described above, and then from that chamber in 186.5 seconds. The deposited substrate is delivered and a new substrate is introduced into the chamber, completing one cycle in a total of 528 seconds. This one cycle of 528 seconds (8 minutes 48 seconds) completes the 6-layer deposition on two substrates. In addition, 15.5 seconds later, open each ejection container of chamber C HM1, CHM2.
- blowing containers have the same structure, and the same piping system described with reference to FIG. 3 is connected to set the same carrier gas flow rate. .
- the temperature of each blowing container may be set according to the characteristics of the organic EL molecules. Further, it is desirable to control the film formation rate and thickness by the temperature of the raw material container.
- the blowing container is made of stainless steel, and the blowing part of the blowing container is made of a stainless steel filter and welded to the main body. Note that the entire inner surface of the blowing container is Al O
- the film deposition system uses the same flow rate of carrier gas in each film formation unit in both modes during film formation and when film formation is stopped, so the pressure in each blowing container constituting each film formation unit Can be kept constant. This means that cross-contamination between blowing containers can be prevented.
- the desired film thickness of each layer is the same (red light emitting layer 'green light emitting layer' blue light emitting layer '
- the electron blocking layer has a film thickness of 20 ⁇ : LOnm)
- the organic EL source molecule concentration in the carrier gas may be the same, but the layer with a large film thickness (the electron transport layer is the hole transport layer and the film thickness is For 50 nm), it is necessary to increase the concentration of organic raw material molecules contained in the carrier gas in proportion to the film thickness. If this is difficult, it is necessary to take measures to increase the thickness of the layer, such as using multiple blowing containers, increasing the opening width of the blowing container, or increasing the carrier gas flow rate.
- a plurality of film forming units are provided, and a plurality of films necessary for the organic EL device are rapidly formed by switching the modes of the plurality of film forming units over time.
- the throughput can be greatly improved and the utilization efficiency of the organic EL materials can be improved.
- the organic EL device when an organic EL device is manufactured by switching 6 layers of organic EL raw material films by switching between three film forming units, the organic EL device can be manufactured at intervals of about 6 minutes.
- the utilization efficiency of EL raw materials was improved to 82%.
- Figs. 4-6 when using two array arrays, six layers can be deposited at intervals of about 8 minutes, and the material utilization efficiency reaches 90%.
- the concentrations of various organic EL raw materials in the carrier gas are short in time. It turned out to change drastically.
- a conventional organic EL raw material In the case of Alq3, the temperature of Alq3 in the carrier gas is measured by FT-IR (Absorption Spectroscopy) while maintaining a temperature of 760 Torr while flowing Ar at a flow rate of lOsccm as the carrier gas is heated to 380 ° C.
- the concentration reached a peak in about 20 minutes (with overshoot), and then it decreased rapidly.
- Such a rapid concentration change makes it difficult to deposit a uniform organic EL film on a molecular basis over a long period of time.
- the evaporating dish in this case had a semicircular cross section formed by breaking a cylindrical pipe closed at both ends.
- the evaporating dish 50 shown in FIG. 7 is composed of a rectangular container having a length (L) of 20 mm, a width (W) of 5 mm, and a height (D) of 5 mm. That is, the illustrated evaporating dish 50 has a bottom surface and side walls erected from the bottom surface in the long side (L) direction and the short side (W) direction, and has an opening for filling the inside with the organic EL material.
- a rectangular parallelepiped material storage space is defined.
- the opening of the evaporating dish 50 has a rectangular shape consisting of a long side and a short side.
- the evaporating dish 50 used in the experiment is a heat-resistant material, for example, a heat-resistant container formed of stainless steel, and serves as a vaporizing means for vaporizing the organic EL raw material.
- the present inventors diligently studied a method that can prevent thermal convection in the evaporating dish 50 and keep the temperature constant, and have developed extremely effective means.
- Ingredients Physically the effect of thermal convection can be reduced by dividing the space for filling the organic EL material inside the evaporating dish 50 into smaller spaces, and as a result, the concentration of the organic EL material in the carrier gas is prolonged. It has been found that it can be kept substantially constant over time. That is, by providing a partition plate (that is, a dividing means, a partition member) extending in the direction of the counter force in the opening force bottom surface of the evaporating dish 50 and dividing the filling space into partial spaces, as described later, The impact could be reduced.
