KR20110057604A - Vacuum evaporating sources with heaters deposited directly on the surface of crucible, the method of manufacturing and evaporator - Google Patents

Abstract

PURPOSE: A heater-integrated molecular beam evaporation source for vacuum deposition, a manufacturing method thereof, and an evaporator using the same are provided to minimize the thermal load of a vacuum system by controlling the temperature of a heater to be similar to the temperature of a crucible. CONSTITUTION: A heater-integrated molecular beam evaporation source for vacuum deposition comprises a PBN(Pyrolytic Boron Nitride) crucible(10), a first heater(20), and a first protective film. The PBN crucible accepts materials. The first heater is deposited on the outer surface of the PBN crucible and forms a pattern proper for heating without influence of magnetic field on a specimen. The first protective film is deposited on the inner surface of the PBN crucible to protect the crucible from the specimen easy to adhere to PBN and partially removed for insulation from the first heater.

Description

Vapor evaporating sources with heaters deposited directly on the surface of crucible, the method of manufacturing and evaporator

The present invention relates to a crucible and a heating part in an evaporation system such as a molecular beam growth apparatus (MBE, Molecular Beam Epitaxy) or an organic light emitting diode deposition apparatus using a method of heating a crucible in a vacuum to deposit a material emitted from the crucible into a sample. It relates to a configured evaporation source and a method of manufacturing the evaporation source. More specifically, a heat generating unit integrated high efficiency evaporation source for heating the crucible directly in contact with the heat generating portion by depositing a heating material on the outer surface of the crucible and patterning it to be suitable for heating to generate a heat generating portion, and injecting a current into the heat generating portion, It relates to a manufacturing method and an evaporator.

Typical methods for forming a thin film on a substrate include physical vapor deposition (PVD), such as vacuum evaporation, ion plating, and sputtering, and chemical vapor deposition by gas reaction. Law). The molecular beam growth apparatus forms a semiconductor thin film by growing atoms or molecules forming a semiconductor material under ultra high vacuum on a substrate by vacuum deposition. In addition, the organic light emitting diode thin film growth apparatus grows a thin film by depositing an organic material constituting the organic light emitting diode by a vacuum deposition method. In addition, in order to form an electrode in the organic light emitting diode, a metal such as aluminum is deposited using a vacuum deposition method.

As described above, in a general deposition apparatus for depositing an organic film and a metal film by using a vacuum deposition method, a substrate is mounted on an upper portion of the deposition chamber, and an evaporation source is disposed below the deposition chamber. The evaporation source includes a crucible containing a deposition material, and a heating unit installed outside the crucible and serving as a heat source for evaporating the deposition material. When power is applied to the heat generating part of the evaporation source, the crucible and the deposition material in the crucible are heated, and the vaporized deposition material is deposited on a substrate mounted on the upper side of the chamber to form an organic film or a metal film on the substrate.

However, since the heat generating part generally used in vacuum as the evaporation source of the deposition apparatus is separated from the crucible, heat is transmitted by radiation and absorption of light. Therefore, the heat transfer efficiency is low and the heat loss is high, which causes a large heat load on the system. In addition, since the temperature of the heat generating portion is considerably higher than the temperature of the crucible, there is a problem in that excessive heat is generated and the upper temperature of the crucible is controlled lower than the temperature of the middle portion of the crucible.

Therefore, the efficiency of heat transfer in the deposition apparatus, the heat loss is minimized, the temperature of the heating portion is controlled to be similar to the temperature of the crucible to minimize the heat load in the vacuum system, the temperature of the top of the crucible is lower than other parts It is desirable to develop an evaporation source that can solve the problem.

Crucibles used at high purity and high temperature are made of PBN (pyrolytic boron nitride), PG (pyrolytic graphite) can be used as a high-purity heating element at high temperature, and its thermal expansion coefficient is similar to that of PBN. Since the process is similar, a high-quality evaporation source can be manufactured by applying a PG heating element to the outside of the PBN crucible.

