CN108987299A - Annealing device and the film manufacturing method for utilizing the annealing device - Google Patents

Annealing device and the film manufacturing method for utilizing the annealing device Download PDF

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Publication number
CN108987299A
CN108987299A CN201710919650.XA CN201710919650A CN108987299A CN 108987299 A CN108987299 A CN 108987299A CN 201710919650 A CN201710919650 A CN 201710919650A CN 108987299 A CN108987299 A CN 108987299A
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gas
heating plate
pressure
substrate
flow
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Granted
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CN201710919650.XA
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CN108987299B (en
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岸本克史
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Samsung Display Co Ltd
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Samsung Display Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H01L21/67109—Apparatus for thermal treatment mainly by convection
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
    • H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The present invention provides a kind of annealing device and the film manufacturing method using the annealing device.The annealing device of an embodiment according to the present invention includes: chamber；First heating plate is configured in the chamber；Second heating plate is configured in the chamber, and is configured in the one side of first heating plate, has multiple slits；And gas injector unit, it is configured to spray gas to the one side of first heating plate, wherein, the area in plane shared by the slit described in the per unit area of the second heating plate central portion is greater than the area in plane shared by the slit described in the per unit area of second heating plate edge part.

Description

Annealing device and the film manufacturing method for utilizing the annealing device
Technical field
The present invention relates to a kind of annealing device and utilize the film manufacturing method of the annealing device.
Background technique
Organic illuminating element is as self-luminous type element and in the case where being applied to display device, and not only visible angle is wide Extensively, contrast is outstanding, but also has the advantages that response speed, brightness, driving voltage good drawing property and can realize multicolor.
Organic illuminating element (organic light emitting device) has the anode in injection hole (hole) It is pressed from both sides between electrode (anode electrode) and the cathode electrode (cathode electrode) for injecting electronics (electron) Structure equipped with the organic film for including hole injection layer, hole transmission layer and luminescent layer.It is applied between described two electrodes When making alive, hole and electronics recombine in luminescent layer and form exciton, from excitation state be changed into ground state with the exciton and It shines.
Summary of the invention
It on the other hand, can as a kind of method for forming organic film between the anode electrode and cathode electrode To enumerate the Solution coating processes such as ink jet printing or nozzle print.The Solution coating processes, can be organic molten by making Liquid is discharged into desired position and makes the inert gas of the organic solution and high temperature and carry out to the organic solution Dry (curing) and drying (baking), to form the organic film.
But the drying and baking process are executed in different chambers, it is thus possible to which can become makes process become multiple The reason of miscellaneous and cost increase.In addition, in the drying and drying course, heating path is according to the row of the organic solution Put position and different, it is thus possible to the problem that organic solution is not dried equably can occur, this problem may be according to base Plate, for example, organic light emitting display panel substrate larger in area and become more serious.
Therefore, project to be solved by this invention is to provide a kind of annealing device, can simplify process and right Organic solution or organic film on substrate are uniformly heat-treated, and are obtained so as to produce the uniformity (uniformity) To the film of raising.
Another project to be solved by this invention is to provide a kind of film manufacturing method, by the organic solution on substrate Or organic film is uniformly heat-treated, so as to so that the uniformity is improved and minimizes impurity content.
Project of the invention is not limited to above-mentioned technical task, and those skilled in the art should can pass through It is clearly understood that unmentioned other technologies project below.
Annealing device for solving an embodiment according to the present invention for described problem includes: chamber；First heating Plate is configured in the chamber；Second heating plate is configured in the chamber, and is configured at the one side of first heating plate On, there are multiple slits；And gas injector unit, it is configured to body of emanating to the one side side spray of first heating plate, Wherein, the area in plane shared by the slit described in the per unit area of the second heating plate central portion is greater than described Area in plane shared by slit described in the per unit area of second heating plate edge part.
The gas injector unit includes multiple first flow path portions, multiple first flow path portion edge and first heating plate The parallel first direction of the one side extend and the flow path along the first direction be provided, and along intersecting with the first direction Second direction separate configuration.
In addition, the slit be along the first direction extend shape, the slit in the first direction The width in centre portion can be greater than the width of the end in the first direction of the slit.
In addition, the multiple slit includes: the first slit, positioned at the center of the second direction of second heating plate Portion；And second slit, compared to the edge part for the second direction that first slit is located at second heating plate, In, the width of first slit can be greater than the width of second slit.
Definition has heat treatment space between first heating plate and second heating plate, can also include first secondary Heater is configured to that more heats can be provided to central portion compared to the edge part of the heat treatment space.
In addition, further includes: substrate setter plate is configured between first heating plate and second heating plate；Air-flow Stopper is configured at first heating plate and the second heating plate time, and matches along the edge of second heating plate It is set to belt shape；Curtain gas ejection section is configured at the outer of the airflow-resistive block in a manner of surrounding the airflow-resistive block Side；Second secondary heater, is configured at the outside of the airflow-resistive block in a manner of surrounding the airflow-resistive block, and is configured to Heat is provided to the heat treatment space side；And hood, it is configured at second heating plate top, wherein the gas Injection unit is configured to body of emanating to the substrate setter plate side spray.
The gas injector unit further include: gas supply source supplies the gas；And feed tube, described Flow path is provided between gas supply source and multiple first flow path portions of the chamber interior, wherein second heating plate With multiple through-holes, the first flow path portion is configured between first heating plate and second heating plate, the gas At least part of supply pipe may be directly connected to the first flow path portion through second heating plate by the through-hole.
In addition, first secondary heater is configured between second heating plate and the hood, described first is secondary Heater extends along the first direction and separates configuration along the second direction, to be multiple, and first pair adds Hot device can be Chong Die with the first flow path portion.
Second heating plate has multiple through-holes, the gas injector unit further include: gas supply source, described in supply Gas；Feed tube provides stream between the gas supply source and multiple first flow path portions of the chamber interior Road；And multiple second flow path portions, it is protruded from the first flow path portion and second heating plate is run through by the through-hole, and It is configured to body of emanating to the substrate setter plate side spray, wherein the first flow path portion is configured at second heating plate and institute It states between hood, the multiple first flow path portion is 2n(herein, n is natural number) is a, and the feed tube includes: One gas service pipes extends along a direction；And two second gas distribution pipes, from first gas distribution pipe branch, In, the flow path length from the gas supply source to each first flow path portion can be identical.
In addition, first secondary heater extends along the first direction and separates configuration along the second direction, and it is 2n+1A, first secondary heater is configured in the two sides in the first flow path portion.
The film manufacturing method of the above-mentioned embodiment according to the present invention for being used to solve another project, comprising: add first Sandwiched discharge has the step of substrate of organic solution between hot plate and second heating plate with multiple slits；And to the base The step of plate side spray emanates body and contacts the gas with the substrate and the gas is discharged by the slit, In, area in plane shared by the slit described in the per unit area of the second heating plate central portion is greater than described the Area in plane shared by slit described in the per unit area of two heating plate edge parts.
After the step of substrate described in sandwiched, further includes the steps that the pressure in the space to manufacture film controls, control The step of making the pressure includes: first time pressure controlling step, is decompressed to lower than the first pressure from first pressure Two pressure；Second of pressure controlling step maintains the second pressure；Third time pressure controlling step, from the second pressure It is decompressed to the third pressure lower than the second pressure；4th pressure controlling step, maintains the third pressure；And the 5th Secondary pressure controlling step is forced into the 4th pressure higher than the third pressure from the third pressure, wherein the first time Pressure controlling step to the 5th pressure controlling step can successively execute in a chamber.
The step of spraying the gas includes: first time gas injection step, sprays gas with first flow；Second of gas Body injecting step sprays gas from first flow decrement to less than the second flow of the first flow；Third time gas Body injecting step maintains the second flow and sprays gas；4th gas injection step, from the second flow be reduced to Less than the second flow flow and spray gas；5th gas injection step maintains the state for not spraying gas；6th Secondary gas injection step, restarts gas injection, and flow is increased to third flow and sprays gas；7th gas injection Step maintains the third flow and sprays gas；And the 8th gas injection step, it is reduced from the third flow to small In the flow and injection gas of the third flow.
In addition, the 5th gas injection step can at least partly be held simultaneously with the third time pressure controlling step Row, the 6th gas injection step can be at least partly performed simultaneously with the 4th pressure controlling step.
In addition, the pressure change rate per unit time in the first time pressure controlling step can be greater than the third Pressure change rate per unit time in secondary pressure controlling step.
In the first time pressure controlling step, second of pressure controlling step and third time pressure controlling step The temperature of the substrate is 35 DEG C or more and 60 DEG C hereinafter, the 4th pressure controlling step and the 5th pressure controlling step In the substrate temperature be 200 DEG C or more and 300 DEG C hereinafter, the third time gas injection step be make the gas and The substrate the organic solution contact the step of, the 7th gas injection step can be make the gas with it is described The step of organic film contact of substrate.
The step of controlling the pressure further includes maintaining the 4th pressure after the 5th pressure controlling step At least part of 6th pressure controlling step of power, the 7th gas injection step can be with the 6th pressure Rate-determining steps are performed simultaneously, and the 8th gas injection step can be at least partly same with the 6th pressure controlling step Shi Zhihang.
In addition, the first time pressure controlling step, second of pressure controlling step and third time pressure control step Rapid execution 5 minutes or more and 10 minutes time below, the 4th pressure controlling step and the 5th pressure control Step execution 15 minutes or more and 25 minutes time below, the 6th time pressure controlling step can execute 5 minutes or more and 15 Time below minute.
