WO2002068732A1 - Tube de recharge pour matériau polycristallin solide, et procédé de production de monocristal au moyen de ce tube - Google Patents

Tube de recharge pour matériau polycristallin solide, et procédé de production de monocristal au moyen de ce tube Download PDF

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Publication number
WO2002068732A1
WO2002068732A1 PCT/JP2002/001796 JP0201796W WO02068732A1 WO 2002068732 A1 WO2002068732 A1 WO 2002068732A1 JP 0201796 W JP0201796 W JP 0201796W WO 02068732 A1 WO02068732 A1 WO 02068732A1
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WO
WIPO (PCT)
Prior art keywords
recharge
raw material
single crystal
solid
tube
Prior art date
Application number
PCT/JP2002/001796
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English (en)
Japanese (ja)
Inventor
Atsushi Iwasaki
Shinobu Takeyasu
Original Assignee
Shin-Etsu Handotai Co., Ltd.
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Filing date
Publication date
Application filed by Shin-Etsu Handotai Co., Ltd. filed Critical Shin-Etsu Handotai Co., Ltd.
Priority to JP2002568821A priority Critical patent/JP4103593B2/ja
Publication of WO2002068732A1 publication Critical patent/WO2002068732A1/fr

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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 solid polycrystalline material recharge tube and a method for producing a single crystal using the same.
  • the present invention relates to a rechargeable tube for additionally filling a solid polycrystalline raw material when producing a single crystal, and a method for producing a single crystal using the same.
  • a single crystal is a semiconductor single crystal, and a silicon single crystal will be described as an example here.
  • a silicon single crystal wafer used as a substrate of a semiconductor integrated circuit is manufactured by, for example, pulling a silicon single crystal by the Czochralski (CZ) method.
  • CZ Czochralski
  • the raw material polycrystalline silicon polycrystalline raw material
  • the graphite ruppo holding the quartz ruppo is heated by a cylindrical graphite heater on its outer periphery, and the polycrystalline silicon is heated. Is melted.
  • the seed crystal is immersed in a silicon melt to form a constricted portion to eliminate dislocations, and then a silicon single crystal is grown to a required diameter and length.
  • a supply pipe is provided to supply the reduced amount of silicon melt in the crucible due to the pulling of the silicon single crystal, and the granular polycrystalline raw material is introduced into the crucible.
  • granular raw material is known in accordance with the amount of melt reduction.
  • CCCZ continuous charge
  • the same amount of granular material as the silicon single crystal growth amount (usually about 0.3 g / sec to 1.0 g Z seconds) must be supplied in small quantities and slowly. Disruption often occurs when the molten metal jumps or causes surface vibration when supplied to the furnace. For this reason, the dislocation of the silicon single crystal during the growth of the silicon single crystal makes it impossible to continue the growth of the silicon single crystal, and it often occurs that the manufacturing cost cannot be reduced. To prevent this, the tip of the supply pipe is squeezed to suppress the supply speed to some extent. This has the disadvantage that the supply rate is limited and the supply time of the granular material becomes too long.
  • a multi-pooling (or recharge pulling (RCCZ)) method is known as a method of reducing the production cost when adding raw materials in a conventional batch method (Fumio Shim ra, Semiconductor Silicon Crystal Technology, B178). -see pl79,1989).
  • a rod-shaped polycrystalline raw material hereinafter referred to as a rod-shaped raw material
  • nugget-shaped raw materials raw materials that can be supplied in large quantities at a time, such as rod-shaped raw materials and bulk polycrystalline raw materials (hereinafter referred to as nugget-shaped raw materials), have been generally used.
  • the applicant of the present invention has to provide a heat-shielding cylinder with a color in a silicon single crystal manufacturing apparatus (Japanese Patent Publication No. 06-0339351), It has been proposed to provide a cylinder with a heater inside (Japanese Patent No. 2785663).
  • a heat shielding member was provided in the silicon single crystal manufacturing apparatus so as to cover above the melt surface.