- a partition plate that is, a dividing means, a partition member
- a partition plate 52 disposed in the evaporating dish 50 is shown as a means for preventing heat convection in the evaporating dish 50.
- the illustrated partition plate 52 is a partition plate (dividing means) that divides the internal space of the evaporating dish 50 illustrated in FIG.
- the illustrated partition plate 52 includes: A long side partition 521 having a height (H) lower than the depth (D) of the internal space, for example 3 mm (H), and four short sides having the same height as the long side partition A side partition piece 522 and a height (H) 4 mm locking piece 54 provided at both ends in the long side direction of the partition plate 52 to contact and support the partition plate 52 to the bottom of the evaporating dish 50 I have.
- the two locking pieces 54 shown in the figure extend in the opposite directions (rearward direction and forward direction in FIG. 8) of both ends of the long side direction cut piece 521 with respect to the short side direction of the evaporating dish 50. Yes.
- the locking piece 54 is provided so as to be higher than the long side direction partition piece 521 and the short side direction partition piece 522 and to protrude below the long side direction partition piece 521. Therefore, the illustrated partition plate 52 is arranged so that a gap 56 is formed between the long side direction partition piece 521 and the short side direction partition piece 522 and the bottom of the evaporating dish 50 as shown in FIG. Is done. In other words, there is a gap 56 between the bottom side end portions of the long side and short side direction partition pieces 521 and 522 that function as a partition member and the bottom portion of the evaporating dish 50, and this gap 56 is the same as that of the evaporating dish 50. A continuous space is formed along the bottom. As shown in FIG. 9, the liquid level 59 at the start of vaporization is lower than the partition plate.
- the partition plate 52 shown in Fig. 8 is arranged in the internal space of the evaporating dish 50, and the evaporating jig 55 is configured.
- the internal space of the evaporating dish 50 is divided into ten partial spaces (partial regions) by the partition plate 52.
- the illustrated evaporating jig 55 is in a state where each partial space is in communication at the bottom.
- a partition plate that is, a partition wall may be brought into contact with the bottom surface of the evaporating dish 50.
- a communication hole may be provided in the partition located in the vicinity of the bottom surface of the evaporating dish 50, or a communication hole may be provided in the bottom surface of the evaporating dish 50 located in the vicinity of the partition plate.
- FIG. 17 shows the change in organic EL material concentration C1 in the carrier gas when the evaporating dish 50 of the present invention provided with a partition plate is used.
- Ar is used as the carrier gas and an organic EL material known as the H material is used is shown.
- curve C1 shows that 200 mg of H material is charged into the evaporating dish 50 shown in Figure 10, held at a temperature of 250 ° C for 5 minutes, and then heated to 470 ° C (right scale).
- the H material concentration change (left scale) in the carrier gas is shown.
- the experiment was performed by placing an evaporating dish 50 in an organic EL raw material container maintained at a pressure of 75 Torr and supplying a carrier gas having a flow rate of lOsccm.
- the maximum concentration is obtained when 20 minutes have elapsed after heating, but this concentration began to decrease within 30 minutes.
- C1 can maintain a concentration of over 900 Oppm for over 100 minutes. In this way, a substantially constant concentration can be maintained over a long period of time.
- the H material vaporized by the evaporation jig of the present invention is supplied to the film forming unit at a constant concentration over a long period of time. It means you can do it. Therefore, by using the vapor deposition jig of the present invention, an extremely thin H material film can be uniformly formed over a long period of time.
- the temperature dependence of the evaporation behavior of the organic EL material (here, H material) is shown, and the pressure of the evaporation jig is kept constant (ie, 30 Torr).
- the temperature is 430 ° C
- the change in the concentration of the H material when it is changed in the range of ⁇ 450 ° C is shown.
- the evaporation jig according to the present invention is filled with 200 mg of H material, and the carrier gas is supplied at a flow rate of lOsccm. Curve C3 shown in Fig.
- Curve C4 shows a change in concentration when heated to 440 ° C while maintaining a pressure of 30 Torr. In this case, the concentration of 9000 ppm can be maintained for 2 hours or more.
