KR101363147B1 - Deposition method and deposition apparatus - Google Patents

Abstract

Shorten the cooling time of the evaporation source.
In the vapor deposition preparation process, the crucible 13 containing the vapor deposition material 30, the heating part 14 for heating the crucible 13, and the vapor deposition material 30 vaporized in the crucible 13 are to be processed. An evaporation source 10 having a nozzle 12 for discharging toward and a target object are disposed in a vacuum chamber. Next, the vapor deposition material 30 stored in the crucible 13 is heated by the heating part 14, gasified vapor deposition material gas is generated, and a vapor deposition film is formed in a to-be-processed object. Next, the gas 26 is supplied into the crucible 13 through the nozzle 12 from the outside of the evaporation source 10, and the heating part 14 is stopped to cool the crucible 13.

Description

Deposition Method and Deposition Apparatus {DEPOSITION METHOD AND DEPOSITION APPARATUS}

TECHNICAL FIELD This invention relates to the technique of a vapor deposition technique and the vapor deposition apparatus used for this, and it is related with the technique especially applicable to the film-forming process of forming a vapor deposition film in a board | substrate.

Japanese Laid-Open Patent Publication No. 2008-115416 (Patent Document 1) discloses a cooling time of a crucible after film formation is completed by moving a reflector for blocking radiant heat from the crucible upwards at the end of film formation and stopping the heater that heats the crucible. A deposition method for reducing this is described.

Japanese Laid-Open Patent Publication 2008-115416

There exists a technique of depositing a vapor deposition film on a board | substrate by arrange | positioning the board | substrate which is a to-be-processed object and an evaporation source in a vacuum chamber. Such a film formation technique is applied to a process of forming an electrode made of a metal film, for example, in a method of manufacturing a flat panel display (FPD) such as an organic EL (Electro Luminescence) display. In the vapor deposition method, vaporization or sublimation is carried out by heating the vapor deposition material stored in the crucible of the evaporation source (hereinafter, vaporization or sublimation is referred to as gasification). A vapor deposition film is formed by transporting the vaporized vapor deposition material to a workpiece (eg, a deposition film formation region of a substrate) disposed outside the evaporation source and solidifying the surface of the workpiece.

In the above vapor deposition method, it is necessary to cool the evaporation source once at the time of exchanging the evaporation material or to maintain the evaporation apparatus, and after exchanging the evaporation material or the like, the temperature is again raised to the evaporation temperature (process temperature). The evaporation source cooling step and the temperature raising step generally require a time of about 5 hours to 10 hours, respectively, and the vapor deposition film can be efficiently formed by reducing the cooling time and the temperature increase time. In particular, in the cooling step, in order to suppress the deposition material from adhering to the wall surface or the cover of the evaporation source (the crucible), the so-called cooling is continued while the heating of the evaporation source is continued slowly until the temperature of the deposition material reaches the evaporation stop temperature. A slow cooling process is performed and this slow cooling process becomes one of the causes which lengthens a cooling time.

As described in the Patent Document 1, in the case of the vapor deposition method in which the reflector is moved to expose the lower side of the crucible in which the vapor deposition material is disposed from the reflector while keeping the upper portion and the lid portion warm, the cooling time of the vapor deposition material is shortened. . However, exposing the crucible heated to a high temperature from the reflector causes a problem of the vapor deposition apparatus due to torsion or melting of the constituent members of the vapor deposition apparatus disposed around the crucible by thermal radiation from the crucible. In particular, in the case of using a vapor deposition material made of a metal, since the vapor deposition temperature (process temperature) becomes a high temperature, for example, 400 ° C to 1000 ° C or higher, the influence of heat radiation from the crucible is increased.

This invention is made | formed in view of the said subject, The objective is to provide the technique which can shorten the cooling time of an evaporation source.

The above and other objects and novel features of the present invention will become apparent from the description and the accompanying drawings.

Outline of representative ones of the inventions disclosed in the present application will be briefly described as follows.

That is, the vapor deposition method in a typical embodiment of the present invention is (a) a crucible for storing a vapor deposition material, a heating part for heating the crucible, and the vapor deposition material vaporized in the crucible toward an object to be processed. And a process of disposing an evaporation source having a nozzle to discharge and a workpiece to be processed in a vacuum chamber. And (b) heating the vapor deposition material stored in the crucible by the heating unit to generate a vaporized vapor deposition material gas to form a vapor deposition film on the workpiece. Moreover, (c) after the said (b) process, the gas is supplied from the outer side of the said evaporation source to the said crucible via the nozzle, and the said heating part is stopped and the said crucible is cooled.

Among the inventions disclosed in the present application, the effects obtained by the representative ones are briefly described as follows.

That is, the cooling time of an evaporation source can be shortened.

BRIEF DESCRIPTION OF THE DRAWINGS It is explanatory drawing which shows the outline | summary of the manufacturing flow of the organic electroluminescence display which is one Embodiment of this invention.
FIG. 2 is an enlarged cross-sectional view showing a schematic structure of an organic EL element of an organic EL display device manufactured by the flow shown in FIG. 1.
It is explanatory drawing which shows the outline | summary of the whole structure of the vacuum vapor deposition apparatus which is one Embodiment of this invention.
It is sectional drawing which shows the whole structure in the film-forming room shown in FIG.
FIG. 5 is an enlarged cross-sectional view of the evaporation source shown in FIG. 4. FIG.
6 is a process flow of the vapor deposition method using the vapor deposition apparatus and the evaporation source shown in FIGS. 3 to 5, the temperature profile of the crucible in each step, the ON-OFF of the heating part in each step, and the gas in each step. It is explanatory drawing which shows the presence or absence of supply.
It is explanatory drawing which shows the temperature profile of the crucible in the cooling process which is the 1st and 2nd comparative example about one Embodiment and embodiment of this invention.
FIG. 8: is sectional drawing which shows the state which supplied the inert gas to the crucible shown in FIG. 4 in the cooling shown in FIG.
FIG. 9: is explanatory drawing which shows an example of the relationship between the temperature of the crucible shown in FIG. 4, and the saturated vapor pressure of vapor deposition material as a partial logarithmic graph.
10 is an explanatory diagram showing a process flow of a vapor deposition method which is a modification to FIG. 6, a temperature profile of the crucible in each step, ON-0FF of a heating unit in each step, and whether or not there is a gas supply in each step; to be.
FIG. 11 is a cross-sectional view showing an entire structure in a film forming room, which is a modification to FIG. 4. FIG.
It is sectional drawing which shows the modification of the film-forming chamber shown in FIG.
It is sectional drawing which shows the modification of the gas supply part shown in FIG.
14 is an enlarged cross-sectional view of the vicinity of the nozzle shown in FIG. 13.
FIG. 15 is a cross-sectional view showing the layout of the gas supply unit during the deposition step of forming the vapor deposition film in the vapor deposition method using the gas supply unit shown in FIG. 13.
It is an expanded sectional view which shows the state which operated the gas supply part shown by FIG. 13 by rotational motion.
FIG. 17 is an enlarged cross-sectional view illustrating each state in which the gas supply unit illustrated in FIG. 16 is further operated. FIG.
It is sectional drawing which shows the structure of the evaporation source used for the cooling process which is a 2nd comparative example shown in FIG.

<State form in this chapter>

In the following embodiments, when necessary for the sake of convenience, the description is divided into a plurality of sections or embodiments, and unless otherwise specified, they are not related to each other, and one of the modifications of some or all of the other, It relates to details, supplementary explanations, and the like.

In addition, in the following embodiment, when mentioning the number of elements, etc. (including number, numerical value, quantity, range, etc.), except when specifically stated and when it is specifically limited to a specific number clearly in principle, etc. It is not limited to the specific number, and may be more than a specific number or may be sufficient as it.

In addition, in the following embodiment, the component (including the element step etc.) is not necessarily essential except the case where it specifically stated, and the case where it seems to be essential in principle.

Similarly, in the following embodiments, when referring to shapes, positional relationships, and the like of components, substantially similar to or similar to the shapes, etc., except when specifically stated and when it is obviously not considered to be in principle. It shall be included. This also applies to the above numerical values and ranges.

In addition, in the whole figure for demonstrating embodiment, the same code | symbol is attached | subjected to the same member as a principle, and the repeated description is abbreviate | omitted. In addition, in order to make drawing easy to understand, hatching may be carried out even in plan view.

In addition, before describing this invention in detail, the meaning of the term in this application is demonstrated as follows.

