JP2013115281A - Vapor phase growth apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vapor phase growth apparatus including a heater for heating a substrate and a current introduction terminal for electrifying the heater, in which thermal diffusion from the current introduction terminal to the outside of the vapor phase growth apparatus can be suppressed effectively.SOLUTION: The vapor phase growth apparatus is configured so that a flow path of refrigerant is provided in a current introduction terminal, and the refrigerant can come into contact with the current introduction terminal body. In addition to the flow path of refrigerant, a cooling container through which the refrigerant flows is provided preferably between the sidewall and the current introduction terminal and/or between the current introduction terminals.

Description

  The present invention relates to a vapor phase growth apparatus, and more particularly to a vapor phase growth apparatus capable of effectively preventing thermal diffusion from a current introduction terminal provided to energize a heater for heating a substrate.

A method for growing a crystal film on a substrate includes a chemical vapor deposition (CVD) method and the like, and a thermal CVD method or the like is known as a CVD method involving substrate heating. In recent years, there has been an increase in the vapor phase growth process performed by heating the substrate under high temperature conditions (for example, 1000 ° C. or higher), and the vapor phase of a group III nitride semiconductor for producing a blue or ultraviolet LED or a blue or ultraviolet laser diode. The growth process is one of them. For example, the growth of a group III nitride semiconductor crystal film was heated to a high temperature of 1000 ° C. or higher using an organometallic gas such as trimethylgallium, trimethylindium, or trimethylaluminum as a group III metal source and ammonia as a nitrogen source. In some cases, the thermal CVD method is used in which a crystal film is vapor-phase grown on a substrate such as silicon (Si), sapphire (Al ₂ O ₃ ), or gallium nitride (GaN). In such a vapor phase growth process, since the substrate is heated at a high temperature, a portion not requiring heating may be heated by heat transfer. Therefore, for example, as described in Patent Document 1, at least a part of the vapor phase growth apparatus may be cooled by a refrigerant.

  The substrate is heated to a temperature necessary for the growth of the crystal film using a heater, and the vapor phase growth reaction is performed by circulating the raw material gas through a reaction furnace formed from the susceptor holding the substrate and the facing of the susceptor. Is called. Usually, the reactor is housed in a reaction vessel and is sealed off from the outside. The heater for heating the substrate is often installed inside the reaction vessel. In order to energize the heater installed inside the reaction vessel, a current supplied from the outside of the reaction vessel is introduced into the reaction vessel. For example, a current is supplied to the heater by a current introduction terminal inserted through the wall of the reaction vessel. In this case, since a reactive or corrosive source gas is circulated inside the reaction vessel, the current introduction terminal of the heater must be electrically insulated without impairing the hermeticity of the reaction vessel.

Japanese Patent No. 3198956 Japanese Patent No. 4540830 Japanese Patent No. 3049927 Japanese Patent No. 3000080

  Such a current introduction terminal is electrically insulated from the surrounding environment without impairing the hermeticity of the reaction vessel, but heat diffuses to the outside through the current introduction terminal and adversely affects external instruments and devices. There is a fear. In particular, the current introduction terminal body for guiding the current from the outside to the heater is made of a conductive material such as a metal or an alloy, but since such a material often has high thermal conductivity, the current introduction terminal body The risk of adversely affecting external instruments and devices due to heat transfer via the is particularly great.

  Therefore, the current introduction terminal is preferably cooled. For example, Patent Documents 2 and 3 show structures that can cool the current introduction terminal. However, in such a structure, there are inclusions and gaps such as a partition wall and an insulating material between the refrigerant flow path and the conductive current introduction terminal body, which hinders efficient cooling of the current introduction terminal body. It was. Further, as an example in which there is no gap between the refrigerant flow path and the conductive current introduction terminal main body, there is a water-cooled electrode described in Patent Document 4, but there is no water cooling between the current introduction terminal and the refrigerant flow path. Inclusions such as tubes and electrical insulation were provided.

  As described above, the conventional techniques as described in Patent Documents 2 to 4 have a problem that the current introduction terminal, in particular, the conductive current introduction terminal main body cannot be efficiently cooled. In particular, in such a conventional technique, cooling is often insufficient when vapor phase growth is performed at a high temperature of, for example, 1000 ° C. or more, like vapor phase growth of a group III nitride semiconductor. Therefore, the problem to be solved by the present invention is that the current introduction terminal main body can be sufficiently cooled, particularly when the current introduction terminal is sufficiently cooled when the vapor phase growth of the group III nitride semiconductor is performed. Another object of the present invention is to provide a vapor phase growth apparatus that can prevent adverse effects on external instruments and devices due to the diffusion of heat to the outside through a current introduction terminal.