  • the nugget raw material when filling the nugget raw material into the quartz tube, the nugget raw material is at room temperature, and if the nugget raw material is directly introduced into a high-temperature melt, the melt scatters in the silicon single crystal manufacturing apparatus, and the silicon single crystal cannot be manufactured. was there. Also, if the melt surface is solidified in order to prevent the melt from scattering, depending on the progress of solidification, damage may be given to the quartz reticulum and the inner surface of the quartz reticulum may be peeled off, and the separated quartz debris may be removed. The phenomenon that the silicon single crystal adheres to the growing silicon single crystal, dislocations are generated in the silicon single crystal, and polycrystallized frequently occurs, and the production efficiency of the silicon single crystal is greatly reduced. . Furthermore, if the solidification proceeds excessively, there is a possibility that the quartz rupture cracks and the melt in the quartz ruppo leaks out.
  • an object of the present invention is to provide a nugget-shaped and / or granular (hereinafter referred to as solid) without taking the conventional raw material supply device into consideration and taking it into and out of a single crystal manufacturing device without attaching the conventional raw material supply device.
  • the raw material can be directly injected into the solidified melt surface in the rutupo, and at the same time, a supply rate suitable for recharging is realized, and the single crystal is produced by performing recharging smoothly and efficiently in a short time.
  • An object of the present invention is to provide an inexpensive solid polycrystalline raw material recharge tube which can improve the resiliency.
  • Another object of the present invention is to provide a method for producing a single crystal capable of safely and efficiently producing a dislocation-free single crystal using the recharge tube. Disclosure of the invention
  • a single crystal production apparatus having a rutupo for storing a crystal melt is detachably provided, and the rutupo is filled with a solid polycrystalline raw material.
  • the rutupo is filled with a solid polycrystalline raw material.
  • a lid for sealing the pipe body, a hook for suspending the main body of the recharge pipe, a recharge pipe wire connecting the hook and the conical valve, and a recharge pipe wire provided at a central portion of the lid;
  • a stopper is provided so as to pass through substantially the center of the recharge pipe main body, and the recharge pipe main body expands outward toward the lower end.
  • the recharge tube of the present invention is a substantially cylindrical rechargeable tube filled with a nugget-like raw material, a granular raw material, or a raw material in which both are mixed, and a single unit in a state where a main body of the recharge tube is suspended by a hook. It can be incorporated into crystal manufacturing equipment. Then, the conical valve connected to the recharge pipe wire separates from the lower end of the recharge pipe main body, and the solid material held in the recharge pipe main body is filled in the ruppo.
  • the solid material can fall along the curved or straight line of the recharge pipe main body and spread along the outside (for example, in a taper shape), and the solid material is smoothly filled without clogging or stagnation. it can. It is also very easy to take in and take out to single crystal manufacturing equipment.
  • the recharge pipe main body is tapered toward the lower end and spreads at an angle of 0.5 to 5.0 °.
  • the angle of the taper is less than 0.5 °, the solid raw material, particularly the nugget-shaped raw material, is not preferable because it becomes clogged or stagnated. If the angle is larger than 5.0 °, the outer diameter of the taper tip of the stone tube becomes too large, which is not preferable. When the angle of the taper portion is 1.0 to 2.0 °, the effect of uniformly filling the solid raw material and the securing of an appropriate outer diameter can both be achieved, which is more preferable.
  • both the recharge tube main body and the conical valve are made of high-purity transparent quartz glass.
  • both the recharge tube body and the conical valve are made of high-purity transparent quartz glass, It is possible to prevent contamination of the bulk material that comes into contact with the inner surface.
  • a flange portion to be supported in the single crystal manufacturing apparatus is integrally attached to the rechargeable tube main body, and the flange portion is made of quartz glass.
  • a flange made of transparent or opaque quartz glass is attached to the recharge tube body at an appropriate position by welding or the like.
  • the position of the support ring (support base) detachably mounted in the single crystal manufacturing equipment can be used between the recharge pipe that supports the flange and fills the solid raw material with the rutupo. The optimal distance can be maintained. Further, when welding the flange portion, it is more preferable to integrate the entire periphery by welding so that the solid raw material can be supported even if it has a high weight.
