WO2011062092A1 - Appareil de tirage de monocristaux - Google Patents

Appareil de tirage de monocristaux Download PDF

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Publication number
WO2011062092A1
WO2011062092A1 PCT/JP2010/069955 JP2010069955W WO2011062092A1 WO 2011062092 A1 WO2011062092 A1 WO 2011062092A1 JP 2010069955 W JP2010069955 W JP 2010069955W WO 2011062092 A1 WO2011062092 A1 WO 2011062092A1
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Prior art keywords
crucible
single crystal
pulling
pulling apparatus
heating element
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PCT/JP2010/069955
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English (en)
Japanese (ja)
Inventor
智博 庄内
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昭和電工株式会社
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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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • 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

Definitions

  • the present invention relates to a single crystal pulling apparatus for pulling and growing a single crystal from a melt.
  • a single crystal of a target material is pulled from a raw material melt that is accommodated in a crucible and heated through the crucible.
  • a raw material is filled in a crucible, and the raw material is melted by heating the crucible by a high-frequency heating method or a resistance heating method.
  • the seed crystal cut in a predetermined crystal orientation is brought into contact with the surface of the raw material melt, and the seed crystal is determined while rotating at a predetermined rotation speed.
  • a single crystal is grown by pulling at a high speed.
  • the crucible be made of molybdenum (Mo) or the like, which is about 1/20 that of iridium.
  • Patent Document 1 describes a single crystal sapphire pulling apparatus in which a Mo crucible is installed in a chamber, and a cylindrical carbon heater and a carbon heat insulator are installed on the outer periphery of the crucible.
  • Patent Document 2 describes a sapphire single crystal pulling growth apparatus that uses low-priced molybdenum (Mo) or tungsten (W) in a crucible so that a carbon felt molded product and carbon felt can be used as a heating chamber forming member. Has been.
  • Mo molybdenum
  • W tungsten
  • Patent Document 3 a crucible (A) made of molybdenum or tungsten is placed inside an iridium crucible (B) so as not to contact each other to form a double structure, and the crucible (B) is heated to a high temperature,
  • the raw material powder can be efficiently melted without causing thermal damage to the crucible (A), and a relatively inexpensive molybdenum or tungsten crucible (A) Describes a sapphire single crystal growth apparatus that can grow a high-quality sapphire single crystal that is free of inclusion even if it is used.
  • the crucible serves both as a container for holding the raw material melt and as a heater for melting the raw material when the crucible itself generates heat. For this reason, in the crucible, a portion where heat is generated and a portion where heat is not generated are mixed, and the temperature gradient of the melt in the crucible becomes steep. For this reason, distortion has occurred in the grown single crystal. Therefore, as disclosed in Patent Document 3, it has been proposed to make the crucible into a double structure and indirectly heat it. However, Patent Document 3 requires the use of an expensive iridium crucible.
  • the present invention makes it possible to use an inexpensive crucible in a single crystal pulling apparatus based on the Czochralski (Cz) method, and relaxes the temperature gradient of the melt in the crucible, thereby straining the grown single crystal.
  • the purpose is to suppress.
  • a single crystal pulling apparatus to which the present invention is applied has a bottom portion and a wall portion rising from a peripheral edge of the bottom portion, and is provided so as to surround a crucible containing a raw material melt and a crucible that is close to but not in contact with the crucible.
  • a first cylindrical member formed, a second cylindrical member made of carbon or a material containing carbon provided so as to surround the first cylindrical member, and an outer side of the second cylindrical member
  • the crucible may be made of molybdenum (Mo), an alloy containing molybdenum (Mo), tungsten (W), or an alloy containing tungsten (W).
  • Mo molybdenum
  • Mo molybdenum
  • Mo molybdenum
  • W tungsten
  • W alloy containing tungsten
  • the first cylindrical member can be characterized by being composed of tantalum (Ta), tungsten (W), or a carbide of at least one of these elements.
  • the second cylindrical member can be characterized by being composed of graphite.
  • the crucible contains an alumina melt as a raw material melt
  • the pulling member pulls a columnar sapphire single crystal from the alumina melt contained in the crucible. it can.