The inventors of the present invention, as a result of diligent studies to solve such problems, found that the current introduction in the vapor phase growth apparatus provided with a heater for heating the substrate and a current introduction terminal for energizing the heater. It has been found that the above-mentioned problems can be solved by providing a flow path for the refrigerant inside the terminal so that the refrigerant can come into contact with the conductive current introduction terminal main body, and the present invention has been achieved.
That is, the present invention is a vapor phase growth apparatus provided with a heater for heating a substrate and a current introduction terminal for energizing the heater, wherein a flow path for the refrigerant is provided inside the current introduction terminal, and the conductivity is improved. The vapor phase growth apparatus is configured so that the refrigerant can come into contact with the current introduction terminal main body.

In the vapor phase growth apparatus according to the present invention, the flow path of the refrigerant is provided inside the current introduction terminal, and the current introduction terminal main body is configured so that the refrigerant can come into contact with the conductive current introduction terminal main body. The current introduction terminal can be sufficiently cooled, for example, when vapor phase growth is performed at a high temperature of, for example, 1000 ° C. or higher, such as vapor phase growth of a group III nitride semiconductor. . Therefore, it is possible to prevent heat from diffusing to the outside through the current introduction terminal and adversely affecting external instruments and devices. In the vapor phase growth apparatus of the present invention, water can also be used as a refrigerant, and the insulation resistance of the current introduction terminal at that time can be 0.2 MΩ or more.
Further, the vapor phase growth apparatus of the present invention has a refrigerant flow path provided between the side wall portion and the current introduction terminal and / or between the current introduction terminal and the current introduction terminal, in addition to the refrigerant flow path provided inside the current introduction terminal. By providing a circulating cooling vessel, the current introduction terminal and its surroundings are also efficiently cooled, so that heat transfer from the heater is also suppressed and the current introduction terminal can be cooled more efficiently.

The present invention is applied to a vapor phase growth apparatus including a heater for heating a substrate and a current introduction terminal for energizing the heater. Hereinafter, although the vapor phase growth apparatus of this invention is demonstrated in detail based on FIGS. 1-10, this invention is not limited by these.
FIG. 1 is a vertical sectional configuration diagram showing an example of the vapor phase growth apparatus of the present invention, and FIG. 2 is a vertical sectional configuration diagram showing another example of the vapor phase growth apparatus of the present invention. 3 is a partially enlarged view of a portion A shown in FIG. 1 and shows a current introduction terminal and a peripheral aspect thereof, and FIG. 4 is a partially enlarged view of the portion A shown in FIG. FIG. 5 shows a configuration different from that of FIG. 3 in the vicinity thereof, FIG. 5 is a configuration diagram of a horizontal section taken along BB in FIG. 1, FIG. 1 is a DD horizontal sectional configuration diagram of FIG. 2, and FIG. 8 is a B′-B ′ horizontal sectional configuration diagram of FIG. 2. 9 is an EE horizontal sectional view of FIG. 3, and FIG. 10 is an FF horizontal sectional view of FIG.

  As shown in FIGS. 1 and 2, the vapor phase growth apparatus of the present invention includes a heater 11 for heating the substrate 5 and a current introduction terminal 12 for energizing the heater 11, as shown in FIGS. 3 and 4. As described above, the refrigerant flow path 21 is provided inside the current introduction terminal 12 so that the refrigerant can come into contact with the conductive current introduction terminal main body 12 a energizing the heater 11.

  Next, the current introduction terminal 12 and its periphery will be described in detail with reference to FIG. The current introduction terminal 12 as shown in FIG. 3 is a conductive current introduction terminal main body that is connected to the power receiving unit 12 d that receives current from an external power source (not shown), the power receiving unit 12 d, and the heater 11 and that conducts current to the heater 11. 12a, a concave space portion 12b provided in the current introduction terminal main body 12a, and a tube portion 12c inserted into the concave space portion 12b. The current introduction terminal main body 12a is preferably rod-shaped, and the cross section perpendicular to the length direction of the current introduction terminal main body 12a is preferably circular, triangular, quadrangular or polygonal, and more preferably circular. However, it is not limited to such a shape. The current introduction terminal body 12a has a cross section perpendicular to the length direction of 5 to 50 mm in diameter and particularly preferably 30 to 300 mm in length, but is not limited to such a size and shape. . The power receiving unit 12d is connected to the current introduction terminal main body 12a, and guides a current from a power source (not shown) to the current introduction terminal main body 12a via the feeder line 26 connected to the power reception unit 12d. Further, a heater 11 is connected to the current introduction terminal main body 12a, and current from a power source (not shown) is supplied to the heater 11 via the power receiving unit 12d and the current introduction terminal main body 12a.

