KR101754260B1 - Drying apparatus and drying method - Google Patents

Abstract

Provided are a drying apparatus and a drying treatment method capable of efficiently removing a solvent in a film of an organic material coated on a substrate in a short period of time and capable of even drying treatment in the plane of the substrate. The drying apparatus 100 includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device 5 for injecting a gas toward the organic material film on the substrate S, and a control part 6. [ The drying apparatus 100 also has a pressure control mechanism for controlling the pressure in the processing vessel 1. [ The plurality of nozzles 51 are configured so that the flow rate of gas and the kind of gas can be independently controlled for each nozzle 51.

Description

[0001] DRYING APPARATUS AND DRYING METHOD [0002]

The present invention relates to a drying apparatus and a drying method which can be used, for example, for drying an organic material film in the process of manufacturing an organic EL device.

An organic EL (electroluminescence) element is a light emitting element that uses luminescence of an organic compound generated by flowing an electric current. A laminate of a plurality of organic functional films (hereinafter, this laminate is referred to as an "EL layer" Quot;) are interposed. Here, the EL layer may be formed from, for example, a hole transporting layer / a light emitting layer / an electron transporting layer / a hole transporting layer / a hole transporting layer / a light emitting layer / an electron transporting layer or a hole transporting layer / Electron injection layer] and the like are stacked in this order.

The EL layer is formed by depositing or applying an organic material on the substrate for each layer. In the case of forming a fine pattern with high precision, it is assumed that it is advantageous to use an inkjet printing method as a coating method.

The organic material film printed on the substrate by the inkjet printing method contains a large amount of solvent, and the reduced-pressure drying treatment is performed to remove the solvent (see, for example, Patent Document 1 and Patent Document 2). The dried organic material film is also baked. By this baking treatment, the organic material film is changed to an organic functional film constituting the EL layer (for example, Patent Document 3).

During the drying process, a large amount of solvent, moisture, and the like are volatilized from the organic material film on the substrate. Therefore, if the volatile components are not removed from the processing vessel of the drying apparatus quickly, the drying efficiency is lowered. The state of the organic material film after drying is known to affect the characteristics of the EL layer. For example, when the dry state of the substrate is uneven in the surface of the substrate during the drying process, the characteristics of the organic EL device in the plane of the substrate are uneven, and when used as an organic EL display, .

However, when the inside of the processing container of the drying apparatus is reduced in pressure, the amount of exhaust gas decreases with a decrease in pressure, and therefore, the amount of exhaust gas decreases in a high vacuum state. Further, in a high vacuum state, since the solvent volatilized from the organic material film forms a molecular flow in the processing vessel, there arises a problem that the solvent stays in the processing vessel.

There has been proposed a drying apparatus for removing a solvent in a coated organic material film by using an inkjet printing method and a drying apparatus having a plurality of spouting nozzles for spraying an inert gas onto a lid member facing a coated surface of a substrate has been proposed For example, Patent Document 4). Patent Document 4 discloses that the size of an ejection port or the number of ejection openings is changed in a lid member opposed to a substrate for the purpose of making the amount of inert gas injected in the surface of the substrate uniform. Patent Document 4 also discloses supplying solvent vapor into the processing vessel to prevent rapid drying of the coating film.

Japanese Patent Publication No. 3951162 (paragraph 0023, etc.) Japanese Patent Publication No. 4168968 (claim 2, etc.) Japanese Patent Publication No. 4148933 (claim 1, etc.) Japanese Patent Application Laid-Open No. 2010-067430 (FIG. 1, etc.)

An object of the present invention is to provide a drying apparatus and a drying method capable of efficiently removing a solvent in a film of an organic material coated on a substrate in a short period of time and capable of performing a uniform drying process in the plane of the substrate .

The inventors of the present invention have conducted studies on the drying of the organic material film applied to the substrate in the reduced-pressure drying process. As a result, it has been found that drying of the organic material film proceeds nonuniformly in the plane of the substrate, And the pattern of the organic material film greatly changed. Based on these findings, the present inventors have conceived that drying can be performed at a uniform rate within the substrate surface by positively changing the flow rate or kind of the gas jetted toward the substrate while controlling the pressure, Thereby completing the invention.

The drying apparatus of the present invention is a drying apparatus for removing a solvent contained in an organic material film applied to a surface of a substrate and drying the same. A drying apparatus of the present invention is a drying apparatus comprising a processing container capable of evacuating vacuum, an exhaust port for exhausting gas in the processing container, a support member for supporting the substrate in the process container, And at least one of the injection flow rate of the gas injected from the plurality of nozzles and the type of the gas is set as a unit independent of one nozzle or a combination of two or more nozzles And a control unit for controlling the control unit.

The drying apparatus of the present invention may be such that the plurality of nozzles eject a drying gas for promoting drying of the organic material film.

In the drying apparatus of the present invention, the plurality of nozzles may spray a drying suppressing gas for suppressing drying of the organic material film.

The drying apparatus of the present invention is characterized in that the plurality of nozzles include a nozzle for spraying a drying gas for promoting drying of the organic material film and a nozzle for spraying a drying suppressing gas for suppressing drying of the organic material film do.

In the drying apparatus of the present invention, the plurality of nozzles may include a nozzle relatively far from the nozzle relatively far from the substrate supported by the support member.

The drying apparatus of the present invention may be such that the nozzle has a cylindrical main body portion having a long length and a gas injection port having a long slit shape along the longitudinal direction of the main body portion. In this case, the plurality of nozzles may include a first nozzle group for jetting gas toward a central portion of the substrate supported by the support member, and a second nozzle group for jetting gas towards the periphery of the substrate .

The drying treatment method of the present invention is a drying treatment method in which a solvent in an organic material film applied to the surface of a substrate is removed and dried. A drying treatment method of the present invention is a drying treatment method comprising a treatment vessel capable of evacuation, an exhaust port for evacuating gas in the treatment vessel, a support member for supporting the substrate in the treatment vessel, And at least one of the injection flow rate of the gas injected from the plurality of nozzles and the type of the gas is set as a unit independent of one nozzle or a combination of two or more nozzles A drying unit having a control unit for controlling the drying unit is used.

The drying treatment method of the present invention may be carried out by maintaining the pressure in the treatment vessel within the range of 0.1 to 100 Pa.

The drying treatment method of the present invention may be such that the injection flow rate of the drying gas for promoting the drying of the organic material film is injected toward the substrate while independently adjusting a single nozzle or a combination of two or more nozzles as a unit.

The drying treatment method of the present invention may be such that the injection flow rate of the drying suppressing gas for suppressing the drying of the organic material film is injected toward the substrate while independently adjusting a single nozzle or a combination of two or more nozzles as a unit.

The drying treatment method of the present invention is characterized in that the mixing ratio of the drying gas for promoting the drying of the organic material film and the drying inhibiting gas for suppressing drying of the organic material film is set to be one nozzle or a combination of two or more nozzles in units And may be ejected toward the substrate while being adjusted independently.

In the drying treatment method of the present invention, the gas may be injected in a pulse shape.

The drying treatment method of the present invention may be such that the organic material film is coated on the substrate by ink jet printing in the production of the organic EL device.

According to the drying apparatus and the drying method of the present invention, the solvent in the organic material film coated on the substrate can be efficiently removed in a short time, and uniform drying can be performed in the plane of the substrate. Therefore, according to the present invention, it is possible to provide, for example, an organic EL device which can improve the productivity of a manufacturing process of the organic EL device and is highly reliable.

1 is a cross-sectional view showing a schematic configuration of a drying apparatus of a first embodiment of the present invention.
Fig. 2 is an explanatory view showing the arrangement of nozzles in the drying apparatus of Fig. 1; Fig.
3 is a characteristic diagram schematically showing a change in pressure in the processing container.
4 is a flow chart schematically showing a manufacturing process of an organic EL device.
5 is a cross-sectional view showing a schematic configuration of a drying apparatus of a second embodiment of the present invention.
Fig. 6 is an explanatory view showing the arrangement of nozzles in the drying apparatus of Fig. 5;
Fig. 7 is a characteristic diagram showing the change in pressure when the N ₂ gas is introduced into the processing vessel and when the processing vessel is not introduced with the N ₂ gas in the middle of the vacuum evacuation.
8 is a characteristic diagram showing the relationship between the N ₂ gas flow rate and the pressure in the processing vessel when N ₂ gas is continuously introduced into the processing vessel.
9 is a characteristic diagram showing the relationship between the N ₂ gas flow rate and the pressure in the processing vessel when N ₂ gas is introduced discontinuously into the processing vessel.
10 is an explanatory diagram showing the position where the drying degree of the substrate surface is observed and the mounting position of the nozzle in the experiment in which the effects of the present invention are confirmed, superimposed on the top view of the substrate.
11 is a cross-sectional view showing a schematic configuration of a drying apparatus of a third embodiment of the present invention.
12 is a perspective view showing the structure of the nozzle in the drying apparatus of Fig.
13 is a cross-sectional view in the direction perpendicular to the longitudinal direction of the nozzle in the drying apparatus of Fig.
14 is an explanatory view showing the arrangement of the nozzles in the drying apparatus of Fig.
Fig. 15 is a view for explaining an example of the gas injection flow rate and the timing of injection when the substrate drying process is performed in the drying apparatus of Fig. 11; Fig.
16 is a cross-sectional view showing a schematic structure of a drying apparatus of a fourth embodiment of the present invention.
17 is a cross-sectional view showing a schematic configuration of a drying apparatus of a fifth embodiment of the present invention.

