Classifications

• • 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
  • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt

Definitions

• the present invention relates to a silicon single crystal production apparatus for growing a single crystal while supplying a bulk material.
• CC-Cz method silicon single crystal manufacturing method for continuously growing single crystals while continuously supplying raw materials into the crucible.
• CC-Cz method silicon single crystal manufacturing method
• the granular material has a spherical shape and a diameter of 0.2 to 5 millimeters.
• the above-mentioned granular silicon raw materials are not generally used.
• it In order for the CC-CZ method to become widespread, it must be a crystal growth technology that can use commonly used raw materials.
• the raw materials used for general purposes are ice or amorphous chunks like crushed glass.
• its dimensions are as large as 10 to 50 millimeters, and there is a variability.
• Such bulk materials are It is extremely difficult to cut out from the storage container and control the supply amount into the crucible. Therefore, the CC-CZ method using bulk materials has not yet been put to practical use.
• a storage unit that stores a large amount of raw materials (50 to 200 kgf) must be able to stably extract raw materials.
• a small amount of supply (30 to: LOOg / min) can be performed, and the supply amount can be controlled with high accuracy (target value ⁇ 10%).
• the structure be as simple as that the device can be manufactured from silicon, quartz or Teflon.
• An object of the present invention is to provide a single crystal manufacturing apparatus provided with a raw material supply device capable of supplying a bulk raw material continuously and with a highly precise control of the supply amount.
• a single crystal manufacturing apparatus is provided with a crucible that accommodates a melt of a crystal raw material and rotates around a vertical axis, and is provided around the crucible.
• the raw material supply device holds the bulk raw material, has a central axis substantially horizontal, and is provided with a storage cylinder provided rotatably around the central axis. It has an inside diameter that allows it to pass to the other end, and is inclined so that the end serving as the outlet is lower in height than the end serving as the inlet, and the rotation of the center shaft is performed. It has a weighing tube provided downstream of the storage tube and a load cell attached to the weighing tube to measure the weight of the bulk material passing through the weighing tube so that it can rotate.
• the bulk raw material held in the storage cylinder whose central axis is almost horizontal opens one of the storage cylinders by rotating the storage cylinder around the central axis. Is discharged from the end.
• This cutting method allows the raw material to be forcibly cut out, regardless of whether the raw material is very irregular, large, and large in size.
• the structure is simple.
• the cut-out amount is adjusted by adjusting the rotation speed of the storage cylinder.
• a method of adjusting the inclination angle of the central axis of the storage cylinder may be used.
• they may be combined.
• the raw material cut out from the storage cylinder is sent into the measuring cylinder.
• the measuring cylinder has an inner diameter that allows the bulk material to pass from one end to the other end.
• the end serving as the inlet for the bulk material discharged from the storage cylinder is closer to the end serving as the other outlet. It is provided at an angle so as to increase its height. Therefore, the bulk raw material discharged from the storage cylinder is moved from the inlet end to the outlet end while sliding in the measuring cylinder by the rotation of the measuring cylinder around the central axis. Move toward the part. Raw materials are arranged in a row as they move. Finally, one by one is discharged from the end on the exit side. The amount of discharge is adjusted by adjusting the number of revolutions of the measuring cylinder. Alternatively, a method of adjusting the inclination angle of the center axis of the measuring cylinder, or a method of combining them may be used.
• a load cell is attached to the measuring cylinder, and the weight of the bulk material discharged from the measuring cylinder is measured.
• the weighing method the following two methods can be considered depending on how to apply the weighing tube load to the load cell.
• Adjustment of the supply amount of the silicon bulk material into the crucible is performed by controlling the rotation speed or the inclination angle of the center of the measuring cylinder based on the measured weight of the load cell. It is done.
• This weighing method allows the raw materials to be transported without difficulty, regardless of the size and the size of the raw materials, even if the raw materials are extremely irregular. It can measure and control with high accuracy. Furthermore, the structure is simple.
• the raw material supply device has a simple structure as described above, the member that comes into contact with the silicon raw material is made of Teflon or quartz in order to reduce the contamination of impurities. Or it can be made in silicon.
• FIG. 1 is a longitudinal sectional view of an apparatus for producing a silicon single crystal equipped with a continuous supply apparatus of a silicon bulk material according to an embodiment of the present invention.
• Fig. 1 is a longitudinal section of the single crystal manufacturing equipment of this embodiment. It is a figure.