  • the pulling member can be characterized by pulling up the columnar sapphire single crystal grown in the c-axis direction from the alumina melt accommodated in the crucible.
  • the present invention in the single crystal pulling apparatus by the Czochralski (Cz) method, it is possible to use an inexpensive crucible, and it is possible to relax the temperature gradient of the melt in the crucible. The distortion of the single crystal can be suppressed.
  • FIG. 1 is a diagram for explaining an example of the configuration of a single crystal pulling apparatus 1 to which the present embodiment is applied.
  • This single crystal pulling apparatus 1 has a heating furnace 10 for growing a sapphire ingot 200 made of a sapphire single crystal as an example of a columnar single crystal.
  • the heating furnace 10 has a cylindrical outer shape, and includes a heat insulating container 11 in which a cylindrical space is formed.
  • the heat insulation container 11 is comprised by assembling the components which consist of a heat insulating material made from zirconia.
  • the heating furnace 10 further includes a chamber 14 that houses the heat insulating container 11 in an internal space.
  • the heating furnace 10 is formed to penetrate the side surface of the chamber 14, and the gas supply pipe 12 that supplies gas from the outside of the chamber 14 to the inside of the heat insulating container 11 through the chamber 14 is formed to penetrate the side surface of the chamber 14. And a gas discharge pipe 13 for discharging gas from the inside of the heat insulating container 11 to the outside through the chamber 14.
  • a crucible 20 that houses an alumina melt 300 as an example of a raw material melt obtained by melting aluminum oxide (Al 2 O 3 ) is disposed below the inside of the heat insulating container 11.
  • the crucible 20 has a shape that opens vertically upward.
  • the crucible 20 has a bottom portion 21 and a wall portion 22 that rises upward from the periphery of the bottom portion 21.
  • the crucible 20 is made of, for example, molybdenum (Mo).
  • a crucible support base 15 having a disk-like outer shape is disposed below the inside of the heat insulating container 11 and below the bottom 21 of the crucible 20.
  • the crucible support base 15 may be made of molybdenum as with the crucible 20.
  • the crucible support base 15 is supported by the shaft 16 from the inner bottom surface of the heat insulating container 11.
  • the shaft 16 may also be made of molybdenum, similar to the crucible 20 and the crucible support 15.
  • the crucible 20 is supported from the inner bottom surface of the heat insulating container 11 by the crucible support base 15 and the shaft 16.
  • the heat generating body 17 as an example of the 2nd cylindrical member provided in the outer side of the crucible 20 inside the heat insulation container 11 and surrounding the wall part 22 of the crucible 20 is provided.
  • the heating element 17 is made of carbon (carbon) such as graphite (graphite). And it is provided inside the heating element 17 and outside the crucible 20 so as to surround the wall portion 22 of the crucible 20, and the constituent material of the heating element 17 is mixed into the alumina melt 300 in the crucible 20.
  • a shield 18 is provided as an example of the first cylindrical member to be prevented. Examples of the constituent material of the shield 18 include metal tantalum (Ta), metal tungsten (W), and carbides of at least one of these elements. Among these, the shield 18 is preferably made of tantalum carbide (tantalum carbide: TaC). That is, the outer side surface of the crucible 20 is surrounded by a cylindrical shield 18 and a heating element 17 provided outside the shield 18.
  • the crucible 20 and the shield 18 are arranged close to each other, but are provided so as not to contact each other.
  • the heating element 17 and the shield 18 are provided in close contact with each other.
  • the heat generating body 17 and the shielding body 18 are being fixed from the inner bottom face or inner top face of the heat insulating container 11 by members (not shown).
  • the crucible 20, the shield 18, and the heating element 17 will be described in detail later.
  • the heating furnace 10 includes a metal heating coil 30 wound around a portion that is outside the side surface on the lower side of the heat insulating container 11 and inside the side surface on the lower side of the chamber 14.
  • the heating coil 30 is disposed so as to face the side surface of the heating element 17 through the heat insulating container 11.
  • the heating coil 30 is configured by, for example, a hollow copper tube.