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.

[First Embodiment]

1 is a cross-sectional view showing a schematic configuration of a single-wafer drying apparatus according to a first embodiment of the present invention. The drying apparatus 100 of the present embodiment is a drying apparatus for drying a glass substrate (hereinafter, simply referred to as "substrate") (S) for an organic EL display as an object to be processed, And then dried.

The drying apparatus 100 of this embodiment includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device 5 for injecting a gas toward an organic material film on a substrate S supported on the base 3 and at least one of a flow rate of a gas jetted from a plurality of nozzles and a kind of gas, Or a control unit 6 for independently controlling the combination of two or more nozzles as a unit. In addition, 'type of gas' includes the mixing ratio (the same shall apply hereinafter). The drying apparatus 100 also has a pressure control mechanism for controlling the pressure in the processing vessel 1. [

<Processing vessel>

The processing container 1 is a pressure-resistant container which can be evacuated. The processing vessel 1 is formed of a metal material. As a material for forming the processing container 1, for example, aluminum, aluminum alloy, stainless steel or the like is used. The processing vessel 1 is provided with a bottom wall 11, four side walls 13 in a prism shape, and a ceiling portion 15.

The side wall 13 is provided with a loading / unloading port 13a for loading / unloading the substrate S into / from the apparatus. The loading / unloading port 13a is for loading / unloading the substrate S with / from the outside of the processing vessel 1. A gate valve (GV) is provided at the loading / unloading outlet (13a). The gate valve GV has a function of opening and closing the loading and unloading port 13a and sealing the processing vessel 1 in a closed state in a hermetic manner and sealing the substrate S ). &Lt; / RTI &gt;

The bottom wall 11 is provided with an exhaust port 11a. The exhaust port 11a is connected to an external exhaust device 19 through an exhaust pipe 17. By driving the exhaust device 19, the interior of the processing vessel 1 can be evacuated to a predetermined degree of vacuum, for example, a pressure of about 0.1 Pa.

<Tape>

Inside the processing container 1, a mounting table 3 as a supporting device is disposed. The mounting table 3 is supported by a plurality of support pillars 21. A plurality of support pillars (21) are fixed to the bottom wall (11). Although not shown, the table 3 has a mechanism for lifting and lowering the substrate S, for example, a lift pin, and has a transfer position for transferring the substrate S, The height position of the substrate S can be adjusted between the position where the substrate S is placed and the processing position where the drying process is performed.

<Pressure control mechanism>

The drying apparatus 100 of the present embodiment is also provided with an exhaust apparatus 19. The exhaust device 19 may be a constituent part of the drying device 100 or an external device different from the drying device 100. The exhaust device 19 has, for example, a vacuum pump such as a turbo molecular pump or a dry pump. The drying apparatus 100 further includes an exhaust pipe 17 connecting the exhaust port 11a and the exhaust device 19 and an APC valve 23 installed in the middle of the exhaust pipe 17. The internal space of the processing container 1 can be evacuated to a predetermined degree of vacuum by operating the vacuum pump of the exhaust device 19 and regulating the opening degree of the APC valve 23. [

The drying apparatus 100 of the present embodiment also includes a pressure gauge 25 for monitoring the pressure in the processing vessel 1. [ The pressure gauge 25 transmits the measurement pressure in the processing vessel 1 to the APC valve 23 as an electric signal.

In this embodiment, the exhaust device 19, the exhaust pipe 17, the APC valve 23, and the pressure gauge 25 constitute a pressure control mechanism for exhausting the inside of the processing container 1 under reduced pressure and regulating it to a predetermined pressure have.

<Gas injection device>

The gas injection device 5 is provided with a plurality of nozzles 51, a gas supply source 53 for supplying gas to the respective nozzles 51, a gas supply source 53 and the respective nozzles 51, And a plurality of pipes 55 for supplying the gas to the gas supply pipe 51. In Fig. 1, six nozzles 51 are representatively shown. The nozzles 51B, the nozzles 51C, the nozzles 51C, the nozzles 51B, the nozzles 51B, the nozzles 51B, the nozzles 51B, Nozzle 51A &quot;. The nozzles 51A are arranged opposite to the upper side of the peripheral portion of the substrate S and the nozzles 51B are arranged on the upper side of the central portion of the rectangular substrate S, Is arranged so as to be opposed to the upper portion of the middle portion between the central portion and the peripheral portion of the substrate S.

The gas supply source 53 is provided with an inert gas supply source 53A and a solvent gas supply source 53B. The inert gas supply source 53A supplies, for example, an inert gas as a drying gas for promoting the drying of the organic material film. As the inert gas, for example, nitrogen gas, argon gas, helium gas, or the like can be used. The solvent gas supply source 53B supplies a solvent gas as a drying suppressing gas for suppressing drying of the organic material film. In addition to the inert gas supply source 53A and the solvent gas supply source 53B, the gas supply source 53 may be provided with a different gas supply source.

The gas injection device 5 is provided with a plurality of mass flow controllers (MFCs) 57 and a plurality of opening / closing valves 59 for controlling the gas flow rate in the middle of the pipe 55. The flow rate or injection speed of the gas injected from the nozzle 51, the kind of the gas, and the like are controlled by the mass flow controller (MFC) 57 and the opening / closing valve 59. 1, representative examples of the piping 55, the on-off valve 59 and the mass flow controller (MFC) 57 are shown. The arrangement position or number thereof is not limited to the contents shown in Fig. 1 Do not.

The plurality of nozzles 51 are provided above the substrate S so that gas can be injected toward the surface of the substrate S. The plurality of nozzles 51 are configured to independently control at least one of a gas flow rate and a gas type. That is, the discharge flow rate of the gas is independently controlled for each nozzle 51 by the combination of the pipe 55, the mass flow controller (MFC) 57 and the opening / closing valve 59. The combination of the piping 55, the mass flow controller (MFC) 57, and the plurality of open / close valves 59 is configured so that the kind of the gas can be switched independently for each nozzle 51 to be sprayed.

[Gas flow rate]

The plurality of nozzles 51 are configured to be capable of injecting an inert gas at an independent injection flow rate. For example, inert gas can be injected at a relatively large flow rate (V1) from the nozzle 51C disposed immediately above the central portion of the substrate S in which the drying of the organic material film is relatively difficult to proceed . The inert gas is injected from the nozzle 51A disposed just above the periphery of the substrate S into the peripheral portion of the substrate S where the drying of the organic material film is relatively easy to be performed at a flow rate V2 relatively smaller than the flow rate V1 can do. An inert gas can be injected from the nozzle 51B at a middle portion between the central portion and the peripheral portion of the substrate S at a flow rate V3 intermediate the flow rate V1 and the flow rate V2. It is also possible that no inert gas is injected to the peripheral portion and the intermediate portion of the substrate S.

The plurality of nozzles 51 are configured to be capable of jetting solvent gas at independent injection flow rates. For example, solvent gas can be injected from the nozzle 51A at a relatively large flow rate V4 to the peripheral portion of the substrate S where drying of the organic material film is relatively easy. In addition, the solvent gas can be jetted from the nozzle 51C at a flow rate V5, which is relatively smaller than the flow rate V4, at the central portion of the substrate S where drying of the organic material film is relatively difficult. The solvent gas can be injected from the nozzle 51B at a middle flow rate V6 between the flow rate V4 and the flow rate V5 at an intermediate portion between the central portion and the peripheral portion of the substrate S. [ It is also possible that the solvent gas is not sprayed to the central portion and the middle portion of the substrate S.

Further, the injection flow rate of the gas is not limited to each of the three flow rates (V1 to V3, V4 to V6), and may be one, two, or four or more stages. Further, it is not limited to the central portion and the peripheral portion of the substrate S, but it is possible to set the flow rate separately for the more subdivided regions and inject the gas.

[Gas type]

The plurality of nozzles 51 are capable of independently injecting an inert gas, a solvent gas, or a mixed gas of an inert gas and a solvent gas (hereinafter sometimes simply referred to as a "mixed gas"). For example, the inert gas can be injected from the nozzle 51C to the central portion of the substrate S where drying of the organic material film is relatively difficult. In addition, the solvent gas can be injected from the nozzle 51A to the peripheral portion of the substrate S where the organic material film is relatively easily dried. Further, a mixed gas of an inert gas and a solvent gas can be injected from the nozzle 51B at an intermediate portion between the central portion and the peripheral portion of the substrate S.

The plurality of nozzles 51 are configured to be capable of injecting the mixed gas in independent mixing ratios. For example, the mixed gas can be injected from the nozzle 51C at a first mixing ratio with a low solvent gas concentration at the central portion of the substrate S where drying of the organic material film is relatively difficult. The mixed gas can be injected from the nozzle 51A at a second mixing ratio higher than the first mixing ratio at a peripheral portion of the substrate S where the organic material film is relatively easily dried. Further, a mixed gas is sprayed from the nozzle 51B at a third mixing ratio which is the middle of the first mixing ratio and the second mixing ratio in the middle portion between the central portion and the peripheral portion of the substrate S .

Further, the mixed gas is not limited to the three stages of the first to third mixing ratios, and may be one, two, or four or more stages. Further, it is not limited to the central portion and the peripheral portion and the intermediate portion of the substrate S, and it is possible to separately inject the gas by setting the kind or the mixing ratio for the finer region.