  The concave space portion 12b is formed by providing a hole that does not penetrate in the length direction of the current introduction terminal main body 12a, and forms a double tube structure together with the tube portion 12c inserted into the concave space portion 12b. . In order to uniformly cool the current introduction terminal main body 12a, the cross-sectional shape of the current introduction terminal main body 12a and the cross-sectional shape of the tube portion 12c are preferably provided so as to be concentric, but the shape and arrangement are limited to such a shape. Never happen. The concave space portion 12b is circular with a cross section perpendicular to the length direction having a diameter of 3 to 48 mm and preferably having a length of 20 to 299 mm, but is limited to such a size and shape. There is no. The tube portion 12c is preferably an annular shape with a cross section perpendicular to the length direction having an outer diameter of 2 to 47 mm and a thickness of 0.5 to 5 mm, but is not limited to such a shape and size. . The tube portion 12c has a gap between the side surface of the concave space portion 12b and the tube portion 12c, and a gap is formed between one end of the tube portion 12c on the heater 11 side and the bottom surface of the concave space portion 12b. However, the size of the gap is preferably 0.5 to 10 mm, but is not limited to such a size. The opening of the concave space 12b can be used as the refrigerant inlet 12f of the refrigerant flow path 21 and the other end of the pipe part 12c can be used as the refrigerant outlet 12g of the refrigerant flow path 21. Another end of the portion 12c can be used as the refrigerant inlet 12f, and the opening of the concave space 12b can be used as the refrigerant outlet 12g. Since the refrigerant flow path 21 having such a structure allows the refrigerant to flow through the entire inside of the current introduction terminal body 12a, the current introduction terminal body 12a can be cooled more efficiently.

  On the other hand, the overall configuration of the vapor phase growth apparatus of the present invention is not limited, and an example thereof is shown in FIGS. In the vapor phase growth apparatus of FIGS. 1 and 2, the vapor phase growth reaction for generating a crystal film is performed inside the reaction vessel 3. The ceiling part 1 and / or the side wall part 2 are preferably constituted by a part of the reaction vessel 3, but are not limited to such a structure. The ceiling 1 is not particularly limited to the installation position or the like as long as it can cover the upper part of the vapor phase growth apparatus and protect the internal components. Inside the reaction vessel 3, a substrate 5 for vapor-phase growth of a crystal film, a heater 11 for heating the substrate 5, a ring-shaped substrate holder 6 for holding the substrate 5, and a disk shape for holding the substrate holder 6 The susceptor 8 and the bearing 15 are provided with a ring-shaped pedestal 20 that rotatably holds the susceptor 8, and these members are housed in a reaction vessel 3 whose outer shape is a disk. The susceptor 8 forms a reaction furnace 10 together with the susceptor facing 9, and the vapor phase growth reaction is performed in the reaction furnace 10. The substrate 5 is disposed with the growth surface on which the crystal film is grown facing downward. However, the present invention is not limited to the downward orientation. For example, the substrate 5 may be disposed upward or laterally. . Further, the present invention is not limited to the vapor phase growth apparatus that supplies the source gas from the central part of the reaction furnace 10 and discharges it from the peripheral part to the outside. For example, the source gas is supplied from one end of the reaction furnace 10. Also, the present invention can be applied to a vapor phase growth apparatus that discharges the reacted gas from the other end to the outside.

  Next, the installation state of the current introduction terminal 12 on the ceiling portion 1 will be described in detail with reference to FIGS. In the embodiment of FIG. 3, two current introduction terminals 12 are connected to each heater 11 in pairs. Since the current introduction terminal 12 has an insulating material 12e provided on the outer side surface of the current introduction terminal main body 12a and is inserted into the through hole provided in the ceiling portion 1 via the insulation material 12e, the current introduction terminal 12 12 is electrically insulated from the ceiling 1. The current introduction terminal 12 may have a flange portion 12h on the outer side surface of the current introduction terminal main body 12a via an insulating material 12e. A sealing material 28 is provided between the flange part 12h and the ceiling part 1, and the sealing part of the ceiling part 1 is not impaired by fixing the flange part 12h to the ceiling part 1 using a fixing screw (not shown) or the like. The current introduction terminal 12 can be attached to the. The through hole into which the current introduction terminal 12 is inserted is preferably provided in the protruding portion 1a provided on the outer surface of the ceiling portion 1, and is preferably provided in the protruding direction of the protruding portion 1a. The protruding portion 1a can be formed by partially increasing the wall thickness of the ceiling portion 1. When the current introduction terminal 12 is inserted into the through hole, the current introduction terminal is electrically insulated from the ceiling portion 1 by providing an insulating material 12e and / or a gap between the current introduction terminal main body 12a and the side surface of the through hole. In the case of providing the insulating material 12e, it is preferable that the insulating material has a thickness of 1 to 10 mm, and in the case of providing a gap, it is preferably a gap of 1 to 10 mm, but it is limited to such a configuration. Absent. The cross section perpendicular to the protruding direction of the protruding portion 1a is preferably circular, triangular, quadrangular, or polygonal, and more preferably circular, but is not limited to such a shape. Although it is preferable that the protrusion part 1a protrudes 20-200 mm from the surface of the ceiling part 1, it is not limited to such a magnitude | size. The above description is applied to a vapor phase growth apparatus (face-down type) in which the crystal growth surface of the substrate is arranged downward. By replacing the “ceiling” with the “bottom”, the crystal growth surface of the substrate Can be applied to a vapor phase growth apparatus (face-up type) in which the substrate is disposed upward.

