KR20140024140A - Apparatus for growing sapphire single crystal - Google Patents

Apparatus for growing sapphire single crystal Download PDF

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Publication number
KR20140024140A
KR20140024140A KR1020120090687A KR20120090687A KR20140024140A KR 20140024140 A KR20140024140 A KR 20140024140A KR 1020120090687 A KR1020120090687 A KR 1020120090687A KR 20120090687 A KR20120090687 A KR 20120090687A KR 20140024140 A KR20140024140 A KR 20140024140A
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South Korea
Prior art keywords
crucible
single crystal
sapphire single
crystal growth
heater
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KR1020120090687A
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Korean (ko)
Inventor
곽만석
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주식회사 케이씨씨
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Priority to KR1020120090687A priority Critical patent/KR20140024140A/en
Publication of KR20140024140A publication Critical patent/KR20140024140A/en

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14—Heating of the melt or the crystallised materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Computer Hardware Design (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention chamber; A crucible installed inside the chamber and filled with alumina raw material; And a heating unit installed inside the chamber and heating the crucible to melt the raw material, wherein the crucible is formed of tungsten material. In addition, the heating unit discloses a sapphire single crystal growth apparatus, characterized in that it comprises a resistance heating heater of graphite material. The sapphire single crystal growth apparatus as described above uses a crucible made of tungsten (W) instead of expensive iridium (Ir), and grows a sapphire single crystal using a graphite heater and a carbon insulator instead of induction heating, thereby insulating a carbon insulator. Since no oxygen gas is released in the atmosphere, a tungsten (W) crucible can be used and the manufacturing cost of single crystal growth can be lowered.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a sapphire single-

The present invention relates to an apparatus for growing sapphire single crystal, and more particularly, to a sapphire single crystal growth apparatus capable of lowering the manufacturing cost of sapphire single crystal growth.

In general, a sapphire single crystal (or alumina single crystal) having a lattice constant similar to that of gallium nitride (GaN) is mainly used as a substrate material in a light emitting diode (LED) chip manufacturing process using a gallium nitride (GaN) compound. have. The Czochralski method (hereinafter referred to as CZ method), the Bernoulli method, the Kirofuros method, the EFG method, the HEM method, and the like can be used to grow the sapphire single crystal. Among them, the CZ method has the advantage that the temperature gradient of the solution is large, so that the growth in the C-axis direction (GaN polar axis direction) is possible, and the crystal growth rate is high, resulting in high productivity. In addition, there is an advantage that the loss of the single crystal ingot can be greatly reduced when the single crystal grown on the C axis is processed into a wafer.

As shown in FIG. 1, the conventional sapphire single crystal growth apparatus 10 is filled with aluminum oxide in an iridium (Ir) crucible 11 located in the heat insulating material container 13, using a high frequency coil 15. The crucible 11 is heated. The aluminum oxide is melted by the heat of the crucible 11 to form the molten metal 2. The seed crystal 5 is connected to the lower end of the lifting rod 3 and the seed crystal 5 is brought into contact with the molten metal 2 and then gradually raised while rotating to grow the sapphire single crystal 1.

However, since the conventional sapphire single crystal growth apparatus 10 uses an induction heating method using an expensive iridium crucible 11 and a high frequency coil 15, the manufacturing cost of sapphire single crystal growth is increased. In addition, the iridium crucible 11 is easily deformed at a high temperature, and should be manufactured by re-melting after use for several months or about 10 to 12 months. The zirconia oxide used as a refractory material also has a short lifetime and is an expensive oxide.

The present invention is to provide a sapphire single crystal growth apparatus that can lower the manufacturing cost of sapphire single crystal growth.

The present invention chamber; A crucible installed inside the chamber and filled with alumina raw material; And a heating unit installed inside the chamber and heating the crucible to melt the raw material, wherein the crucible is formed of tungsten material.

In addition, the heating unit discloses a sapphire single crystal growth apparatus, characterized in that it comprises a resistance heating heater of graphite material.

The heater may include a first heater installed at an outer circumference of the crucible and heating a side surface of the crucible; And a second heater installed below the crucible and heating the bottom surface of the crucible.

The sapphire single crystal growth apparatus further includes a sapphire single crystal growth apparatus installed inside the chamber and further including a shield surrounding the crucible and the heating unit.

In addition, the shield discloses a sapphire single crystal growth apparatus, characterized in that the graphite material.