The present invention is to solve the problems of the prior art, an object of the present invention by depositing a heating material on the surface of the crucible in a vacuum deposition system to directly transfer the heat of the heating portion by the heat conduction to the crucible to increase the efficiency of heat transfer An evaporation source, a manufacturing method of the evaporation source, and an evaporator are provided.

As a technical solution for achieving the object of the present invention, the first aspect of the present invention is made of a PBN for containing the material used in the deposition system for depositing a material such as organic matter or metal to the sample in a vacuum A heat generating unit integrated evaporation source including a crucible and a PG deposited and patterned on the outer surface of the PBN crucible for heating is presented.

According to a second aspect of the present invention, a crucible made of PBN for holding the material used in a deposition system for depositing a material such as an organic substance on a sample in a vacuum, and an outer surface of the PBN crucible are patterned to be suitable for heating. A first passivation layer comprising a PG deposited to protect the crucible from a sample that is deposited on an inner surface of the PBN crucible and adheres well to PBN, such as aluminum; A heating unit integrated evaporation source including an heating unit and an insulating unit for electrically insulating the first passivation layer is provided. Some materials, such as aluminum, change from a liquid state to a solid state during cooling, so that they adhere well to the PBN crucible, and thus, when the crucible is cooled, the crucible is damaged due to a difference in thermal expansion coefficient between the sample and the crucible. Since these samples do not adhere well to PG, the problem of crucible breakage can be solved by forming a PG film inside the crucible.

According to a third aspect of the present invention, in the invention of the first aspect of the present invention, a PBN cap body having a discharge port formed therein for covering an opening of the PBN crucible and corresponding to the discharge port on an outer surface of the PBN cap body A heat generating unit-integrated evaporation source is provided that includes a second heat generating portion consisting of a hole and a patterned PG deposited for heating.

According to a fourth aspect of the present invention, in the invention of the second aspect of the present invention, a PBN cap body having a discharge port formed therein for covering an opening of the PBN crucible, and corresponding to the discharge port on an outer surface of the PBN cap body And a second heat generating portion comprising PG deposited and patterned to be suitable for heating and heating, and PG for protecting the crucible from a sample deposited on the inner surface of the PBN lid and adhered well to PBN, such as aluminum. A heat generating unit integrated evaporation source including a second protective film to be formed and an insulating part for electrically insulating the second heating part and the second protective film is provided.

In a fifth aspect of the present invention, a method for producing an evaporation source of the first to fourth aspects of the present invention is presented.

According to a sixth aspect of the present invention, an evaporator which utilizes a power supply electrode as a support when mounting the heat generating unit integrated evaporation source on a vacuum flange is presented.

In a seventh aspect of the present invention, there is provided an evaporator further comprising a spacing device designed to minimize the contact area to prevent the evaporation source from being moved or broken when the heating unit integrated evaporation source is mounted on the vacuum flange. .

According to the molecular beam evaporation source for vacuum unit integrated vacuum thin film deposition of the heat generating unit, it is possible to minimize heat load in the vacuum system by maximizing heat transfer efficiency, minimizing heat loss, and controlling the temperature of the heat generating unit to be similar to the temperature of the crucible. And, there is an effect that can solve the problem that the upper temperature of the crucible is controlled lower than other parts. In addition, it is possible to prevent the PBN crucible from being damaged from a sample that adheres well to PBN, such as aluminum. In addition, it is possible to improve the use efficiency of the sample by arranging the discharge port well on the lid body.

Hereinafter, with reference to the accompanying drawings, the configuration of the invention according to an embodiment of the present invention will be described in detail.

1 is a schematic configuration diagram of a first embodiment of a heat generating unit integrated high efficiency evaporation source of the present invention. As shown in FIG. 1, in a deposition system for depositing a material such as an organic material or a metal on a sample in a vacuum, a crucible made of PBN (Pyrolytic Boron Nitride) for containing the material 30 ( 10) and a first heating part 20 composed of PG (pyrolytic graphite) pyrolytic graphite (PG) deposited on the outer surface of the PBN crucible 10 so as to be suitable for heating.