  • the heating coil 30 is wound in a spiral shape and has a cylindrical shape when viewed as a whole. That is, the inner diameter on the upper side and the inner diameter on the lower side of the heating coil 30 are substantially the same. Thereby, the space formed in the inside by the wound heating coil 30 is cylindrical.
  • the central axis of the heating coil 30 passing through the columnar space is substantially perpendicular to the horizontal direction, that is, along the vertical direction.
  • the heating furnace 10 includes a lifting rod 40 as an example of a lifting member that extends downward from above through through holes provided in the upper surfaces of the heat insulating container 11 and the chamber 14, respectively.
  • the pulling rod 40 is attached so as to be able to move in the vertical direction and rotate around the axis.
  • a sealing material (not shown) is provided between the through hole provided in the chamber 14 and the lifting rod 40.
  • a holding member 41 for attaching and holding a seed crystal 210 (see FIG. 2 described later) serving as a base for growing the sapphire ingot 200 is attached to an end portion of the pulling bar 40 on the vertically lower side. Yes.
  • the single crystal pulling apparatus 1 includes a pulling drive unit 50 for pulling the pulling bar 40 vertically upward (in the direction of arrow A) and a rotation driving unit 60 for rotating the pulling bar 40 in the direction of arrow B.
  • the pulling drive unit 50 is composed of a motor or the like, and can adjust the pulling speed of the pulling bar 40 in the direction of arrow A.
  • the rotation driving unit 60 is also composed of a motor or the like so that the rotation speed of the lifting rod 40 in the direction of arrow B can be adjusted.
  • the single crystal pulling apparatus 1 includes a gas supply unit 70 for supplying gas into the chamber 14 via the gas supply pipe 12.
  • the gas supply unit 70 can supply an inert gas such as nitrogen or argon.
  • the gas supply unit 70 can also adjust the flow rate of the gas supplied into the chamber 14.
  • the single crystal pulling apparatus 1 includes an exhaust unit 80 that exhausts gas from the inside of the chamber 14 via the gas exhaust pipe 13.
  • the exhaust unit 80 includes, for example, a vacuum pump or the like, and can decompress the chamber 14 and exhaust the gas supplied from the gas supply unit 70.
  • the single crystal pulling apparatus 1 includes a coil power supply 90 that supplies a high-frequency alternating current (referred to as a high-frequency current in the following description) to the heating coil 30.
  • the coil power supply 90 can set the presence / absence of supply of a high-frequency current to the heating coil 30, the amount of current to be supplied, and the frequency of the high-frequency current supplied to the heating coil 30.
  • the single crystal pulling apparatus 1 includes a weight detection unit 110 that detects the weight of the sapphire ingot 200 that grows on the lower side of the pulling bar 40 via the pulling bar 40.
  • the weight detection unit 110 includes, for example, a conventionally known load cell.
  • the single crystal pulling apparatus 1 includes a control unit 100 that controls operations of the pulling drive unit 50, the rotation drive unit 60, the gas supply unit 70, the exhaust unit 80, and the coil power supply 90 described above. Further, the control unit 100 calculates the crystal diameter of the sapphire ingot 200 to be pulled up based on the weight signal output from the weight detection unit 110 and feeds it back to the coil power supply 90.
  • FIG. 2 is a diagram showing an example of the configuration of a sapphire ingot 200 manufactured using the single crystal pulling apparatus 1 shown in FIG.
  • the sapphire ingot 200 includes a seed crystal 210 that serves as a base for growing the sapphire ingot 200, a shoulder 220 that extends under the seed crystal 210 and is integrated with the seed crystal 210, and a lower portion of the shoulder 220.
  • a straight body portion 230 extending and integrated with the shoulder portion 220, and a tail portion 240 extending under the straight body portion 230 and integrated with the straight body portion 230 are provided.
  • a single crystal of sapphire grows in the c-axis direction from the upper side, that is, from the seed crystal 210 side to the lower side, that is, from the tail part 240 side.
  • the shoulder part 220 has a shape in which the diameter gradually increases from the seed crystal 210 side toward the straight body part 230 side.