Gasification refers to the phase transition to the gas phase by heating a solid or liquid material. Phase transition to the gas phase includes vaporization (phase transition from liquid phase to gas phase) and sublimation (phase transition from gas phase to gas phase without passing through a liquid phase). In the present specification, when referred to as gasification, vaporization or sublimation means. use. Moreover, the material which vaporizes the material which vaporizes by vaporizing, and the material which vaporizes by sublimating is called a sublimation material.

Vapor deposition, a vapor deposition method, or a vapor deposition process means taking out the material gas vaporized in the heating container to the outside of a heating container, and solidifying on the surface of a to-be-processed object and forming into a film. In addition, the film formed by vapor deposition is a vapor deposition film, and the material used as a raw material of a vapor deposition film is a vapor deposition material, and the vaporization vaporization material is called vapor deposition material gas.

In addition, an evaporation source refers to the apparatus which vaporizes vapor deposition material and extracts vapor deposition material gas. Therefore, the evaporation source includes a heating container for storing the vapor deposition material and a blowout port for ejecting the vapor deposition material gas.

In addition, a vapor deposition apparatus means the apparatus which performs a vapor deposition process on to-be-processed objects, such as a board | substrate, for example. Therefore, the vapor deposition apparatus includes, in addition to the above-mentioned evaporation source, a holding unit for holding the object to be processed, and an airtight chamber such as a vacuum chamber for storing the evaporation source and the object to be processed.

Moreover, in the following embodiment, as an application example of the evaporation source, the vapor deposition apparatus provided with an evaporation source, and the vapor deposition method using the same, the case where the manufacturing method of the organic electroluminescent display apparatus which this inventor specifically examined was applied to the electrode formation process is given concretely. Explain.

<Method for Manufacturing Organic EL Display Device>

BRIEF DESCRIPTION OF THE DRAWINGS It is explanatory drawing which shows the outline | summary of the manufacturing flow of the organic electroluminescence display of this embodiment. 2 is an expanded sectional view which shows the outline structure of the organic electroluminescent element of the organic electroluminescence display manufactured by the flow shown in FIG.

As shown in FIG. 1, the manufacturing method of the organic electroluminescent display apparatus of this embodiment has the board | substrate preparation process and the organic electroluminescent element formation process which forms an organic electroluminescent element on a board | substrate. In addition, the organic EL element forming step includes an organic layer forming step and a second electrode forming step. Briefly using FIG. 2, in the board | substrate preparation process (refer FIG. 1), the board | substrate (glass substrate) 1 which has the surface 1a located in the display surface side, and the back surface 1b on the opposite side to the surface 1a. Prepare. For example, a plurality of active elements made of TFT (Thin Film Transistor) or the like is formed in an array shape on the back surface 1b (not shown). Next, in the first electrode forming step (see FIG. 1), the conductive film 3 serving as an anode, for example, of the organic EL element 2a is formed on the back surface 1b of the substrate 1 (active element such as TFT or the like). Is formed. In the element structure called bottom emission, since the conductive film 3 is formed on the display surface side of the organic EL element 2a, it is made of a material such as IT0 (Indium Tin 0xide) that is transparent to visible light. In the element structure called top emission, since the 2nd electrode side becomes a display surface, you may form the electrically conductive film 3 from the laminated film of the high reflectivity aluminum alloy film and the ITO film with high hole injection property. Next, in the organic layer forming step (see FIG. 1), the organic layer 4 is formed on the conductive film 3. The organic layer 4 is a laminated film in which organic films having different functions, such as a hole transporting layer 4a, a light emitting layer 4b, and an electron transporting layer 4c, are sequentially stacked. Next, in the second electrode forming step (see FIG. 1), a conductive film 5 serving as an electrode having a polarity (for example, a cathode) opposite to the conductive film 3 is formed on the organic layer 4. The conductive film 5 is made of, for example, a metal thin film such as aluminum (Al) in a bottom emission structure, or a silver (Ag) or magnesium (Mg) alloy in a top emission structure.

Thus, the organic EL element 2a has a structure in which the organic layer 4 is sandwiched between an anode (conductive film 3) and a cathode (conductive film 5), and an organic layer is formed from each by flowing a current through the cathode and anode. Inject electrons and holes in (4). The injected electrons and holes pass through the hole transport layer 4a or the electron transport layer 4c, respectively, and are bonded in the light emitting layer 4b. The light emitting material of the light emitting layer 4b is excited by the energy of the bonding, and light is generated when the light emitting material of the light emitting layer 4b returns to the ground state from the excited state. A plurality of such organic EL elements 2a are formed on the back surface 1b of the substrate 1, and the display device is formed by each of the organic EL elements 2a or a combination of the plurality of organic EL elements 2a. The pixel (pixel) of the phosphorescent organic EL display device 2 is constituted.

Here, among the laminated films constituting the organic EL element 2a, the organic layer 4 or the conductive film 5 is disposed in the vacuum chamber by placing the substrate 1, which is an object, and an evaporation source, and the organic layer, which is a deposition film, on the substrate 1. (4) and the conductive film 5 are formed. That is, the organic layer 4 and the conductive film 5 are formed by what is called a vacuum vapor deposition method (vacuum vapor deposition method).

 <Overall Configuration of Vacuum Deposition Apparatus>

Next, the whole structure of the vacuum vapor deposition apparatus used for the organic layer formation process and 2nd electrode formation process shown in FIG. 1, and the process flow of the film formation process of the organic layer 4 and the conductive film 5 shown in FIG. 2 are demonstrated. do. 3 is an explanatory diagram showing an outline of an entire configuration of a vacuum vapor deposition apparatus according to the present embodiment.

The vapor deposition apparatus (vacuum vapor deposition apparatus) 100 shown in FIG. 3 is the transfer chamber 101 which delivers the board | substrate 1, the some film-forming chamber 102 which is a process chamber which forms a vapor deposition film, respectively, and the some film-forming chamber. It has the conveyance chamber 103 which distributes and conveys the board | substrate 1 to. In FIG. 3, the structure which the unit which consists of the some film-forming chamber 102 and the conveyance chamber 103 was connected through the delivery chamber 101 by plurality (three in FIG. 3) is shown. Each of these delivery chambers 101, the conveyance chamber 103, and the film formation chamber 102 is connected to exhaust apparatuses (not shown), such as a vacuum pump, and is made into the airtight chamber which can be maintained under reduced pressure. In particular, the film formation chamber 102 which performs the vacuum vapor deposition process is a vacuum chamber which can maintain a room pressure in the reduced pressure state (so-called high-vacuum state) of about ^10-3 Pa- ^10-5 Pa, for example.

Among the plurality of transfer chambers 101, the transfer chamber 101 on the inlet side is a loader portion 101a. For example, the substrate 1 on which the conductive film 3 shown in FIG. Carried in 101a). The robot 103a is arrange | positioned as the board | substrate conveying apparatus in the conveyance chamber 103, for example, and the board | substrate 1 is each film-forming chamber 102 from the delivery chamber 101 (loader part 101a) by the robot 103a. ) Is distributed and returned. Each deposition chamber 102 is provided with an evaporation source 10 having evaporation materials (not shown in FIG. 3) serving as raw materials for the organic layer 4 or the conductive film 5 shown in FIG. 2, respectively. For example, a vapor deposition film is laminated | stacked sequentially and formed into a film under the vacuum conditions of about 10 <^-3> Pa ~ 10 <^-5> Pa. Specifically, first, in the first film formation chamber 102, an organic layer 4, which is a vapor deposition film to be the hole transport layer 4a, is formed on the conductive film 3, which is the anode (first electrode) illustrated in FIG. 2. . The board | substrate 1 after film-forming is taken out to the conveyance chamber 103 by the robot 103a, and is conveyed to the 2nd film-forming chamber 102. In the second film forming chamber 102, an organic layer 4, which is a vapor deposition film to be the light emitting layer 4b, is formed on the hole transport layer 4a shown in FIG. 2. The board | substrate 1 after film-forming is taken out to the conveyance chamber 103 by the robot 103a, and is conveyed to the 3rd film-forming chamber 102. In the third film formation chamber 102, an organic layer 4, which is a vapor deposition film to be the electron transporting layer 4c, is formed on the light emitting layer 4b shown in FIG. 2. The board | substrate 1 after film-forming is taken out to the conveyance chamber 103 by the robot 103a, and is conveyed to the 4th film-forming chamber 102. In the fourth film forming chamber 102, a conductive film 5, which is a vapor deposition film that serves as a cathode (second electrode), is formed on the electron transport layer 4c shown in FIG. 2. And the board | substrate 1 formed into the conductive film 5 is conveyed by the robot 103a to the delivery chamber 101 of the exit side which is the unloader part 101b, and further protects from moisture and oxygen in air | atmosphere. By performing the sealing process for the purpose, the organic electroluminescence display 2 shown in FIG. 2 is obtained. In the sealing treatment step, the sealing substrate 7 is disposed on the organic EL element 2a with the sealing material 6 interposed therebetween.