The PBN crucible 10 is generally manufactured by pyrolytic gaseous boron compound and gaseous nitrogen compound by CVD (chemical vapor deposition). The PBN crucible 10 is characterized by a non-invasive tissue. Therefore, since the PBN crucible 10 does not have a hole, a substance cannot enter and stick, and chemical resistance is also favorable.

The first heating part 20 of the PG, which is deposited on the outer surface of the PBN crucible 10 and is patterned for heating (for example, a symmetrical pattern) so as not to affect a sample by a current, is connected to a power source. It is heated to a high temperature by injecting a current.

As in the first embodiment of the present invention, by directly depositing the PG on the outer surface of the PBN crucible 10, and forming the symmetrical pattern of the PG suitable for heating, the integral evaporation source is attached to the heating portion and the crucible Since the evaporation source is integrally formed with the PBN crucible 10 as a contact heating part, heat can be efficiently transferred through heat conduction to the material 30 directly contacting the inside of the PBN crucible 10. have.

2 is a schematic structural diagram of a second embodiment of the present invention. As shown in FIG. 2, according to the second embodiment of the present invention, the PG is deposited on the outer surface and the inner surface of the PBN crucible 10 in the first embodiment to form a heating part and a protective film. According to a second embodiment of the present invention, in a deposition system for depositing a material such as an organic material or a metal on a sample in a vacuum, a crucible 10 made of PBN for containing the material 30 and the PBN crucible ( 10) the first heating part 20 composed of PG deposited and patterned (for example, a symmetrical pattern) suitable for heating so that a magnetic field due to electric current does not affect the sample on the outer surface of the external surface, and PBN like aluminum Insulating the first protective film made of PG deposited on the inner surface of the PBN crucible, the first heat generating part 20 and the first protective film 40 to protect the PBN crucible from the sample adhered well to In order to prevent the PG, the first insulation 50 is removed.

For example, the insulating part 50 may be formed by depositing PG in and out of the PBN crucible, and then removing a part of the PG deposited to electrically insulate the first heat generating part 20 and the first passivation layer 40. By this, the insulation part 50 can be formed.

According to the second embodiment of the present invention, when cooling the material 30 adhering to the PBN, such as aluminum, it is possible to prevent the PBN crucible 10 from being damaged by the difference in the coefficient of thermal expansion, thereby rapidly cooling the material. Can be. For example, in a crucible of 500 cc or more, it takes more than 8 hours to cool down to 100 degrees Celsius at a temperature higher than the melting point of aluminum at 660 degrees Celsius without a first protective film. Cooling in time is possible.

3 is a schematic diagram of the invention of the third embodiment of the present invention. As shown in FIG. 3, the 3rd Embodiment of this invention is a structure of the invention of the said 1st or 2nd embodiment further including the lid body in which the discharge port was formed which covers the opening part of the said PBN crucible. . That is, in the configuration of the first embodiment of the present invention, the PBN cap body 70, which covers the opening of the PBN crucible 10, and has a discharge port 60 for discharging material, and the PBN cap body 70 A second heat generation composed of PG deposited and patterned (for example, a symmetrical pattern) suitably for heating so that a hole corresponding to the discharge hole 60 and a magnetic field due to an electric current do not affect the sample on the outer surface of the It is the structure containing the part 80.

When voltage is applied to the first and second heat generating units, the thickness of the PG deposited on the lid and the thickness of the PG deposited on the PBN crucible are maintained so that the temperature of the PBN lid is kept higher than the temperature of the PBN crucible. It is preferable to adjust the ratio of the heating part and the pattern of the heating part.