[Nozzle height position]

In the drying apparatus 100 of the present embodiment, the height positions of the plurality of nozzles 51 can be individually set. In other words, the plurality of nozzles 51 are arranged in such a manner that the distance to the substrate S supported on the mounting table 3 is at least the distance between the nozzles 51A relatively far from the nozzles 51C relatively close to each other, And a nozzle 51B. The height position of each nozzle 51 can be achieved by mounting an adapter (extension pipe) (not shown) between the pipe 55 and the nozzle 51 which are introduced into the processing vessel 1, for example. By changing the distance between the nozzle 51 and the substrate S in this way, it is possible to control the intensity and amount of the gas reaching the surface of the substrate S, for example, even when the same gas is jetted at the same speed . In the example shown in Fig. 1, a nozzle 51C is disposed at a height position H1, at which the distance to the substrate S is relatively close to the central portion of the substrate S in which drying of the organic material film is relatively difficult have. A nozzle 51A is disposed at a height position H2 that is higher than the height position H1 and relatively far from the substrate S at the periphery of the substrate S where the drying of the organic material film is relatively easy . A nozzle 51B is disposed at a height position H3 which is higher than the height position H1 and lower than the height position H2 in the middle portion between the central portion and the peripheral portion of the substrate S. [

Further, the height position of the nozzle 51 is not limited to the three positions of the height positions H1 to H3, and may be one, two, or four or more. Further, it is possible to spray the gas by setting the height position of the nozzle 51 individually for the more subdivided area, not limited to the middle part and the middle part of the substrate S and the middle part.

[Arrangement of Nozzle]

Fig. 2 is a plan view of the substrate S for explaining the arrangement of the nozzles 51 in the drying apparatus 100 of Fig. 2, the arrangement of the nozzles 51 is projected on the upper surface of the substrate S. In Fig. 2, formation regions of the organic material film pattern-coated on the substrate S by the ink-jet printing method are indicated by R1 to R4. Here, each of the regions R1 to R4 corresponds to the size of the organic EL product, for example, the organic EL display. That is, the organic material films are separately formed in the surface of the substrate S so that four organic EL devices can be manufactured from one substrate S. Nine nozzles 51 are uniformly arranged in the formation regions R1 to R4 of the four organic material films, respectively. In this manner, the nozzle 51 can be disposed in consideration of the layout of the organic material film formed on the substrate S.

Further, the present invention is not limited to the four regions R1 to R4 of the substrate S, and it is possible to inject the gas by individually setting the arrangement of the nozzles 51 with respect to the more subdivided regions. As another example of the arrangement, although not shown, the number of the nozzles 51 is relatively increased in the upper portion of the central portion of the substrate S where drying of the organic material film is relatively difficult, The number of the nozzles 51 may be relatively reduced above the periphery of the peripheral portion of the substrate S where drying is relatively easy. Further, it is preferable that the position or the gas flow rate of the nozzle 51 can be changed depending on the type or shape of the substrate S.

<Control section>

1, the respective components of the drying apparatus 100, for example, the exhaust device 19, the APC valve 23, the mass flow controller (MFC) 57, the on-off valve 59, , And is controlled by being connected to the control unit (6). The control unit 6 includes a controller 61 having a CPU, a user interface 62, and a storage unit 63. The controller 61 has a computer function, and controls the components in the drying apparatus 100 as a whole. The user interface 62 is constituted by a keyboard for performing a command input operation or the like for the process manager to manage the drying apparatus 100 and a display for visually displaying the operating status of the drying apparatus 100 and the like. The storage unit 63 stores a recipe in which a control program (software) or processing condition data for realizing various processes executed in the drying apparatus 100 under the control of the controller 61 is recorded. The user interface 62 and the storage unit 63 are connected to the controller 61. [

If desired, an arbitrary recipe is called from the storage unit 63 by an instruction from the user interface 62 and is executed by the controller 61 so that the desired Drying treatment is carried out. That is, the control unit 6 sends control signals to the exhaust device 19 and the APC valve 23 to maintain the inside of the processing container 1 at a predetermined pressure. The control unit 6 also sends out control signals to the plurality of mass flow controllers (MFCs) 57 and the on-off valves 59 to control the flow rates of the gases jetted from the plurality of nozzles 51 and One is adjusted independently for each nozzle 51 or for each combination of two or more nozzles 51. The recipe such as the control program or the processing condition data may be stored in a computer-readable storage medium such as a CD-ROM, a hard disk, a flexible disk, a flash memory, or the like. Alternatively, it may be transmitted from another apparatus, for example, via a dedicated line at any time and used online.

[Drying Treatment Method]

Next, the drying process of the organic material film on the surface of the substrate S, which is performed using the drying apparatus 100, will be described with reference to Fig. The drying treatment method of this embodiment performs a drying treatment on the organic material film applied to the surface of the substrate S in the treatment vessel 1 of the drying apparatus 100. [ During the drying process, the control unit 6 controls the gas injection device 5 including the plurality of nozzles 51 by individually adjusting the injection flow rate of gas, the kind of gas, etc. for each nozzle 51, (S). The injection of at least one of the inert gas and the solvent gas from the respective nozzles 51 may be continuous or discontinuous (intermittent). The drying treatment is carried out in such a manner that the pressure in the treatment vessel 1 is controlled within the range of 0.1 to 100 Pa, preferably 0.3 to 10 Pa, in order to promote the volatilization of the solvent contained in the organic material film and to improve the drying efficiency . In this embodiment, by performing the gas injection by the gas injection device 5 and the pressure control in the processing vessel 1 in relation to each other, it is possible to lower the solvent concentration in the atmosphere while making the inside of the processing vessel 1 highly vacuumed The drying efficiency of the organic material film on the surface of the substrate S is improved, and the drying treatment can be performed in a short time.

3 is a characteristic diagram schematically showing the pressure change in the process of evacuating the inside of the processing vessel 1 under reduced pressure. The vertical axis of FIG. 3 represents the pressure in the processing vessel 1, and the horizontal axis represents time. In the drying apparatus 100, by operating the exhaust device 19, the inner space of the processing container 1 can be evacuated to a predetermined degree of vacuum. For example, when the exhaust device 19 is operated, a pressure drop occurs in the processing vessel 1, for example, as indicated by a curve A in Fig. Here, it is assumed that the preferable pressure range in the drying process for the organic material film is within the range of the pressures (P1 to P2) in Fig. The values of the pressures P1 and P2 may be set according to the amount of solvent in the organic material film on the surface of the substrate S and the pressure P1 is preferably set within a range of 10 to 100 Pa, The pressure P2 is preferably set within a range of 0.1 to 0.3 Pa, for example. If the pressure P1 in the processing vessel 1 exceeds 100 Pa, the drying efficiency of the organic material film is lowered. If the pressure P2 in the processing vessel 1 is lower than 0.1 Pa, the drying of the region (for example, peripheral portion) which is likely to dry in the plane of the substrate S is excessively advanced, And the like. It is also difficult to control the degree of drying of the organic material film on the substrate S if the pressure in the processing vessel 1 fluctuates greatly beyond the range of P1 to P2, It is difficult to grasp the degree of drying, and there is a possibility of causing unevenness of processing among a plurality of substrates S. Therefore, when the drying process for the substrate S is performed from the time point t1 to the time point t2, for example, the pressure in the range from t1 to t2 is within the range of P1 to P2, ) In the processing vessel 1 is preferable.

The pressure in the processing vessel 1 can be controlled within a certain range by controlling the flow rate of the introduced gas by the mass flow controller (MFC) 57 and the opening degree of the APC valve 23. [ In the drying treatment method of the present embodiment, in order to introduce gas continuously or discontinuously into the processing vessel 1 by the gas injection apparatus 5, the control unit 6 controls the pressure and the gas flow rate in the following procedure . For example, in Fig. 3, the gas injection is continuously performed at the time t1 when the pressure in the processing vessel 1 has dropped to P1 and at the time t2 when the drying process is terminated I do. 3, at the same time when the pressure in the processing vessel 1 is lowered to P1, the gas is injected and the gas is injected during the period from the time point t2 at which the drying processing is terminated And then stopped. In the case where the introduction of the gas is discontinuously performed, it is preferable to switch the gas introduction and the stop at intervals within the range of, for example, 10 to 100 seconds.

As described above, the gas is continuously or discontinuously introduced while maintaining the inside of the processing container 1 in a high vacuum state in the range of the pressures P1 to P2. The drying process can be performed in a short period of time by promoting the discharge of the solvent in the atmosphere in the processing container 1 by using the air stream of the gas thus introduced.

[Procedure of drying treatment]

Next, the procedure of the drying process using the drying apparatus 100 configured as described above will be described. First, as the previous step, the organic material film is printed on the substrate S in a predetermined pattern by an external inkjet printing apparatus (not shown). Next, the gate valve GV is opened, and the substrate S on which the organic material film is printed is transferred to the mounting table 3 of the drying apparatus 100 by an external transfer device (not shown).

Subsequently, the gate valve (GV) of the drying apparatus 100 is closed and the exhaust apparatus 19 is operated to exhaust the inside of the processing vessel 1 under reduced pressure. The pressure in the processing vessel 1 is monitored by the pressure gauge 25, and the degree of opening of the APC valve 23 is controlled to reduce the pressure to a predetermined degree of vacuum. In this way, a drying process for removing the solvent contained in the organic material film formed on the substrate S can be performed. During this drying process, the gas injection device 5 provided with the plurality of nozzles 51 capable of individually controlling the injection flow rate of the gas, the kind of the gas, etc., while controlling the pressure in the processing vessel 1, S can be efficiently dried in a short period of time while uniformizing the degree of drying of the organic material film in the plane of the substrate S by spraying gas toward the surface of the substrate S. In addition, by introducing gas into the processing vessel 1 by using the gas injection device 5, airflow is generated in the processing vessel 1, so that the exhaust of the solvent staying in the processing vessel 1 is promoted .