  • a guide is provided for fitting the inner surface of the recharge tube main body to fix the lid, and the guide and the stopper are made of tetrafluoroethylene.
  • the lid By making the guide and stopper made of tetrafluoroethylene, the lid can be attached in close contact with the main body of the rechargeable pipe, and foreign matter such as dust in the work room can enter inside the main body of the recharge pipe from above. Can be prevented.
  • the diameter of the main body of the recharge tube is 25 to 60% of the diameter of the truss.
  • the diameter (outer diameter) of the recharge tube main body By setting the diameter (outer diameter) of the recharge tube main body to 25 to 60% of the diameter (outer diameter) of the quartz tube, it is easy to handle, and a recharge tube capable of uniformly and efficiently filling solid raw materials can be obtained. can get.
  • the diameter of the main body of the recharge tube is smaller than 25% of the diameter of the quartz tube, the amount of solid raw material that can be held by the main body of the recharge tube at one time is not preferable.
  • it is larger than 60% the space between the outer periphery of the recharge pipe and the inner periphery of the stone pipe becomes narrow, and the space for charging the raw material becomes small, which is not preferable.
  • a grown single crystal is taken out of a single crystal manufacturing apparatus, and the recharge tube holding the solid raw material is placed in the single crystal manufacturing apparatus.
  • the solid material in the recharge tube is introduced into the crystal manufacturing equipment and solidified by lowering the heating power of the heater after the entire surface of the residual melt in the rutu is solidified, and then increasing the heating power of the heater on the solidified surface.
  • all the solid-state raw materials in the rutupo are melted, and single crystal growth is performed again to grow a plurality of single crystals, thereby forming a single crystal.
  • the heating power (solidification power) of the heater when solidifying the melt surface remaining in the quartz crucible after growing the single crystal is 40 to 40% of the power (melting power) when the raw material is melted. It is about 70%, and after heating the entire surface of the melt, the heating power is raised all at once to the melting point, preventing the solidification from proceeding excessively, reducing the damage to the inner surface of the quartz tube, and peeling
  • the phenomenon that dislocations are generated in the single crystal due to the crushed quartz chips and polycrystallized can be reduced. By this operation, dislocation-free single crystals can be produced safely and efficiently.
  • the recharge tube when the solid material is filled by the recharge tube, the recharge tube is supported by a metal support ring (support table) detachably provided in the single crystal manufacturing apparatus, and solidified. After bringing the melt surface in contact with the conical valve at the distal end portion of the recycle pipe by raising the rotopo, it is preferable to fill the solid raw material by lowering the rotopo.
  • the support ring can be made of the same quartz glass as the recharge tube main body, it is easily broken or cracked, and the metal (for example, stainless steel) has sufficient strength to support the rechargeable tube main body. Is obtained.
  • the support ring be detachable in the single crystal manufacturing apparatus, because maintenance and repair in the event of breakage or a change in the diameter of the reticle tube body are facilitated.
  • the flange portion of the recharge tube rests on the support ring provided in this manner, and the recharge tube stops. further Raise the solidified melt surface to contact the conical valve at the tip of the refill pipe by raising the quartz loop, loosen the load that suspends the wire of the recharge pipe, and lower the quartz loop. As a result, the solid raw material in the refill tube is smoothly filled on the solidified surface in the quartz tube.
  • the solid raw material is additionally charged by repeating the operation of charging the solid raw material with the use of the refill pipe a plurality of times.
  • FIG. 1 is a schematic cross-sectional view showing a solid raw material pipe 20 of the present invention
  • FIG. 2 is a view showing a state where a polycrystalline raw material is filled in a quartz tube using the polycrystalline raw material recharging apparatus of the present invention.
  • Fig. 3 is a schematic cross-sectional view showing a state in which a quartz reticule is filled with a polycrystalline raw material using a recharge device having a different conical valve.
  • Figure 4 is a schematic cross-sectional view showing a conical valve filling a polycrystalline raw material into a quartz tube using a different recharging device.