4 is a schematic structural diagram of a fourth embodiment of the present invention. 4th Embodiment of this invention This invention is a structure which further includes the cover body in the opening part in the structure of said 1st or 2nd embodiment. That is, in the configuration of the second embodiment of the present invention, the PBN cap body 70 with the discharge opening 60 for covering the opening of the PBN crucible 10 and the outer surface of the PBN cap body 70 A second heat generating part including a hole corresponding to the discharge hole 60 and a PG deposited and patterned (for example, a symmetrical pattern) suitable for heating so that a magnetic field generated by a current does not affect the sample during heating; 80), and a second protective film 90 made of PG deposited on the inner surface of the PBN crucible so that the sample which adheres well to the PBN, such as aluminum, does not adhere to the lid body, and the second heat generating part 80 In order to electrically insulate the second passivation layer 90, the second insulation part 100 including PG is removed.

Also in this case, it is preferable that the temperature of the PBN lid 70 is maintained higher than the temperature of the PBN crucible 10 when a current is supplied to each of the heat generating units.

5 is a flowchart illustrating a first embodiment and a third embodiment of a method for manufacturing a heat generating unit integrated high efficiency evaporation source according to the present invention. As shown in FIG. 5, the method of manufacturing a heating unit integrated high efficiency evaporation source of the present invention includes preparing a PBN crucible in a method of manufacturing an evaporation source of a vacuum deposition system (S100) and 500 micrometers on an outer surface of the PBN crucible. Forming a first heating layer by depositing a PG of less than a meter (S110), and a pattern suitable for heating without a magnetic field due to current in the first heating layer formed on the outer surface of the PBN crucible (for example For example, the method may include forming a symmetric pattern (S120).

In addition, a third embodiment of the method of manufacturing the heat generating unit integrated high efficiency evaporation source of the present invention comprises the steps of preparing a PBN lid body covering the PBN crucible, the discharge port for evaporation (S130), and the PBN lid body Forming a second heating layer by depositing PG of 500 micrometers or less on an outer surface of the SB, and a hole corresponding to an outlet of the PBN capping body in a second heating layer formed on an outer surface of the PBN capping body; The method may further include forming a pattern (eg, a symmetrical pattern) suitable for heating without affecting the sample by the magnetic field due to overcurrent (S150).

When the current is supplied to each of the heating layers, it is preferable that the temperature of the PBN lid is kept higher than the temperature of the PBN crucible.

Forming a first heating layer by depositing PG of 500 micrometers or less on the outer surface of the PBN crucible (S110) may be formed by a CVD technique, the current generated in the first heating layer formed on the outer surface of the PBN crucible Forming a pattern (for example, a symmetrical pattern) suitable for heating without the magnetic field affecting the sample (S120) is removed by a mechanical method or by heating the PG to 400 degrees Celsius or more by laser beam It can form by the technique of removing a part.

6 is a flowchart illustrating a second embodiment and a fourth embodiment of a method for manufacturing a heat generating unit integrated high efficiency evaporation source according to the present invention. As shown in FIG. 6, according to the second embodiment of the method of manufacturing the heat generating unit integrated high efficiency evaporation source of the present invention, in the first embodiment, PG is deposited on the inner surface of the PBN crucible to further form a protective film. It is done.

According to a second embodiment of the present invention, the method of manufacturing a heating unit integrated high-efficiency evaporation source includes preparing a PBN crucible (S200) in a method of manufacturing an evaporation source of a vacuum deposition system (S200) and 500 micrometers on the inner and outer surfaces of the PBN crucible. Depositing a PG of less than one meter (S210) and forming a pattern (for example, a symmetric pattern) suitable for heating without affecting the sample by a magnetic field caused by current in the first heating layer formed on the outer surface of the PBN crucible And forming an insulating part for electrically insulating the first heating layer and the first passivation layer (S230).

In addition, a fourth embodiment of the method for manufacturing the heat generating unit integrated high efficiency evaporation source of the present invention comprises the steps of preparing a PBN cap body covering the PBN crucible, the outlet for evaporation (S240), and the PBN cap body Depositing PG of 500 micrometers or less on the inner and outer surfaces of S250 and a magnetic field formed by a hole and a current corresponding to the outlet of the PBN lid in a second heating layer formed on the outer surface of the PBN lid; Forming a pattern suitable for heating (for example, a symmetrical pattern) without affecting the sample (S260), and forming an insulator for electrically insulating the second heating layer and the second protective film. (S270).