  • the straight body portion 230 has such a shape that the diameters thereof are substantially the same from the upper side to the lower side.
  • the diameter of the straight body 230 is set to a value slightly larger than the diameter of the desired sapphire single crystal wafer.
  • the tail part 240 has the shape which becomes convex shape from upper direction to the downward direction, when the diameter reduces gradually toward the downward direction from the upper part. 2 shows an example in which the tail 240 has a convex shape protruding below the straight body 230. However, when manufacturing conditions are varied, a broken line in FIG. As shown, it may have a concave shape that is recessed below the straight body portion 230.
  • the reason why the sapphire ingot 200 having a crystal grown in the c-axis direction is manufactured is as follows.
  • a blue LED substrate material, a polarizer holding member of a liquid crystal projector, and the like are cut out from an ingot so that the plane ((0001) plane) perpendicular to the c-axis of the sapphire single crystal is the main plane.
  • the sapphire single crystal ingot grown in the c-axis direction for cutting out the wafer.
  • the sapphire ingot 200 in which the crystal is grown in the c-axis direction is manufactured in consideration of the convenience in the subsequent process.
  • the single crystal pulling apparatus 1 shown in FIG. 1 can pull not only the sapphire ingot 200 grown in the c-axis direction but also the sapphire ingot 200 grown in the a-axis direction, for example.
  • sapphire it is possible to pull up various oxide single crystals, and it is also possible to pull up single crystals other than oxides.
  • FIG. 3 is a perspective view showing an example of the configuration of the crucible 20, the heating element 17, and the shield 18 shown in FIG. Below, the positional relationship of the crucible 20, the heat generating body 17, and the shielding body 18 is demonstrated.
  • the crucible 20 is made of molybdenum.
  • the crucible 20 may be substantially made of only molybdenum material or made of only tungsten (W) material.
  • an alloy of molybdenum and tungsten (Mo—W), and other metal elements such as niobium and tantalum may be contained. If it is made of an alloy of molybdenum and tungsten (Mo—W), it preferably contains 10% to 40% by mass of tungsten. Any crucible 20 using these is cheaper than iridium.
  • the bottom portion 21 has a circular shape and has a substantially uniform thickness (for example, about 2 mm to 7 mm) over the entire area. Further, the wall portion 22 has a cylindrical shape, and this also has a substantially uniform thickness (for example, about 2 mm to 7 mm) over the entire region.
  • the inner diameter of the crucible 20 is determined by the diameter of the single crystal to be grown. For example, when growing a sapphire single crystal having a diameter of about 150 mm (about 6 inches), the inner diameter of the crucible 20 is about 220 mm.
  • Heating element 17 When a part of the magnetic flux generated by the high-frequency current supplied to the heating coil 30 crosses the heating element 17 through the heat insulating container 11, the heating element 17 blocks the change of the magnetic field on the wall surface of the heating element 17. As a result, an eddy current is generated in the heating element 17.
  • the heating element 17 is provided for heating and melting the raw material charged in the crucible 20, it needs to be stable at a temperature near the melting point of the raw material charged in the crucible 20.
  • the melting point of alumina is about 2040 ° C.
  • the temperature of the alumina melt 300 is heated from 2100 ° C. to 2400 ° C.
  • Graphite has a sufficient heat resistance with a melting point of 3500 ° C. or higher. Further, graphite has an electrical resistance that efficiently induces induction heating. Therefore, in the present embodiment, graphite is used as the heating element 17.
  • the heating element 17 is not limited to graphite, and may be any material that satisfies the above requirements, and is preferably a material containing carbon. Since the thickness of the heating element 17 is affected by the frequency of the high-frequency current supplied from the coil power supply 90, the thickness is preferably in the range of 5 mm to 30 mm in the present invention. If it is thicker than 30 mm, the heat generation efficiency of the heat generator 17 is lowered.
  • the heating element 17 becomes too thick, a portion that does not generate heat is generated, and heat is taken away from this, so that the heating efficiency of the heating element 17 is not good.
  • the thickness is less than 5 mm, the heat generation efficiency of the heat generator 17 is lowered. That is, if the heating element 17 becomes too thin, the portion that generates heat is reduced, so that the high-frequency current supplied to the heating coil 30 is less likely to be reflected in the heat generation amount.