The first time gas injection step to the 8th gas injection step continuously performs in one chamber, The first time pressure controlling step is to the 5th pressure controlling step and the first time gas injection step to In eight gas injection steps, 1mm or more and 20mm are maintained separated by a distance between the substrate and second heating plate Hereinafter, in the first time pressure controlling step into third time pressure controlling step, 90 weights of the organic solution total weight % or more is measured by gasification and by slit discharge, the second pressure can be 0.1torr or more and 10torr hereinafter, described the Three pressure can be 10-4Torr or more and 10-2Torr is hereinafter, the 4th pressure can be 700torr or more.
In addition, definition has heat treatment space between the substrate and second heating plate, the second flow is tool There is the flow of 1 times or more of value of the every 1 minute heat treatment space volume, the third flow can be with every 1 minute The flow of 5 times or more of value of the heat treatment space volume.
The specific item of other embodiments is included in detailed description and attached drawing.
The annealing device of an embodiment according to the present invention, by as heat treatment object substrate top/ Lower part configures heating plate and prevents vaporized organic solvent vapor from condensing again, so as to so that the impurity content in film is minimum Change.In addition, by being configured to different from the slit arrangement density in edge part in the central portion of upper Heating Plate, so as to improve Drying uniformity.
In addition, the drying process and baking process of substrate continuously perform in a chamber, so as to so that process is simple Change and shorten production time per piece (tact time), and can prevent during substrate introduces/draws process chamber there may be Pollutant attachment.
In addition, the film manufacturing method of an embodiment according to the present invention, it can form that the uniformity is improved and impurity contains Measure the film being minimized.
The effect of embodiment according to the present invention is not limited to the content of explanation listed above, includes in this specification More effects.
Detailed description of the invention
Fig. 1 is the exploded perspective view of the annealing device of an embodiment according to the present invention.
Fig. 2 is the sectional side view of the annealing device of Fig. 1.
Fig. 3 is the sectional side view in the another location of the annealing device of Fig. 1.
Fig. 4 is the second heating plate for showing Fig. 1 and the perspective view of the first secondary heater.
Fig. 5 is the plan view of the second heating plate of Fig. 4.
Fig. 6 is the perspective view for showing the gas injector unit of Fig. 1.
Fig. 7 is the first flow path portion of Fig. 6 and the bottom isometric view in second flow path portion.
Fig. 8 is the sectional view cut according to the A-A ' line of Fig. 6.
Fig. 9 is the exploded perspective view of annealing device according to another embodiment of the present invention.
Figure 10 is the sectional side view of the annealing device of Fig. 9.
Figure 11 is the second heating plate for showing Fig. 9 and the perspective view of the first secondary heater.
Figure 12 is the perspective view for showing the gas injector unit of Fig. 9.
Figure 13 is the first flow path portion of Figure 12 and the bottom isometric view of third flow path portion.
Figure 14 is the sectional view cut according to the B-B ' line of Figure 12.
Figure 15 to Figure 21 is the figure for illustrating the film manufacturing method of an embodiment according to the present invention.
Figure 22 to Figure 25 is the figure for showing the result according to experimental example.
Symbol description
100: 200: the first heating plate of chamber
300: the second heating plates 400: substrate setter plate
500: gas injector unit
Specific embodiment
Advantages and features of the invention and the method for realizing them, by referring to hereinafter together with attached drawing specifically Bright embodiment becomes more clear.However, the present invention can be presented as various embodiments different from each other, be not limited to Lower the disclosed embodiments, however, embodiment is used for the purpose of making disclosure of the invention become complete and making belonging to the present invention The those skilled in the art of technical field are completely understood by the scope of the present invention and provide, and present invention is limited only to the models of claim It encloses.
Element (elements) is located at other yuan when either layer is regarded as being located at " top (on) " of other elements or layer The case where being folded with other layers or other elements immediately above or intermediate of part be all completely contained in.On the contrary, element is regarded as When positioned at " (directly on) directly above ", indicate in intermediate not sandwiched other elements or the situation of layer.Entirely illustrating In book, identical reference marks indicates identical constituent element."and/or" includes each and one of the project being previously mentioned Above all combinations.
As " following (below) " of spatially opposite term, " lower section (beneath) ", " lower part (lower) ", " on Side (above) ", " top (upper) " etc. as shown, can in order to relatively easily describe an element or constituent element with Correlation between other elements or constituent element and use.The direction one illustrated in spatially opposite term and figure It rises in use, being understood to include the term of the opposite directions of element.For example, turning over by the element illustrated in figure In the case where, the element for being described as " lower section (below or the beneath) " of other elements can be placed to other elements " top (above) ".Therefore, in the direction of lower section and top can be all completely contained in by schematical term " lower section ".
In the present specification, the 1st direction X refers to any one direction in plane, the 2nd direction Y refer in the plane with The direction that 1st direction X intersects, the 3rd direction Z refer to the direction vertical with the plane.
In the present specification, " heat treatment ", which refers to, intentionally executes temperature control to heat treatment object.At the heat Reason can with about 0 DEG C or more or about 35 DEG C or more or about 50 DEG C or more or about 60 DEG C or more or about 100 DEG C with Upper or about 150 DEG C or more or about 200 DEG C or more or about 300 DEG C or more temperature execute.
Hereinafter, being described with reference to the embodiment of the present invention.
Fig. 1 is the exploded perspective view of the annealing device of an embodiment according to the present invention.Fig. 2 is by the heat treatment of Fig. 1 The sectional side view that device is cut according to second direction Y is the sectional side view for cutting the position that can show feed tube 650. Fig. 3 is the sectional side view for cutting the annealing device of Fig. 1 according to second direction Y, is to cut to show the first secondary heater The sectional side view of 710 position.
Referring to figs. 1 to Fig. 3, the annealing device 1000 according to the present embodiment includes: chamber 100；First heating plate 200 with Second heating plate 300, is configured in chamber 100；Substrate setter plate 400 is configured at the first heating plate 200 and the second heating plate Between 300；And gas injector unit 600, spray gas.
Chamber 100 can provide the state space for carrying out heat treatment procedure.For example, chamber 100 will during carrying out process It is isolated from outside inside it, so as to be configured to carry out independent pressure control and temperature control in state space System.Though not illustrating in figure, the substrate introducing portion and/or substrate of shape of slit could be formed in the side wall of chamber 100 Lead division.
Substrate setter plate 400 is configured inside chamber 100.The offer of substrate setter plate 400 can steadily be disposed as heat The space of the substrate (not shown) of processing target object etc..Although Fig. 1 etc. illustrates, display base plate setter plate 400 is in four sides in the plane The case where shape, but the present invention is not limited thereto, it in the plane can also be with rounded etc..Substrate setter plate 400 passes through lifting Device 450 can be supported and go up and down.Lifting device 450 can be elevating lever etc..
First heating plate 200 can be configured at the lower part of substrate setter plate 400 in chamber 100.First heating plate 200 can To be to provide the inferior part inferior part of heat from substrate downside (not shown).The shape of first heating plate 200 in the plane can be Shape corresponding with substrate setter plate 400.First heating plate 200 can pass through lifting device 450 with substrate setter plate 400 together Fixed and lifting.That is, even if in the case where lifting device 450 works, the first heating plate 200 and substrate setter plate 400 it Between can also be maintained scheduled distance separated by a distance.
Hereinafter, also referring to the constituent element that annealing device 1000 is explained in more detail in Fig. 4 to Fig. 8.
Fig. 4 is the second heating plate 300 for showing Fig. 1 and the perspective view of the first secondary heater 710.Fig. 5 be Fig. 4 second plus The plan view of hot plate 300.
Referring to figs. 1 to Fig. 5, the second heating plate 300 can be configured at the top of substrate setter plate 400 in chamber 100.The Two heating plates 300 can be from substrate upside (not shown) and provide the upper Heating Plate of heat.Second heating plate 300 and first adds Space between hot plate 200 is defined as heat treatment space 500.It can be using sandwiched as heat treatment mesh in heat treatment space 500 Mark the substrate (not shown) etc. of object.That is, substrate (not shown) can be located in the first heating plate 200 and the second heating plate 300 Between in the state of be heat-treated.Accordingly, the substrate can be inhibited to be bent, and vaporized solvent vapo(u)r can be prevented again It condenses and pollutes the substrate.
Shape in the plane of second heating plate 300 can be shape corresponding with substrate setter plate 400.Second heating plate 300 can have multiple through-hole 300h and multiple slits 310.Shape in the plane of each through-hole 300h can be generally circular. It is inserted in each through-hole 300h by the feed tube 650 of aftermentioned gas injector unit 600.
Multiple slits 310 can form the air-flow flowed from a side of the second heating plate 300 to the other side.With multiple narrow Second heating plate 300 of seam 310 can play the function as plate washer (baffle plate).Multiple slits 310 can be The shape extended along first direction X.
In an illustrative embodiment, 310 institute of slit in the per unit area of the central portion 300C of the second heating plate 300 The area in plane accounted for can be greater than in the per unit area of the edge part 300E of the second heating plate 300 shared by slit 310 Plane on area.In the present specification, " edge part " of certain constituent element refers to positioned at " the center of the constituent element Part around portion ".That is, edge part refers to the region for surrounding central portion from outside.