<Configuration of the deposition chamber and evaporation source>

Next, the structure of the evaporation source 10 arrange | positioned in the film-forming chamber 102 and the film-forming chamber 102 shown in FIG. 3 is demonstrated. 4 is a cross-sectional view showing the entire configuration of the film formation chamber shown in FIG. 3, and FIG. 5 is an enlarged cross-sectional view showing the evaporation source shown in FIG. 4.

As shown in FIG. 4, the film formation chamber 102 is connected to a vacuum pump VP, and an exhaust path (exhaust pipe) VL for discharging gas in the film deposition chamber 102 is connected. The valve V1 is disposed between the vacuum pump VP and the film forming chamber 102. When the valve V1 is opened, the pressure in the film forming chamber 102 is about 10 ⁻³ Pa to about 10 ⁻⁵ Pa, for example. The pressure can be reduced until the pressure is reduced (so-called high vacuum). That is, the film formation chamber 102 is a vacuum chamber. In the deposition chamber 102, an evaporation source 10 for discharging the vaporized vapor deposition material gas toward the substrate 1 and a substrate holder 21 for holding the substrate 1 are disposed. In addition, the deposition chamber 102 is connected to the gas supply path GL introduced into the deposition chamber 102 from the outside of the deposition chamber 102 and the gas supply path GL, and the inert gas is introduced into the evaporation source 10. The gas supply part 25 provided with the gas discharge port GN to supply is arrange | positioned.

From the surface 11a of the housing 11 of the evaporation source 10, a plurality of nozzles 12, which are discharge ports of the vapor deposition material gas 30a, are exposed from the housing 11. On the other hand, the substrate 1 and the mask (deposition mask) 22 are held in the substrate holding part 21. The board | substrate 1 is arrange | positioned so that the back surface 1b which is a formation surface of a vapor deposition film may face the surface 11a which is an arrangement surface of the vapor deposition material gas outlet of the evaporation source 10 via the mask 22. As shown in FIG. Moreover, the some opening part 22a is formed in the mask 22 corresponding to the position which forms the organic electroluminescent element 2a shown in FIG. 2, and the vapor deposition film formation area | region of the board | substrate 1 is a mask in the opening part 22a. Each is exposed from (22). In addition, the positional relationship between the substrate 1 and the evaporation source 10 is that the back surface 1b of the substrate 1 is the surface 11a which is an arrangement surface of the vapor deposition material gas outlet (nozzle 12) of the evaporation source 10. It should just face through the mask 22, and is not limited to the aspect shown in FIG. In FIG. 4, the system called the face down deposit system which arrange | positions the some nozzle 12 on the surface 11a which is the upper surface of the evaporation source 10 is shown. As a modification other than the aspect shown in FIG. 4, the face up deposit system which arrange | positions the nozzle 12 in the lower surface side of the evaporation source 10, or the side deposit which arrange | position the nozzle 12 in the side surface of the evaporation source 10 is shown. Applicable to the method.

Moreover, the evaporation source 10 is equipped with the crucible 13 which is a heating container which heats the vapor deposition material 30. As shown in FIG. Moreover, around the crucible 13, the heating part (heater) 14 which heats the vapor deposition material 30 arrange | positioned inside the crucible 13 is provided. Moreover, around the crucible 13, the heat retention part (reflector) 15 which improves the heat retention efficiency of the crucible 13 is arrange | positioned.

As shown in FIG. 5, the housing 11 which the evaporation source 10 has is equipped with the cover part 11c and the main body part 11d. The lid part 11c and the main body part 11d are being fixed by fastening means, such as a screw which is not shown in figure. The crucible 13, the heating part 14, and the heat retaining part 15 are accommodated in the main body part 11d, and when the cover part 11c is removed, these members can be taken out. Moreover, in this embodiment, since the surface 11a which opposes the board | substrate 1 shown in FIG. 4 is arrange | positioned on the upper surface side of the housing 11, the opening part 11c is formed in the cover part 11c, and the opening part 11e is provided. ), The nozzle 12 is exposed.

Moreover, the crucible 13 is equipped with the cover part 13c and the main body part 13d. The cover part 13c and the main body part 13d are fixed by fastening means, such as a screw which is not shown in figure. The vapor deposition material 30 is accommodated in the bottom of the main body part 13d, and for example, when the lid part 13c is removed, the vapor deposition material 30 can be taken out and replaced outside of the crucible 13. . Moreover, when the lid part 13c and the main body part 13d are fixed in the overlapping state, the inside of the crucible 13 becomes a sealed space except the opening part 13e which is an ejection opening of the vapor deposition material gas 30a. In this embodiment, since the example of the structure which takes out vapor deposition material gas 30a from above the crucible 13 is shown, the opening part 13e is formed in the cover part 13c of the crucible 13. As shown in FIG. In addition, in this embodiment, since the example of the structure which discharges vapor deposition material gas 30a toward the board | substrate 1 from the opening part 13e of the crucible 13 is shown, the opening part 13e has the structure of vapor deposition material gas 30a. The nozzle 12 which is a discharge port is attached. The nozzle 12 is arrange | positioned in the position overlapping with the opening part 11e formed in the cover part 11c of the housing 11, and the nozzle 12 is exposed in the opening part 11e. In addition, although the structure of the evaporation source 10 is not limited to the aspect shown to FIG. 4 and FIG. 5, various modifications can be applied, but it is simplified in order to make it easy to understand the operation in each process of the vapor deposition method mentioned later. The structure is shown.

Moreover, the heating part 14 which heats the vapor deposition material 30 and the crucible 13 is arrange | positioned so that the circumference | surroundings of the crucible 13 may be enclosed. In this embodiment, the heating part 14 is a heater which heats the vapor deposition material 30 and the crucible 13, for example by a Joule heating system. In addition, although the example which arrange | positions the heating part 14 along the side surface of the crucible 13 is shown in FIG.4 and FIG.5, the arrangement | positioning of the heating part 14 is not limited to the example shown in FIG.4 and FIG.5. For example, the heating part 14 can be arrange | positioned also on the lid part 13c of the crucible 13, and below the crucible 13, for example. In addition, although the example which uses a coil-shaped heater as the heating part 14 is shown in FIG. 4 and FIG. 5, the structure of the heating part 14 is not limited to the example shown in FIG. 4 and FIG. For example, a plate-shaped heater (plate heater) can be arranged around the crucible 13.

Moreover, the heat retention part 15 which improves the heat retention efficiency of the crucible 13 is arrange | positioned around the crucible 13 and the heating part 14. The heat insulating part 15 is made of, for example, a plurality of metal plates, and is disposed to surround the crucible 13 except for the opening 13e. Moreover, at least the surface (inner surface) which faces the crucible 13 of each metal plate is mirror-finished. That is, the heat insulation part 15 has a function which reflects the radiation from the crucible 13 and the heating part 14, and improves the heat retention efficiency of the crucible 13 arrange | positioned inside the heat insulation part 15. . Moreover, since the heat insulation part 15 reflects the radiation from the crucible 13 and the heating part 14, the twist or melting | fusing by radiant heat to the member (for example, the body 11) of the outer side of the heat insulation part 15 is carried out. It has a function as a protection member which suppresses generation | occurrence | production.

In addition, a thermocouple TC is disposed in the evaporation source 10. For example, the thermocouple TC is disposed between the crucible 13 and the heat retaining portion 15, and is fixed in a state in which the temperature around the crucible 13 can be measured. The temperature signal detected by the thermocouple TC is transmitted to the outside of the deposition chamber 102 and based on the temperature signal, the temperature of the crucible 13 and the temperature of the deposition material 30 disposed in the crucible 13 are determined. I can figure it out.

In addition, the vapor deposition material 30 is a raw material of the vapor deposition film formed in the board | substrate 1, For example, it is the organic material which comprises the organic layer 4 shown in FIG. 2, or the metal material which comprises the electrically conductive film 5. Is done. When the vapor deposition material 30 is heated by the heating unit 14 included in the evaporation source 10, the vapor deposition material 30 vaporizes (vaporizes or sublimes) to form the vapor deposition material gas 30a. When the vapor deposition material 30 vaporizes, the inside of the crucible 13 becomes a pressure of, for example, about 10 ⁰ Pa to about 10 ¹ Pa. For this reason, the vapor deposition material gas 30a is blown out of the evaporation source 10 via the opening 11e and the nozzle 12 which were formed in the crucible 13 by the pressure difference inside and outside the crucible 13, It is emitted toward the substrate 1 which is disposed opposite to the nozzle 12.