  • the thickness of the heating element 17 is preferably 10 mm to 20 mm.
  • Graphite is easy to exfoliate and has a vapor pressure when heated from 2100 ° C. to 2400 ° C. And carbon particles which carbon gas and carbon gas solidified are generated.
  • the generated carbon gas and carbon particles are mixed into the alumina melt 300 in the crucible 20, it is taken into the sapphire single crystal and becomes a crystal defect. Further, the carbon gas and the carbon particles reduce the alumina melt 300 to generate oxygen (O 2 ) and carbon monoxide (CO). For this reason, it reacts with molybdenum in the crucible 20 to produce molybdenum oxide rich in sublimation. Thereby, the crucible 20 corrodes and the life of the crucible 20 is shortened.
  • the shield 18 is located between the outer wall portion 22 of the crucible 20 and the heating element 17, so that the constituent material of the heating element 17 (for example, carbon gas and carbon particles when the heating element 17 is graphite) is contained in the crucible 20. To be mixed into the alumina melt 300. For this reason, the shield 18 needs to be stable at a temperature near the melting point of the raw material charged into the crucible 20 and, for example, when the heating element 17 is graphite, it may not be decomposed by carbon gas and carbon particles. preferable.
  • the constituent material of the heating element 17 for example, carbon gas and carbon particles when the heating element 17 is graphite
  • Tantalum carbide is a carbide material with a high melting point of 3873 ° C. and stable at high temperatures. Therefore, it is not decomposed by carbon gas and carbon particles. Therefore, in this embodiment, tantalum carbide is used.
  • the shield 18 is not limited to tantalum carbide, and may be any material that satisfies the above requirements, and is preferably a material containing carbide.
  • the crucible 20 and the shield 18 are arranged close to each other, but are provided so as not to contact each other. Since the shield 18 is heated by heat conduction or heat radiation from the heating element 17, when the crucible 20 and the shield 18 come into contact with each other, the temperature of the contacted portion of the crucible 20 increases, and the inside of the crucible 20 The temperature gradient of the alumina melt 300 becomes steep. On the other hand, the heating element 17 and the shielding body 18 may be in contact with each other, but when the heating element 17 and the shielding body 18 are locally in contact with each other, the portion becomes high temperature. Therefore, it is preferable that the heating element 17 and the shield 18 are in close contact with each other, or are arranged close to each other without contact.
  • the thickness of the shield 18 is preferably in the range of 0.1 mm to 10 mm. If the thickness is more than 10 mm, processing becomes difficult and the cost increases. On the other hand, if the thickness is less than 0.1 mm, the strength as the shield 18 becomes fragile and may be damaged when taken out from the single crystal pulling apparatus 1 (at the time of handling). Disappear.
  • the thickness of the shield 18 is preferably in the range of 0.3 mm to 5 mm.
  • the heating element 30 is heated by the heating coil 30, and the shield 18 disposed in close contact with or in close proximity to the heating element 17 causes the heat conduction from the heating element 17 and / or Or it is heated by thermal radiation.
  • positioned in proximity to the shield 18 is heated by the thermal radiation from the heated shield 18.
  • the crucible 20 serves only as a container for holding the alumina melt 300, and the heating element 17 serves as a heater. That is, the crucible 20 is indirectly heated.
  • the temperature gradient of the alumina melt 300 in the crucible 20 is reduced as compared with the case where the crucible 20 also serves as a heater by induction heating. . Thereby, generation
  • the length of the side surface of the heating element 17 may be shorter than the length of the wall part 22 of the crucible 20, but preferably the length of the wall part 22 of the crucible 20 or longer and the upper end of the heating element 17. It is sufficient in terms of efficiency to heat the crucible 20 that the lower end and the lower end are set so as to protrude from the upper end and the lower end of the crucible 20, respectively.
  • the shield 18 is interposed between the crucible 20 and the heating element 17. However, since the heat capacity of the shield 18 is small, the shield 18 can be a sufficient heat source for heating the crucible 20. Absent. Therefore, most of the heat for heating the crucible 20 is supplied from the heating element 17.