• a crucible 2 is provided at the center of the chamber 1, and a lid 1 a is mounted on the upper portion of the crucible 2.
• a support shaft 4 for rotatably and vertically movingly supporting the graphite crucible 3 a heater 8 as a heating means, and a heater 8 are provided around the heater 8. Insulation material 9 is arranged.
• Crucible 2 is made of quartz and set in graphite crucible 3.
• the crucible 2 is provided with a cylindrical partition 6, which divides the silicon melt 5 in the crucible 2 into an outer raw material melting section and an inner crystal growing section. You The partition 6 is provided with a through-hole 7.
• the columnar silicon single crystal 12 grows from the seed crystal 11 and is lifted by the silicon melt 5.
• the pulling device 40 includes a wire 10 and a wire 10 to which the seed crystal 11 is attached via a pulling chamber 1b and a shield chuck. , And a wire winding device 13 and a gate valve 14.
• the raw material supply device 20 has a box 21 provided on an upper portion of the chamber 1 and communicating with the inside of the chamber 1.
• An opening / closing lid S 1 for refilling the silicon bulk material S 0 is provided at an upper portion of the box 21, and a 0 ring 32 for the seal is provided. It is bolted to the box 21 via this.
• the storage cylinder 22 is provided inside the box 21, and can be rotated around the center axis by a drive mechanism (not shown). The angle of inclination of the central axis can be adjusted around the center.
• the height of the inlet end of the silicon bulk material 30 is higher than the height of the outlet side end.
• the drive mechanism (not shown) allows the rotary motion about the center axis to be performed by using a drive mechanism (not shown).
• shut 25 that guides the silicon bulk material 30 discharged from the storage tube 22 to the measuring tube 24. It is provided.
• a load cell 28 for measuring the weight of the silicon bulk material 30 is attached to the measuring cylinder 24. At the moment when the silicon bulk material 30 is discharged from the measuring cylinder 24, the measured value is reduced by the weight of the discharged silicon bulk material 30. By calculating the cumulative value of the reduction amount within a predetermined time, the supply amount of the silicon bulk material 30 to the crucible 2 can be measured.
• the first guide tube 27 is provided below the outlet of the measuring tube, and guides the raw material from the measuring tube 24 downward.
• the second guide tube 28 supplies the raw material into the silicon melt in the raw material melting section via the gate valve 29.
• the second guide pipe 28 passes through the silicon melt 5 of the outer raw material melting section, which is divided by the partition 6 by the raw material supply device 20, Then, the silicon bulk material 30 is charged. The amount is equivalent to the growth amount of the single crystal.
• the silicon bulk material 30 charged in the storage tube 22 is discharged from the opening of the storage tube 22 by the rotation of the storage tube 22. Then, it is supplied to the measuring cylinder 24 via the shot 25.
• the inlet end of the measuring tube 24 is set so that the height is higher than the outlet end, so supply to the inlet end of the measuring tube 24. Due to the rotational movement of the measuring tube 24, the silicon bulk material 30 moves in the measuring tube in the axial direction toward the lower end on the outlet side.
• the silicon bulk material 30 discharged from the outlet end of the measuring cylinder 2 '4 passes through the first guide tube 27 and the second guide tube 28 and then into the crucible 2.
• the amount of the silicon bulk material 30 charged into the silicon melt surface is determined by the speed at which the silicon bulk material 30 in the measuring cylinder 24 moves in the measuring cylinder in the axial direction. Is determined by
• the moving speed of the raw material in the measuring cylinder can be adjusted by the rotation speed of the measuring cylinder. Therefore, while monitoring the measured value of the load cell 26 attached to the measuring cylinder 24, the amount of input is adjusted by adjusting the rotation speed of the measuring cylinder 24.
• the gate valve 29 When refilling the silicon bulk material 30 into the storage cylinder 22, the gate valve 29 is closed, and the central axis of the storage cylinder 22 is centered on the inclined axis 23. Rotate the storage tube so that it is vertical. Then, the opening / closing lid 31 at the top of the box 21 is opened to replenish the silicon bulk material 30.
• the storage tube 22 the measuring tube 24, the cut 25, and the first guide tube that the silicon bulk material 30 comes into contact with If the second guide tube 28 and the second guide tube 28 are made of Teflon, quartz, or silicon, it is possible to prevent impurities from being mixed.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Crystallography & Structural Chemistry (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Crystals, And After-Treatments Of Crystals (AREA)
• Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

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Cited By (5)

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Citations (2)

• 1990
  • 1990-03-02 JP JP2051326A patent/JPH03252386A/ja active Pending
• 1991
  • 1991-03-01 KR KR1019910701501A patent/KR920701531A/ko not_active Withdrawn
  • 1991-03-01 WO PCT/JP1991/000273 patent/WO1991013192A1/ja active Application Filing
  • 1991-03-01 DE DE19914190411 patent/DE4190411T1/de not_active Withdrawn

Patent Citations (2)

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