<Deposition method>

Next, the vapor deposition method of this embodiment using the vapor deposition apparatus and evaporation source shown in FIGS. 3-5 is demonstrated. 6 is a process flow of the vapor deposition method using the vapor deposition apparatus and the evaporation source shown in FIGS. 3 to 5, the temperature profile of the crucible in each step, the ON-OFF of the heating part in each step, and the gas in each step. It is explanatory drawing which shows the presence or absence of supply. In addition, in this application, the temperature around the crucible 13 is measured by the thermocouple TC shown, for example in FIG. 4 and FIG. 5, and this is regarded as the temperature of the crucible 13. As shown in FIG. Therefore, for example, although the temperature of the crucible shown in FIG. 6 is strictly the temperature of the thermocouple provided in the evaporation source 10, it demonstrates as the temperature of the crucible 13 in the following description.

As shown in FIG. 6, the vapor deposition method of this embodiment forms the vapor deposition preparation process which prepares to form a vapor deposition film in the board | substrate 1 shown in FIG. 4, the vapor deposition process of forming a vapor deposition film in the board | substrate 1, and forms a vapor deposition film. 4 and a cooling step of cooling the crucible 13 and the evaporation material, and a maintenance step of maintaining the evaporation apparatus and the evaporation source after the cooling step.

First, in a vapor deposition preparation process, the vapor deposition film is prepared in the board | substrate 1 shown in FIG. In detail, as shown in FIG. 4, after storing the vapor deposition material 30 in the crucible 13 of the evaporation source 10, the nozzle 12 faces the rear surface 1b of the substrate 1 to be processed. It is arrange | positioned (fixed) in the film-forming chamber 102 which is a vacuum chamber. Thereafter, the valve V1 connected to the exhaust path VL is opened, and the gas in the deposition chamber 102 is exhausted by the vacuum pump VP, so that the pressure in the deposition chamber 102 is, for example, 10 ^−3. Reduce the pressure until you get a vacuum of about Pa-10 ^-5 Pa. Moreover, the board | substrate 1 is conveyed in the film-forming chamber 102 from the conveyance chamber 103 shown in FIG. 3, and the back surface 1b of the board | substrate 1 is made by the board | substrate holding part 21 as shown in FIG. The substrate 1 is supported to face the nozzle 12 through the mask 22. Moreover, an electric current flows through the heating part 14, and the crucible 13 and the vapor deposition material 30 arrange | positioned in the crucible 13 are heated. Thereby, the temperature of the crucible 13 (temperature of the deposition material 30) rises from the temperature T1 to the temperature (process temperature) T2 at the time of forming a vapor deposition film in a vapor deposition process, as shown in FIG. do. At this time, the valve V2 of the gas supply part 25 shown in FIG. 4 is closed, and gas is not supplied from a gas supply part. In addition, in this process, some time is required for the pressure reduction process which reduces the inside of the film-forming chamber 102 to predetermined vacuum degree, and the temperature raising process which raises the crucible 13 to temperature T2. For example, even when the pressure reduction step and the temperature raising step are performed in parallel, a time of about 5 hours to about 10 hours is required until the transition to the vapor deposition step. Moreover, the time required for a temperature rising process changes with the temperature T2 which is the process temperature of a vapor deposition process. For example, when forming the vapor deposition film which consists of metal materials, such as magnesium (Mg), since temperature T2 needs to be 500 degreeC or more, the time required for a temperature rising process becomes long.

Next, in the vapor deposition process shown in FIG. 6, a vapor deposition film is formed in the back surface 1b of the board | substrate 1 shown in FIG. Specifically, the vapor deposition material 30 is heated inside the evaporation source 10 to generate a vaporized (vaporized or sublimed) vapor deposition material gas 30a. The vapor deposition material gas 30a is discharged from the nozzle 12 of the evaporation source 10 toward the substrate 1. The vapor deposition material gas 30a discharged from the nozzle 12 is blown around the vapor deposition film formation area of the board | substrate 1 which opposes the nozzle 12. As shown in FIG. The vapor deposition film is formed by solidifying (condensing and depositing) the vapor deposition material gas 30a on the surface of the vapor deposition film formation region having a lower temperature than the inside of the evaporation source 10.

By the way, in the said vapor deposition preparation process, time of about 5 hours-about 10 hours is required. For this reason, from the viewpoint of improving the efficiency of the entire vapor deposition method, the substrate 1 is sequentially replaced while the pressure in the deposition chamber 102 shown in FIG. 4 and the temperature of the vapor deposition material 30 are maintained. It is preferable to form a vapor deposition film. In other words, after the deposition film is formed on the first substrate 1, the pressure in the deposition chamber 102 and the temperature of the deposition material 30 are maintained and the second substrate 1 is replaced with the second substrate 1. It is preferable to form a vapor deposition film in the substrate 1. That is, it is preferable to form a vapor deposition film continuously about the some board | substrate 1 without stopping a vapor deposition process as much as possible.

However, there is a limit to the number of substrates 1 that can be processed continuously, and the deposition process may be stopped. For example, when the vaporization of the vapor deposition material 30 shown in FIG. 4 advances and the remaining amount becomes small, it is necessary to exchange it with the new vapor deposition material 30. In this case, since the cover portion 13c of the crucible 13 shown in FIG. 5 needs to be opened to arrange a new deposition material 30, the pressure in the deposition chamber 102 and the temperature of the deposition material 30 are adjusted. It is difficult to maintain. In addition, the deposition process may be stopped due to some problem. In this case, depending on the cause of the problem, it becomes difficult to maintain the pressure in the deposition chamber 102 and the temperature of the vapor deposition material 30. In addition, when performing maintenance of each member in the film-forming chamber 102, it is necessary to stop a vapor deposition process. For example, when the evaporation process takes a long time, the vapor deposition material gas 30a may be deposited and deposited in the evaporation source 10 or the deposition chamber 102. When deposits of the vapor deposition material 30 adhered in the evaporation source 10 or in the deposition chamber 102 increase, it becomes a detrimental factor in forming the vapor deposition film, and thus, the work of removing the deposits regularly is necessary. In the maintenance process shown in FIG. 6, a vapor deposition process is stopped and the above operation (maintenance operation) is performed.

In the maintenance process shown in FIG. 6, since it is difficult to maintain the pressure of the deposition chamber 102 shown in FIG. 4 and the temperature of the vapor deposition material 30 as mentioned above, the crucible shown in FIG. 4 before a maintenance process is performed. The cooling process (refer FIG. 6) which lowers the temperature of (13) is performed. After the maintenance process is completed, as shown in FIG. 6, the deposition preparation process is performed again to prepare a vapor deposition film on the new substrate 1. Hereinafter, the detailed embodiment for shortening a cooling time in the cooling process of this embodiment shown in FIG. 6 is demonstrated. In addition, the board | substrate 1 (refer FIG. 4) in which the vapor deposition film was formed in the vapor deposition process shown in FIG. 6 is taken out from the film-forming chamber 102 (refer FIG. 4) to the conveyance chamber 103 (refer FIG. 3) before a cooling process. Hereinafter, the detail of the cooling process after taking out the board | substrate 1 from the film-forming chamber 102 is demonstrated.

<Details of the cooling process>

FIG. 7: is explanatory drawing which shows the temperature profile of the crucible in the cooling process which is a 1st and 2nd comparative example about this embodiment and this embodiment. 8 is sectional drawing which shows the state which supplied the inert gas to the crucible shown in FIG. 4 in the cooling shown in FIG. 9 is explanatory drawing which shows an example of the relationship between the temperature of the crucible shown in FIG. 4, and the saturated vapor pressure of vapor deposition material as a partial logarithmic graph.

18 is sectional drawing which shows the structure of the evaporation source used for the cooling process which is a 2nd comparative example shown in FIG. In addition, since the vapor deposition apparatus used for the 1st comparative example shown in FIG. 7 is the same as that of this embodiment except the gas supply part 25 shown in FIG. 4 is not arrange | positioned, FIG. It demonstrates with reference.