  • the length of the side surface of the cylindrical heating element 17 is shorter than the length of the wall portion 22 of the crucible 20 (height of the crucible 20), heat is generated in the upper part or / and the lower part of the wall portion 22 of the crucible 20. Sufficient heat radiation from the body 17 (including the shield 18) cannot be received, and a steep temperature gradient may be generated in the crucible 20 or the alumina melt 300.
  • the shield 18 is provided to prevent the constituent material of the heating element 17 (for example, when the heating element 17 is graphite, carbon gas and carbon particles) from being mixed into the crucible 20.
  • the upper end of the shield 18 is set higher than the upper end of the heating element 17. That is, the upper end of the shield 18 is preferably higher than the upper end of the heating element 17.
  • the upper end of the shield 18 may be lower than the upper end of the wall portion 22 of the crucible 20, but it is more preferable that the upper end of the wall portion 22 of the crucible 20 be provided at a height higher than that.
  • the lower end of the shield 18 may be at least within the range of the wall portion 22 of the crucible 20, and may be set lower than the lower end of the wall portion 22 of the crucible 20.
  • the lower end of the shield 18 only needs to be within the range of the side surface of the heating element 17, and may be set lower than the lower end of the heating element 17. That is, the shield 18 is provided so as to separate the crucible 20 and the heating element 17 in the opening portion of the crucible 20 provided vertically upward. This is because the constituent material of the heating element 17 is mixed into the alumina melt 300 in the crucible 20 through the opening of the crucible 20 provided vertically upward. This is because it is sufficient that the shield 18 can suppress the mixing of the constituent materials of the heating element 17.
  • FIG. 4 is a flowchart for explaining an example of a procedure for manufacturing the sapphire ingot 200 shown in FIG. 2 using the single crystal pulling apparatus 1 shown in FIG.
  • a melting step is performed in which solid aluminum oxide filled in the crucible 20 in the chamber 14 is melted by heating (step 101).
  • a seeding step is performed in which temperature adjustment is performed in a state where the lower end portion of the seed crystal 210 is in contact with the aluminum oxide melt, that is, the alumina melt 300 (step 102).
  • the shoulder 220 is formed below the seed crystal 210 by pulling it upward (in the direction of arrow A in FIG.
  • a shoulder forming step is executed (step 103). Subsequently, a straight body part forming step is performed in which the straight body part 230 is formed below the shoulder part 220 by pulling upward through the seed crystal 210 while rotating the shoulder part 220 (step 104). Further, the tail forming step of forming the tail 240 below the straight body 230 by pulling up and separating from the alumina melt 300 while rotating the straight body 230 through the seed crystal 210 and the shoulder 220. Is executed (step 105).
  • step 106 the cooling process which stops and cools the heating of the alumina melt 300 in the crucible 20 is executed (step 106), and after the obtained sapphire ingot 200 is cooled, it is taken out of the chamber 14 and a series of manufacturing is performed. Complete the process.
  • the sapphire ingot 200 thus obtained is first cut at the boundary between the shoulder 220 and the straight body 230 and at the boundary between the straight body 230 and the tail 240, and the straight body 230 is cut out. .
  • the cut out straight body portion 230 is further cut in a direction orthogonal to the longitudinal direction to form a sapphire single crystal wafer.
  • the main surface of the obtained wafer is the c-plane ((0001) plane).
  • the obtained wafer is used for manufacturing blue LEDs and polarizers.
  • a c-axis ( ⁇ 0001>) seed crystal 210 is prepared.
  • the seed crystal 210 is attached to the holding member 41 of the pulling rod 40 and set at a predetermined position.
  • the crucible 20 is filled with a raw material of aluminum oxide, that is, an alumina raw material, the crucible 20 is placed on the crucible support 15, and the heat insulating container 11 is assembled in the chamber 14.
  • the inside of the chamber 14 is decompressed using the exhaust unit 80 in a state where the gas supply from the gas supply unit 70 is not performed.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14 to bring the inside of the chamber 14 to normal pressure.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14.