The central portion 300C of second heating plate 300 and the substrate (not shown) that can be configured in substrate setter plate 400 Central portion overlapping in plane, the edge part 300E of the second heating plate 300 can be and the side in the plane of substrate (not shown) The part of edge overlapping.
For example, multiple slits 310 include: the first slit 311, positioned at the center of the second direction Y of the second heating plate 300 Portion；And second slit 312, the edge part of the second direction Y of the second heating plate 300 is located at relative to the first slit 311, In, the width t of the first slit 311311aThe width t of the second slit 312 can be greater than312.In the present specification, " the width of slit Degree " refers to the width of the slit on the direction perpendicular to slit extending direction.For example, the width t of the first slit 311311aIt can To be the width t of the second slit 3123122 times or more.
In the case where the substrate as heat treatment object includes organic solvent, during heat treatment at least partially Organic solvent is gasified, so as to be discharged by the slit 310 of the second heating plate 300.At this point, the central portion of the substrate is upper Portion, that is, the top of the edge part of the central portion of heat treatment space 500 and the substrate, that is, the edge part of heat treatment space 500 Between, the saturation state of the organic solvent vapor may be different.The present invention is not limited thereto, for example, organic solvent is in institute The vaporized amount of central portion for stating substrate (not shown) can be greater than organic solvent in the vaporized amount in the edge part of the substrate, And it can be greater than in the vapour pressure of the organic solvent in the central portion region of the substrate in the edge part region of the substrate The organic solvent vapour pressure.That is, the central portion region of heat treatment space 500 is compared to edge part region, it is vaporized Organic solvent relatively faster reaches saturation state, so as to inhibit further to gasify.
According to the annealing device 1000 of the present embodiment, make to be equivalent to narrow in the region of the central portion of substrate (not shown) Area shared by seam 310 is greater than area shared by the slit 310 being equivalent in the region in the substrate edges portion, therefore can be with structure The amount of organic solvent vapor as the discharge of slit 310 by the second heating plate 300 is different according to the region of substrate.Such as It is configured to, passes through in the vaporized organic solvent of central portion of the second direction Y of the substrate with relatively wide area The discharge rapidly of the first slit 311, in contrast, in the vaporized organic solvent in edge part of the second direction Y of the substrate The velocity of discharge compared to central portion it is slow.Accordingly, it on the entire area of the substrate as heat treatment object, can be improved organic The degree of solvent gasification, that is, drying uniformity.
In addition, in the case where the substrate as heat treatment object includes organic solvent, in order to make the entire area of substrate It equably dries, substrate center portion can be different from gas injection amount required by edge part.The present invention is not limited thereto, example Such as, in the slit 310 of the second heating plate 300 in the case where central portion and edge part have uniform width, in order to ensure dry The dry uniformity can require the gas for penetrating more various flow to edge part side spray relative to central portion.On the contrary, according to the present embodiment Annealing device 1000 has as the slit 310 of the second heating plate 300 has in central portion than edge part wider width Although penetrating the gas of more various flow to central portion side spray compared to edge part, the effect of drying uniformity can also ensure that.Cause This, can penetrate more process gas, institute to the central portion side spray of the substrate of the organic solution Relatively centralized comprising organic solvent Heat treatment can be effectively performed.
In some embodiments, first slit 311 is the shape extended to first direction X, the first party of slit 310 To the width t of the central portion of X311aThe width t of some end of the first direction X of the first slit 311 can be greater than311b.For example, The width t of central portion311aIt can be the width t of end311b2 times or more.
According to the annealing device 1000 of the present embodiment, it is configured to make 310 row of slit by the second heating plate 300 The amount of organic solvent vapor out is different according to substrate (not shown) region.Such as be configured to, the of the substrate The vaporized organic solvent of central portion of one direction X is by the first discharge rapidly of slit 310 with relatively wide area, with this On the contrary, the velocity of discharge in the vaporized organic solvent in edge part of the first direction X of the substrate is slow compared to central portion.According to The drying uniformity of organic solvent can be improved on the entire area of substrate in this.It is different from shown in figure, the first slit 311 Width can also tend to end from the central portion of first direction X and gradually become smaller.
In addition, annealing device 1000 includes the first secondary heater 710, so as to be configured to compared to heat treatment space 500 edge part is capable of supply that relatively more heats to central portion side.
In an illustrative embodiment, the first secondary heater 710 is configured in the second heating plate 300.First secondary heating Device 710 is configured in the second heating plate 300 and will be between aftermentioned hood 910.First secondary heater 710 may be at Second heating plate 300 abuts and contact or state spaced apart by a predetermined distance.
First secondary heater 710 can be the micro-heater with subtle thickness along the first direction X shape extended.The One secondary heater 710 separates configuration along first direction X and second direction Y, thus the first secondary heater 710 can be it is multiple.
The heat provided by the first secondary heater 710 can be different according to the region of heat treatment space 500.For example, the One secondary heater 710 and the central portion of heat treatment space 500 overlap, in contrast, in the edge part of heat treatment space 500 The first secondary heater 710 can not be configured.The present invention is not limited thereto, for example, the central portion region of the substrate compared to Edge part region, vaporized organic solvent relatively faster reach saturation state, so as to inhibit further to gasify.
According to the annealing device 1000 of the present embodiment, it is configured to make to supply to the region for the central portion for being equivalent to the substrate The heat answered is greater than the heat supplied to the region for the edge part for being equivalent to the substrate, so as to be configured to make from the base The amount of the organic solvent vapor of plate gasification is different according to the region of substrate (not shown).For example, in the central portion quilt of the substrate More heats are provided and the gasification of the organic solvent vapor that induces relatively large number of amount, in contrast, on the side of the substrate Edge can produce the organic solvent vapor of relatively small number of amount.Meanwhile by increasing the temperature section in thermal treatment zone 500 Add, so as to so that the saturated vapour pressure of 500 central portion of thermal treatment zone is greater than the saturated vapor of 500 edge part of thermal treatment zone Pressure, and have can induce organic solvent more vaporized effect.Accordingly, it can be improved on the entire area of substrate The drying uniformity of solvent.
Fig. 6 is the perspective view for showing the gas injector unit of Fig. 1.Fig. 7 is first flow path portion 610 and the second flow path of Fig. 6 The bottom isometric view in portion 620.Fig. 8 is the sectional view cut according to the A-A ' line of Fig. 6.
Referring to figs. 1 to Fig. 8, gas injector unit 600 includes: gas supply source 670, is configured at outside chamber 100；First Flow path portion 610 is being configured between the first heating plate 200 and the second heating plate 300 in chamber 100；And feed tube 650, the flow path between gas supply source 670 and first flow path portion 610 is provided.
Gas supply source 670 is configured at outside chamber 100 and storage technology gas, and is configured to supply to the inside of chamber 100 Answer process gas.The process gas may include inert gas, and inert gas is as long as the low and stable substance of reactivity It is not particularly limited, for example, it may be nitrogen (N2) or argon gas (Ar) or be to nitrogen or argon gas doping hydrogen (H2) and/ Or the gas of CO gas (CO).
Feed tube 650, which is provided, is transferred to multiple first flow path portions for the process gas provided from gas supply source 670 610 flow path.Feed tube 650 can run through the second heating plate 300 by the through-hole 300h of second heating plate 300.
In an illustrative embodiment, feed tube 650 can be the form that following form is repeated as many times, that is, grade Join (cascade) form: a pipe for being connected to 670 side of gas supply source is branched off into two pipes, and above-mentioned is branched into two Pipe be branched off into two pipes again respectively.For example, feed tube 650 includes: first gas distribution pipe 651, along a direction (example Such as, third direction Z) extend；And two the second distribution pipes 652, is directly connected in from 651 branch of first gas distribution pipe One flow path portion 610.In this case, second gas distribution pipe 652 and first flow path portion 610 are respectively 2nIt is a, second gas Distribution pipe 652 can run through the through-hole 300h of the second heating plate 300.Herein, n is natural number.By will be from gas supply source 670 feed tube 650 to first flow path portion 610 is configured to cascade form, can make accordingly from gas supply source 670 to 2n The flow path length of a second gas distribution pipe 652 is actually all the same.Accordingly, can make to be supplied to second gas distribution pipe 652 And the process gas in first flow path portion 610 flow and supply at the time of it is practically identical.In the present specification, " flow path is long Degree " refers to the length of gas flow paths.
In addition, prolonging from the position that second gas distribution pipe 652 is directly connected to first flow path portion 610 to first direction X The flow path length of the one end first direction X in the first flow path portion 610 stretched and the flow path length of the other end to first direction X can be with It is mutually the same.However, the shape of feed tube 650 and configuration are not limited thereto, various modifications can be carried out.
First flow path portion 610 extend along the first direction X parallel with one side (the upper surface of the drawing) of the first heating plate 200 and Flow path to first direction X is provided.Y separates configuration in a second direction in first flow path portion 610, so that first flow path portion 610 can be with It is multiple.The one end in first flow path portion 610 and/or the other end can be and the second flow path portions 620 of the extension of Y in a second direction It is in fluid communication with each other.First flow path portion 610 can overlap along third direction Z with the first secondary heater 710.
First flow path portion 610 is configured to distribute from the received process gas of feed tube 650 to first direction X And penetrate the process gas to substrate (not shown) side spray as heat treatment object.For example, first flow path portion 610 is constituted To emanate body to 200 side of the first heating plate and/or 400 side spray of substrate setter plate, first flow path portion 610 be can have for making work Skill gas injection is to its external jet port 610h.Jet port 610h is that external opening is extended to from first flow path portion 610, can It is formed in the position for the body that is easy to emanate to 400 side spray of substrate setter plate.Section shape in first flow path portion 610 is generally circular In the case where, jet port 610h can be located at the semicircle of 200 side of the first heating plate in first flow path portion 610, that is, under on drawing On the semicircle of side.