In the cooling process shown in FIG. 6, the heating part 14 shown in FIG. 4 is stopped, and the temperature of the crucible 13 is cooled from the temperature T2 which is process temperature to the temperature T1 which can perform maintenance work. The temperature T1 can be equal to, for example, room temperature (ambient temperature around the vapor deposition apparatus), but an impurity film such as an oxide film is formed on each member such as the evaporation source 10 (see FIG. 5) during the maintenance work. If it can suppress a thing and can work, it is not limited to this. Therefore, in FIG. 6, although the temperature at the start of heating in a vapor deposition preparation process and the temperature used as the end point of a cooling process in a cooling process are shown as temperature T1, respectively, this temperature T1 is exactly the same temperature. It does not have to be, but may have some width. For example, it can be made into about 30 to 60 degreeC higher than room temperature. The temperature T2 varies depending on the vaporization temperature of the vapor deposition material 30 (see FIG. 5), but may be, for example, about 400 ° C. to over 1000 ° C.

Here, the following aspects are considered as a cooling process which is a 1st comparative example concerning this embodiment. That is, it is the method of immediately stopping the heating part 14 (refer FIG. 5) immediately after starting a cooling process, and reducing the temperature of the crucible 13 (FIG. 5) by natural cooling. In this case, like the cooling curve P2 shown in FIG. 7, for example, the temperature of the crucible 13 can be cooled to the temperature T1 about 4 hours-8 hours. By the way, in this 1st comparative example, since the vaporization of the vapor deposition material 30 shown in FIG. 5 is not stopped at the stage immediately after cooling start, and the temperature of the crucible 13 falls rapidly, the wall surface in the crucible 13 is reduced. However, there is a problem that the deposition material 30 is deposited on the inner surface of the lid portion 13c and is easy to attach. As described above, if the deposition material 30 is deposited on the wall surface or the inner surface of the lid portion 13c in the crucible 13, it becomes an inhibitory factor for forming a uniform film quality deposition film in the deposition step shown in FIG. In addition, when the vapor deposition material 30 precipitates at the junction between the lid portion 13c and the main body portion 13d, the precipitate functions as an adhesive and it becomes difficult to separate the lid portion 13c from the main body portion 13d. . Moreover, when removing a precipitate, since it is necessary to remove by a machining, maintenance work becomes complicated. As described above, in the cooling step, it is necessary to suppress deposition of the vapor deposition material 30 on the wall surface of the crucible 13 or the inner surface of the lid portion 13c.

Therefore, as an embodiment which suppresses precipitation of the vapor deposition material 30 in a cooling process, the cooling process which is a 2nd comparative example with respect to this embodiment is considered. That is, in the 2nd comparative example, as shown in FIG. 18, the heating part 14 is divided into several block, and it is comprised so that each block can turn ON-OFF independently. In the example shown in FIG. 18, the upper block 14a arrange | positioned around the lid part 13c of the crucible 13, and the lower block 14b arrange | positioned around the vapor deposition material 30 arrange | positioned in the crucible 13 are shown. Dividing by). And in the cooling process which is a 2nd comparative example, after the start of a cooling process, the lower block 14b of the heating part 14 stops, but the upper block 14a does not stop. That is, in the second comparative example, while the heating by the upper block 14a is continued, the temperature of the deposition material 30 reaches the temperature T3 (see FIG. 7) at which gasification of the deposition material 30 stops. The crucible 13 and the deposition material 30 are gradually cooled until it is. Thereafter, the upper block 14a is also stopped and cooled by natural cooling until the entire temperature of the crucible 13 reaches the temperature T1. According to this second comparative example, the heating of the lid portion 13c is continued until the vaporization of the vapor deposition material 30 is stopped, thereby preventing the deposition material 30 from adhering to the lid portion 13c. can do. However, as shown by the cooling curve P3 in FIG. 7, since the cooling rate becomes slow (for example, about 2 hours-about 3 hours) from the temperature T2 to the temperature T3 (slow cooling period), Until it reaches temperature T1 which is an end point of a cooling process, time of about 5 hours-about 10 hours is required, for example.

In addition, as a 3rd comparative example (not shown), during the cooling process, the thermal insulation part 15 shown in FIG. 5 is moved upwards, and the circumference | surroundings of the vapor deposition material 30 of the crucible 13 are the thermal insulation part 15 ), And the structure which heat-retains the circumference | surroundings of the cover part 13c by the heat retention part 15 is also considered. However, since the thermal insulation part 15 has a function as a protection member which suppresses generation | occurrence | production of twisting and melting by radiant heat in the member (for example, the body 11) of the outer side of the thermal insulation part 15, In the third comparative example, the heat or the like 11 disposed around the crucible 13 is damaged by heat radiation from the crucible 13, which causes a problem of the vapor deposition apparatus.

In view of the problems of the respective comparative examples described above, the inventors of the present invention studied the technology of suppressing the deposition of the vapor deposition material 30 in the cooling step and shortening the cooling time, and found out the configuration of the present embodiment. This inventor pays attention to the relationship between generation | occurrence | production of the vapor deposition material gas 30a (refer FIG. 4), and saturated vapor pressure, and raises the pressure in the crucible 13 in a cooling process, and reduces gasification of the vapor deposition material 30, The configuration to stop was found. That is, as shown in FIG. 8, in the cooling process, the gas (inert gas) 26 is supplied from the gas supply part 25 to the crucible 13 through the nozzle 12, and the pressure in the crucible 13 is vapor-deposited. By making it higher than the saturated vapor pressure of the material 30, gasification of the vapor deposition material 30 can be reduced or stopped. Moreover, as a supply method of the gas 26, the method of supplying the gas 26 to the whole inside the film-forming chamber 102 which is a vacuum chamber is also considered. However, in this case, foreign matter remaining in the film formation chamber 102 may be wound up by the gas 26 and mixed in the crucible 13. Therefore, it is preferable to selectively supply the gas 26 toward the crucible 13 from the viewpoint of preventing foreign matter mixing, and locally increase the pressure in the crucible 13. In this embodiment, as shown in FIG. 8, the gas discharge port GN of the gas supply part 25 is arrange | positioned in the film-forming chamber 102, and is arrange | positioned toward the opening part of the nozzle 12 of the evaporation source 10. As shown in FIG. Moreover, the gas supply path GL of the gas supply part 25 is led to the exterior of the film formation chamber 102, and is connected to the gas supply source TG arrange | positioned outside of the film formation chamber 102. As shown in FIG. In the gas supply source TG, an inert gas source such as argon (Ar) or nitrogen (N ₂ ) is stored, for example. Moreover, between the gas supply source TG and the gas discharge port GN, the valve V2 which adjusts the presence or absence of gas supply and a flow volume is arrange | positioned, and is connected with the gas supply path GL. Accordingly, when the valve V2 is opened at or after the cooling process is started, the gas 26 is supplied to the inside of the crucible 13 through the nozzle 12 from the outside of the evaporation source 10. Moreover, since the gas discharge port GN of the gas supply part 25 is arrange | positioned in the film-forming chamber 102, and is arrange | positioned toward the opening part of the nozzle 12 of the evaporation source 10, the gas 26 is the crucible 13 It can be selectively supplied in the chamber to locally raise the pressure in the crucible 13. Moreover, the flow volume of the gas 26 and the supply pressure of the gas 26 can be adjusted by the opening degree of the valve V2, for example.

As shown in FIG. 9, the saturated vapor pressure of the vapor deposition material 30 (refer FIG. 8) is sufficiently small compared with standard atmospheric pressure (about 101 kPa), and the pressure in the crucible 13 at the time of starting a cooling process is for example. It is 100 Pa or less even when a crucible temperature is 1100 degreeC. For this reason, even if the pressure of the gas 26 (refer FIG. 8) to supply is a small value with respect to standard atmospheric pressure, if the pressure higher than the pressure in the crucible 13 in the vapor deposition process shown in FIG. Can be pressurized. Moreover, since the pressure in the crucible 13 becomes higher than the pressure of the space outside the crucible 13, a part of the gas 26 supplied in the crucible 13 is discharged | emitted from the nozzle 12 to the outside of the crucible 13 However, by continuously supplying the gas 26 from the gas supply portion 25 toward the nozzle 12, the pressure in the crucible 13 can be maintained higher than the saturated vapor pressure of the deposition material 30. That is, according to the present embodiment, the gasification of the vapor deposition material 30 can be stopped or significantly reduced by supplying gas into the crucible 13 through the nozzle 12 from the outside of the evaporation source 10 in the cooling step. have. For this reason, for example, as shown in FIG. 6, when the heating part 14 (refer FIG. 8) is stopped at the start of a cooling process, even if the temperature of the crucible 13 abruptly falls, vapor deposition material 30 is carried out. ) (See FIG. 8) can be suppressed. In addition, as in the cooling curve P3 according to the second comparative example shown in FIG. 7, it is not necessary to provide a slow cooling period, so that the cooling time can be greatly shortened (for example, to be less than half with respect to the second comparative example). Can be. Moreover, according to this embodiment, since a cooling time can be shortened without moving the heat insulation part 15 in a cooling process, it radiates to radiant heat to the member (for example, the body 11) of the outer side of the heat insulation part 15. It can suppress generation | occurrence | production of torsion and fusion by it.