  FIG. 4 is a diagram showing an aspect different from that of FIG. 3 in the current introduction terminal and its surroundings. However, as a difference from the aspect of FIG. 3, the current introduction terminal 12 is directly on the outer side surface of the current introduction terminal main body 12a. It has a flange portion 12h provided, has an insulating material 12e between the flange portion 12h and the ceiling portion 1, between the flange portion 12h and the insulating material 12e, and between the insulating material 12e and the ceiling portion 1. Each is provided with a sealing material 28. As shown in the embodiment of FIGS. 3 and 4, the current introduction terminal 12 is detachably attached to the ceiling portion 1. As shown in FIGS. 3 and 4, the current introduction terminal 12 can be detachably attached to the ceiling portion 1 by the flange portion 12h. However, the insertion method is not limited, and the current introduction terminal 12 (for example, the insulating material 12e). ) And the side surface of the through hole provided in the ceiling portion 1, and a spiral can be provided on each of the through holes and the current introduction terminal 12 can be screwed into the through hole.

  In addition, a refrigerant flow pipe 23 is connected to the refrigerant inlet 12f and the refrigerant outlet 12g of the refrigerant flow path 21 using a connection joint 24, and the refrigerant is supplied and discharged. By connecting the refrigerant flow pipe 23 connected to the refrigerant outlet 12g of the current introduction terminal 12 to the refrigerant inlet 12f of another current introduction terminal 12, the refrigerant flow paths 21 of the plurality of current introduction terminals 12 are connected in series. Is also possible. In addition, by using an electrically insulating material for at least a part of the refrigerant flow pipe 23, the current introduction terminal 12 is electrically insulated from another current introduction terminal 12 or an external device (not shown) such as a refrigerant supply source. can do. For example, when the coolant is water or an aqueous solution, it is preferable that the electrical insulation portion of the coolant circulation pipe 23 has a small inner diameter and a long length in terms of electrical insulation from the coolant to the outside. Specifically, the inner diameter of the electrical insulating portion of the refrigerant flow tube 23 is usually 10 mm or less, preferably 5 mm or less, and the length is usually 0.5 m or more, preferably 1 m or more.

  As the refrigerant flowing in the refrigerant flow path 21 provided in the current introduction terminal 12, water such as tap water can be used, and ion-exchanged water or pure water is preferably used, but is not limited thereto. There is nothing. Further, the insulation resistance of the current introduction terminal 12 is 0.2 MΩ or more, preferably 0.5 MΩ or more when water is used as the refrigerant. The insulation resistance is measured, for example, between the current introduction terminal main body 12a and the ground electrode (not shown) of the vapor phase growth apparatus or the ground electrode (not shown) of the ground pipe connected to the refrigerant flow pipe 23. .

  Next, the cooling container 4 will be described in detail. In the vapor phase growth apparatus of the present invention, a cooling container through which a refrigerant flows can be provided between the side wall portion and the current introduction terminal and / or between the current introduction terminal and the current introduction terminal. In the vapor phase growth apparatus shown in FIGS. 1 and 2, a cooling container 4 in which a refrigerant is circulated is provided adjacent to the ceiling portion 1 and close to the current introduction terminal 12. More specifically, The current introduction terminal 12 is inserted into a through hole provided in the protruding direction of the protruding portion 1a of the ceiling portion 1, and the cooling container 4 is provided adjacent to the outer side surface of the protruding portion 1a. The cooling container 4 that cools the ceiling portion 1 is provided with refrigerant inlets and outlets (30, 31) so that the refrigerant flows from the peripheral edge of the reaction furnace 10 toward the center. It is not limited to the flowing configuration. In order to perform cooling uniformly, a partition plate may be provided in the middle of the flow path to make the refrigerant flow uniform.