In addition, it discloses a sapphire single crystal growth apparatus, characterized in that the inner wall of the shield is coated with silicon carbide (SiC).

The sapphire single crystal growth apparatus according to the present invention has the following effects.

(1) The present invention has the effect of lowering the manufacturing cost of single crystal growth by growing a sapphire single crystal using a crucible made of tungsten (W) instead of the existing expensive iridium (Ir).

(2) The present invention grows the sapphire single crystal by using resistance heating by graphite heater instead of the conventional high frequency induction heating, tungsten (W) crucible can be used because the oxygen gas is not released from the carbon material insulation, This has the effect of lowering the manufacturing cost.

1 is a sectional view schematically showing a conventional sapphire single crystal growth apparatus.
2 is a sectional view schematically showing a sapphire single crystal growth apparatus according to a preferred embodiment of the present invention.
3 is a flowchart showing a sapphire single crystal growth process procedure using the CZ method.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

Prior to the description of the present invention, the sapphire single crystal growth apparatus for growing sapphire single crystal in aluminum oxide melt is exemplified, but it is not limited thereto, and it can be understood that the present invention can also be applied to a silicon single crystal growth apparatus mainly used to make semiconductor silicon wafers. .

2 is a sectional view schematically showing a sapphire single crystal growth apparatus according to a preferred embodiment of the present invention.

As shown in FIG. 2, the sapphire single crystal growth apparatus 100 according to the preferred embodiment of the present invention includes a chamber 110, a crucible 120, and a heating unit 130 to grow the sapphire single crystal 1. Is used.

The chamber 110 is a predetermined layer for growing a sapphire single crystal (or alumina single crystal) 1 used as a substrate material in a light emitting diode (LED) chip manufacturing process using a gallium nitride (GaN) compound. Provide a confined space for the processes to be performed. Here, the method of growing the sapphire single crystal 1 includes the Czochralski method (hereinafter referred to as CZ method), the Bernoulli method, the Kirupros method, the EFG method, the HEM method and the like. Among them, the present invention uses the Czochralsk (CZ) method in which seed crystals 5, which are single crystals, are immersed in the molten aluminum oxide 2, and the crystals are grown while being slowly pulled up.

In addition, the inner wall of the chamber 110 is provided with a heat insulator 111 to block the heat to heat the crucible 120 to the outside of the chamber 110 by the heater 130 to be described later. For example, the upper, lower and side portions of the crucible 110 is insulated using the heat insulating material 111. Here, the heat insulating material 111 may use a variety of materials, it is preferable to use a carbon (Carbon) material that can be used for a long time because of excellent heat insulating properties and less deformation.

In addition, the inner wall of the heat insulating material 111 is provided with a shield (113) surrounding the outside of the crucible 120 and the heater 130 to be described later, the dust generated from the heat insulating material 111 to the inside of the crucible (120). To prevent mixing. Here, the shield 113 may use a variety of materials, it is preferable to use a graphite (Graphite) material that is the same material as the heater 130.

In addition, the inner wall of the shield 113 is preferably coated with silicon carbide (SiC) to a thickness of approximately 50 ~ 200㎛ in order to suppress the reaction of oxygen and graphite volatilized from the raw material.

The crucible 120 is installed inside the chamber 110 and filled with an alumina raw material for growing the sapphire single crystal 1. The alumina raw material filled in the crucible 120 is heated by the heater 130 to be in the molten state (2).

In the present invention, by using the crucible 120 of tungsten (W) material instead of the existing expensive iridium (Ir), it is possible to lower the manufacturing cost of sapphire single crystal growth.

Meanwhile, in addition to tungsten (W), an inexpensive molybdenum (Mo) crucible 120 may be used. However, when a molybdenum (Mo) crucible 120 is used, molybdenum (Mo) and alumina raw materials react to form a crystal. There is a problem that molybdenum (Mo) precipitates occur. Therefore, in the present invention, a crucible 120 made of tungsten (W) is used instead of molybdenum (Mo).

In addition, the crucible 120 is supported by the lower crucible support shaft 121, the crucible support shaft 121 is rotated by a drive means (not shown) to rotate the crucible 120 while moving the solid-liquid interface Keep this same height. Here, the crucible support shaft 121 is also preferably made of the same tungsten (W) material as the crucible 120. In addition, it is preferable that the seed holder and the seed shaft 3 also use a tungsten (W) material.