Subsequently, the gas injection by the gas injection device 5 and the exhaust by the exhaust device 19 are stopped and the inside of the process container 1 is raised to a predetermined pressure. Thereafter, the gate valve (GV And the substrate S is taken out of the processing container 1 by an external transfer device (not shown). By the above procedure, the drying process for one substrate S is completed.

[Example of Application to Manufacturing Process of Organic EL Device]

In the production of the organic EL device, a plurality of organic functional films are formed as an EL layer between the anode and the cathode. The drying apparatus 100 of the present embodiment can be applied to the production of an organic EL element having any lamination structure. Here, the case where an organic EL element having a hole injecting layer / a hole transporting layer / a light emitting layer / an electron transporting layer / an electron injecting layer is produced from an anode side to an anode side as an EL layer is described as a specific process by the drying apparatus 100 .

Fig. 4 schematically shows a manufacturing process of the organic EL device. In this example, the organic EL device is manufactured by the processes of STEP1 to STEP8. In STEP 1, an anode (pixel electrode) is formed on the substrate S in a predetermined pattern by, for example, a vapor deposition method or the like. Next, in STEP 2, a partition (bank) made of an insulating material is formed between the positive electrodes. As the insulating material for forming the barrier rib, for example, a polymer material such as a photosensitive polyimide resin can be used.

Subsequently, in STEP3, a hole injection layer is formed on the anode formed in STEP1. First, an organic material to be a material of the hole injection layer is printed on the anode partitioned by each partition by the inkjet printing method. Subsequently, the thus-printed organic material film is subjected to a reduced-pressure drying process for removing the solvent by using the drying apparatus 100. Subsequently, the substrate S after the drying treatment is transferred to a baking apparatus and subjected to a baking treatment to form a hole injecting layer.

Subsequently, in STEP4, a hole transport layer is formed on the hole injection layer formed in STEP3. First, an organic material to be a material of the hole transport layer is printed on the hole injection layer by an inkjet printing method. The organic material film printed in this way is subjected to a reduced pressure drying treatment for removing the solvent by using the drying apparatus 100. [ Subsequently, the substrate S after the drying treatment is transferred to a baking apparatus and baked to form a hole transporting layer.

Subsequently, in STEP5, a light emitting layer is formed on the hole transporting layer formed in STEP4. First, an organic material to be a material of the light emitting layer is printed on the hole transporting layer by the inkjet printing method. The organic material film printed in this way is subjected to a reduced pressure drying treatment for removing the solvent by using the drying apparatus 100. [ Subsequently, the substrate S after the drying treatment is transferred to a baking apparatus and subjected to a baking treatment to form a light emitting layer. Further, when the light emitting layer is composed of a plurality of layers, the above process is repeated.

Subsequently, an electron transport layer (STEP6), an electron injection layer (STEP7) and a cathode (STEP8) are sequentially formed on the light emitting layer by, for example, vapor deposition method to obtain an organic EL element.

In such a manufacturing process of the organic EL device, the drying apparatus 100 can be suitably applied to STEP3 (hole injection layer formation), STEP4 (hole transport layer formation), and STEP5 (light emission layer formation). That is, after the organic material film which is the previous stage of each layer is printed by the inkjet printing method, the organic material film can be subjected to the reduced pressure drying treatment using the drying apparatus 100. In this case, since the drying apparatus 100 is provided with the gas injection device 5 having a plurality of nozzles 51 capable of individually regulating the flow rate of the gas and the kind of the gas, the drying apparatus 100 is excellent in a short period of time Drying efficiency is obtained.

As described above, by using the drying apparatus 100, the drying process necessary for forming the EL layer can be efficiently performed with high throughput in the manufacturing process of the organic EL device.

[Second Embodiment]

Next, the drying apparatus of the second embodiment of the present invention will be described with reference to Figs. 5 and 6. Fig. 5 is a cross-sectional view showing a schematic structure of the drying apparatus 101 according to the second embodiment. Fig. 6 is a plan view of the substrate S for explaining the arrangement of the nozzles 51 in the drying apparatus 101 of Fig. As a main difference from the drying apparatus 100 of the first embodiment, in the drying apparatus 101 of the present embodiment, at least one of the gas flow rate and the gas type can be adjusted for each combination of the plurality of nozzles 51 have. Hereinafter, differences from the drying apparatus 100 of the first embodiment will be mainly described. In the drying apparatus 101 of this embodiment, the same components as those of the first embodiment are denoted by the same reference numerals, and description thereof is omitted.

The drying apparatus 101 of the present embodiment includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device (5A) for injecting a gas toward an organic material film on a substrate (S) to be supported; and at least one of a flow rate of a gas jetted from the plurality of nozzles and a kind of gas, And a control unit (6) for independently controlling the combination of the two units as a unit. Further, the drying apparatus 101 is provided with a pressure control mechanism for controlling the pressure in the processing vessel 1.

The structure of the processing container 1, the mounting table 3, the pressure control mechanism, and the control unit 6 in the drying apparatus 101 of this embodiment is the same as that of the drying apparatus 100 of the first embodiment.

<Gas injection device>

The gas injection device 5A has a plurality of nozzles 51, a gas supply source 53 for supplying gas to each nozzle 51, a gas supply source 53 and each nozzle 51, And a plurality of pipes 55 for supplying the gas to the gas supply pipe 51. In Fig. 5, eleven nozzles 51 are representatively shown. The gas injection device 5A includes a plurality of mass flow controllers (MFCs) 57 and a plurality of opening / closing valves 59 for controlling the gas flow rate in the middle of the pipe 55. The flow rate or injection speed of the gas injected from the nozzle 51, the kind of the gas, and the like are controlled by the mass flow controller (MFC) 57 and the opening / closing valve 59. 5, representative examples of the pipe 55, the on-off valve 59, and the mass flow controller (MFC) 57 are shown. The positions and the number of these are not limited to the contents shown in Fig. 5 Do not.

In the present embodiment, the plurality of nozzles 51 includes a plurality of combinations, and at least one of the gas flow rate and gas type can be adjusted independently for each combination. In Fig. 5, two combinations (nozzle groups 52) constituted by a plurality of nozzles 51 are representatively shown. When it is necessary to distinguish each of the nozzle groups 52 for convenience of explanation, the nozzle group 52A, the nozzle group 52B, and the nozzle group 52A are indicated from the left side toward the paper surface of FIG. Here, the nozzle group 52B is disposed so as to oppose to the upper portion of the central portion of the rectangular substrate S, and the nozzle group 52A is arranged to face the upper side of the peripheral portion of the substrate S. It is also possible to set the nozzle groups 52 individually for the more subdivided regions, not limited to the central portion and the peripheral portion of the substrate S.

The gas supply source 53 is provided with an inert gas supply source 53A and a solvent gas supply source 53B. The configuration of the gas supply source 53 is the same as that of the first embodiment.

In the present embodiment, a plurality of nozzles 51 are provided above the substrate S so that gas can be jetted toward the surface of the substrate S. The plurality of nozzle groups 52 are configured so that the flow rate of gas and the kind of gas can be adjusted independently for each nozzle group 52. That is to say, the combination of the pipe 55, the mass flow controller (MFC) 57 and the opening / closing valve 59 is arranged so as to control the flow rate of the gas independently for each nozzle group 52. The combination of the pipe 55 and the plurality of open / close valves 59 is configured so that the kind of the gas can be switched independently for each nozzle group 52 so as to be injected.

[Gas flow rate]

The plurality of nozzle groups 52 are configured to be capable of injecting inert gas at independent injection flow rates. For example, inert gas can be injected at a relatively large flow rate V7 from the nozzle group 52B disposed immediately above the center portion of the substrate S in which the drying of the organic material film is relatively difficult to proceed have. An inert gas is supplied from the nozzle group 52A disposed immediately above the periphery of the substrate S to the peripheral portion of the substrate S where the drying of the organic material film is relatively easy to proceed at a flow rate V8 relatively smaller than the flow rate V7 It can be sprayed. It is also possible that no inert gas is injected into the peripheral portion of the substrate S.

The plurality of nozzle groups 52 are configured to be capable of jetting solvent gas at independent injection flow rates. For example, solvent gas can be injected from the nozzle group 52A at a relatively large flow rate V9 to the peripheral portion of the substrate S where drying of the organic material film is relatively easy. In addition, the solvent gas can be jetted from the nozzle group 52B at a flow rate V10, which is relatively smaller than the flow rate V9, at the central portion of the substrate S where drying of the organic material film is relatively difficult. It is also possible not to spray the solvent gas in the central portion of the substrate S.

The injection flow rate of the gas is not limited to two stages but may be one stage or three or more stages. Further, it is not limited to the central portion and the peripheral portion of the substrate S, and it is possible to set the flow rate separately for the more subdivided regions and to inject the gas.

[Gas type]

The plurality of nozzle groups 52 are configured to be capable of jetting an inert gas, a solvent gas, or a mixed gas of an inert gas and a solvent gas (hereinafter sometimes simply referred to as a "mixed gas") independently of each other. For example, an inert gas can be injected from the nozzle group 52B to the central portion of the substrate S where drying of the organic material film is relatively difficult. In addition, the solvent gas can be injected from the nozzle group 52A to the peripheral portion of the substrate S where drying of the organic material film is relatively easy.