  • FIG. 5 is a schematic cross-sectional view showing a state where a polycrystalline raw material is filled in a quartz rupture using a recharge device without a stopper.
  • the recharge tube 20 has a solid polycrystalline silicon inside.
  • Tube 2 1 (recharge tube body) for holding raw material, conical valve 22 detachable at the lower end of quartz tube 21, and detachable at the upper end of quartz tube 21
  • a lid 23 that is provided so as to seal the solid material in the quartz tube 21 and a guide 24 that fits on the inner surface of the quartz tube 21 and fixes the lid 23 to the quartz tube 21
  • a hook 26 for suspending the quartz tube 21 from the pulling wire of the silicon single crystal manufacturing device 10
  • a stainless steel recharge tube wire 27 connecting the hook 26 to the conical valve 22
  • a stopper 25 is provided at the center of the tube 23 so that the discharge tube wire 27 passes through the approximate center of the quartz tube 21 and a quartz tube in the silicon single crystal manufacturing apparatus 10 21 is provided with a flange portion 28 for supporting the same.
  • the quartz tube 21 is made of high-purity transparent quartz glass, and has a tapered portion 21a that widens toward the lower end.
  • the length L2 of the tapered portion 21a is preferably about 20 to 40% of the total length L1 of the recharge tube 20.
  • the angle ⁇ 1 to be attached to the taper portion is preferably 0.5 to 5.0 °, more preferably 0.5 to 3.0 °.
  • the angle ⁇ 1 of the tapered portion 21a is smaller than 0.5 °, the solid raw material, in particular, the nugget raw material is undesirably clogged or clogged.
  • the angle ⁇ 1 of the tapered portion 2 la is larger than 5.0 °, the outer diameter at the tip of the tapered portion 21 a of the quartz tube 21 increases, and the support ring 1 attached to the single crystal manufacturing apparatus 10 In order to escape 2d, the diameter of the quartz tube 21 will inevitably be reduced, and the internal volume of the quartz tube 21 will have to be reduced, and the solid material will be less filled, which is preferable. Absent.
  • the angle ⁇ 1 of the tapered portion 21 a is increased, the flange 28 must necessarily have a larger protrusion from the quartz tube 21. A large flange is required, and the production of the recycle pipe 20 becomes complicated. Furthermore, if the angle ⁇ 1 of the tapered portion 2 la is greater than 3.0 °, the production cost of the quartz tube 21 is high, but the clogging and stagnation of the solid raw material is smaller than in the case of less than that. Not so effective No improvement can be expected. When the angle ⁇ 1 of the tapered portion 21a is 1.0 to 2.0 °, clogging and stagnation of the solid-shaped material can be effectively prevented, and the inner volume is reduced and the production cost is reduced as much as possible. It becomes possible. In consideration of such points, in the present embodiment, the length L2 of the tapered portion 21a is about 30% of the total length L1 of the recharge tube, and the angle ⁇ 1 is 1.15 °.
  • an example of the purity of the transparent quartz glass, which is the material of the recharge tube 20 is as follows: 81 is 14 111 (parts per million by weight, the same applies hereinafter), ⁇ & is 0.4 ppm, (11 is 0.0 5 ppm or less, 6 is 0.2 ppm, K and Li are 0.6 ppm each, Na is 0.7 ppm, Ding is 1.l ppm, and OH is 5 ppm or less It is needless to say that the purity is preferably smaller than the above-mentioned value, and the physical properties are, for example, a density of 2.2 ⁇ 10 3 kg / m 3 , a tensile strength of 4.9 ⁇ 10 r, kg f / m 2 (4. 80 X 10 7 P a), the compressive strength is 1. lxl 0 8 kg ⁇ / m 2 (1. 08 X 10 9 P a), a softening point of 1 683.C.