The heating unit 130 is installed in the chamber 110 and heats the crucible 120 to melt the alumina raw material filled in the crucible 120. The heating unit 130 is made of a graphite material and includes a heater (described by reference numeral 130) which is supplied with power and generates heat by resistance. The reason why the use of tungsten (W) or molybdenum (Mo) crucible in the conventional high frequency induction heating is not possible is as follows. In the conventional induction heating furnace, zirconia refractories, which are insulators that are not affected by magnetic induction, should be used as a heat insulator, and the refractory releases a small amount of oxygen gas by decomposition reaction at a high temperature of 2000 ° C or higher. Oxygen gas is easily oxidized with tungsten (W) at a high temperature to generate an oxide, which acts as a source of contamination of the molten aluminum oxide, or the crucible surface is rapidly oxidized, causing problems that cannot be used for a long time. Therefore, in the present invention, the sapphire single crystal 1 is grown by using the graphite heater 130 and the carbon insulating material 111 instead of the conventional high frequency induction heating, so that oxygen gas is not emitted, and thus a tungsten (W) crucible may be used. It is possible to reduce the production cost of single crystal growth.

The heater 130 includes a first heater 131 and a second heater 132 to heat the sides and the bottom of the crucible 120.

The first heater 131 may be formed on the outer circumference of the crucible 120 so as to heat the side surface of the crucible 120 and may have a cylindrical shape surrounding the outer circumferential surface of the crucible 120.

The second heater 132 may be positioned in the lower portion of the crucible 120 so as to heat the lower surface of the crucible 120 and may have a disc shape in which the crucible support shaft 121 penetrates the center thereof. Here, in the case of the alumina melt, the viscosity is about 0.05 Pa.s at a melting temperature of 2050 ° C., which is higher than that of other oxides, so that the heat conduction is low, so that natural convection occurs when only the first heater 131 is heated to heat the side of the crucible 120. There is a problem that is not formed. The second heater 132 for heating the lower part of the crucible 120 is installed together and heated to shorten the melting time and easily form natural convection.

3 is a flowchart showing a sapphire single crystal growth process procedure using the CZ method.

As shown in FIG. 3, first, an alumina raw material is filled in a crucible 120 made of tungsten (W) material (S101), a heat insulating material 111 is assembled, and a vacuum is used to remove oxygen in the chamber 110. Vacuum to 10 -3 torr with a pump (not shown). In the present invention, by using the crucible 120 of tungsten (W) material instead of the existing expensive iridium (Ir), it is possible to lower the manufacturing cost of sapphire single crystal growth. Next, argon (Ar) gas or inert gas is injected into the chamber 110 to replace the inside of the chamber 110 with an argon atmosphere (S102). Next, power is supplied to the heater 130 to completely melt the raw material filled in the crucible 120 (S103). At this time, by simultaneously operating the first heater 131 for heating the side of the crucible 120 and the second heater 132 for heating the lower part of the crucible 120, it is possible to shorten the melting time and easily form natural convection have. In the present invention, it is possible to lower the manufacturing cost of sapphire single crystal growth by using resistance heating by the heater 130 made of graphite instead of conventional high frequency induction heating. Next, when the raw material is melted, the inside is observed by a CCD camera (not shown) to check whether convection is formed, and when the convection is formed, a seed touch for contacting the seed crystals 5 to the alumina molten metal 2 gradually. The process proceeds (S104). At this time, when the temperature of the heater 130 is too high, the seed crystal 5 is melted, and thus the temperature of the heater 130 is adjusted while observing the surface of the seed crystal 5. On the contrary, if the temperature of the heater 130 is too low, there is a problem that the seed crystals 5 are rapidly grown after being in contact with the surface of the molten metal 2 and growing into polycrystals instead of single crystals. Next, when the seed touch process is completed, a shoulder process of simultaneously growing the diameter of the single crystal 1 in the horizontal direction and the vertical direction to the desired target diameter while reducing the heat generation of the heater 130 is performed (S105). In the shoulder process, a process of controlling the growth rate of the single crystal is performed by changing the weight of the crystal. Next, when the shoulder process is completed, the body process of growing the body portion 13 while gradually pulling the single crystal 1 in the vertical direction to the desired length is performed (S106). Next, when the body process is completed, a tail process is performed to reduce the diameter in order to separate the single crystal 1 from the solution, and a cut off completely separates the single crystal 1 from the melt after the tail process. The process proceeds (S107). When this process is completed, the heater 130 is lowered to a temperature at a rate of 40 ~ 50 ℃ / h (S108). Finally, after the power of the heater 130 is off (off), a natural cooling process of gradually cooling the single crystal (1) at room temperature while continuing to inject the inert gas (S109).