The process gas sprayed from first flow path portion 610 can have about 35 DEG C or more and 300 DEG C of temperature below or About 35 DEG C or more and 60 DEG C of temperature below or about 200 DEG C or more and 300 DEG C of temperature below.By at the heat of substrate To substrate-side spray technology gas in science and engineering sequence, especially drying process, the organic solvent of the substrate can be significantly improved Gasification rate, and can prevent vaporized solvent vapo(u)r from condensing again and polluting the substrate.For example, induction is vaporized molten Agent steam is discharged by slit 310 and improves gasification rate, and can prevent from condensing again.In addition, abundant in organic solvent Subsequent heat treatment process after gasification can be easier to make hot place accordingly to substrate-side spray technology gas that is, in baking process Manage the not discharged residual solvent steam discharge in space 500.
Though also, the present invention is not limited thereto, and is to be used to form having for organic illuminating element in the organic solution In the case that the solution of machine layer and the substrate are organic illuminating element manufacture substrate, by the heat treatment procedure in substrate, To substrate-side spray technology gas especially in baking process, (the In Pixel of the uniformity in pixel can be improved to have Uniformity, IPU) effect.
For example, in the case where discharging organic solution to pixel region and being dried to it and execute baking process, Gasification rate in the edge part of a pixel can be faster than the gasification rate of the central portion in a pixel.In a pixel It is interior, if increased in the gasification rate difference of edge part and central portion, there can be the edge for the organic film being formed in pixel The problem of thickness in portion and the difference in thickness of central portion become larger.However, the annealing device 1000 of embodiment according to the present invention, By the way that the water based on process gas can be formed to substrate-side spray technology gas in heat treatment procedure, especially baking process Square to air-flow, edge part in a pixel and the film thickness at central portion can be made to be formed uniformly accordingly.That is, logical In the case where crossing solution coating process formation organic luminous layer, it may have be capable of forming the organic luminous layer with flat surfaces Effect.
In some embodiments, annealing device 1000 can also include: airflow-resistive unit 800, the second secondary heater 720 and/or exhaust unit 900.
Airflow-resistive unit 800 plays the space for making to carry out heat treatment procedure, that is, in heat treatment space 500 and chamber 100 The effect isolated each other of other spaces.Accordingly, the pollution of the substrate as caused by impurity in chamber 100 (not shown) can be made most Smallization.For example, airflow-resistive unit 800 may include airflow-resistive block 810 and curtain gas ejection section 830.
Airflow-resistive block 810 can be configured at the first heating plate 200 and the second heating along the edge of the second heating plate 300 Between plate 300.Airflow-resistive block 810 can be least partially overlapped with substrate setter plate 400 and the second heating plate 300.Air-flow Stopper 810 can be configured to substantially quadrangle belt shape and surround heat treatment space 500.810 pairs of airflow-resistive block heat treatments The side in space 500 carries out physical blockage (Blocking), so as to so that open space minimizes.
Curtain gas ejection section 830 can be configured at outside airflow-resistive block 810 in a manner of surrounding airflow-resistive block 810 Side.Curtain gas ejection section 830 may be configured as, to 810 side of airflow-resistive block, specifically, to substrate setter plate 400 by means of Lifting device 450 and the region direction that abuts with substrate setter plate 400 of airflow-resistive block 810 sprays gas curtain gas in the case where rising Body (curtain gas).For example, curtain gas ejection section 830 (can not schemed from the curtain gas source of supply outside chamber 100 Show) it receives curtain gas and sprays curtain gas.The curtain gas can be inert gas.Curtain gas ejection section 830 is logical It crosses to form gas gas curtain, can prevent the air-flow connected between the inside and outside of heat treatment space 500.
Second secondary heater 720 is configured at 810 outside of airflow-resistive block in a manner of surrounding airflow-resistive block 810, and can Heat is provided to be configured to 500 side of heat treated space.For example, the second secondary heater 720 can be arranged in 100 inside of chamber Wall and from substrate (not shown) side provide heat side heater.
Gas in chamber 100 is discharged in exhaust unit 900, so as to so that the pressure control in chamber 100 becomes easy.Example Such as, exhaust unit 900 may include hood 910, exhaust pump 920 and exhaust pipe 930.
Exhaust pump 920 is configured at outside chamber 100, and can be by connecting inside exhaust pipe 930 and chamber 100.Row Tracheae 930 connects 100 inside of chamber and exhaust pump 920, to provide the channel for discharging the gas trapped from hood 910. Exhaust pump 920 can be acted on by pressure makes the gas inside chamber 100 can control chamber accordingly to 100 outside drain of chamber Pressure inside 100.For example, exhaust pump 920 is and making the gas inside chamber 100 to 100 outside drain of chamber to chamber It is depressurized inside 100, so as to be formed as steaming 100 inside atmosphere of chamber with the saturation for the organic solvent to gasify Vapour pressure is identical or lower, accordingly, the gasification of organic solvent can be made to become easy.In addition, exhaust pump 920 can be induced by gas The discharge of the organic solvent of change.Exhaust pump 920 can enumerate dry pump or turbine pump etc..
Hood 910 can be with the adjacent configuration of the ceiling of chamber 100.For example, can be configured at the second heating plate 300 and The top of feed tube 650.Hood 910, which can be trapped effectively, to be added by the slit 310 of the second heating plate 300 from second The mobile gas in the upward side in 300 downside of hot plate.For example, from the organic solvent of substrate gasification (not shown) and from gas injection list The process gas of 600 injection of member can be trapped and be discharged by hood 910 after being discharged by the slit 310 of the second heating plate 300. Area in the plane of hood 910 can be bigger than the area in the plane of the second heating plate 300.That is, hood 910 can be with The second heating plate 300 is completely covered.In addition, as shown in Fig. 2 etc., in the case where hood 910 has inclined surface, it is possible to reduce From the edge side of the second heating plate 300 rise air-flow and from center side rise air-flow between path difference.
Hereinafter, illustrating annealing device according to another embodiment of the present invention.However, omit to according to Fig. 1's etc. The explanation of the identical composition of the annealing device of embodiment, about these, the those skilled in the art of the technical field of the invention It can be clearly understood that by attached drawing.
Fig. 9 is the exploded perspective view of annealing device according to another embodiment of the present invention.Figure 10 is the heat treatment of Fig. 9 The sectional side view of device.Figure 11 is the second heating plate for showing Fig. 9 and the perspective view of the first secondary heater.
Referring to Fig. 9 to Figure 11, according to the annealing device 1001 of the present embodiment, first flow path portion 611 is configured at second and adds The top of hot plate 301, this point are the points different from the annealing device 1000 of embodiment according to Fig. 1 etc..
Second heating plate 301 can have multiple through-hole 301h and multiple slits 330.In the plane of each through-hole 301h Shape can be roughly circular.Multiple through-hole 301h separate configuration along first direction X and second direction Y, can substantially be formed as Matrix array.Can be inserted in each through-hole 301h will aftermentioned gas injector unit 601 third flow path portion 630.
Multiple slits 330 can form the air-flow flowed from 301 1 side of the second heating plate to the other side.With multiple slits 330 the second heating plate 301 can play function identical with plate washer.Multiple slits 330 may include: main slit 350, have The shape extended along first direction X；And secondary slit 360, there is the shape that Y extends in a second direction.Main slit 350 and pair are narrow Seam 360 can substantially form the slit of mesh shape.
In an illustrative embodiment, in the per unit area of the central portion of the second heating plate 301 shared by slit 330 Area in plane can be greater than in the per unit area of 301 edge part of the second heating plate in plane shared by slit 330 Area.
For example, multiple main slits 350 include: the first main slit 351, in the second direction Y of the second heating plate 301 Centre portion；And the second main slit 352, compared to the edge part for the second direction Y that the first main slit 351 is located at the second heating plate 301, Wherein, the width t of the first main slit 351351aThe width t of the second main slit 352 can be greater than352.For example, the first main slit 351 Width t351aIt can be the width t of the second main slit 3523522 times or more.It accordingly, can be on the entire area of substrate Improve the drying uniformity of organic solvent.
In some embodiments, a first main slit 351 is the shape extended along first direction X, and the first main slit The width t of the central portion of 351 first direction X351aSome end of the first direction X of the first main slit 351 can be greater than Width t351b.For example, the width t of central portion351aIt can be the width t of end351b2 times or more.Accordingly, in the entire of substrate On area, the drying uniformity of organic solvent can be improved.With difference as shown in the figure, the width of the first main slit 351 can also be with Tend to end from the central portion of first direction X to gradually become smaller.
In addition, annealing device 1001 includes the first secondary heater 711, so as to be configured to compared to heat treatment space 500 edge part is capable of supply that relatively more heats to central portion.
In an illustrative embodiment, the first secondary heater 711 is configured in the second heating plate 301.First secondary heating Device 711 is configured between the second heating plate 301 and hood 910.First secondary heater 711 may be at and the second heating plate 301 abut and contact or state spaced apart by a predetermined distance.First secondary heater 711 is along the first direction X shape extended and edge Second direction Y separates configuration, so that the first secondary heater 711 can be multiple.