When the current is supplied to each of the heating layers, it is preferable that the temperature of the PBN lid is kept higher than the temperature of the PBN crucible.

Referring to FIG. 7, when the material is deposited using a general evaporation source without a lid on a rectangular substrate having a diagonal length of 600 mm, the outlet of the evaporation source is disposed 560 mm below the center of the substrate and 350 mm away from the side. When rotating while depositing, the uniformity of the deposited material is about 90%, and the rate of evaporated material reaching the substrate is about 15%. The remaining 85% will not reach the substrate and will be consumed by sticking to the inner wall of the vacuum system.

As shown in FIG. 8, when the three outlets are formed in the lid body so that the direction of the outlet is directed to three points on the substrate, the uniformity of the sample is improved to about 95%, and the evaporated material is The rate of reaching the substrate is about 24%. The use of a lid with a large number of outlets can increase the use efficiency of the material by about 60% over an evaporation source without a lid.

In the case of a general crucible in which the heating element does not exist in the lid, the temperature of the upper part of the crucible is lower than that of the middle part. In the case of using a lid without a heating part in such a common crucible, the material evaporated from the crucible is condensed on the lid again, which causes a problem that the outlet is blocked. Sieve cannot be used.

The evaporation source manufactured in the embodiment of the present invention may be mounted on the vacuum flange 200 in which the electrode for power supply 400 and the thermocouple (T / C) electrode are mounted as shown in FIG. 9. In this case, the power supply electrode is connected to supply power to the first heating element and the second heating element, and the thermocouple electrode is connected to measure the temperature of the evaporation source. The structure can be simplified by using a power supply electrode as a support. The spacer 300 serves to fix the evaporation source so that the evaporation source does not move and has a structure of minimizing contact with the evaporation source in order to minimize heat loss.

The spacer 300 may be configured, for example, as shown in FIG. 10.

The technical scope of the present invention regarding the heat generating unit integrated high-efficiency evaporation source and its manufacturing method described above is not limited to the above-described embodiments. Naturally, various predictable embodiments included in the technical idea of the present invention are included. For example, PBN may be further deposited on the outside of the first heating element and the second heating element to protect the heating element applied to the first to fourth embodiments. At this time, the PBN is not deposited on the portion for connection with the power supply electrode.

1 is a schematic configuration diagram of a first embodiment of a heat generating unit integrated high efficiency evaporation source of the present invention.

2 is a schematic diagram of a second embodiment of the heat generating unit integrated high efficiency evaporation source of the present invention.

3 is a schematic diagram of a third embodiment of the heat generating unit integrated high efficiency evaporation source of the present invention.

4 is a schematic configuration diagram of a fourth embodiment of the heat generating unit integrated high efficiency evaporation source of the present invention.

5 is a flowchart illustrating a first embodiment and a third embodiment of a method for manufacturing a heat generating unit integrated high efficiency evaporation source according to the present invention.

6 is a flowchart illustrating a second embodiment and a fourth embodiment of a method for manufacturing a heat generating unit integrated high efficiency evaporation source according to the present invention.

7 is a schematic diagram of an example (a) of a system for vacuum deposition using a general evaporation source and uniformity and material use efficiency (b) of a deposited thin film.

8 is a schematic diagram of an example (a) of a system for vacuum deposition using the heat generating unit integrated high efficiency evaporation source and the uniformity and material use efficiency (b) of the deposited thin film.

9 is a block diagram of an evaporator employing the evaporation source of the present invention.

10 is a configuration diagram illustrating the spacer of FIG. 9.