In addition, as in the present embodiment, when the gas 26 is supplied into the crucible 13, the cooling time can be further shortened than in the first comparative example shown in FIG. 7. The gas 26 supplied into the crucible 13 is in contact with the wall surface and the vapor deposition material 30 in the crucible 13, and heat exchange is performed. The gas 26 whose temperature has risen due to heat exchange moves upward of the crucible 13, and a part of the gas 26 is discharged from the nozzle 12 to the outside of the crucible 13. On the other hand, since the gas 26 newly supplied from the gas discharge port GN of the gas supply part 25 has a lower temperature than the gas 26 discharged from the nozzle, the gas 26 easily enters the crucible 13. In this way, the gas 26 which has risen in temperature by heat exchange is discharged to the outside, and the heat exchange proceeds by supplying the gas 26 having a relatively low temperature therein, thereby facilitating the temperature reduction of the crucible 13. For this reason, as shown in FIG. 7, the cooling curve P1 in the cooling process of this embodiment can shorten cooling time compared with the cooling curve P2 in the case of natural cooling. For example, in the example of the cooling curve P1 shown in FIG. 7, the time (cooling time) in which the temperature of the crucible 13 falls from the temperature T2 to the temperature T1 is about 2.5 hours-about 5 hours.

<Preferred sun>

Next, the particularly preferable aspect in the vapor deposition apparatus and vapor deposition method of above-mentioned this embodiment is demonstrated including a modification. FIG. 10 is an explanatory diagram showing a process flow of a vapor deposition method which is a modification to FIG. 6, a temperature profile of the crucible in each step, ON-OFF of a heating part in each step, and whether or not gas is supplied in each step. FIG. to be. FIG. 11 is a cross-sectional view showing an entire configuration in a film forming room as a modification of FIG. 4. FIG. 12 is sectional drawing which shows the modification of the film-forming chamber shown in FIG.

First, it is preferable that the gas 26 shown in FIG. 8 is an inert gas from the viewpoint of suppressing generation | occurrence | production of an impurity by reacting with the vapor deposition material 30 arrange | positioned in the crucible 13 and the crucible 13 itself. Here, the inert gas means that the impurity is less likely to produce impurities than the deposition material 30 disposed in the crucible 13 or the atmosphere gas outside the deposition chamber 102 which is a vacuum chamber with respect to the crucible 13 itself. As the so-called rare gas, nitrogen is also included. Moreover, according to the constituent material of the crucible 13 and process temperature (temperature T2 shown in FIG. 6), a preferable gas species differs. For example, when the temperature T2 is higher than 800 ° C. and the crucible 13 is formed of a metal material such as molybdenum (Mo), tantalum (Ta), tungsten (W), impurities are generated. Since it is easy to become, it is preferable to use gas 26 as argon (Ar) gas. On the other hand, when the crucible 13 is formed of a ceramic such as alumina or boron nitride, or carbon (c), if the crucible 13 does not generate impurities by reacting with the deposition material 30, it is made of nitrogen (N ₂ ) gas which is cheaper than argon gas. It is desirable to. In the case of forming a deposited film temperature (T2) is formed at a temperature lower than 400 ℃ of an organic material, it may be a nitrogen gas or carbon dioxide (CO ₂₎ gas.

In addition, from the viewpoint of shortening the cooling time, as shown in FIG. 6, it is preferable to continuously supply the gas 26 until the temperature of the crucible 13 reaches the temperature T1. When the supply of the gas 26 is stopped in the middle of the cooling step and the temperature T1 is reached by natural cooling, the cooling rate decreases when the temperature of the atmosphere and the temperature of the crucible 13 are close to each other. However, by continuously supplying the gas 26, since the heat exchange by the gas 26 continues even when the ambient temperature and the temperature of the crucible 13 are close to each other, the cooling time can be further shortened than in the case of natural cooling. However, from a viewpoint of reducing the cost of the gas 26 used in a cooling process, it is preferable to switch the gas 26 in the middle of a cooling process. For example, as described above, when the temperature T2 is higher than 800 ° C., and the crucible 13 is formed of a metal material such as molybdenum, tantalum, tungsten or the like, the gas is started at the start of the cooling step. Argon gas is supplied as (26). And when the temperature of the crucible 13 becomes 400 degrees C or less, for example, the kind of gas 26 will be switched and it will be made into nitrogen gas and carbon dioxide gas which are cheaper than argon gas, for example. In this case, cooling time can be shortened and the manufacturing cost at the time of forming a vapor deposition film can be reduced.

On the other hand, from the viewpoint of reducing the amount of use of the gas 26, as in the modification shown in FIG. 10, the supply of the gas 26 is stopped in the middle of the cooling process, and then the temperature of the crucible 13 is increased by natural cooling. It is preferable to reach (T1). In this case, even if the temperature of the crucible 13 stops supply of the gas 26, it is preferable to stop supply of the gas 26 at the stage where the temperature of the crucible 13 fell to the temperature which becomes small enough for the vaporization material 30 to vaporize. Do. As an embodiment for performing the vapor deposition method as shown in FIG. 10, for example, as shown in FIG. 11, the sensor 27 and the crucible 13 which measure the vapor deposition material gas 30a in the film-forming chamber 102 are shown. The temperature sensor (not shown) which measures the temperature of the () is installed in advance. And in the vapor deposition preparation process shown in FIG. 10, the temperature (gasification temperature) of the crucible 13 when the sensor 27 detects vapor deposition material gas 30a is electrically connected with the sensor 27 and a temperature sensor. It records in the control part 28 connected. In the cooling step, the temperature of the crucible 13 is measured, and at the stage where the temperature is lowered to the gasification temperature or lower, for example, the control unit 28 closes the valve V2 to supply the gas 26. Stop. Moreover, as another embodiment, in the vapor deposition process and cooling process shown in FIG. 10, the sensor 27 (refer FIG. 11) continuously measures the detection ratio (detection amount in a set measurement range) of the vapor deposition material gas 30a. do. And when the detection ratio of the vapor deposition material gas 30a detected in a cooling process becomes below a preset reference value (for example, 1/10-1/100 or less of the detection ratio in a vapor deposition process), a valve ( The supply of the gas 26 is stopped by closing V2). Thus, when supply of the gas 26 is stopped in the middle of a cooling process, cooling time becomes long compared with the example shown in FIG. 6, but the usage-amount of the gas 26 can be reduced.

In addition, in the cooling process of this embodiment, supply of the gas 26 from the gas supply part 25 and stopping the heating part 14 stop the vapor deposition material 30 in the crucible 13 and the crucible 13. It is preferable to stop the heating section 14 after the supply of the gas 26 is started for cooling. As shown in FIG. 9, since the saturated vapor pressure of the vapor deposition material 30 is very small, when the supply of the gas 26 is started, the quantity of the vapor deposition material 30 which vaporizes in a short time will be reduced significantly. However, from the viewpoint of more reliably suppressing deposition of the deposition material 30 on the wall surface or the inner surface of the lid portion 13c in the crucible 13, the timing of stopping the heating portion 14 is determined by the gas 26. It is preferable to carry out after starting supply. In addition, the timing which stops the heating part 14 can be determined by the elapsed time after starting supply of the gas 26, for example. Moreover, as a method of more reliably suppressing precipitation of the vapor deposition material 30, after confirming that the detection amount of the vapor deposition material gas 30a is small enough using the sensor 27 shown in FIG. The method of stopping (14) is effective.