  For example, the cooling container 4 of FIGS. 1 and 2 is provided with an opening lid 22 ′ that can open the inside of the cooling container 4, and the opening lid 22 ′ is attached to the cooling container 4 via a sealing material 28. Yes. A plurality of opening lids 22 ′ are preferably provided, and the number of opening lids 22 ′ is preferably not limited to a plurality. However, by providing a plurality of opening lids 22 ′, the cooling container 4 can be provided without opening all the opening lids 22 ′. Various parts such as inspection, cleaning, and maintenance can be performed by opening various parts inside. At least during vapor phase growth, all the opening lids 22 ′ are closed, the cooling container 4 is sealed, and the refrigerant is circulated. As shown in FIGS. 1 and 2, not only the cooling vessel 4 provided close to the current introduction terminal 12 but also another cooling vessel 4 ′ at the lower part of the reaction vessel 3 for cooling the facing 9 of the susceptor. Can be provided.

  As shown in FIG. 2, the vapor phase growth apparatus of the present invention can include a plurality of open lids equipped with a plurality of current introduction terminals and / or a plurality of cooling containers. In the vapor phase growth apparatus of FIG. 1, the cooling container 4 is manufactured integrally with the side wall portion 2, but in the vapor phase growth apparatus of FIG. 2, the opening lid 22 provided on the ceiling portion 1 and the cooling container 4 are integrated. It is produced as. In the vapor phase growth apparatus of FIG. 2, an opening lid 22 is provided on the ceiling 1 (reaction vessel 3), and the inside of the reaction vessel 3 can be opened. Since the current introduction terminal 12 and / or the cooling container 4 are mounted on the opening lid 22, when the opening lid 22 is removed, the cooling container 4 and / or the current introduction terminal 12 are also removed at the same time. Inspection, cleaning, maintenance, etc. can be facilitated. Preferably, the plurality of current introduction terminals 12 and / or the plurality of cooling containers 4 are attached to the opening lid 22 so that the plurality of current introduction terminals 12 and / or the plurality of cooling containers 4 are removed when the opening lid 22 is removed. By providing a plurality of such opening lids 22, it is possible to open various locations inside the reaction vessel 3 without opening all the opening lids 22, and work such as inspection, cleaning, and maintenance However, the present invention is not limited to such a configuration.

  Next, the reaction vessel 3 in which the vapor phase growth reaction for generating the crystal film is performed and the inside thereof will be described in detail with reference to FIGS. The substrate 5 is held by the substrate holder 6 with the growth surface facing downward. However, the substrate 5 may be held upward, and the orientation of the growth surface is not particularly limited. The substrate holder 6 can hold one substrate having a diameter of 2 inches, 3 inches, 4 inches, or 6 inches, but is not particularly limited to a substrate of these sizes. The susceptor 8 held rotatably can be rotated by the rotational driving force transmitted from the rotational driver 17. When the susceptor 8 is rotated, the rotational driving force from the rotational driver 17 is transmitted via a rotational drive shaft 18 that is rotatably sealed so as not to impair the sealing performance of the reaction vessel 3 by means such as a magnetic fluid seal. The rotation drive shaft 18 is transmitted to the rotary plate 19 fixed to the tip of the susceptor 8 side. Gears are provided on the peripheral edge of the susceptor 8 and the peripheral edge of the rotating plate 19, respectively. When these gears mesh with each other, the rotational driving force from the rotary driver 17 is transmitted to the susceptor 8, and the susceptor 8 rotates. To do. By rotating the susceptor 8 in this way, a crystal film having a uniform film quality and film thickness can be obtained.

  The susceptor 8 forms a reaction furnace 10 together with the susceptor facing 9, and the reaction furnace 10 is housed in the reaction vessel 3 and sealed, and the reaction furnace 10 is provided with a raw material gas inlet 13. The vapor phase growth reaction is performed by supplying the source gas from the source gas introduction unit 13 while heating the substrate 5 with the heater 11 that generates heat by the current introduced from the current introduction terminal 12. A crystal film is formed. The raw material gas used for the vapor phase growth reaction is directly discharged from the reaction gas discharge unit 14 as a reaction gas. For example, in FIG. 1, the source gas from the source gas introduction unit 13 provided in the center of the reaction furnace 10 is blown out radially from the source gas introduction unit 13 and supplied horizontally to the growth surface of the substrate 5. However, it is not limited to such a form. The substrate holder 6 may be provided with a soaking plate 7 in order to uniformly transfer the heat from the heater 11 to the substrate 5. It is preferable that the susceptor 8 is always rotated during the vapor phase growth reaction, and the rotation direction and rotation speed of the susceptor 8 can be arbitrarily set by changing the rotation direction and rotation speed of the rotation driver 17. In order to obtain a uniform film thickness and film quality between the substrates, the substrate holders 6 are arranged on the same circumference with respect to the center of the reaction furnace 10, and the distances from the source gas introduction unit 13 are made equal. However, it is not particularly limited.