  • the gas supplied in the melting step may be the same as or different from that in the preparation step.
  • the rotation driving unit 60 rotates the pulling rod 40 at the first rotation speed.
  • the coil power supply 90 supplies a high frequency current to the heating coil 30.
  • a high frequency current is supplied from the coil power supply 90 to the heating coil 30, the magnetic flux repeatedly generates and disappears around the heating coil 30.
  • the crucible 20 when the bottom 21 and the wall 22 of the crucible 20 are heated and the aluminum oxide accommodated in the crucible 20 is heated beyond its melting point (2054 ° C.), the crucible 20 The alumina raw material, that is, aluminum oxide is melted to form an alumina melt 300.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14.
  • the gas supplied in the seeding step may be the same as or different from that in the melting step. However, as in the melting step, mixing of oxygen is not preferable.
  • the pulling drive unit 50 lowers the pulling rod 40 to a position where the lower end of the seed crystal 210 attached to the holding member 41 comes into contact with the alumina melt 300 in the crucible 20 and stops it. In this state, the coil power supply 90 adjusts the current value of the high-frequency current supplied to the heating coil 30 based on the weight signal from the weight detection unit 110.
  • the shoulder forming step the high frequency current supplied from the coil power supply 90 to the heating coil 30 is adjusted, and then held for a while until the temperature of the alumina melt 300 is stabilized, and then the lifting rod 40 is moved to the first rotational speed. Pull up at the first pulling speed while rotating.
  • the seed crystal 210 is pulled up while being rotated with its lower end immersed in the alumina melt 300, and a shoulder 220 that expands vertically downward is formed at the lower end of the seed crystal 210. It will be done. Note that the shoulder forming step is completed when the diameter of the shoulder 220 becomes about several mm larger than the desired diameter of the wafer.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14.
  • the gas supplied in a straight body part formation process may be the same as a shoulder part formation process, and may differ. However, as in the melting step, mixing of oxygen is not preferable.
  • the coil power supply 90 continues to supply a high frequency current to the heating coil 30 to heat the alumina melt 300 through the crucible 20.
  • the pulling drive unit 50 pulls the pulling rod 40 at the second pulling speed.
  • the second pulling speed may be the same as or different from the first pulling speed in the shoulder forming step.
  • the rotation drive unit 60 rotates the pulling rod 40 at the second rotation speed.
  • the second rotation speed may be the same speed as the first rotation speed in the shoulder forming step, or may be a different speed.
  • the shoulder 220 integrated with the seed crystal 210 is pulled up while being rotated while the lower end of the shoulder 220 is immersed in the alumina melt 300.
  • the trunk portion 230 is formed.
  • the diameter of the straight body 230 may be equal to or larger than the desired diameter of the wafer.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14.
  • the gas supplied in the tail portion forming step may be the same as or different from that in the straight body portion forming step.
  • mixing of oxygen is not preferable.
  • the coil power supply 90 continues to supply a high-frequency current to the heating coil 30 to heat the alumina melt 300 through the crucible 20.
  • the pulling drive unit 50 pulls the pulling rod 40 at the third pulling speed.
  • the third pulling speed may be the same as the first pulling speed in the shoulder forming process or the second pulling speed in the straight body forming process, or may be a speed different from these. Good.
  • the rotation drive unit 60 rotates the pulling rod 40 at the third rotation speed.
  • the third rotation speed may be the same as the first rotation speed in the shoulder forming process or the second rotation speed in the straight body forming process, or may be different from these. Also good.
  • the pulling drive unit 50 increases the pulling speed of the pulling bar 40 and pulls the pulling bar 40 further upward, thereby lowering the lower end of the tail 240. Pull away from melt 300. Thereby, the sapphire ingot 200 shown in FIG. 2 is obtained.
  • the gas supply unit 70 supplies a predetermined gas into the chamber 14.
  • the gas supplied in the cooling step may be the same as or different from the tail forming step.
  • mixing of oxygen is not preferable.
  • the coil power supply 90 stops the supply of the high-frequency current to the heating coil 30 and stops the heating of the alumina melt 300 through the crucible 20.