- Curve C5 shows the change in concentration when heated to 450 ° C while maintaining a pressure of 30 Torr, a concentration of 13000 ppm can be achieved, and the organic EL material substantially filled with this concentration is substantially Therefore, it can be maintained until it is completely vaporized from the evaporation jig.
- the pressure-dependent characteristics of the evaporation behavior of the H material which is an organic EL material
- the evaporation jig according to the present invention is maintained at a temperature of 440 ° C., and Ar is supplied as a carrier gas to the evaporation jig at a flow rate of lOsccm.
- the evaporation jig is filled with 200 mg of H material, as in FIGS. 17 and 18.
- Curves C6, C7, and C8 show the evaporation characteristics of the H material with the evaporation jig maintained at 75 Torr, 30 Torr, and 20 Torr, respectively.
- the concentration of the H material in the carrier gas increases, and in any case, the concentration of the H material in the carrier gas substantially increases. Can be kept constant.
- FIG. 11 (a) shows a plan view of the evaporation jig 55 according to the second embodiment of the present invention.
- the evaporation tray 50 is a partition that forms a partition member. The board is divided into seven partial areas in the horizontal direction and nine partial areas in the vertical direction, for a total of 63 partial areas.
- FIG. 11 (a) is described as the short side direction of the evaporation jig 55
- the vertical direction in FIG. 11 (a) is described as the long side direction of the evaporation jig 55.
- FIG. 11 (b) which is a cross-sectional view taken along the line AA ′ of FIG. 11 (a)
- the evaporating dish 50 of the evaporating jig 55 is disposed inside.
- the dish member 62 is formed of a material having good thermal conductivity, excellent mechanical strength, and a low thermal expansion coefficient, such as Cu-W, Al-Mg-Zn, etc., and the inner surface is made of YO, AlO, carbon. Etc.
- the covering member 66 is made of a highly heat-insulating stainless steel or the like.
- the illustrated evaporating dish 50 includes a dish member 62, a heat pipe unit 64, a covering member 66, and a heat insulating member 68. Further, as shown, a heater 70 is provided at the bottom of the evaporating dish 50.
- a first partition 72 having a height that does not reach the bottom of the plate member 52 is provided to define the seven partial areas. Yes. Note that a heat pipe is not provided in the illustrated first partition 72.
- FIGS. 11 (c) and 11 (d) the second and third partitions 74 and 76 arranged along the lines B-B 'and C-C' in FIG. 11 (a). Is shown respectively.
- the second partition 74 is embedded with a heat pipe 741 that is lowered in the right direction in FIG. 11 (c).
- the third partition 76 shown in FIG. 11 (d) is embedded with a heat pipe 761 that decreases in the left direction. .
- the heat pipes 741 and 761 embedded in the second and third partition portions 74 and 76 are inclined so that the liquid flows inside. Is attached.
- the partition portions 74 and 76 having the right and left lower heat pipes 741 and 761 are alternately arranged in the dish member 52 of FIG. Therefore, the partition plate shown in FIG. 11 is configured by connecting the first to third partition portions 72, 74, and 76.
- each of the heat pipes 741 and 761 is coated with Y 2 O or the like so as not to cause a decomposition effect on the solvent by the catalyst.
- FIG. 11 (e) there is shown a cross section of the partition plate along the line D-D 'in Fig. 11 (a). As is apparent from the figure, the second and third partition portions are shown. 74 and 76 are alternately arranged, and these second and third partitions 74 and 76 are respectively provided with right-down and left-down The pipes 741 and 761 are buried!
- the second and third partition parts 74 and 76 are arranged in the dish member 62 so that the bottom part force of the dish member 62 also has a predetermined interval, that is, does not contact the bottom part of the dish member 62. Has been placed. Therefore, in this structure, each partial region defined by the first to third partition portions 72, 74, and 76 communicates with the bottom of the plate member 62, so that the organic EL material is liquefied. In this case, the surface of the liquefied organic EL material is kept constant in each partial region.
- the partition plate shown in FIGS. 11 (a) to 11 (e) is a first plate in which a heat pipe is not embedded as a spacer between the second and third partition portions 74 and 76. It can be easily created by interposing the partition 72.
- These first to third partition plates are formed of a material having good thermal conductivity, excellent mechanical strength, and a small thermal expansion coefficient, such as Cu-W, Al-Mg-Zn, etc.