  Although the material which comprises the ceiling part 1 (reaction container 3) and the cooling container 4 includes a metal or an alloy, it is not limited to these materials. The ceiling 1 (reaction vessel 3) has a high temperature inside the reaction vessel 3, in which a reactive or corrosive source gas is circulated, shuts the reaction furnace 10 from the outside air, and controls the vapor phase growth reaction. In some cases, the pressure of the reactor 10 may be changed to reduced pressure, normal pressure, or increased pressure. Therefore, the material is preferably a metal or alloy having heat resistance, corrosion resistance, and strength, but is not limited to these materials. Never happen. The cooling container 4 is assumed to be a metal or alloy having heat resistance, corrosion resistance, and strength, since the coolant circulating in the cooling container 4 is assumed to be high temperature. The material is not limited. The substrate holder 6, the susceptor 8, the facing surface 9 of the susceptor, and the rotating plate 19 are preferably carbon materials or carbon materials coated with a ceramic material, but are not particularly limited. The rotary drive shaft 18 is preferably a metal, an alloy, a metal oxide, a carbon-based material, a ceramic-based material, a carbon-based material coated with a ceramic material, or a combination thereof, but is not particularly limited. The heater 11 is preferably a carbon heater or a ceramic heater, but is not limited to these heaters. The current introduction terminal main body 12a and the power receiving portion 12d are preferably made of a metal or alloy having conductivity, the tube portion 12c and the flange portion 12h are preferably made of metal or alloy, and the insulating material 12e is a resin having electrical insulation. Alternatively, it is preferably a ceramic material, but is not limited to these materials. The bearing 15 is preferably a ceramic material, but is not limited to a ceramic material. The refrigerant flow pipe 23 is preferably a resin having electrical insulation, but is not limited to a resin having electrical insulation. The sealing material 28 is preferably a metal, an alloy, or a resin, but is not limited to such a material.

Here, examples of the resin include glass epoxy or fluororesin, but are not limited thereto. Examples of the fluororesin include, but are not limited to, Teflon (registered trademark) or Viton (registered trademark). Examples of metals include, but are not limited to, aluminum, nickel or copper. Examples of alloys include stainless steel or inconel, but are not limited thereto. Examples of the carbon-based material include carbon, pyrolytic graphite (PG), and glassy carbon (GC), but are not limited thereto. Examples of the ceramic material include, but are not limited to, alumina, silicon carbide (SiC), silicon nitride (Si ₃ N ₄ ), and boron nitride (BN).

  The material constituting the ceiling 1 (reaction vessel 3) and the cooling vessel 4 is particularly preferably stainless steel. The current introduction terminal body 12a is particularly preferably made of stainless steel, copper or nickel, and most preferably made of nickel. It is particularly preferable that the tube portion 12c and the flange portion 12h are made of stainless steel, the power receiving portion 12d is made of copper, and the insulating material 12e is made of glass epoxy or alumina. The substrate holder 6, the susceptor 8, the susceptor facing 9 and the rotating plate 19 are SiC coated carbon, the heater 11 is a carbon heater, the bearing 15 is alumina, the rotary drive shaft 18 is stainless steel, the refrigerant flow pipe 23 is Teflon (registered trademark), The sealing material 28 is particularly preferably copper or Viton (registered trademark).

  EXAMPLES Next, although an Example demonstrates this invention concretely, this invention is not limited by these.

[Example 1]
(Production of vapor phase growth equipment)
A vapor phase growth apparatus as shown in FIGS. 1, 3, 5 to 7, 9, and 10 was manufactured. A susceptor 8 (made of SiC coated carbon, diameter 720 mm, thickness 11 mm, capable of holding six 6-inch substrates) and substrate holder 6 (made of SiC-coated carbon, capable of holding one 6-inch diameter sapphire substrate) 6 pieces were held by the susceptor 8 described above.