The plurality of nozzle groups 52 are configured to be capable of injecting the mixed gas in independent mixing ratios. For example, the mixed gas can be injected from the nozzle group 52B at a first mixing ratio with a low solvent gas concentration at a central portion of the substrate S where drying of the organic material film is relatively difficult. The mixed gas can be injected from the nozzle group 52A at a second mixing ratio higher than the first mixing ratio to the peripheral portion of the substrate S where the drying of the organic material film is relatively easy.

The mixing ratio of the mixed gas is not limited to two stages but may be one stage or three or more stages. Further, it is possible to spray the gas by setting the type or concentration individually for the finer regions, not limited to the central portion and the peripheral portion of the substrate S.

[Nozzle height position]

In the present embodiment, the height positions of the plurality of nozzles 51 in the nozzle group 52 can be individually set. In the example shown in Fig. 5, the height positions of the plurality of nozzles 51 included in the nozzle group 52B opposed to the central portion of the substrate S, in which drying of the organic material film is relatively difficult, is changed. That is, the nozzle group 52B is arranged so that the distance to the substrate S supported on the mounting table 3 is at least a relatively high height position H4, a relatively far height position H5, H4 and a height position H6 lower than the height position H5.

In the example shown in Fig. 5, the height positions of the nozzles 51 included in the nozzle group 52A are all set to the same height position H5.

In the case of changing the height position of the nozzle 51 in the nozzle group 52, it is not limited to three, but may be two or four or more. It is also possible to separately inject the gas by setting the height position of the nozzle 51 with respect to the more subdivided area of the substrate S.

[Arrangement of Nozzle]

In Fig. 6, the arrangement of the nozzles 51 is shown projected on the upper surface of the substrate S. Fig. 6, the nozzle group 52B is disposed so as to oppose to the upper portion of the central portion of the rectangular substrate S, and the nozzle group 52A is arranged above the peripheral portion of the substrate S Respectively. Specifically, eight nozzle groups 52A are arranged so as to surround the nozzle group 52B having 25 nozzles 51. The nozzle group 52A includes the nozzle group 52A1 and the nozzle group 52A2 and the number of the nozzles 51 included therein is 15 nozzle groups 52A1 and the nozzle group 52A2 The nozzle group 52A1 and the nozzle group 52A2 are common in terms of the function of jetting the gas onto the substrate S. [

In Fig. 6, formation regions of the organic material film pattern-coated on the substrate S by the ink-jet printing method are indicated by R1 to R4. Here, each of the regions R1 to R4 corresponds to the size of the organic EL product, for example, the organic EL display. That is, the organic material films are separately formed in the plane of the substrate S so that four organic EL products can be manufactured from one substrate S. The plurality of nozzles 51 are equally arranged by 25 for each of the formation regions R1 to R4 of the four organic material films. In this manner, the nozzle 51 can be disposed in consideration of the layout of the organic material film formed on the substrate S.

Further, the present invention is not limited to the four regions R1 to R4 of the substrate S, and it is possible to inject the gas by individually setting the arrangement of the nozzles 51 with respect to the more subdivided regions. As another example of the arrangement, although not shown, the number of the nozzles 51 is relatively increased in the upper portion of the central portion of the substrate S where drying of the organic material film is relatively difficult, The number of the nozzles 51 may be relatively reduced above the periphery of the peripheral portion of the substrate S where drying is relatively easy.

The drying process in the drying apparatus 101 of the present embodiment is a method in which at least one of the gas flow rate and gas type is individually controlled by the control unit 6 in units of the nozzle group 52A or the nozzle group 52B Except that the gas is injected toward the surface of the substrate S while the gas is injected toward the surface of the substrate S. The drying of the organic material film in the plane of the substrate S by spraying the gas toward the surface of the substrate S using the gas injection device 5A while controlling the pressure in the process container 1 during the drying process It can be efficiently dried in a short period of time.

Other configurations and effects in this embodiment are the same as those in the first embodiment. Further, the drying apparatus 101 can be applied to the manufacturing process of the organic EL element similarly to the first embodiment.

Next, with reference to Figs. 7 to 9, experimental results on which the present invention is based will be described. 7 to 9 show the pressure (Pa) (log scale) in the processing vessel 1, and the horizontal axis shows time (seconds). In the following experiment, the same drying apparatus as the drying apparatus 100 of Fig. 1 was used.

7 is a characteristic diagram showing changes in pressure when the N ₂ gas is introduced into the processing container 1 and when the N ₂ gas is not introduced during the evacuation of the inside of the processing container 1 by operating the exhaust device 19. 7 shows the change in pressure when no N ₂ is introduced during the drying process and the curve B shows the change in the pressure during the drying process from the point when the pressure in the process container 1 dropped to 10 Pa. And the N ₂ gas was continuously introduced at a flow rate of 180 ml / min (sccm) to the end of the reaction. 7, it was confirmed that the pressure can be kept substantially constant by adjusting the opening degree of the APC valve 23 while introducing N ₂ gas into the processing vessel 1 by the mass flow controller (MFC) 57 .

8 shows the relationship between the flow rate of N ₂ gas when the N ₂ gas is introduced continuously into the processing vessel 1 and the flow rate of N ₂ gas when the inside of the processing vessel 1 is evacuated while the exhaust system 19 is operated, And pressure. 8 shows the pressure change when N ₂ gas is continuously introduced at a flow rate of 100 ml / min (sccm) from the time when the pressure in the processing vessel 1 is lowered to 10 Pa to the end of the drying processing. It has been confirmed from Fig. 8 that the pressure can be kept substantially constant by adjusting the opening degree of the APC valve 23 while introducing N ₂ gas into the processing vessel 1 by the mass flow controller (MFC) 57 .

Figure 9 is, by operating the exhaust unit (19) processing vessel (1) N ₂ gas flow rate and the process vessel 1 in the case where, while a reduced pressure evacuating the inside, introducing N ₂ gas discontinuously into the processing container 1, And the pressure in the chamber. 9 shows the pressure change when the N ₂ gas is discontinuously introduced at a flow rate of 100 ml / min (sccm) during the period from the time when the pressure in the processing vessel 1 is lowered to 10 Pa to the termination of the drying treatment Respectively. 9, while the N ₂ gas is introduced into the processing vessel 1, the pressure is maintained at about 1 Pa. While the introduction of the N ₂ gas is stopped, the pressure is maintained at about 0.3 Pa. As described above, the opening degree of the APC valve 23 is adjusted while the N ₂ gas is introduced into the processing vessel 1 by the mass flow controller (MFC) 57, so that the pressure is maintained within a predetermined range, for example, 0.3 Pa To 1 Pa. &Lt; tb &gt;&lt; TABLE &gt;

Next, with reference to FIG. 10, experimental results confirming the effects of the present invention will be described. In this experiment, the same drying apparatus as the drying apparatus 100 of Fig. 1 was used. 10 is a plan view of the substrate S. Fig. 10 shows the position at which the drying degree of the surface of the substrate S is observed and the mounting position of the nozzle 51 when the drying process of the substrate S is performed in the processing vessel 1 of the drying apparatus used in the experiment, Are superimposed on a plan view of the substrate (S). In Fig. 10, the regions corresponding to the sizes of the organic EL products, for example, the organic EL display, are denoted by symbols R1 and R2. The size of the substrate S was 920 mm on the long side and 730 mm on the short side.

The nozzles 51 can be disposed directly above the four positions S 1, S 2, S 3, and S 4 on the substrate S and gas can be injected toward the substrate S . The distance L between the nozzles 51 was set to 250 mm. In this experiment, when the pressure in the processing vessel 1 is controlled at 1.4 Pa and N ₂ gas is introduced at 180 mL / min (sccm) from each nozzle 51 and when no gas is introduced at all . The position S1 of the central portion of the region R1 where the drying progresses slowly in the plane of the substrate S and the position S5 of the corner portion of the region R1 where the drying progresses fast in the plane of the substrate S, The time until the organic material film reached a predetermined degree of drying and the drying was completed was measured.

As a result, the time to completion of drying was 53 seconds when N ₂ gas was introduced at the position S1, and 68 seconds when N ₂ gas was not introduced. In the position S5, the time when N ₂ gas was introduced was 55 seconds, and the time when N ₂ gas was not introduced was 54 seconds. From this result, in the case where N ₂ gas was not introduced, the difference in drying time between the position S1 at the center of the area R1 and the position S5 at the corner was large. However, by introducing N ₂ gas, the time to completion of drying for the position S1 and the position S5 could be equalized. Therefore, it was confirmed that the rate of progress of drying in the plane of the substrate S can be made uniform by introducing N ₂ gas.

[Third Embodiment]

Next, the drying apparatus of the third embodiment of the present invention will be described with reference to Figs. 11 to 14. Fig. 11 is a cross-sectional view showing a schematic structure of the drying apparatus 102 according to the third embodiment. Fig. 12 is a perspective view for explaining the configuration of one nozzle 51 in the drying apparatus 102 of Fig. 11, and Fig. 13 is a cross-sectional view in a direction perpendicular to the longitudinal direction of the nozzle 51. Fig. 14 is an explanatory diagram showing the arrangement of the nozzles 51 viewed from the side of the placement table 3 (on the side of the substrate S) below. As a main difference from the drying apparatus 100 of the first embodiment, in the drying apparatus 102 of the present embodiment, the nozzle 51 has a pipe shape. Hereinafter, differences from the drying apparatus 100 of the first embodiment will be mainly described. In the drying apparatus 102 of this embodiment, the same components as those of the first embodiment are denoted by the same reference numerals and description thereof is omitted.