In addition, as shown in FIG. 4, in the vapor deposition process, it is necessary to arrange | position the gas supply part 25 so that the path | route (emission path) from which the vapor deposition material gas 30a may be discharged toward the board | substrate 1 from the nozzle 12 may be avoided. There is. For this reason, as shown in FIG. 4, the gas discharge port GN of the gas supply part 25 is arrange | positioned apart from the nozzle 12, and the vapor deposition material gas 30a which reaches from the nozzle 12 to the board | substrate 1 is shown. With respect to the axis line (virtual line) AL of the discharge path of, it is preferable that the discharge angle from the gas discharge port GN is disposed to be inclined. Thereby, a vapor deposition film can be stably formed in the board | substrate 1, without performing the operation | work which retracts the gas discharge port GN at the time of a vapor deposition process. In other words, in the aspect shown in FIG. 4, supply of the gas 26 (refer FIG. 8) can be started, without moving the position of the gas discharge port GN when moving from a vapor deposition process to a cooling process. In addition, since it is not necessary to move the position of the gas discharge port GN when moving from a vapor deposition process to a cooling process, the relationship between the position of the nozzle 12 and the gas discharge port GN, and the emission angle of the gas 26 is Can be adjusted with high precision. As a result, the gas 26 can be reliably discharged toward the nozzle 12 in the cooling step. Thus, in this embodiment, since it is not necessary to move the position of the gas discharge port GN when moving from a vapor deposition process to a cooling process, the gas supply path GL is comprised by metal piping, for example. .

Moreover, it is preferable to close the valve V1 connected to the exhaust path VL in a cooling process. When the cooling step is performed while the valve V1 is closed, the gas 26 can be convection in the film forming chamber 102 shown in FIG. 8 because the cooling step can be performed while the exhaust gas in the film forming chamber 102 is stopped. do. For this reason, cooling of the crucible 13 can be accelerated | stimulated and the cooling time can be shortened further. Moreover, as an aspect which further promotes the convection of the gas in the film-forming chamber 102 in a cooling process, it purges gas 31 separately from the gas supply part 25 in the film-forming chamber 102 like the modification shown in FIG. The purge gas supply part 32 which supplies ()) can be arrange | positioned. According to the structure shown in FIG. 12, the supply amount of the purge gas 31 supplied from the purge gas supply source TP is controlled independently of the gas 26 supplied from the gas supply part 25 by adjusting the opening degree of the valve V3. Therefore, the purge gas 31 can be convection efficiently in the film forming chamber 102. As the gas 26, the purge gas 31 is preferably an inert gas from the viewpoint of suppressing the generation of impurities, and particularly preferably the same gas as the gas 26.

<Other Modifications>

Next, modifications other than the above-described modifications will be described. FIG. 13 is a sectional view showing a modification of the gas supply unit shown in FIG. 8, and FIG. 14 is an enlarged sectional view of the vicinity of the nozzle shown in FIG. 15 is sectional drawing which shows the layout of the gas supply part in the vapor deposition process of forming a vapor deposition film in the vapor deposition method using the gas supply part shown in FIG. 16 and 17 are enlarged cross-sectional views illustrating respective states in which the gas supply units shown in FIGS. 13 to 15 are operated.

The gas supply part 25 shown in FIG. 8 and the gas supply part 35 shown in FIGS. 13-17 differ from the following point. First, the gas supply part 35 shown in FIGS. 13-18 is connected to the stopper part (nozzle cap) NC which the gas supply path GL covers the opening part of the nozzle 12 in a cooling process. The stopper portion NC is provided with a through hole constituting a part of the gas supply path GL, and as shown in FIG. 14, the tip of the through hole discharges the gas 26 into the crucible 13. It is a discharge port GN.

In the vapor deposition method using the gas supply part 35, the opening part of the nozzle 12 is covered with the stopper part NC of the gas supply part 35 in the cooling process shown in FIG. At this time, the gas discharge port GN (see FIG. 14) of the gas supply part 35 is disposed inside the nozzle 12 or inside the crucible 13. When the valve V2 shown in FIG. 3 is opened in this state, the gas 26 can be supplied to the crucible 13 more reliably than the gas supply part 25 shown in FIG. When covering the opening part of the nozzle 12 with the stopper part NC of the gas supply part 35, the nozzle 12 and the stopper part NC may be closely contacted and the opening part of the nozzle 12 may be completely closed. However, as shown in FIG. 14, it is more preferable to provide a clearance gap without making the nozzle 12 and the stopper part NC contact. As mentioned above, in the cooling process, the gas 26 which rose by heat exchange in the crucible 13 collects upwards. Thus, by providing a gap between the nozzle 12 and the stopper NC, the gas 26 having risen in temperature can be discharged from the gap to the outside of the evaporation source 10, so that the gas 26 having a relatively low temperature enters the inside. By supplying, heat exchange advances and the temperature fall of the crucible 13 can be accelerated | stimulated. In addition, although the gas discharge port GN of the gas supply part 35 is shown in the inside of the nozzle 12 in FIG. 14, when the gas discharge port GN is arrange | positioned on the opening part of the nozzle 12, Since the gas 26 can be supplied to the crucible 13 reliably, the gas discharge port GN may be disposed outside the nozzle 12. However, when the distance between the gas discharge port GN and the opening part of the nozzle 12 becomes large, since some part of the gas 26 may spread to the outer side of the nozzle 12, the gas discharge port GN may be a nozzle ( It is preferable to arrange | position in the vicinity of the opening part of 12, and it is especially preferable to arrange | position in the opening part of the nozzle 12 or in the crucible 13.

In addition, in this modification, since the stopper NC is disposed on the nozzle 12 which is the discharge port of the vapor deposition material gas 30a (see FIG. 15) after the start of the cooling process, the vapor deposition material is disposed on the surface of the stopper NC. 30 (refer FIG. 13) may precipitate. In this way, even when the deposition material 30 is deposited on the surface of the stopper part NC, the gap between the nozzle 12 and the stopper part NC is provided so that the stopper part NC and the nozzle 12 are separated. Adhesion by a precipitate can be suppressed. In addition, from the viewpoint of more reliably suppressing deposition of the deposition material 30 on the surface of the plug portion NC, as shown in FIG. 14, the heating portion 36 is provided in the plug portion NC, and the plug portion is provided. It is preferable to heat (NC).

By the way, as shown in FIG. 13, since the stopper NC of the gas supply part 35 is arrange | positioned so that the nozzle 12 may be covered in a cooling process, in the vapor deposition process shown in FIG. 6, for example, in FIG. As shown, it is necessary to move the stopper NC from the nozzle 12. Therefore, in the modified example shown in FIGS. 13-17, the state which can move the position of the stopper part NC at the time of the transition from the vapor deposition process shown in FIG. 6 to a cooling process, and the transition from a cooling process to a maintenance process is shown. I support it. For example, in the example shown to FIGS. 13-17, the stopper part NC is fixed to the support part SB which supports the stopper part NC and the gas supply path GL connected to the stopper part NC. have. In addition, the fixing method of the stopper part NC is not specifically limited, For example, you may form the stopper part NC and the support part SB integrally. The support part SB is movable in the state which fixed the stopper part NC (supported state), for example, when it moves to a cooling process from a vapor deposition process, it moves as shown to FIG. 16 and FIG. First, as shown in FIG. 16, it operates by rotational movement so that the stopper part NC may be located on the nozzle 12 using a part of support part SB as a support point. Next, as shown in FIG. 17, the whole support part SB moves downward with the stopper part NC, and covers the opening part of the nozzle 12 with the stopper part NC as shown in FIG. In this state, the valve V2 shown in FIG. 13 is opened to supply the gas 26. In addition, when shifting from the cooling process shown in FIG. 6 to a maintenance process, operation | movement opposite to the operation shown in FIG. 17 and FIG. 16 is performed. Moreover, since the gas supply path GL is connected to the stopper part NC moving at the time of implementing a process, at least one part of the gas supply path GL is comprised by the piping which can be deformed with the movement of the stopper part NC. do.

In addition, since the said modification is the same as embodiment shown in FIG. 1 thru | or FIG. 9 except the above-mentioned difference, overlapping description is abbreviate | omitted. Moreover, the modified example shown in FIGS. 13-17 can also be applied combining the various modified examples mentioned above.

As mentioned above, although the invention made by this inventor was demonstrated concretely based on embodiment, this invention is not limited to the said embodiment, Needless to say that it can be variously changed in the range which does not deviate from the summary.

For example, in the said embodiment, although the deposition method called what is called a point source system which formed the vapor deposition film using the evaporation source 10 provided with the one nozzle 12 as an aspect of an evaporation source was mentioned and demonstrated, It can be set as the vapor deposition method which arrange | positions and arrange | positions the some evaporation source 10 in the film-forming chamber 102. FIG. In this case, since the range where the vapor deposition material gas 30a reaches becomes wider, the efficiency of the vapor deposition process can be improved.