  The current introduction terminal main body 12a is a nickel bar having a cross section perpendicular to the length direction having a diameter of 13 mm and a length of 182 mm. A concave space 12b concentrically with the above-described cross section of the current introduction terminal main body 12a (a cross section perpendicular to the length direction is a circle having a diameter of 8 mm, a length of 160 mm) is provided, and a tube portion 12c (length) Stainless steel tube with a cross section perpendicular to the direction of an outer diameter of 4 mm and a wall thickness of 1 mm, a power receiving part 12 d (made of copper), an insulating material 12 e (an outer diameter of 26 mm, a wall thickness of 6.5 mm, a cylinder with a length of 38 mm) The current introduction terminal 12 was manufactured by providing a flange 12h (diameter 70 mm, thickness 13 mm, stainless steel). A gap of 2 mm was generated between the side surface of the concave space portion 12b and the tube portion 12c, and between one end of the tube portion 12c on the heater 11 side and the bottom surface of the concave space portion 12b. The opening of the concave space 12b was used as the refrigerant inlet 12f of the refrigerant flow path 21, and the other end of the pipe 12c was used as the refrigerant outlet 12g.

  The ceiling part 1 was provided with a protruding part 1a protruding 64 mm from the surface thereof, and a through hole having a diameter of 26 mm was provided in the protruding direction of the protruding part 1a. The current introduction terminal 12 manufactured as described above was inserted into the through hole, and the flange portion 12h was fixed to the ceiling portion 1 via the copper sealant 28 using a fixing screw (not shown). The insulating material 12e of the current introduction terminal 12 is in contact with the side surface of the through hole, a gap of 6.5 mm is generated between the current introduction terminal main body 12a and the side surface of the protruding portion 1a, and the current introduction terminal 12 is electrically insulated from the ceiling portion 1. It was. A power supply line 26 for supplying a current from an external power source (not shown) is fixed to the power receiving unit 12 d of the current introduction terminal 12 with a power supply line fixing bolt 25. Further, the carbon heater 11 was connected to the current introduction terminal main body 12 a by the heater fixing screw 27.

(Insulation resistance measurement)
Using such a vapor phase growth apparatus, the insulation resistance of the current introduction terminal 12 was measured. First, two current introduction terminals 12 connected to one heater 11 were taken as one set, and an arbitrary set of current introduction terminals 12 was selected. This set of current introduction terminals 12 is connected in series with a refrigerant flow pipe 23 (made of Teflon (registered trademark), outer diameter 6 mm, inner diameter 4 mm, length 0.5 m), and the remaining refrigerant inlet (12f) and refrigerant outlet ( 12g) Refrigerant circulation pipes 23 (made of Teflon (registered trademark), outer diameter 6 mm, inner diameter 4 mm, length 1.2 m) are connected to each, and a stainless steel ground pipe (not shown) is connected to each refrigerant circulation pipe 23. Connected. An arbitrary one of the set of current introduction terminals 12 connected in this way is selected, and an insulation resistance measuring instrument is connected between the current introduction terminal main body 12a and the ground electrode (not shown) of the vapor phase growth apparatus, Another insulation resistance measuring device was connected between the current introduction terminal main body 12a and the ground electrode (not shown) of the ground pipe.

Next, room temperature tap water is used as a coolant, and this is passed through each current introduction terminal 12 at a flow rate of 1 L / min and through the cooling container 4 at a flow rate of 19 L / min. The inside of the container 3 was kept at atmospheric pressure. At this time, the insulation resistance value of the current introduction terminal main body 12a and the insulation resistance measuring instrument connected to the ground electrode of the vapor phase growth apparatus is 1 MΩ or more (range over), and the current introduction terminal main body 12a and the ground pipe are grounded. The insulation resistance value indicated by the insulation resistance measuring instrument connected to the pole was 5 MΩ.
Then, the temperature of the heater 11 was raised to 1180 ° C. while flowing hydrogen from the source gas introduction part 13 and held for 60 minutes. After the holding, the temperature of the current introduction terminal 12 was stabilized at 27 ° C., and the refrigerant temperature at the refrigerant outlet 12 g of the current introduction terminal 12 was stabilized at 28 ° C. Also, the insulation resistance value shown by the insulation resistance measuring instrument connected to the current introduction terminal body 12a and the ground electrode of the vapor phase growth apparatus is stable at 0.6 MΩ, and is connected to the current introduction terminal body 12a and the ground electrode of the ground pipe. The insulation resistance value shown by the insulation resistance measuring instrument was stable at 1 MΩ.

(Vapor phase growth experiment)
Gallium nitride (GaN) was grown on the surface of the substrate 5 using such a vapor phase growth apparatus. First, room temperature tap water is used as a refrigerant, and this is passed through each current introduction terminal 12 at a flow rate of 1 L / min and through the cooling vessel 4 at a flow rate of 19 L / min. The inside of 3 was kept at atmospheric pressure.