Claims (15)

In the evaporation source used in the vacuum deposition system, PBN (pyrolytic boron nitride) crucibles for holding materials, And a first heat generating part deposited on an outer surface of the PBN crucible and having a pattern suitable for heating without a magnetic field generated by a current affecting a sample. The method according to claim 1, And a first protective film that is partially deposited to protect the crucible from a sample deposited on the inner surface of the PBN crucible and adheres well to PBN, such as aluminum, and is electrically insulated from the first heating element. The method according to claim 1, A PBN cap body covering the opening of the PBN crucible and having an outlet for evaporation, deposited on the outer surface of the PBN cap body, and a magnetic field due to a hole and a current corresponding to the outlet of the PBN cap body affects the sample. It further comprises a second heat generating portion is formed a pattern suitable for heating, When the current is applied to the heat generating portion, the heat generating unit integrated high efficiency evaporation source, characterized in that the temperature is configured to be maintained higher than the temperature of the first heat generating portion. The method of claim 3, It further includes a second protective film deposited on the inner surface of the PBN cap body to protect the cap body from a sample adhered to the PBN, such as aluminum, and partially removed to electrically insulate the first heating unit and the second heating unit. High efficiency evaporation source integrated with a heating unit. The method according to any one of claims 1 to 4, The heat generating unit and the protective film is a heat generating unit integrated high efficiency evaporation source, characterized in that made of pyrolytic graphite (PG) of 500 micrometers or less. The method according to any one of claims 1 to 4, The heat generating unit integrated high efficiency evaporation source, characterized in that the pattern of the heat generating portion is symmetrical. The method according to claim 3 or 4, The discharge port is composed of one or more, each discharge port has a funnel form, the center line is an integrated high efficiency evaporation source, characterized in that is made to face different parts of the sample. Preparing a PBN crucible, Depositing pyrolytic graphite of 500 micrometers or less on the outer surface of the PBN crucible to form a first heating layer; And forming a pattern suitable for heating in the first heating layer formed on the outer surface of the PBN crucible without affecting the sample. The method according to claim 8, Covering the PBN crucible, preparing a PBN cap body formed with a discharge port for evaporation, Forming a second heating layer by depositing pyrolytic graphite of 500 micrometers or less on an outer surface of the PBN cap body; The heat generating portion further comprises the step of forming a pattern suitable for heating in the second heating layer formed on the outer surface of the PBN cap body and the magnetic field due to the hole and the current corresponding to the discharge port of the PBN cap body does not affect the sample Manufacturing method of integrated high efficiency evaporation source. The method according to claim 8, Forming a first passivation layer by simultaneously depositing pyrolytic graphite of 500 micrometers or less on the inner and outer surfaces of the PBN crucible; The method of claim 1, further comprising the step of forming an insulating part to electrically insulate the first heating layer and the first passivation layer. The method according to claim 10, Preparing a PBN cap body in which an outlet for evaporation is formed, Forming a second heating layer and a second protective film by depositing pyrolytic graphite of 500 micrometers or less on the inner and outer surfaces of the PBN cap body at the same time; Forming a pattern suitable for heating in the second heating layer formed on the outer surface of the PBN cap body by a hole and a current corresponding to the outlet of the PBN cap body without affecting the sample; And forming an insulating part on a second protective film formed on an inner surface of the PBN lid to electrically insulate the second heating layer and the second protective film. The method according to any one of claims 8 to 11, The method of manufacturing an integrated high efficiency evaporation source, characterized in that the pattern of the heating layer is symmetrical. The method according to claim 9 or 11, When the current is applied to the heat generating layer, the integrated high efficiency evaporation source manufacturing method characterized in that the temperature of the PBN cap body is configured to be maintained higher than the temperature of the PBN crucible. A heating unit integrated evaporation source, A vacuum flange for mounting the heating unit integrated evaporation source, A power supply electrode for supplying power to the heat generating unit integrated evaporation source, And the power supply electrode is used as a support for mounting the heat generating unit integrated evaporation source on the vacuum flange. The method according to claim 14, Evaporator, characterized in that further comprising a spacer designed to minimize the contact area in order to prevent the movement and to prevent damage when mounted on the vacuum flange by tilting the heating unit integral evaporation source.

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