The drying apparatus 102 of this embodiment includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device 5B for injecting a gas toward the organic material film on the substrate S supported by the nozzle 51 and at least one of the flow rate of the gas jetted from the plurality of nozzles 51 and the kind of gas, ) Or a combination of two or more nozzles 51 as a unit. Further, the drying apparatus 102 is provided with a pressure control mechanism for controlling the pressure in the processing vessel 1.

The configuration of the processing container 1, the mounting table 3, the pressure control mechanism, and the control unit 6 in the drying apparatus 102 of this embodiment is the same as that of the drying apparatus 100 of the first embodiment.

<Gas injection device>

The gas injection device 5B includes a plurality of nozzles 51, a gas supply source 53 for supplying gas to each nozzle 51, a gas supply source 53 and each nozzle 51, 51 for supplying the gas to the gas supply pipe. In Fig. 11, eleven nozzles 51 are representatively shown. The gas injection device 5B includes a plurality of mass flow controllers (MFCs) 57 and a plurality of opening / closing valves 59 for controlling the gas flow rate in the middle of the pipe 55. [ The flow rate or injection speed of the gas injected from the nozzle 51, the kind of the gas, and the like are controlled by the mass flow controller (MFC) 57 and the opening / closing valve 59. 11, representative ones are shown for the pipe 55, the on-off valve 59 and the mass flow controller (MFC) 57, and the positions or the number of these positions are not limited to those shown in Fig. 11 .

As shown in Fig. 12, the nozzle 51 has a main body portion 51a having a long cylindrical shape. The main body portion 51a of the nozzle 51 is formed with a gas injection port 51b having a long slit shape along the longitudinal direction thereof. As shown in Fig. 13, in the present embodiment, one gas injection opening 51b is formed in the lower portion of the main body portion 51a, and two gas injection openings 51b in total are formed in the side portion. The three gas injection openings 51b are formed so as not to overlap each other at an angle of 90 degrees in the circumferential direction of the main body portion 51a. The inner space of the cylindrical main body portion 51a acts as a gas diffusion space for diffusing the gas. Since the inert gas, the solvent gas, or the mixed gas thereof can be injected in the form of a line by the gas injection port 51b having a long slit shape, the injection unevenness does not occur, The gas can be uniformly injected toward the fuel cell. Further, the number of the gas injection ports 51b may be one in the circumferential direction of the main body portion 51a, or two to four or more gas injection ports 51b may be formed at an arbitrary angle. The gas injection port 51b may be divided into a plurality of portions in the longitudinal direction of the main body portion 51a.

In this embodiment, the plurality of nozzles 51 includes a plurality of combinations, and at least one of the gas flow rate and gas type can be adjusted independently for each combination. In Fig. 11, two combinations (nozzle groups 52) constituted by a plurality of nozzles 51 are representatively shown. When it is necessary to distinguish each of the nozzle groups 52 for convenience of description, the nozzle group 52C, the nozzle group 52D, and the nozzle group 52C are denoted from the left side toward the paper of Fig. 14, the nozzle group 52D is arranged so as to oppose to the upper portion of the central portion of the rectangular substrate S, and the nozzle group 52C is disposed above the peripheral portion of the substrate S As shown in Fig. It is also possible to set the nozzle groups 52 individually for the more subdivided regions, not limited to the central portion and the peripheral portion of the substrate S.

[Arrangement of Nozzle]

In Fig. 14, the position of the substrate S is projected by arranging the nozzles 51. Fig. 14, the nozzle group 52D is disposed so as to oppose to the upper portion of the central portion of the rectangular substrate S, and the nozzle group 52C is arranged above the peripheral portion of the substrate S Respectively. Specifically, the nozzle group 52D having the five nozzles 51 is arranged so as to surround the nozzle group 52C having the sixteen nozzles 51 around the nozzle group 52D. The nozzle group 52C includes a plurality of nozzles 51 having different lengths of the main body portion 51a and the gas injection ports 51b, but there is no substantial difference therebetween.

In addition, the nozzle 51 may be arranged in consideration of the layout of the organic material film formed on the substrate S. Further, it is possible to inject the gas by setting the arrangement of the nozzles 51 individually for the more subdivided area, not limited to the two areas of the central part and the peripheral part of the substrate S. As another example of the arrangement, although not shown, the number of the nozzles 51 is relatively increased in the upper portion of the central portion of the substrate S where drying of the organic material film is relatively difficult, The number of the nozzles 51 may be relatively reduced above the periphery of the peripheral portion of the substrate S where drying is relatively easy.

The gas supply source 53 is provided with an inert gas supply source 53A and a solvent gas supply source 53B. The configuration of the gas supply source 53 is the same as that of the first embodiment.

In this embodiment, the plurality of nozzles 51 are provided above the substrate S so that gas can be injected toward the surface of the substrate S. The plurality of nozzle groups 52 are configured so that the flow rate of gas and the kind of gas can be adjusted independently for each nozzle group 52. That is to say, the combination of the pipe 55, the mass flow controller (MFC) 57 and the opening / closing valve 59 is arranged so as to control the flow rate of the gas independently for each nozzle group 52. The combination of the pipe 55 and the plurality of open / close valves 59 is configured so that the kind of the gas can be switched independently for each nozzle group 52 so as to be injected.

[Gas flow rate]

The plurality of nozzle groups 52 are configured to be capable of injecting inert gas at independent injection flow rates. For example, inert gas can be injected at a relatively large flow rate V11 from the nozzle group 52D disposed immediately above the center portion of the substrate S in which the drying of the organic material film is relatively difficult to proceed, have. An inert gas is supplied from the nozzle group 52C disposed just above the periphery of the substrate S to the periphery of the substrate S where the organic material film is relatively easily dried, and a flow rate V12, which is relatively smaller than the flow rate V11, As shown in FIG. It is also possible that no inert gas is injected into the peripheral portion of the substrate S.

The plurality of nozzle groups 52 are configured to be capable of jetting solvent gas at independent injection flow rates. For example, solvent gas can be jetted from the nozzle group 52C at a relatively large flow rate V13 to the peripheral portion of the substrate S where drying of the organic material film is relatively easy. In addition, solvent gas can be jetted from the nozzle group 52D at a flow rate V14 relatively smaller than the flow rate V13 at the central portion of the substrate S where drying of the organic material film is relatively difficult. It is also possible not to spray the solvent gas in the central portion of the substrate S.

The injection flow rate of the gas is not limited to two stages but may be one stage or three or more stages. Further, it is not limited to the central portion and the peripheral portion of the substrate S, and it is possible to set the flow rate separately for the more subdivided regions and to inject the gas.

[Gas type]

The plurality of nozzle groups 52 are configured to be capable of jetting an inert gas, a solvent gas, or a mixed gas of an inert gas and a solvent gas (hereinafter sometimes simply referred to as a "mixed gas") independently of each other. For example, the inert gas can be injected from the nozzle group 52D to the central portion of the substrate S where drying of the organic material film is relatively difficult. In addition, solvent gas can be injected from the nozzle group 52C to the peripheral portion of the substrate S where drying of the organic material film is relatively easy.

The plurality of nozzle groups 52 are configured to be capable of injecting the mixed gas in independent mixing ratios. For example, the mixed gas can be injected from the nozzle group 52D at a first mixing ratio with a low solvent gas concentration at a central portion of the substrate S where drying of the organic material film is relatively difficult. The mixed gas can be injected from the nozzle group 52C at a second mixing ratio higher than the first mixing ratio to the peripheral portion of the substrate S where the drying of the organic material film is relatively easy.

The mixing ratio of the mixed gas is not limited to two stages but may be one stage or three or more stages. Further, it is possible to spray the gas by setting the type or concentration individually for the finer regions, not limited to the central portion and the peripheral portion of the substrate S.

The drying process in the drying device 102 of the present embodiment is a process in which at least one of the gas flow rate and gas type is individually controlled by the control unit 6 in units of the nozzle group 52C or the nozzle group 52D Except that the gas is injected toward the surface of the substrate S while the gas is injected toward the surface of the substrate S. The drying of the organic material film in the plane of the substrate S is performed by spraying the gas toward the surface of the substrate S using the gas injection device 5B while controlling the pressure in the process container 1 during the drying process, It is possible to efficiently dry it in a short time while uniformizing the degree of uniformity.

[Procedure of drying treatment]

Next, the procedure of the drying process using the drying apparatus 102 will be described. First, as the previous step, the organic material film is printed on the substrate S in a predetermined pattern by an external inkjet printing apparatus (not shown). Next, the gate valve GV is opened, and the substrate S on which the organic material film is printed is transferred to the mounting table 3 of the drying apparatus 102 by an external transfer device (not shown).

Subsequently, the gate valve (GV) of the drying apparatus 102 is closed and the exhaust apparatus 19 is operated to exhaust the inside of the processing vessel 1 under reduced pressure. The pressure in the processing vessel 1 is monitored by the pressure gauge 25, and the degree of opening of the APC valve 23 is controlled to reduce the pressure to a predetermined degree of vacuum. In this way, a drying process for removing the solvent contained in the organic material film formed on the substrate S can be performed. During this drying process, by using the gas injection device 5B having a plurality of nozzles 51 capable of individually controlling the injection flow rate of the gas, the kind and the ratio of the gas, and the like, while controlling the pressure in the processing vessel 1, By spraying the gas toward the surface of the substrate S, it is possible to efficiently dry the substrate S in a short time while uniformizing the degree of drying of the organic material film in the plane of the substrate S. In addition, by introducing gas into the processing vessel 1 using the gas injection device 5B, an airflow is generated in the processing vessel 1, thereby promoting the discharge of the solvent staying in the processing vessel 1 .