  Next, the temperature of the heater 11 was raised to 1050 ° C. while flowing hydrogen from the source gas introduction unit 13 to clean the substrate 5. Subsequently, the temperature of the heater 11 is lowered to 510 ° C., and a buffer layer having a thickness of 20 μm made of GaN is grown on the substrate using trimethyl gallium (TMG) and ammonia as source gases and hydrogen as a carrier gas. After the buffer layer growth, the supply of only TMG was stopped, and the temperature of the heater 11 was raised to 1050 ° C. Thereafter, hydrogen and nitrogen were supplied as carrier gases in addition to TMG and ammonia from the source gas introduction unit 13 to grow undoped GaN for 1 hour. Immediately before the end of undoped GaN growth, the temperature of the current introduction terminal 12 was 27 ° C., the refrigerant temperature at the refrigerant outlet 12g of the current introduction terminal 12 was 28 ° C., and the refrigerant temperature at the refrigerant outlet 31 of the cooling vessel 4 was 38 ° C. It was. After the growth of undoped GaN was completed, the substrate 5 was allowed to cool to near room temperature and taken out from the reaction vessel 3.

  The vapor phase growth of GaN as described above was repeated 10 times. However, the vapor phase growth apparatus operated normally in all the growths, and there was no abnormality in external devices such as the power supply and current control device connected to the heater 11. There was no abnormality such as leakage. Next, the current introduction terminal 12 was removed from the vapor phase growth apparatus and inspected, but no abnormality such as discoloration or corrosion was confirmed.

  The present invention is suitable as a vapor phase growth apparatus for a thermal CVD method or the like, and particularly suitable as a vapor phase growth apparatus for a group III nitride semiconductor used for manufacturing a blue or ultraviolet light emitting diode or laser diode. is there.

It is a vertical cross-section block diagram which shows an example of the vapor phase growth apparatus of this invention. It is a vertical cross-section block diagram which shows an example different from FIG. 1 of the vapor phase growth apparatus of this invention. It is the elements on larger scale of the A section shown in FIG. 1, and is a figure which shows the aspect of a current introduction terminal and its periphery. FIG. 4 is a partially enlarged view of a portion A shown in FIG. 1 and is a view showing a mode different from FIG. It is a BB horizontal cross-section block diagram of FIG. It is CC horizontal cross-section block diagram of FIG. 1, FIG. FIG. 3 is a DD horizontal cross-sectional configuration diagram of FIGS. 1 and 2. It is a B'-B 'horizontal cross-section block diagram of FIG. It is the EE horizontal electric surface block diagram of FIG. FIG. 4 is a configuration diagram of an FF horizontal electric surface in FIG. 3.

DESCRIPTION OF SYMBOLS 1 Ceiling part 1a Protrusion part 2 Side wall part 3 Reaction container 4, 4 'Cooling container 5 Substrate 6 Substrate holder 7 Soaking plate 8 Susceptor 9 Face of susceptor 10 Reactor 11 Heater 12 Current introduction terminal 12a Current introduction terminal main body 12b Concave shape Space portion 12c tube portion 12d power receiving portion 12e insulating material 12f refrigerant inlet 12g refrigerant outlet 12h flange portion 13 source gas introduction portion 14 reaction gas discharge portion 15 bearing 16 bearing groove 17 rotation driver 18 rotation drive shaft 19 rotation plate 20 mount 21 Refrigerant flow path 22, 22 'Opening lid 23 Refrigerant flow pipe 24 Connection joint 25 Feed line fixing bolt 26 Feed line 27 Heater fixing screw 28 Sealing material 29 Flow of refrigerant 30 Refrigerant inlet 31 Refrigerant outlet

Claims (6)

  A vapor phase growth apparatus comprising a heater for heating a substrate and a current introduction terminal for energizing the heater, wherein a flow path for a refrigerant is provided inside the current introduction terminal, and a conductive current introduction terminal main body The vapor phase growth apparatus is configured so that the refrigerant can come into contact therewith.   The vapor phase growth apparatus according to claim 1, wherein the current introduction terminal is inserted into a through hole provided in the ceiling portion.   The vapor phase growth apparatus according to claim 2, wherein the current introduction terminal is detachably attached to the ceiling portion.   The vapor phase growth apparatus according to claim 1, further comprising a cooling container through which a refrigerant flows between the side wall portion and the current introduction terminal and / or between the current introduction terminal and the current introduction terminal.   5. The vapor phase growth apparatus according to claim 4, wherein the ceiling portion includes a plurality of opening lids equipped with a plurality of current introduction terminals and / or a plurality of cooling containers.   The vapor phase growth apparatus according to claim 1, wherein the refrigerant is water.

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