The heat provided by the first secondary heater 711 can be different according to the region of heat treatment space 500.For example, First secondary heater 711 and the central portion of heat treatment space 500 overlap, in contrast, at the edge of heat treatment space 500 Portion can not configure the first secondary heater 711.Accordingly, it compared to the edge part of substrate, can be induced in central portion relatively more The gasification of the organic solvent vapor of amount, and can be in the drying uniformity of the entire area of substrate raising organic solvent.
Figure 12 is the perspective view for showing the gas injector unit of Fig. 9.Figure 13 is first flow path portion 611 and the third stream of Figure 12 The bottom isometric view in road portion 630.Figure 14 is the sectional view cut according to the B-B ' line of Figure 12.
Referring to Fig. 9 to Figure 14, gas injector unit 601 includes: gas supply source 670, be configured to storage technology gas and Process gas is supplied inside to chamber 100；First flow path portion 611 is configured at the top of the second heating plate 301 in chamber 100； Feed tube 650, provides the flow path between gas supply source 670 and first flow path portion 611, and gas injector unit 601 may be used also To include the third flow path portion 630 protruded from first flow path 611.
The process gas provided from gas supply source 670 can be transferred to multiple first-class by the offer of feed tube 650 The flow path in road portion 611.In an illustrative embodiment, feed tube 650 includes first gas distribution pipe 651 and two second Gas service pipes 652, so as to be cascade form.In this case, second gas distribution pipe 652 and first flow path portion 611 be respectively 2nA, second gas distribution pipe 652 can run through the through-hole 301h of the second heating plate 301.Herein, n is nature Number.Accordingly, the flow and the supply that are supplied to the process gas of second gas distribution pipe 652 and first flow path portion 611 can be made Etching it is practically identical.
It is 2 in first flow path portion 611nIn a schematical embodiment, the first secondary heater 711 can be 2n+1It is a.? First secondary heater 711 is distributed in the two sides of the second direction Y in first flow path portion 611, every side.
For the shape and configuration of feed tube 650, explanation was carried out together with Fig. 6 etc., therefore omit weight Multiple explanation.
On the other hand, first flow path portion 611 extends along first direction X and provides the flow path along first direction X.First flow path Y separates configuration in a second direction in portion 611, so as to be multiple.Multiple first flow path portions 611 can be configured at the second heating plate 301 top.That is, multiple first flow path portions 611 can be configured between the second heating plate 301 and hood 910.
Multiple third flow path portions 630 can be protruded from first flow path portion 611 to 301 side of the second heating plate.Third flow path portion 630 can receive process gas from 611 branch of first flow path portion.Although Fig. 9 is illustrated compared under the second heating plate 301 The case where downside end in face, third flow path portion 630 protrudes downwards, but the present invention is not limited thereto, third flow path The downside end in portion 630 actually can also be in same level with the lower surface of the second heating plate 301.
Third flow path portion 630 is configured to will be from the flowing of the received process gas in first flow path portion 611 to third party It is guided to the downside of Z and penetrates the process gas to substrate (not shown) side spray as heat treatment object.For example, third Flow path portion 630 is configured to body of emanating to 200 side of the first heating plate and/or 400 side spray of substrate setter plate, third flow path portion 630 can have for spraying process gas to its external jet port 630h.Jet port 630h is formed as holding gas The position easily penetrated to 400 side spray of substrate setter plate and form.For example, jet port 630h can be arranged in third flow path portion The inclined shape of 630 side wall and downward side.
Make the shared relatively large feed tube 650 of spatial volume and first flow path portion 611 be configured at second to add The top of hot plate 301, and by being configured to the third flow path portion 630 protruded from first flow path portion 611 through the second heating plate 301 and penetrate process gas to 400 side spray of substrate setter plate, so as to so as to be defined within the first heating plate 200 and the second heating Thermal coefficient (heat conductivity) in heat treatment space 500 between plate 301 actually maintains evenly.Accordingly, It can inhibit the heat loss of process gas and heat possessed by process gas is completely transmitted to substrate (not shown).Separately Outside, in heat treatment space 500, for example, it is configured without the equal other pipe in the first flow path portion 611 with metal material, from And it can prevent the sinuous flow for the process gas being not intended to, therefore can improve in the entire area of the substrate organic molten The drying uniformity of agent, and the difference of exhaust pathway can also be reduced.Moreover, in heat treatment space 500, for example, simultaneously The equal other pipe in the first flow path portion 611 with metal material is not configured, so as to prevent vaporized organic solvent from steaming Vapour is attached to the pipe and condenses again and pollute substrate.
Hereinafter, being illustrated to the film manufacturing method of an embodiment according to the present invention.
It include that sandwiched discharge has between the first heating plate and the second heating plate according to the film manufacturing method of the present embodiment The step of substrate of machine material layer；And to the substrate-side spray gas the step of, and the step of substrate described in sandwiched it After can also include the steps that control cavity indoor pressure.
Firstly, the step of illustrating substrate described in sandwiched.
Figure 15 is the sectional side view of annealing device the step of showing sandwiched substrate.Figure 16 is the base of amplification display Figure 15 The figure of plate.
The step of 5 and Figure 16 referring to Fig.1, sandwiched substrate 10 may include: the substrate 10 for preparing discharge and having organic solution 1 The step of；Substrate 10 is introduced into chamber 100 and substrate 10 is configured to the step in substrate setter plate 400；And it uses The step of lifting device 450 rises substrate setter plate 400, the first heating plate 200 and substrate 10.
Substrate 10 may include: bulk substrate (BASE SUBSTRATE) 3；And organic solution 1, it is disposed to matrix base On plate 3.In some embodiments, substrate 10 can also include the electrode layer 4 and pixel definition film being configured on bulk substrate 3 (PDL:Pixel Define Layer) 5.Although it is not shown, but in some embodiments, substrate 10 can also include being located in Addition organic layer (not shown) between electrode layer 4 and organic solution 1.
Organic solution 1 can discharge organic substance solution on bulk substrate 3 and be formed.Although the present invention is not limited to This, but the organic solution is the solution for being used to form the organic layer of organic illuminating element, and is organic light emission in the substrate Element manufacture in the case where substrate, organic solution 1 can be including hole injection layer substance, hole transmission layer substance and/or More than one in luminescent layer substance.
Substrate setter plate 400 can rise to the position abutted with airflow-resistive block 810, at this point, by substrate setter plate 400, the definition space heat treatment space 500 that the gentle flow resistance block 810 of the second heating plate 300 surrounds.Heat treatment space 500 is real The space of heat treatment is executed in matter to substrate 10, can be divided with other spaces inside chamber 100 and independently execute precision Temperature control or process gas gas flow optimized.For example, airflow-resistive block 810 carries out the side of heat treatment space 500 Physical blockage, so as to which so that open space minimizes, 830 using gas gas curtain of curtain gas ejection section can be prevented The air-flow of connection is formed between the inside and outside of heat treatment space 500.
It is in by 450 substrate 10 of lifting device in the state of rising, the upper surface of substrate 10 and the second heating plate 300 Lower surface between can be about 1mm or more separated by a distance and 20mm hereinafter, about 10mm.If substrate 10 and second adds Between hot plate 300 is separated by a distance 1mm or more, then substrate 10 can be prevented to be damaged because of the injection pressure of process gas, and Stable air-flow is formed, so as to inhibit to generate the sinuous flow being not intended to.In addition, if separated by a distance be 20mm hereinafter, if from The heat that second heating plate 300 provides can be effectively transmitted to substrate 10.Accordingly, in the first heating plate 200 and the second heating It can be with sandwiched substrate 10 between plate 300.
The annealing device used in the present embodiment can be and be filled according to the heat treatment of the embodiment of Fig. 1 or Fig. 9 etc. It sets, therefore omits repeated explanation.
Then, illustrate the step of spraying gas to the substrate-side.
Figure 17 is shown in the flow of process gas and the chart of cavity indoor pressure variation in the step of injection gas.Figure 18 be the sectional side view for showing the annealing device of the step S200 by spraying gas dry substrate.Figure 19 is amplification display The figure of the substrate of Figure 18.
Firstly, referring to Fig.1 7, it may include: to be dried by spraying gas according to the step of injection gas of the present embodiment The step S200 of substrate；And the step S300 of substrate is dried by spraying gas.
Referring to Fig.1 7 to Figure 19, make substrate 10 dry (curing) and penetrating process gas to 10 side spray of substrate (S200).The step S200 for keeping substrate 10 dry can be the step of making the organic solution 1 of substrate 10 gasify.In this step S200 In, substrate 10 can be with about 35 DEG C or more and 60 DEG C of temperature below are heat-treated, but the present invention is not limited thereto.Separately Outside, the step S200 for alloing organic solution 1 dry executes about 5 minutes or more and 10 minutes time below.In this step In S200, the about 90 weight % or more of the organic solution 1 of substrate 10, overall weight can be gasified.
In the step S200 for making organic solution 1 dry above by spray technology gas, mentioned from gas supply source 670 The process gas of confession, can be by the feed tube 650 including first gas distribution pipe 651 and second gas distribution pipe 652 And first flow path portion 610 and penetrated by the spray-hole in first flow path portion 610 to 10 side spray of substrate.The process gas sprayed Body can be contacted with the organic solution 1 of substrate 10.In this case, between substrate 10 and the lower surface of the second heating plate 300 Can maintain about 1mm or more and 20mm separated by a distance hereinafter, about 10mm.