Hereinafter, a gas injection control method when the substrate S is dried while jetting a gas in a pulse shape using the drying apparatus 102 will be described with reference to FIG. Fig. 15 shows an example of the gas injection flow rate and the timing of injection when the drying process of the substrate S is performed while the gas is sprayed in the form of a pulse to the drying apparatus 102. Fig. In this example, only inert gas such as nitrogen gas is used as the gas. 14, a nozzle group 52D disposed opposite to the upper side of the central portion of the rectangular substrate S, a nozzle group 52C disposed opposite to the upper side of the peripheral portion of the substrate S, And the inert gas is injected toward the substrate S at different timings. In an initial stage of the drying process for one substrate S, an inert gas is alternately injected in a pulse shape from the nozzle group 52D and the nozzle group 52C to the injection flow rate V21. The pulse period at this time is T1 and the pulse width is D1. In the next step of the drying process for one substrate S, an inert gas is alternately injected in a pulse shape from the nozzle group 52D and the nozzle group 52C to the injection flow rate V22. The pulse period at this time is T2 and the pulse width is D2. In a further stage of the drying process for one substrate S, an inert gas is alternately jetted in a pulse shape from the nozzle group 52D and the nozzle group 52C to the jet flow rate V23. The pulse period at this time is T3 and the pulse width is D3. Thus, in the drying apparatus 102, it is possible to vary the injection flow rates (V21 to V23) in accordance with the stage of the drying process for one substrate (S), and to change the duty ratio so as to inject the gas. The pulse widths T1 to T3 and the pulse widths D1 to D3 may be different in the nozzle group 52D and the nozzle group 52C and the pressure in the processing vessel 1, , The temperature, the kind of the solvent, the kind of the organic material film on the substrate S, and the like. Further, the injection flow rate, the pulse period, and the pulse width may be kept constant without changing.

After the drying process for one substrate S is completed, the gas injection by the gas injection device 5B and the exhaust by the exhaust device 19 are then stopped. After the inside of the processing container 1 is raised to a predetermined pressure, the gate valve GV of the drying device 102 is opened and the substrate S is transferred to the processing container 1 (not shown) by an external transfer device . By the above procedure, the drying process for one substrate S is completed.

Other configurations and effects in this embodiment are the same as those in the first embodiment. Further, the drying apparatus 102 can be applied to the manufacturing process of the organic EL element similarly to the first embodiment.

[Fourth Embodiment]

Next, the drying apparatus of the fourth embodiment of the present invention will be described with reference to Fig. 16 is a cross-sectional view showing a schematic structure of the drying apparatus 103 according to the fourth embodiment. As a main difference from the drying apparatus 100 of the first embodiment, in the drying apparatus 103 of this embodiment, at least one of the flow rate of gas and the kind of gas can be adjusted for each combination of the plurality of nozzles 51 have. In addition, the plurality of nozzles 51 have nozzles 51 which are not perpendicular to the upper surface of the plate-like substrate S but obliquely inject gas. Hereinafter, differences from the drying apparatus 100 of the first embodiment will be mainly described. In the drying apparatus 103 of this embodiment, the same components as those of the first embodiment are denoted by the same reference numerals, and description thereof is omitted.

The drying apparatus 103 of the present embodiment includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device 5C for injecting a gas toward the organic material film on the substrate S to be processed and a nozzle 51 for injecting at least one of the injection flow rate and gas kind of the gas injected from the plurality of nozzles 51, Or a combination of two or more nozzles 51 as a unit. The drying apparatus 103 is also provided with a pressure control mechanism for regulating the pressure in the processing vessel 1. [

The structure of the processing container 1, the mounting table 3, the pressure control mechanism, and the control unit 6 in the drying apparatus 103 of this embodiment is the same as that of the drying apparatus 100 of the first embodiment.

<Gas injection device>

The gas injection device 5C includes a plurality of nozzles 51, a gas supply source 53 for supplying gas to the respective nozzles 51, a gas supply source 53 for connecting the respective nozzles 51, 51 for supplying the gas to the gas supply pipe. In Fig. 16, eleven nozzles 51 are representatively shown. The gas injection device 5C includes a plurality of mass flow controllers (MFCs) 57 for controlling the gas flow rate and a plurality of opening / closing valves 59 at the middle of the pipe 55. [ The flow rate or injection speed of the gas injected from the nozzle 51, the kind of the gas, and the like are controlled by the mass flow controller (MFC) 57 and the opening / closing valve 59. 16, representative ones are shown for the pipe 55, the on-off valve 59, and the mass flow controller (MFC) 57. The positions or the number of these positions are not limited to those shown in FIG. 16 .

In this embodiment, as shown in Fig. 16, the plurality of nozzles 51 includes a nozzle 51 for jetting a gas perpendicularly to the upper surface of a flat substrate S, a nozzle 51 for obliquely injecting gas, (51). Specifically, the plurality of nozzles 51 arranged above the central portion of the rectangular substrate S are arranged so as to be capable of jetting gas substantially vertically to the upper surface of the substrate S. On the other hand, the plurality of nozzles 51 arranged opposite to the upper side of the peripheral portion of the substrate S eject gas at an angle of 30 DEG to 45 DEG to the upper surface of the flat substrate S, . Therefore, even if the injection flow rate of the gas is the same, it is possible to inject the inert gas directly to the central portion of the substrate S, in which drying of the organic material film is relatively difficult, S, the injection force of the inert gas can be weakened.

Further, in the present embodiment, the plurality of nozzles 51 include a plurality of combinations, and at least one of the gas flow rate and the gas kind can be independently controlled for each combination. 16, two combinations (nozzle groups 52) constituted by a plurality of nozzles 51 are representatively shown. When it is necessary to distinguish each of the nozzle groups 52 for convenience of explanation, the nozzle group 52E, the nozzle group 52F, and the nozzle group 52E are denoted from the left side toward the paper surface of Fig. 16, the nozzle group 52F is disposed so as to oppose to the upper portion of the central portion of the rectangular substrate S, and the nozzle group 52E is arranged above the peripheral portion of the substrate S As shown in Fig. It is also possible to set the nozzle groups 52 individually for the more subdivided regions, not limited to the central portion and the peripheral portion of the substrate S.

The gas supply source 53 is provided with an inert gas supply source 53A and a solvent gas supply source 53B. The configuration of the gas supply source 53 is the same as that of the first embodiment.

In this embodiment, the plurality of nozzles 51 are provided above the substrate S so that gas can be injected toward the surface of the substrate S. The plurality of nozzle groups 52 are configured so that the flow rate of gas and the kind of gas can be adjusted independently for each nozzle group 52. That is to say, the combination of the pipe 55, the mass flow controller (MFC) 57 and the opening / closing valve 59 is arranged so as to control the flow rate of the gas independently for each nozzle group 52. The combination of the pipe 55 and the plurality of open / close valves 59 is configured so that the kind of the gas can be switched independently for each nozzle group 52 so as to be injected.

[Gas flow rate]

The plurality of nozzle groups 52 are configured to be capable of injecting inert gas at independent injection flow rates. For example, inert gas can be injected at a relatively large flow rate V31 from the nozzle group 52F disposed immediately above the central portion of the substrate S in which the drying of the organic material film is relatively difficult to proceed have. An inert gas is supplied from the nozzle group 52E disposed immediately above the periphery of the substrate S to the periphery of the substrate S where the drying of the organic material film is relatively easy, As shown in FIG. It is also possible not to inject inert gas to the peripheral portion of the substrate S.

The plurality of nozzle groups 52 are configured to be capable of jetting solvent gas at independent injection flow rates. For example, solvent gas can be jetted from the nozzle group 52E at a relatively large flow rate V33 to the peripheral portion of the substrate S where drying of the organic material film is relatively easy. In addition, the solvent gas can be jetted from the nozzle group 52F at a flow rate V34, which is relatively smaller than the flow rate V33, at the central portion of the substrate S where drying of the organic material film is relatively difficult. It is also possible not to spray the solvent gas in the central portion of the substrate S.

The injection flow rate of the gas is not limited to two stages but may be one stage or three or more stages. Further, it is not limited to the central portion and the peripheral portion of the substrate S, and it is possible to set the flow rate separately for the more subdivided regions and to inject the gas.

Other configurations and effects in this embodiment are the same as those in the first embodiment. Further, the drying apparatus 103 can be applied to the manufacturing process of the organic EL element similarly to the first embodiment.

[Fifth Embodiment]

Next, a drying apparatus according to a fifth embodiment of the present invention will be described with reference to Fig. 17 is a cross-sectional view showing a schematic configuration of the drying apparatus 104 according to the fifth embodiment. As a main difference from the drying apparatus 100 of the first embodiment, in the drying apparatus 104 of the present embodiment, at least one of the gas injection flow rate and the gas type can be adjusted by using the combination of the plurality of nozzles 51 as a unit Consists of. The plurality of nozzles 51 are configured so as to be capable of jetting gas in a parallel or oblique direction, not perpendicular to the upper surface of the flat substrate S. Hereinafter, differences from the drying apparatus 100 of the first embodiment will be mainly described. In the drying apparatus 104 of this embodiment, the same components as those of the first embodiment are denoted by the same reference numerals, and description thereof is omitted.