- the outer surface is covered with YO, Al 2 O, carbon, etc.
- the partition plate shown in FIG. 11 has a thickness of 0.5 to 2 mm and forms a partial region having a size of 2 to 5 mm ⁇ 2 to 5 mm.
- the size of the pan member is 123 mm long, 72 mm short, 30 mm deep, and the second and third partitions (corresponding to 74 and 76 in Fig. 11) have a diameter of 2 mm.
- the heat pipe was embedded with a thickness of 3 mm, while the first partition (corresponding to 72) had a thickness of 2 mm.
- the partial area surrounded by the first to third partition parts 72, 74, and 76 is a rectangular shape of 5mm x 3mm (the space between the partition plates embedded in the heat pipe is 5mm), totaling 200 parts The region was arranged.
- FIG. 11 (f) there is shown a modification of the upper end portion of the plate member 62 shown in Figs. 11 (b) and 11 (e).
- the organic EL raw material was liquefied, it went up along the inner wall of the evaporating dish 50 and leaked to the outside.
- FIGS. 11 (b) and 11 (e) it is not necessary to bend the upper end portion of the dish member 62 to the inside of the evaporating dish 50.
- Some EL raw materials were observed to be insufficient.
- the upper end of the dish member 62 is simply bent to the inside of the evaporating dish 50 as shown in Fig. 11 (f).
- an evaporating jig (also referred to as an evaporating vessel) 55 according to another embodiment of the present invention will be described.
- the illustrated evaporation jig 55 has a structure suitable for flowing a carrier gas uniformly. More specifically, the illustrated evaporating jig 55 includes an evaporating dish 50 having a short side direction and a long side direction as described in connection with FIG. And a partition 72 arranged. As is clear from this, FIG. 12 shows a cross section in the short side direction of the evaporating dish 50, as in FIG. 11 (b).
- the partition 72 is configured not to contact the bottom of the evaporating dish 50, and as a result, the partial area defined by the partition 72 is communicated with the bottom of the evaporating dish 50.
- the illustrated evaporation tray 50 includes the plate member 62, the heat pipe unit 64, the covering member 66, the heat insulating member 68, and the heater 70, and the evaporation illustrated in FIG. Same as a dish.
- the illustrated evaporation jig 55 is provided with an upstream filter portion 82 provided on the upstream side in the short axis direction and a downstream filter portion 84 provided on the downstream side in the short axis direction.
- the upstream filter section 82 and the downstream filter section 84 are formed of Al 2 O 3.
- a slit-shaped filter is provided.
- the upstream filter unit 82 is coupled to a carrier gas supply source via a valve Val, a flow control system (FCSa), and a valve Va2, while the downstream filter unit 84 is coupled to a blowing container. Yes.
- a carrier gas is caused to flow in the short side direction of the illustrated evaporation jig (evaporation vessel) 55.
- the upstream filter section 82 and the downstream filter section 84 operate as a carrier gas supply means for transporting the raw material evaporated and vaporized by the evaporation jig 55 onto a substrate (not shown).
- the gas pressure in the evaporation container is maintained at about 20 Torr, and the gas discharged from the downstream filter unit 84 to the blowout container is maintained at a pressure higher than lOTorr and supplied at a gas flow rate of lOccZmm. Is done.
- the pressure drop in the upstream filter section 82 and the downstream filter section 84 is adjusted to be 700 Torr and lOTorr or less (preferably 5 Torr), respectively!
- the evaporating dish 50 has a width of 10 cm or 20 cm in the long side direction, if the gas of lOccZmin is flowed at a width of 5 mm, the total gas flow rate is 200 ccZmin or 400 ccZ min. Become.
- a baffle plate 83 is installed inside the gas supply port so that the gas flows uniformly. It was.
- the concentration determined by temperature can be maintained almost constant over a long period of time.
- the evaporation characteristic of the H material increases as the pressure decreases, and the concentration of the H material in the carrier gas increases. At any pressure, the concentration of the H material in the carrier gas can be kept substantially constant.
- FIG. 13 the relationship between the concentration of H material and the pressure when the temperature of the evaporation jig 55 shown in FIGS. 7 to 10, 11, and 12 is kept constant is shown.