Figure 18 illustrates the case where using annealing device 1000 according to the embodiment of Fig. 1 etc., but in other implementations Also the annealing device 1001 according to the embodiment of Fig. 9 etc. can be used in example.In this case, from gas supply source 670 The process gas of offer, can be by the feed tube including first gas distribution pipe 651 and second gas distribution pipe 652 650, first flow path portion 611 and third flow path portion 630 are penetrated to 10 side spray of substrate.
The process gas after contacting with organic solution 1, can be by the slit 310 of the second heating plate 300 at heat Manage the outside drain in space 500.For example, the process gas can be mobile from the upward side in the downside of the second heating plate 300, and can To be captured by hood 910.
It, can be by the slit 310 of the second heating plate 300 to heat in addition, from the organic solvent vapor that organic solution 1 gasifies The outside drain of processing space 500.For example, the organic solvent vapor can be from the upward sidesway in downside of the second heating plate 300 It is dynamic, and can be captured by hood 910.
It is configured to according to multiple slits 310 of the second heating plate 300 of the annealing device of the present embodiment, second Area shared by slit 310 is greater than in the edge part of the second heating plate 300 in the per unit area of the central portion of heating plate 300 Area shared by slit 310 in per unit area.Accordingly, it can be effectively discharged out organic solvent vapor, and there is outstanding do Dry characteristic.
In addition, according to the film manufacturing method of the present embodiment, although with the organic layer baking step S300 that will be discussed below The drying steps S200 of organic solution is executed in the same chamber, but still may insure to the organic solution 1 in substrate 10 Outstanding drying uniformity, therefore process can be simplified.
In an illustrative embodiment, 10 drying steps S200 of substrate may include the first time gas injection successively executed Step SF1, second of gas injection step SF2, third time gas injection step SF3, the 4th gas injection step SF4 and Five gas injection step SF5.
First time, gas injection step SF1 can be the step of starting spray technology gas with first flow F1." flow " Refer to the amount of injection (volume) of the gas in per unit time.That is, " flow " refers in per unit time from gas injection list The total amount for the process gas that member 600 is flowed into substrate heat treatment space.In other words, " flow " can refer to per unit time The amount of the interior gas provided from gas supply source 670.
Then, second of gas injection step SF2 can be make flow reduce from first flow F1 to second flow F2 and The step of spray technology gas.Second flow F2 can be the flow less than first flow F1.Second of gas injection step SF2 It can be performed simultaneously completely with the first time pressure controlling step SP1 that will be discussed below.
Then, third time gas injection step SF3 can be maintain second flow F2 and the step of spray technology gas.? In this specification, it further includes not changing stream intentionally that " maintaining flow ", which refers to, which not only includes the case where indicating that the numerical value of flow is constant, Amount and the case where flow changes in 10% range of analog value.
Third time gas injection step SF3 completely can be with second of pressure controlling step SP2 being described below simultaneously It executes.According to second of pressure controlling step SP2, the atmosphere inside chamber 100 can be made to be formed as the organic molten of organic solution 1 The easier state of the gasification of agent, and can be promoted organic with enough flow (that is, second flow F2) spray technology gas The gasification of solution 1 and the discharge for guiding organic solvent vapor.That is, third time gas injection step SF3 and second of pressure control Step SP2 is dry diffusing step, can be the step of executing actual drying to organic solution 1.
In an illustrative embodiment, second flow F2 can be about 1 with 500 volume of every 1 minute heat treatment space Times or more or about 2 times or more or about 20 times or more value flow.In the third time as drying substrates step S200 In gas injection step SF3, by making second flow F2 within the above range, so as to guide the suitable of organic solvent vapor Benefit discharge.
Then, the 4th gas injection step SF4 can be from second flow F2 and gradually decrease flow and spray technology gas The step of body.For example, the 4th gas injection step SF4 can be and gradually decrease flow from second flow F2 and interrupt injection work The step of skill gas.Accordingly, the high vacuum in chamber 100 may be implemented.
Then, the 5th gas injection step SF5 can be the step of maintaining the not state of spray technology gas.Pass through Four times gas injection step SF4 and the 5th time gas injection step SF5 can make inside chamber 100 in high vacuum state.
In some embodiments, 10 drying steps S200 of substrate further include to the pressure of film making space (that is, chamber) into The step of row control, the pressure controlling step can also include the first time pressure controlling step SP1 successively executed, second Pressure controlling step SP2 and third time pressure controlling step SP3.Pressure control can be executed by the operation of exhaust pump 920.
First time pressure controlling step SP1 can be decompressed to the step of second pressure P2 from first pressure P1.First pressure P1 can be the pressure in the chamber 100 after substrate 10 is introduced into.For example, first pressure P1 can be about 700torr or more, or The atmospheric pressure of person about 760torr or more.In addition, second pressure P2 can be the pressure less than first pressure P1.For example, the second pressure Power P2 can be about 0.1torr or more and 10torr hereinafter, about 0.1torr or more and 1torr or less.
First time pressure controlling step SP1 is initial depressurization steps, can be in chamber 100 atmosphere depressurize and start into The step of row is dried under reduced pressure process.First time pressure controlling step SP1 can execute about 30 seconds or more and 90 seconds time below.
Then, second of pressure controlling step SP2 can be the step of maintaining second pressure P2.In the present specification, " dimension Hold pressure " refer to and not only include the case where indicating that the numerical value of pressure is constant, further include do not control pressure intentionally and pressure corresponding The case where changing in 10% range of value.
The substantial vacuum state being depressurized can be maintained inside second of pressure controlling step SP2, chamber 100 (that is, second pressure P2 state).Accordingly, be formed as 100 inside atmosphere of chamber and the organic solution 1 as dry object The saturated vapour pressure of organic solvent is identical or lower, accordingly, the gasification of organic solvent can be made to become easy.
Secondly, third time pressure controlling step SP3 can be the step of being decompressed to third pressure P3 from second pressure P2.The Three pressure P3 can be the pressure less than second pressure P2.For example, third pressure P3 can be about 10-4Torr or more and 10- 2Torr is hereinafter, about 10-3torr.It can achieve high vacuum shape inside third time pressure controlling step SP3, chamber 100 State.It can be less than to control in first time pressure in the pressure change rate per unit time of third time pressure controlling step SP3 and walk Pressure change rate per unit time in rapid SP1.For example, third time pressure controlling step SP3 can be with the 4th gas Body injecting step SF4 and the 5th time gas injection step SF5 is at least partly performed simultaneously.
In first time pressure controlling step SP1 into third time pressure controlling step SP3, the organic solution 1 of substrate 10 About 90% or more of total weight can be by gasification and with the discharge of organic solvent vapor state.In organic solution 1 not by gasification and The solid component of remaining and remaining organic solvent can form the organic layer 2 being described below on bulk substrate 3.For the first time Pressure controlling step SP1 to third time pressure controlling step SP3 can be in about 5 minutes or more and 10 minutes Time Continuous below Ground executes.
In some embodiments, the sandwiched substrate 10 the step of after can also include using curtain gas ejection section 830 The step of spraying curtain gas.By the flow for the curtain gas that curtain gas ejection section 830 is sprayed, can be by first-class 30% or more and 100% or less of the process gas flow that road portion 610 is sprayed.For example, the flow of curtain gas can be less than work The flow of skill gas.The flow of curtain gas and process gas is adjusted within the above range, it can be by heat treatment space 500 and outer Portion's isolation, accordingly, can prevent impurity to be attached to substrate 10, and can prevent the loss of process gas and stablize process gas Ground is used in the heat treatment of substrate 10.
Figure 20 is the sectional side view for showing the annealing device by spraying the step of gas dries substrate.Figure 21 be the figure of the substrate of amplification display Figure 20.
7, Figure 20 and Figure 21 referring to Fig.1 dry substrate 11 and penetrating process gas to 11 side spray of substrate (baking)S300.The step of step S300 of drying substrate 11 can be the membrane property of organic layer 2 of control base board 11.At this In step S300, the organic solution 1 that organic layer 2 can be Figure 19 is dried and about 90 weight % or more remain in base after being gasified Organic film on structure base board 3.In this step S300, substrate 11 can be with about 200 DEG C or more and 300 DEG C of temperature below obtain heat Processing, but the present invention is not limited thereto.In addition, the step S300 that organic layer 2 is dried can execute about 20 minutes with The upper and 40 minutes time below.
By spraying in the step S300 that the process gas dries organic layer 2, provided from gas supply source 670 Process gas, can by feed tube 650 and first flow path portion 610 and by the spray-hole in first flow path portion 610 to 11 side spray of substrate is penetrated.The process gas sprayed can be contacted with the organic layer 2 of substrate 11.In this case, substrate 11 and second heating plate 300 lower surface between can maintain about 1mm or more and 20mm separated by a distance hereinafter, about 10mm.That is, connecting in a chamber 100 to the step S200 of the step S300 dried of organic layer 2 and dry organic solution 1 Continuous to execute, 11 position of substrate risen by riser 450 is constant, can be fixed state.
The process gas used in this step S300, can with organic solution is made by the dry organic solution Process gas used in the step S200 of gasification is same or different.Figure 20 has been illustrated using the implementation according to Fig. 1 etc. The case where annealing device 1000 of example, but the heat treatment of the embodiment according to Fig. 9 etc. also can be used in other embodiments Device 1001.