The following experiment was performed to grow the sapphire single crystal by the process method proposed in the present invention.

Example 1

A tungsten crucible 120 having a diameter of 300 mm and a height of 300 mm was filled with 80 kg of alumina raw material, and the sapphire single crystal 1 was grown using seed crystals in the A-axis direction. Inert gas was continuously injected into the chamber 110 to suppress the reaction between the gas generated while the raw material melted and the graphite heater 130 and the heat insulating material 111. The crystal growth rate was 2.0 mm / hr, and the sapphire single crystal 1 was grown into a cylindrical shape having a diameter of 200 mm.

Example 2

In the same manner as in Example 1, seed crystals in the C-axis direction were used to grow the sapphire single crystal 1.

Through Examples 1 and 2, the A-axis growth single crystal was corrugated in a 90 degree vertical direction to prepare a C-axis ingot, and the C-axis growth single crystal was corrugated in the axial direction to prepare an ingot. . The ingot prepared as described above was cut to 2 mm thickness to polish the surface, and then subjected to polarization inspection to observe defects. As a result of observation, no crystal defects such as subgrain, low angle grain boundary, and bubble were found in both A and C axes. This can be confirmed that the level of polycrystalline usable as the substrate for the LED.

Therefore, the sapphire single crystal growth apparatus 100 of the present invention uses the crucible 120 made of tungsten (W) instead of the existing expensive iridium (Ir), and instead of the induction heating, the graphite heater 130 and the carbon insulation ( By growing the sapphire single crystal 1 using 111), since the oxygen gas is not released from the carbonaceous heat insulating material, it becomes an atmosphere in which a tungsten (W) crucible can be used, and the manufacturing cost of sapphire single crystal growth can be lowered.

While the present invention has been described in connection with certain exemplary embodiments, it will be understood by those skilled in the art that various changes may be made without departing from the scope of the present invention. In addition, the description in parentheses in the description of the claims is intended to prevent obscuration of the description, and the scope of the claims of the claims should be construed to include all the items in parentheses.

100: sapphire single crystal growth device
110: chamber
111: heat insulation
113: Shield
120: crucible
121: crucible support shaft
130: heating unit (heater)
131: first heater
132: second heater

Claims (6)

chamber;
A crucible installed inside the chamber and filled with alumina raw material; And
Is installed inside the chamber, and includes a heating unit for melting the raw material by heating the crucible,
The crucible is sapphire single crystal growth apparatus, characterized in that made of tungsten material. The method of claim 1, wherein the heating unit,
Sapphire single crystal growth apparatus comprising a resistance heating heater of graphite material. The method of claim 2, wherein the heater,
A first heater installed at an outer circumference of the crucible and heating a side surface of the crucible; And
Sapphire single crystal growth apparatus is installed in the lower portion of the crucible, comprising a second heater for heating the lower surface of the crucible. 2. The sapphire substrate according to claim 1,
Sapphire single crystal growth apparatus is installed in the chamber, characterized in that it further comprises a shield surrounding the outside of the crucible and the heating unit. 5. The method of claim 4,
Sapphire single crystal growth apparatus, characterized in that the shield is made of a graphite material. 5. The method of claim 4,
Sapphire single crystal growth apparatus, characterized in that the inner wall of the shield is coated with silicon carbide (SiC).
KR1020120090687A 2012-08-20 2012-08-20 Apparatus for growing sapphire single crystal KR20140024140A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102215441B1 (en) * 2020-08-31 2021-02-10 에스케이씨 주식회사 A pparatus for measuring a insulation material and method of applying the same
US11856678B2 (en) 2019-10-29 2023-12-26 Senic Inc. Method of measuring a graphite article, apparatus for a measurement, and ingot growing system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11856678B2 (en) 2019-10-29 2023-12-26 Senic Inc. Method of measuring a graphite article, apparatus for a measurement, and ingot growing system
KR102215441B1 (en) * 2020-08-31 2021-02-10 에스케이씨 주식회사 A pparatus for measuring a insulation material and method of applying the same

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