- Fig. 13 shows Torr on the upper scale and lZP (lZTorr) on the lower scale.
- characteristic C9 represents the relationship between the pressure when H material is heated to 430 ° C and the concentration of H material in the carrier gas.
- characteristics C10 and C11 are 440 ° C and 460 °, respectively.
- C shows the characteristics when H material is heated.
- the slopes of the characteristics C12 to C14 represent the activation energy Ea in constant pressure states of lOTorr, 20 Torr, and 30 Torr, respectively. 1. 893 eV, 1. 894 eV, and 1. 892 eV.
- the evaporation amount of the H material that is, the concentration of the H material can be expressed by the following equation (1).
- V (%) (Ko / P) X e " Ea / kT (1)
- Ko is a constant (% 'Torr)
- P is the pressure (Torr)
- Ea is active I spoon energy (eV).
- Tables 1, 2, and 3 show lOccZmin at pressures of 10, 20, and 30 Torr, respectively.
- FIG. 15 there is shown an evaporation jig 55 according to a fourth embodiment of the present invention.
- the solid organic EL raw material is filled and melted by heating to become a liquid state.
- the organic EL raw material is unavoidably exposed to air, so the quality of the solid organic EL raw material may deteriorate due to oxidation or the like. It is done.
- liquefaction container 86 has a configuration in which a liquefaction container 86 is connected to an evaporation jig 55.
- the illustrated liquid container 86 has an inclined bottom surface and is connected to the evaporation jig 55 via a pipe 87 having a valve VL. Further, the liquefaction vessel 86 is provided with a heater for heating the solid organic EL raw material filled therein.
- the solid organic EL material is filled. Subsequently, the solid organic EL raw material is baked in the liquid vessel 86 while flowing Ta or Ar from atmospheric pressure.
- the temperature of the liquefaction vessel 86 is slowly increased under atmospheric pressure, and the organic EL raw material is liquefied at, for example, 250 ° C.
- the valve VL is opened, and the liquid organic EL raw material evaporates from the liquid container 86 due to its own weight via the pipe 87 attached near the bottom of the liquid container 86. Filled with ingredient 55. If the viscosity of the liquid organic EL raw material is large and difficult to flow, it can be avoided to pressurize it with gas and push the liquid organic EL raw material from the liquefaction vessel 86 to the evaporation jig 55.
- the liquid organic EL raw material can be filled with 55 liters of an evaporation jig that does not contact the liquid organic EL raw material with air.
- a partition plate is provided in the liquefaction vessel 86 in the same manner as the evaporation vessel 55, so that the organic EL raw material is supplied. It is also possible to employ a configuration in which heating is performed uniformly.
- the evaporation jig 55 is used in the film forming apparatus shown in FIGS. 1 to 6 has been described.
- the evaporation jig according to the present invention is limited to this. It can be applied to other types of film forming equipment.
- the evaporation jig according to the present invention is vaporized. It can be similarly applied as a means.
- the evaporation jig according to the present invention is a blowout that blows out a carrier gas containing a vaporized raw material as a film forming portion toward the substrate as described in FIGS. 1 to 6 and Prior Application 1. It can be used to supply the vaporized raw material in the carrier gas to other film forming mechanisms such as a plasma apparatus using microwave excitation as well as a structure.
- the evaporation jig according to the present invention can be used as a vapor deposition jig in a vapor deposition apparatus.
- FIG. 16 there is shown an example in which the evaporation jig 55 of the present invention is applied to a vapor deposition apparatus (that is, a vacuum vapor deposition apparatus).
- the illustrated vapor deposition apparatus includes the vapor deposition jig 55 of the present invention and a substrate 30 (for example, a glass substrate) mounted in a face-down manner on the stage 262 so as to face the vapor deposition jig 55. is doing.
- the evaporation jig 55 shown in the figure is similar to the evaporation jig 55 shown in FIG. 11.
- the plate member 62, the heat pipe unit 64, the covering member 66 that covers the heat pipe 64, and the covering member 66 It is comprised by the heat insulation member 68 provided in the outer periphery. Furthermore, the distance di between the substrate 30 and the upper end of the evaporation jig 55 is set to 3 to 20 cm (for example, 5 cm).