The process gas after contacting with organic layer 2 can pass through 310 heat treated of slit of the second heating plate 300 The outside drain in space 500.For example, the process gas can be mobile from the upward side in the downside of the second heating plate 300, and can be with It is captured by hood 910.
In addition, adding the organic solvent vapor of gasification from organic layer 2 and/or remaining in the residual in heat treatment space 500 Solvent vapo(u)r can pass through the outside drain in the 310 heat treated space 500 of slit of the second heating plate 300.For example, described chase after The organic solvent vapor and/or residual solvent steam of aerating, can be mobile from the upward side in the downside of the second heating plate 300, and It can be captured by hood 910.
According to the film manufacturing method of the present embodiment, although the drying steps S200 of the organic solution and the drying of organic layer Step S300 is continuously performed in the same chamber 100, but can still form the gas of the horizontal direction as caused by process gas Stream, accordingly, can control the membrane property of film thickness of edge part and central portion etc. in a pixel, easily so as to so that work Sequence is simplified.
In an illustrative embodiment, 11 baking step S300 of substrate may include the 6th gas injection successively executed Step SF6, the 7th time gas injection step SF7 and the 8th time gas injection step SF8.
6th time gas injection step SF6 can be the initial baking step for restarting spray technology gas.6th time Gas injection step SF6 can be the step of gradually increasing flow and spray technology gas.For example, the 6th gas injection step SF6 can be the step of making the flow of process gas be gradually increased to third flow F3 and spray technology gas.
Then, the 7th gas injection step SF7 can be maintain third flow F3 and the step of spray technology gas.
7th gas injection step SF7 can be with the 6th pressure controlling step SP6 being described below at least partly It is performed simultaneously.It can be with enough flows (that is, third flow F3) sprays the process gas of high temperature and dries organic layer 2, especially The air-flow of horizontal direction can be formed by the process gas.
In an illustrative embodiment, third flow F3 can be about 5 with 500 volume of every 1 minute heat treatment space Times or more or about 10 times or more or about 100 times or more of value flow.In the 7th as substrate baking step S300 In secondary gas injection step SF7, by keeping third flow F3 within the said range, so as to make center in a pixel Film thickness at portion and edge part is more uniformly formed.
Then, the 8th gas injection step SF8, which can be, gradually decreases flow from third flow F3 and sprays gas Step.It gradually decreases flow for example, the 8th gas injection step SF8 can be from third flow F3 and interrupts process gas spray The step of penetrating, stabilizing 2 surface of organic layer of substrate 11.
In some embodiments, 11 baking step S300 of substrate further includes the steps that the pressure in the space of control manufacture film, The step of controlling the pressure can also include the 4th time pressure controlling step SP4 and the 5th time pressure control step successively executed Rapid SP5, but also may include the 6th pressure controlling step SP6.
4th pressure controlling step SP4 can be the step of maintaining third pressure P3.I.e., it is possible to be to maintain chamber 100 The step of internal high vacuum state.For example, the 4th pressure controlling step SP4 can be with above-mentioned 6th gas injection step SF6 is at least partly performed simultaneously.
5th pressure controlling step SP5 can be the step of being forced into the 4th pressure P4 from third pressure P3.4th pressure Power P4 may be greater than the pressure of third pressure P3.For example, the 4th pressure P4 can be about 700torr or more, Huo Zheyue The atmospheric pressure of 760torr or more.4th pressure P4 and first pressure P1 can be same or different.
4th time pressure controlling step SP4 and the 5th time pressure controlling step SP5 can be at about 15 minutes or more and 25 It is consecutively carried out in time below minute.
6th pressure controlling step SP6 can be the step of maintaining the 4th pressure P4.I.e., it is possible to be made in chamber 100 Portion maintains the step of atmospheric pressure.In this case, the 6th pressure controlling step SP6 can be sprayed with the 7th gas Step SF7 is penetrated at least partly to be performed simultaneously.In turn, the 6th pressure controlling step SP6 can be with the 8th gas injection Step SF8 is at least partly performed simultaneously.6th time pressure controlling step SP6 can execute about 5 minutes or more and 15 minutes or less Time.
In the 4th time pressure controlling step SP4 to the 6th times pressure controlling step SP6, the organic of substrate 11 can control The membrane properties such as the film thickness of layer 2.For example, making the thickness of the central portion for the organic layer 2 being located in a pixel and the thickness of edge part It spends difference to reduce, so as to improve the uniformity in pixel (IPU), but the present invention is not limited thereto.
Previous drying process is required to the characteristic of the vaporized a large amount of organic solvent vapor of smooth discharge, and dries Procedure calls temperature control features, therefore there are problems that being difficult executing these processes in a chamber.However, according to this reality The annealing device and film manufacturing method for applying example make to provide the passing away of vaporized organic solvent vapor and process gas The second heating plate (upper Heating Plate) slit arranging density be configured to central portion be greater than edge part, show accordingly by While the discharge characteristic of a large amount of organic solvent vapor of gasification, there is the process gas of injection high temperature and be easier to control film The effect of characteristic.Accordingly, previous drying process and baking process can be continuously performed in a chamber, therefore can subtracted Less according to the extraction to exterior thereto and the production time per piece being re-introduced into (tact time) and the possibility of pollution that substrate can be made It minimizes.
Hereinafter, the effect of annealing device and film manufacturing method according to the present invention is described in detail by experimental example.
[experimental example 1: the film uniformity characteristic of the drying process based on process gas flow]
The organic illuminating element manufacture panel including two 3.7 inches is introduced in the annealing device according to Fig. 1 Size be 300mm × 300mm substrate.The substrate be discharge have including methyl benzoate (methyl benzoate) with And the state of the organic solution of ethyl phthalate (diethyl phthalate).In addition, by conversion process gas flow into It has gone the drying of organic solution, and the measurement result of the uniformity in pixel (In Pixel Uniformity, IPU) has been shown in In Figure 22.The temperature of first heating plate and the second heating plate is 40 DEG C.Experiment condition is, in the feelings of not spray technology gas Condition and the case where with the injection of the flow of 0.2L/min, 0.5L/min, 1L/min, 1.5L/min, 2L/min.In spray technology In the case where gas, nitrogen 60 seconds of 40 DEG C of injection.
The uniformity refers in pixel gasified in a pixel than organic solvent after remaining organic layer interior thickness The ratio of area in plane shared by the part of big thickness.That is, referring to that the uniformity closer to 100%, get over by film thickness in pixel It is uniform and flat.
Figure 22 is the result that the uniformity (In Pixel Uniformity, IPU) in pixel is measured under each experiment condition.
Referring to Figure 22 it has been confirmed that with process gas flow increase, the uniformity increases in pixel.I.e., it is known that dry The process gas of dry step injection has influence to the improvement of the uniformity in the pixel of organic layer.
[experimental example 2: the residual organic solvent steam content based on process gas flow]
The organic illuminating element manufacture panel including two 3.7 inches is introduced in the annealing device according to Fig. 1 Size be 300mm × 300mm substrate.The substrate be discharge have including methyl benzoate (methyl benzoate) with And the state of the organic solution of ethyl phthalate (diethyl phthalate).In addition, by 40 DEG C of nitrogen with 0.2L/min with And the flow of 2L/min sprays and measures the content of remaining organic solvent in chamber, as the result is shown in Figure 23.Except this it Outside, experiment condition is identical as experimental example 1.The content of residual organic solution is determined with residual gas analyzer (RGA).
Figure 23 is, (left side) and sprays work with the flow of 2L/min the case where to flow spray technology gas with 0.2L/min The result that the partial pressure of the organic solution vapor of residual is measured in the time-based chamber of the case where skill gas (right side).
It referring to Figure 23, can be confirmed in the case where process gas flow is 2L/min, residual organic solvent in chamber Each component content is lower.
[experimental example 3: according to the film uniformity characteristic of the baking process of process gas flow]
The organic illuminating element manufacture panel including two 3.7 inches is introduced in the annealing device according to Fig. 1 Size be 300mm × 300mm substrate.The substrate is the state that discharge has the organic solution including hole injecting material. In addition, 40 DEG C of nitrogen is sprayed 60 seconds with the flow of 2L/min, to dry organic solution.In addition to this, drying condition It is identical as experimental example 1.Then, it has been carried out by transformation nitrogen temperature, injecting time and injection flow to hole injection layer Drying.
Then, after discharge is including the organic solution of hole transporting material on hole injection layer, the back tender is repeated The baking process of sequence and hole transmission layer.
Figure 24 shows the uniformity in the pixel to the hole injection layer and hole transmission layer that are formed by the above process The result being measured.Table 1 is shown in the experiment condition that experimental example 3 uses.
[table 1]
Figure 24 (a) is surveyed to the uniformity in the pixel under each experiment condition (In Pixel Uniformity, IPU) Fixed result.
Referring to table 1 and Figure 24 (a) it has been confirmed that even if the temperature in process gas is identical as process gas injecting time In the case where, when the injection flow of process gas is larger, the uniformity increases in pixel.I.e., it is possible to know, sprayed in baking step The process gas penetrated contributes and influences the improvement of thickness uniformity in pixel on the control of the membrane property of organic layer.
Figure 24 (b) is, the case where to flow spray technology gas with 2L/min (on) sprayed with the flow of 20L/min The case where process gas (under) under the result that is measured of organic film section profile (section profile).For pixel The section profile of interior organic film is determined in short side direction and longitudinal direction.Measurement to section profile, uses essence Close surface profile measurement system (presision surface profile measurement system) SNU is surveyed It is fixed.