  • the pulling drive unit 50 stops the pulling of the pulling rod 40 and the rotation driving unit 60 stops the rotation of the pulling rod 40. At this time, a small amount of aluminum oxide that did not form the sapphire ingot 200 remains as the alumina melt 300 in the crucible 20.
  • the alumina melt 300 in the crucible 20 with the stop of heating is gradually cooled and solidified in the crucible 20 after falling below the melting point of aluminum oxide to become aluminum oxide solid. Then, the sapphire ingot 200 is taken out from the chamber 14 with the chamber 14 sufficiently cooled.
  • the crucible 20 is indirectly heated without directly heating the wall portion 22 of the crucible 20 by the heating coil 30. For this reason, compared with the case where the wall part 22 of the crucible 20 is directly heated with the heating coil 30, the temperature gradient of the melt in the crucible 20 can be relieved. Therefore, distortion generated in the single crystal grown by the rapid temperature gradient can be suppressed.

Abstract

L'invention concerne un appareil (1) de tirage de monocristaux comportant un four (10) de chauffe destiné à faire croître un lingot (200) de saphir composé d'un monocristal de saphir. Un creuset (20) destiné à contenir un bain (300) de fusion d'alumine est placé en position inférieure à l'intérieur d'un récipient (11) thermiquement isolant. L'appareil (1) de tirage de monocristaux comporte également un corps (17) de chauffe qui est placé à l'intérieur du récipient (11) thermiquement isolant mais à l'extérieur du creuset (20) de façon à entourer une partie (22) de paroi du creuset (20). L'appareil (1) de tirage de monocristaux comporte de plus un corps (18) de protection qui est placé à l'intérieur du corps (17) de chauffe mais à l'extérieur du creuset (20) de façon à entourer la partie (22) de paroi du creuset (20) dans le but d'empêcher le matériau constitutif du corps (17) de chauffe de se mélanger au bain (300) de fusion d'alumine à l'intérieur du creuset (20). Par conséquent, un creuset économique peut être utilisé dans un appareil de tirage de monocristaux faisant appel à la méthode de Czochralski (Cz), et la déformation dans un monocristal de croissance peut être limitée en réduisant le gradient de température du bain de fusion à l'intérieur du creuset.
PCT/JP2010/069955 2009-11-20 2010-11-09 Appareil de tirage de monocristaux WO2011062092A1 (fr)

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WO2014073163A1 (fr) * 2012-11-06 2014-05-15 信越半導体株式会社 Dispositif de fabrication de monocristal

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JP5772719B2 (ja) * 2012-05-23 2015-09-02 住友金属鉱山株式会社 酸化物単結晶育成装置
KR101547329B1 (ko) * 2013-03-21 2015-08-25 주식회사 사파이어테크놀로지 사파이어 단결정 성장장치 및 성장방법
JP6182938B2 (ja) * 2013-04-03 2017-08-23 シンフォニアテクノロジー株式会社 誘導加熱溶解装置
USD771167S1 (en) 2013-08-21 2016-11-08 A.L.M.T. Corp. Crucible
JP6302192B2 (ja) * 2013-09-04 2018-03-28 株式会社福田結晶技術研究所 単結晶の育成装置及び育成方法
WO2015064505A1 (fr) * 2013-10-30 2015-05-07 株式会社アライドマテリアル Creuset et procédé de production de saphir monocristallin l'utilisant
CN104451862B (zh) * 2015-01-16 2017-09-01 苏州恒嘉晶体材料有限公司 一种蓝宝石单晶炉和蓝宝石引晶方法
KR102271712B1 (ko) * 2020-09-28 2021-07-01 한화솔루션 주식회사 히터를 포함하는 잉곳 성장 장치 및 잉곳 성장 장치용 히터의 제조 방법

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WO2014073163A1 (fr) * 2012-11-06 2014-05-15 信越半導体株式会社 Dispositif de fabrication de monocristal
JP2014091670A (ja) * 2012-11-06 2014-05-19 Shin Etsu Handotai Co Ltd 単結晶製造装置

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TW201128003A (en) 2011-08-16

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