- an organic EL material having an average free path of about 10 m at 10 _4 Torr is deposited on the substrate mounted on the stage 262 in a face-down state (with the film formation side down).
- the organic EL raw material is filled in the evaporation jig 55 through the pipe 87 with a liquefied container force (not shown).
- the substrate 30 is mounted on the stage 262 while maintaining a temperature of 100 ° C.
- Such an evaporation apparatus can also be suitably applied to film formation of metallic lithium (Li) having a low vapor pressure, which is not merely a film formation of an organic EL material.
- Li melting point 179 ° C Li is heated to 200-250 ° C in the evaporation jig 55 while vapor deposition is performed by reducing the pressure to 1 X 10 _5 Torr in an Ar atmosphere, and the Ar atmosphere pressure is set to lOTorr. Can be stopped. If the evaporation jig 55 of the present invention is used, the evaporation amount is evaporated uniformly over time in a large area, so that vapor deposition with a uniform thickness can be performed even on different substrates. It can be carried out.
- the present invention can be applied to organic EL film formation to obtain a high-quality organic EL device. Furthermore, the present invention can also be applied to film formation for various display devices and the like that require high quality and long life as well as film formation for organic EL. Furthermore, in the above-described embodiments, the case where the planar shape of the small opening of the evaporation jig is a rectangle has been described. However, the shape is not limited to a rectangle, but a square, a regular triangle, a regular pentagon, a regular hexagon, a regular octagon, and other polygons.
- the partition plate is not limited to a plate shape as long as it has a structure capable of preventing thermal convection, and may have another shape such as a corrugated plate shape, a rod shape, or a mesh shape.
- the structure can prevent thermal convection. It ’s okay. In this case, the communication structure at the bottom can be omitted.
- the structure can prevent thermal convection. There is no problem.
- the evaporation vessel itself and the partition plate or column are made of material with good heat conduction, and those surfaces that come into contact with the molten liquid should be surfaces with less catalytic effect on the organic EL material. preferable.
- the surface having little catalytic effect include a passive film such as alumina yttria, carbon, and fluorocarbon.
- the shape of the container is preferably such that the evaporation area does not vary even when the liquid level drops.
- the inner surface is vertical, such as a cube, a rectangular parallelepiped, a cylinder, or a polygonal column.
- the partitioning member should have a configuration in which the evaporation area does not change even when the liquid level drops.
- the amount of evaporation is sensitive to pressure and temperature, it is necessary to strictly control the pressure and temperature to be constant.
- the carrier gas is supplied to the liquid surface so that the temperature and flow rate are constant. Therefore, it is preferable to provide a filter such as a slit filter at the entrance and exit of the evaporation container.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroluminescent Light Sources (AREA)
- Physical Vapour Deposition (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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US11/992,229 US20090087545A1 (en) | 2005-09-20 | 2006-09-19 | Film Forming Apparatus, Evaporating Jig, and Measurement Method |
JP2007536495A JP5358778B2 (ja) | 2005-09-20 | 2006-09-19 | 成膜装置、蒸発治具、及び、測定方法 |
Applications Claiming Priority (2)
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JP2005-272283 | 2005-09-20 | ||
JP2005272283 | 2005-09-20 |
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WO2007034790A1 true WO2007034790A1 (ja) | 2007-03-29 |
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ID=37888833
Family Applications (1)
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PCT/JP2006/318530 WO2007034790A1 (ja) | 2005-09-20 | 2006-09-19 | 成膜装置、蒸発治具、及び、測定方法 |
Country Status (6)
Country | Link |
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US (1) | US20090087545A1 (ja) |
JP (1) | JP5358778B2 (ja) |
KR (1) | KR20080046267A (ja) |
CN (1) | CN101268210A (ja) |
TW (1) | TWI421367B (ja) |
WO (1) | WO2007034790A1 (ja) |
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Also Published As
Publication number | Publication date |
---|---|
US20090087545A1 (en) | 2009-04-02 |
TW200722550A (en) | 2007-06-16 |
JP5358778B2 (ja) | 2013-12-04 |
KR20080046267A (ko) | 2008-05-26 |
TWI421367B (zh) | 2014-01-01 |
CN101268210A (zh) | 2008-09-17 |
JPWO2007034790A1 (ja) | 2009-03-26 |
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