Referring to table 1 and Figure 24 (b) it has been confirmed that with the flow spray technology gas of 2L/min, in picture Plain edge part, organic film surface are formed as heaving to downside.I.e., it is possible to confirm that the thickness of organic film is sharply in pixel edge portion Reduce.On the contrary, it has been confirmed that with the flow spray technology gas of 20L/min, with the 2L/min the case where compared with, Thickness in pixel edge portion reduces relatively fewer.I.e., it is possible to know, in the process gas that baking step sprays to organic layer Membrane property controls the improvement for contributing and influencing thickness uniformity in pixel.
[experimental example 4: according to the pneumatic measurement of the horizontal direction of process gas flow]
It is manufactured according to the annealing device of the embodiment of Fig. 1 to the organic illuminating element including two 3.7 inches to using The case where nitrogen is sprayed with 2L/min with the substrate that the size of panel is 300mm × 300mm and the feelings that nitrogen is sprayed with 20L/min The air velocity of the horizontal direction of condition is simulated experiment, and by it as the result is shown in Figure 25.
Figure 25 is, the case where with the flow spray technology gas of 2L/min (on) and with the flow spray technology of 20L/min The case where gas (under) under according to 3.7 inch faceplate panel positions to air velocity carry out simulated experiment result.By positions of panels After being divided into 9 regions along the long side direction and being divided into 9 regions along short side direction, totally 81 regions are simulated Experiment.
Referring to Figure 25 it has been confirmed that according to the flow of process gas, in panel in same position, horizontal gas flow speed is produced Raw difference.In the case where the flow injection with 2L/min, the average speed of horizontal gas flow is 0.028m/s, with 20L/min Flow injection in the case where, the average speed of horizontal gas flow is 0.15m/s.I.e., it is possible to know, increase in the flow of process gas In the case where adding, entire surface plate suqare is capable of forming about big 5 times or so of horizontal gas flow.
More than, although being illustrated centered on the embodiment of the present invention, this is only exemplary, and the present invention is simultaneously It is not limited to this, for the those skilled in the art in fields of the present invention, it is possible to understand that do not departing from implementation of the present invention In the range of the intrinsic propesties of example, it can carry out in various modifications and application not enumerated above.For example, in implementation of the invention The each component that example is specifically presented can be with deformation implementation.In addition, the difference about this deformation and application, should be interpreted that packet Contained in the scope of the present invention that claims define.

Claims (10)

1. a kind of annealing device, comprising:
Chamber；
First heating plate is configured in the chamber；
Second heating plate is configured in the chamber, and is configured in the one side of first heating plate, has multiple slits； And
Gas injector unit is configured to body of emanating to the one side side spray of first heating plate,
Area in plane shared by the slit described in the per unit area of the central portion of second heating plate is greater than in institute State the area in plane shared by slit described in the per unit area of the edge part of the second heating plate.
2. annealing device according to claim 1, wherein
The gas injector unit, comprising:
Multiple first flow path portions extend along the first direction parallel with the one side of first heating plate and provide along described The flow path of first direction, and configuration is separated along the second direction intersected with the first direction,
The slit is the shape extended along the first direction,
The width of the central portion in the first direction of the slit is greater than the end in the first direction of the slit Width.
3. annealing device according to claim 2, wherein
The multiple slit includes:
First slit, positioned at the central portion of the second direction of second heating plate；And
Second slit, compared to the edge part for the second direction that first slit is located at second heating plate,
The width of first slit is greater than the width of second slit.
4. annealing device according to claim 2, wherein
Definition has heat treatment space between first heating plate and second heating plate, and includes:
First secondary heater is configured to that more heat can be applied to central portion compared to the edge part of the heat treatment space Amount；
Substrate setter plate is configured between first heating plate and second heating plate；
Airflow-resistive block is configured between first heating plate and second heating plate, along second heating plate Edge is configured to belt shape；
Curtain gas ejection section is configured at the outside of the airflow-resistive block in a manner of surrounding the airflow-resistive block；
Second secondary heater is configured at the outside of the airflow-resistive block in a manner of surrounding the airflow-resistive block, and constitutes To provide heat to the heat treatment space side；And
Hood is configured at the top of second heating plate,
The gas injector unit is configured to body of emanating to the substrate setter plate side spray.
5. annealing device according to claim 4, wherein
The gas injector unit further include:
Gas supply source supplies the gas；And
Feed tube provides stream between the gas supply source and multiple first flow path portions of the chamber interior Road,
Second heating plate has multiple through-holes,
The first flow path portion is configured between first heating plate and second heating plate,
At least part of the feed tube through second heating plate and is directly connected in described by the through-hole First flow path portion,
First secondary heater is configured between second heating plate and the hood,
First secondary heater extend along the first direction and separated along the second direction be configured to it is multiple,
First secondary heater is Chong Die with the first flow path portion.
6. annealing device according to claim 4, wherein
Second heating plate has multiple through-holes,
The gas injector unit further include:
Gas supply source supplies the gas；
Feed tube provides stream between the gas supply source and multiple first flow path portions of the chamber interior Road；And
Multiple second flow path portions protrude from the first flow path portion and run through second heating plate, and structure by the through-hole It emanates body as to the substrate setter plate side spray,
The first flow path portion is configured between second heating plate and the hood, and the multiple first flow path portion is 2n It is a, wherein n is natural number,
The feed tube includes:
First gas distribution pipe extends along a direction；And
Two second gas distribution pipes, from first distribution pipe branch,
Flow path length from the gas supply source to each first flow path portion is all the same,
First secondary heater extends along the first direction and separates configuration along the second direction, and is 2n+1It is a,
First secondary heater is configured at the two sides in the first flow path portion.
7. a kind of film manufacturing method, wherein include:
Sandwiched discharge has the step of substrate of organic solution between the first heating plate and second heating plate with multiple slits； And
The gas is contacted with the substrate to substrate-side injection gas, and the gas is discharged by the slit Step,
Area in plane shared by the slit described in the per unit area of the central portion of second heating plate is greater than in institute State the area in plane shared by slit described in the per unit area of the edge part of the second heating plate.
8. film manufacturing method according to claim 7, wherein
After the step of substrate described in sandwiched further include:
The step of pressure of film making space is controlled,
The step of controlling the pressure include:
First time pressure controlling step is decompressed to the second pressure lower than the first pressure from first pressure；
Second of pressure controlling step maintains the second pressure；
Third time pressure controlling step is decompressed to the third pressure lower than the second pressure from the second pressure；
4th pressure controlling step, maintains the third pressure；And
5th pressure controlling step is forced into the 4th pressure higher than the third pressure from the third pressure,
The first time pressure controlling step to the 5th pressure controlling step successively executes in a chamber,
The step of spraying the gas include:
First time gas injection step sprays gas with first flow；
Second of gas injection step sprays gas from first flow decrement to less than the second flow of the first flow Body；
Third time gas injection step maintains the second flow and sprays gas；
4th gas injection step sprays gas from the flow of second flow decrement to less than the second flow；
5th gas injection step maintains the state for not spraying gas；
6th gas injection step restarts to spray gas, and flow is increased to third flow and sprays gas；
7th gas injection step maintains the third flow and sprays gas；And
8th gas injection step sprays gas from the flow of third flow decrement to less than the third flow,
The 5th gas injection step is at least partly performed simultaneously with the third time pressure controlling step,
The 6th gas injection step is at least partly performed simultaneously with the 4th pressure controlling step.
9. film manufacturing method according to claim 8, wherein
The step of controlling the pressure further includes maintaining the 4th pressure after the 5th pressure controlling step 6th pressure controlling step,
It is described in the first time pressure controlling step, second of pressure controlling step and third time pressure controlling step The temperature of substrate be 35 DEG C or more and 60 DEG C hereinafter,
The temperature of 4th pressure controlling step and the substrate in the 5th pressure controlling step be 200 DEG C with It is upper and 300 DEG C hereinafter,
The third time gas injection step is the step of contacting the organic solution of the gas and the substrate,
The 7th gas injection step be the step of contacting the organic film of the gas and the substrate,
The first time pressure controlling step, second of pressure controlling step and third time pressure controlling step execute 5 points More than clock and 10 minutes time below,
4th pressure controlling step and the 5th pressure controlling step execute 15 minutes or more and 25 minutes or less Time,
6th pressure controlling step execution 5 minutes or more and 15 minutes time below,
The 7th gas injection step is at least partly performed simultaneously with the 6th pressure controlling step,
The 8th gas injection step is at least partly performed simultaneously with the 6th pressure controlling step.
10. film manufacturing method according to claim 8, wherein
The first time gas injection step to the 8th gas injection step continuously performs in one chamber,
In the first time pressure controlling step to the 5th pressure controlling step and the first time gas injection step Extremely in the 8th gas injection step, the maintenance 1mm or more separated by a distance between the substrate and second heating plate And 20mm hereinafter,
In the first time pressure controlling step into the third time pressure controlling step, the 90 of the organic solution total weight Weight % or more is discharged by gasification and by the slit,
The second pressure be 0.1torr or more and 10torr hereinafter,
The third pressure is 10-4Torr or more and 10-2Torr hereinafter,
4th pressure is 700torr or more,
Definition has heat treatment space between the substrate and second heating plate,
The second flow is the flow with 1 times or more of value of the every 1 minute heat treatment space volume,
The third flow is the flow with 5 times or more of value of the every 1 minute heat treatment space volume.
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