Moreover, in the said embodiment, although the aspect which discharge | emits vapor deposition material gas 30a from the fixed evaporation source 10 was demonstrated as an aspect of an evaporation source, as a modification, the evaporation source 10 and the board | substrate 1 are moved relatively. It is applicable to the embodiment which forms a vapor deposition film in the board | substrate 1, making it possible. Thus, the method of forming a vapor deposition film, moving the evaporation source 10 and the board | substrate 1 relatively, even if the area of the vapor deposition film formation surface of the board | substrate 1 which is a to-be-processed object is large, the film thickness and film quality of a vapor deposition film are uniform. It is advantageous in that it can be done. Moreover, in the vapor deposition method using the vapor deposition apparatus which moves a vaporization source and a board | substrate relatively, as shown in FIG. 4, the axis (virtual line) of the discharge path | route of the vapor deposition material gas 30a from the nozzle 12 to the board | substrate 1 is shown. With respect to AL, the release angle from the gas discharge port GN does not have to be inclined. In this case, although not shown, the evaporation source is moved at or before the start of the cooling process, or the gas outlet of the gas supply is relatively moved, so that the gas outlet of the gas supply is opposite to the opening of the nozzle of the evaporation source. Place it in place. Thereafter, when gas is selectively supplied from the gas supply part toward the crucible, the pressure in the crucible can be locally increased.

The present invention can be widely used for products for forming vapor deposition films such as organic EL displays and lighting, and vapor deposition apparatuses.

One… Board
1a ... surface
1b ... If
2… Organic EL display device (display device)
2a ... Organic EL device
3, 5... Conductive film
6 ... Sealant
7 ... Sealing substrate
4… Organic layer
4a ... Hole transport layer
4b ... The light-
4c... Electron transport layer
10, 10A ... Evaporation source
11 ... Ore
11a ... if
11c ... The lid portion
11d... The body portion
11e... Opening
12... Nozzle
13 ... Crucible
13c... The lid portion
13d... The body portion
13e ... Opening
14 ... Heating section
14a ... Upper block
14b... Lower block
15... Thermal insulation part (reflector)
21 ... The substrate-
22... Mask
22a ... Opening
25, 35... Gas supply portion
26 ... gas
27 ... sensor
28 ... The control unit
30 ... Deposition material
30 ... Deposition material gas
31 ... Purge gas
32 ... Purge gas supply
36 ... Heating section
100 ... Deposition apparatus
101 ... Delivery room
101a ... The loader section
101b... Unloader portion
102... The Tent of Meeting
103 ... Conveying room
103a... Robot (substrate conveying device)
GL ... Gas supply path
GN… Gas outlet
NC… Stopper
P1, P2, P3... Cooling curve
SB… Support
T1, T2, T3... Temperature
TC… thermocouple
TG… Gas source
TP… Purge gas source
V1, V2, V3... valve
VL… Exhaust path
VP… Vacuum pump

Claims (15)

(a) preparing a evaporation source having a crucible containing a vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging the vaporization material vaporized in the crucible toward an object to be processed;
(b) heating the vapor deposition material stored in the crucible by the heating unit to generate a vaporized vapor deposition material gas to form a vapor deposition film on the workpiece;
(c) after the step (b), selectively supply gas through the nozzle from the gas supply unit disposed outside the evaporation source to the inside of the crucible to locally increase the pressure inside the crucible, Stopping the part to cool the crucible;
In the step (c), the gas discharge port for supplying the gas into the crucible is spaced apart from the nozzle,
And the discharge angle of the gas from the gas discharge port is inclined with respect to the axis of the discharge path of the deposition material gas from the nozzle to the workpiece. The method of claim 1,
And the gas supplied into the crucible in the step (c) is an inert gas. (a) preparing a evaporation source having a crucible containing a vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging the vaporization material vaporized in the crucible toward an object to be processed;
(b) heating the vapor deposition material stored in the crucible by the heating unit to generate a vaporized vapor deposition material gas to form a vapor deposition film on the workpiece;
(c) after the step (b), selectively supply gas through the nozzle from the gas supply unit disposed outside the evaporation source to the inside of the crucible to locally increase the pressure inside the crucible, Stopping the part to cool the crucible;
In the step (c), the gas supply unit for supplying the gas into the crucible, in the step (c), comprises a stopper covering the opening of the nozzle,
The gas supply path of the gas supply unit is connected to a through hole formed in the plug portion, and the gas outlet of the gas supply unit is in the opening of the nozzle, in the opening of the nozzle, or the crucible in the step (c). And disposed within. The method of claim 3, wherein
In the said (c) process, the said stopper part is heated, The vapor deposition method characterized by the above-mentioned. The method according to claim 1 or 3,
In the step (c), the gas is continuously supplied until the temperature of the crucible reaches a temperature that is the end point of the cooling. (a) preparing a evaporation source having a crucible containing a vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging the vaporization material vaporized in the crucible toward an object to be processed;
(b) heating the vapor deposition material stored in the crucible by the heating unit to generate a vaporized vapor deposition material gas to form a vapor deposition film on the workpiece;
(c) after the step (b), selectively supply gas through the nozzle from the gas supply unit disposed outside the evaporation source to the inside of the crucible to locally increase the pressure inside the crucible, Stopping the part to cool the crucible;
In the step (c), the gas is continuously supplied until the temperature of the crucible reaches a temperature which becomes the end point of the cooling,
In the said (c) process, the vapor deposition method characterized by switching the kind of said gas in the middle of the said cooling. The method according to claim 1 or 3,
In the step (c), the supply of the gas is stopped before the temperature of the crucible reaches a temperature at which it is the end point of the cooling. (a) preparing a evaporation source having a crucible containing a vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging the vaporization material vaporized in the crucible toward an object to be processed;
(b) heating the vapor deposition material stored in the crucible by the heating unit to generate a vaporized vapor deposition material gas to form a vapor deposition film on the workpiece;
(c) after the step (b), selectively supply gas through the nozzle from the gas supply unit disposed outside the evaporation source to the inside of the crucible to locally increase the pressure inside the crucible, Stopping the part to cool the crucible;
In the step (c), the supply of the gas is stopped before the temperature of the crucible reaches a temperature which becomes the end point of the cooling,
And a sensor for detecting a timing of stopping the supply of the gas. A vacuum chamber, an evaporation source disposed in the vacuum chamber, a gas supply part for supplying gas into the evaporation source, and a holding part for holding a workpiece in the vacuum chamber,
The evaporation source
A crucible accommodating vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging vapor deposition material gas vaporized in the crucible toward the target object,
The gas-
A gas supply path for introducing the gas into the vacuum chamber from the outside of the vacuum chamber, and a gas outlet for supplying the gas into the crucible from the nozzle of the evaporation source,
The gas outlet of the gas supply unit is disposed apart from the nozzle,
And a discharge angle of the gas from the gas discharge port is inclined with respect to an axis of the discharge path of the deposition material gas from the nozzle to the workpiece. The method of claim 9,
And the gas supply part is connected to a source of inert gas, and the inert gas is discharged from the gas outlet. A vacuum chamber, an evaporation source disposed in the vacuum chamber, a gas supply part for supplying gas into the evaporation source, and a holding part for holding a workpiece in the vacuum chamber,
The evaporation source
A crucible accommodating vapor deposition material, a heating part for heating the crucible, and a nozzle for discharging vapor deposition material gas vaporized in the crucible toward the target object,
The gas-
A gas supply path for introducing the gas into the vacuum chamber from the outside of the vacuum chamber, and a gas outlet for supplying the gas into the crucible from the nozzle of the evaporation source,
The gas supply part has a stopper covering an opening of the nozzle,
The stopper is fixed to the support for moving the stopper from the opening of the nozzle,
The gas supply path is connected to a through hole formed in the stopper;
And the gas outlet of the gas supply part is disposed on the opening of the nozzle, in the opening of the nozzle or in the crucible when the stopper is disposed at a position covering the opening of the nozzle. The method of claim 11,
The stopper part is provided with a heating part for heating the stopper part. The vapor deposition method according to claim 3, 6 or 8, wherein the gas supplied into the crucible in the step (c) is an inert gas. The method according to claim 3, 6, or 8, wherein in the step (c), the position of the evaporation source or the gas outlet of the gas supply unit is moved relatively until the crucible starts cooling. And a gas is supplied from the gas supply part to the inside of the crucible through the nozzle from the gas supply part so as to face the opening of the nozzle. The vapor deposition apparatus according to claim 11, wherein the gas supply part is connected to a source of an inert gas, and the inert gas is discharged from the gas discharge port.

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