The drying apparatus 104 of this embodiment includes a processing container 1 capable of vacuum evacuation, a mounting table 3 as a supporting member for supporting the substrate S in the processing container 1, A gas injection device 5D for injecting a gas toward the organic material film on the substrate S to which at least one of the nozzles 51 is injected and at least one of the injection flow rate and gas kind of the gas injected from the plurality of nozzles 51, As a unit. The drying apparatus 104 is also provided with a pressure control mechanism for controlling the pressure in the processing vessel 1. [

The structure of the processing container 1, the mounting table 3, the pressure control mechanism, and the control unit 6 in the drying apparatus 104 of this embodiment is the same as that of the drying apparatus 100 of the first embodiment.

<Gas injection device>

The gas injection device 5D includes a plurality of nozzles 51, a gas supply source 53 for supplying gas to the respective nozzles 51, a gas supply source 53 and the nozzles 51, 51 for supplying the gas to the gas supply pipe. The gas injection device 5D is provided with a plurality of mass flow controllers (MFCs) 57 and a plurality of opening / closing valves 59 for controlling the gas flow rate in the middle of the pipe 55. [ The flow rate or injection speed of the gas injected from the nozzle 51, the kind of the gas, and the like are controlled by the mass flow controller (MFC) 57 and the opening / closing valve 59. 17, representative ones are shown for the pipe 55, the on-off valve 59 and the mass flow controller (MFC) 57, and the positions and the number of these positions are not limited to those shown in FIG. 17 .

In this embodiment, as shown in Fig. 17, the plurality of nozzles 51 are arranged so as to oppose to the upper portion of the central portion of the rectangular substrate S, and also to the upper surface of the plate S So that the gas is injected in parallel or in a direction inclined at a predetermined angle. That is, the inert gas can be injected obliquely at an angle of, for example, 30 to 45 degrees from a position opposed to the central portion of the substrate S in a radial direction or horizontally downward . Therefore, the injection amount of the inert gas or the solvent gas can be made uniform within the plane of the substrate S.

Further, in this embodiment, the plurality of nozzles 51 constitute one combination unit. In Fig. 17, one combination (nozzle group 52G) composed of a plurality of nozzles 51 is shown. The nozzle group 52G is arranged so as to be opposed to the upper portion of the central portion of the rectangular substrate S. Further, the present invention is not limited to the central portion of the substrate S, but a plurality of nozzle groups 52 may be provided.

The gas supply source 53 is provided with an inert gas supply source 53A and a solvent gas supply source 53B. The configuration of the gas supply source 53 is the same as that of the first embodiment.

Other configurations and effects in this embodiment are the same as those in the first embodiment. Further, the drying apparatus 104 can be applied to the manufacturing process of the organic EL element similarly to the first embodiment.

Although the embodiment of the present invention has been described in detail for the purpose of illustration, the present invention is not limited to the above embodiment, and various modifications are possible. For example, the manufacturing process of the organic EL device is not limited to that shown in Fig. 4. For example, the EL layer may be formed from a positive electrode side to a negative electrode side in the order of [hole transporting layer / light emitting layer / electron transporting layer] / Hole transporting layer / light emitting layer / electron transporting layer], the drying apparatuses 100 to 104 of the present invention can be similarly applied.

In the drying apparatus 100 of the first embodiment, at least one of the gas injection flow rate and the gas type can be independently adjusted using the nozzles 51 as a unit, and the drying apparatuses 101 - 104), at least one of the jet flow rate of the gas and the kind of the gas can be adjusted independently by using the nozzle group 52 as a unit. However, in another embodiment, at least one of the flow rate of gas and the kind of gas may be independently adjustable in a state where the nozzle 51 and the nozzle group 52 are mixed.

1: Processing vessel
3: Wit
5, 5A: Gas injection device
6:
11: bottom wall
13: Side wall
15: ceiling
15a: Exhaust
17: Exhaust pipe
19: Exhaust system
21: Support pillars
23: APC valve
25: Manometer
51: Nozzle
53: gas supply source
53A: inert gas source
53B: Solvent gas source
55: Piping
57: Mass flow controller
59: Opening and closing valve
61:
62: User Interface
63:
100, 101: Drying apparatus
S: substrate
GV: Gate valve

Claims (24)

A drying apparatus for removing a solvent contained in an organic material film applied to a surface of a substrate and drying the same,
A processing container capable of vacuum evacuation,
An exhaust port for exhausting the gas in the processing container,
A supporting member for supporting the substrate in the processing container;
A gas injection device having a plurality of nozzles for injecting a gas toward the substrate supported by the support member;
And a control unit that independently adjusts at least one of a flow rate of the gas jetted from the plurality of nozzles and a kind of the gas to one nozzle or a combination of two or more nozzles as a unit,
Wherein the control unit maintains the pressure during the drying process while introducing the gas into the processing vessel within a range of 0.1 to 100 Pa,
The control unit starts to introduce gas into the processing container when the pressure in the drying process reaches the upper limit of the range after starting decompression exhaust in the processing container and continues the gas introduction and decompression and exhaustion until the end of the drying process And the drying device. The method according to claim 1,
Wherein the plurality of nozzles eject a drying gas for promoting drying of the organic material film. The method according to claim 1,
Wherein the plurality of nozzles eject a drying inhibiting gas that suppresses drying of the organic material film. The method according to claim 1,
Wherein the plurality of nozzles include a nozzle for ejecting a drying gas for promoting drying of the organic material film and a nozzle for ejecting a drying suppressing gas for suppressing drying of the organic material film. 5. The method according to any one of claims 1 to 4,
Wherein the plurality of nozzles includes a nozzle relatively far from the nozzle relatively far from the substrate supported by the support member. The method according to claim 1,
Wherein the nozzle has a cylindrical main body portion having a long length and a gas injection port having a long slit shape is formed along the longitudinal direction of the main body portion. The method according to claim 6,
Wherein the plurality of nozzles includes a first nozzle group for jetting a gas toward a central portion of the substrate supported by the support member and a second nozzle group for jetting gas toward the periphery of the substrate. A processing container capable of vacuum evacuation,
An exhaust port for exhausting the gas in the processing container,
A supporting member for supporting the substrate in the processing container;
A gas injection device having a plurality of nozzles for injecting a gas toward the substrate supported by the support member;
And a controller that independently adjusts at least one of a jet flow rate of the gas jetted from the plurality of nozzles and a kind of the gas as a unit or a combination of two or more nozzles as a unit, In which a solvent in an organic material film applied to a surface of a substrate is removed and dried,
The pressure during the drying process carried out while introducing the gas into the processing vessel is maintained within the range of 0.1 to 100 Pa,
The introduction of gas into the processing vessel is started when the pressure in the drying process reaches the upper limit of the above range after the decompression exhaust in the processing vessel is started and the gas introduction and decompression and exhaustion are continued until the end of the drying processing . &Lt; / RTI &gt; delete 9. The method of claim 8,
Wherein a spraying flow rate of the drying gas for promoting drying of the organic material film is sprayed toward the substrate while independently adjusting a single nozzle or a combination of two or more nozzles as a unit. 11. The method according to claim 8 or 10,
Wherein the spraying flow rate of the drying suppressing gas for suppressing the drying of the organic material film is sprayed toward the substrate while independently adjusting a single nozzle or a combination of two or more nozzles as a unit. 11. The method according to claim 8 or 10,
Wherein a mixing ratio of a drying gas for promoting drying of the organic material film and a drying inhibiting gas for suppressing drying of the organic material film is adjusted independently with a single nozzle or a combination of two or more nozzles as a unit, &Lt; / RTI &gt; 11. The method according to claim 8 or 10,
Wherein the gas is sprayed in a pulse shape. 11. The method according to claim 8 or 10,
Wherein the organic material film is applied onto the substrate by ink jet printing in the production of the organic EL device. The method according to claim 1,
Wherein the control unit maintains the pressure during the drying process within a range of 0.3 to 1 Pa. 16. The method according to claim 1 or 15,
Characterized in that when the pressure reaches the upper limit of the above range after starting decompression exhaust in the processing vessel, continuous introduction of gas into the processing vessel is started and the continuous introduction of the gas is continued until the end of the drying processing Lt; / RTI &gt; 16. The method according to claim 1 or 15,
Wherein when the pressure reaches an upper limit of the range after starting decompression exhaust in the processing vessel, the introduction of gas into the processing vessel for ejecting pulsed gas from the plurality of nozzles is started. 18. The method of claim 17,
Wherein said pulse-type gas ejection varies the injection flow rate, pulse period, or pulse width of said gas at an interval within a range of 10 to 100 seconds. The method according to claim 1,
Wherein the flow rate of the gas is set stepwise. 9. The method of claim 8,
Wherein the pressure during the drying process is maintained within a range of 0.3 to 1 Pa. The method according to claim 8 or 20,
Characterized in that when the pressure reaches the upper limit of the above range after starting decompression exhaust in the processing vessel, continuous introduction of gas into the processing vessel is started and the continuous introduction of the gas is continued until the end of the drying processing Lt; / RTI &gt; The method according to claim 8 or 20,
Wherein the introduction of the gas into the processing container for ejecting the pulsed gas from the plurality of nozzles is started when the pressure reaches the upper limit of the range after starting the reduced pressure exhaust in the processing container . 23. The method of claim 22,
Wherein said pulse-type gas ejection varies the injection flow rate, pulse period, or pulse width of said gas at intervals within a range of 10 to 100 seconds. 9. The method of claim 8,
Wherein the flow rate of the gas is set stepwise.

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