  • the diameter (outer diameter) R1 of the quartz tube 21 is designed to be 25 to 60% of the diameter (outer diameter) R11 of the quartz tube 11a. If it is less than 25%, the amount of the solid raw material that the quartz tube 21 can hold at a time decreases, and in this case, recharging may be repeated, but the number of times of recharging is increased, which is not preferable. If it is larger than 60%, the solid raw material may be filled left and right, and the space between the outer circumference of the quartz tube 21 and the inner circumference of the quartz tube 11a will be narrowed, and the solid raw material will be charged. This is not preferable because the space used for the operation becomes small.
  • the diameter R11 of the stone crucible 11a is 24 inches (0.6096m)
  • the diameter R1 of the quartz tube 21 is 40%, 9.6 inches (0%). 2438m).
  • the conical valve 22 is made of high-purity transparent quartz glass.
  • the quartz tube 21 is filled with a solid material in a state where the conical valve 22 is attached to the lower end of the quartz tube 21 and closed.
  • the angle ⁇ 2 between the generatrix of the peripheral surface 22a of the conical valve 22 and the bottom surface 22b is preferably set to 40 to 70 °. If the angle ⁇ 2 is smaller than 40 °, as shown in FIG.
  • the angle ⁇ 2 of the conical valve 22 is 54 °.
  • the solid raw material can be smoothly and uniformly filled in the quartz tube 11a.
  • the symbol L 3 indicates the total height of the conical valve 22.
  • the guide 24 is made of tetrafluoroethylene, and is integrally attached to the back of the lid 23 with a screw 24a as shown in FIG.
  • the guide 24 attaches the quartz tube 21 and the lid 23 in close contact.
  • the guide 24 may be fixed to the upper end of the quartz tube 21 with screws or the like.
  • the stopper 25 is made of tetrafluoroethylene, and is attached so that the recharge tube wire 27 passes substantially through the center.
  • the stopper 25 and the recharge tube wire 27 are moved along a notch (not shown) extending from one location on the circumference of the lid 23 to the center, and are fixed to the approximate center of ⁇ 23.
  • the rectilinear pipe wire 27 is positioned so as to substantially pass through the center of the quartz tube 21.
  • the recharge tube 20 will roll and the isolation valve 13 (The silicon single crystal manufacturing equipment 10 will be used to remove the silicon single crystal from the pull chamber 12 and the quartz tube. And a main chamber 11 including a crystal growth furnace 11b centered on 11a. Can be blocked (see Figure 5).
  • the stopper 25 By attaching the stopper 25 to almost the center of the recharge pipe 20, the recharge pipe 20 does not roll, does not lose its balance, and is prevented from falling down by inclining. Quartz roots 1 1a are evenly filled.
  • the flange 28 is made of quartz glass, and as shown in Fig. 2, an optimal distance P between the quartz tube 21 and the quartz tube 11a for uniformly filling the solid material is maintained. In addition, the entire circumference is integrated by welding at an appropriate position to support high weight.
  • the raw material is held in the recharge pipe 20.
  • nugget-like raw materials with high purity and high dissolution rate are often used as raw materials, but when growing silicon single crystals that do not require purity, inexpensive granular raw materials are appropriately mixed with nugget-like raw materials. In some cases, only granular raw materials are present in some cases. There are cases where only the nugget-shaped raw material, the nugget-shaped raw material, the granular raw material, and the granular raw material alone are used, but each is called a solid raw material.
  • the recharge tube 20 holding the solid raw material is introduced into the silicon single crystal manufacturing apparatus 10.
  • the isolation valve 13 is closed, and the interior of the main chamber 11 is isolated from the atmosphere.
  • the recharge tube 20 enters the silicon single crystal manufacturing equipment 10
  • the air in the pull chamber 11 is exhausted, and the recharge tube 20 can be inserted into the main champer 11 with the air shut off.
  • a support ring 12 d is provided above the isolation valve 13 in the silicon single crystal manufacturing apparatus 10, and the flange portion 28 of the recharge pipe 20 is placed on the support ring 12 d And a solid raw material can be charged.
  • the silicon melt (residual melt) remaining in the quartz tube 1a is solidified only on the surface, and the solidified surface A is filled with the raw material.
  • the solid raw material can be filled in the most preferable state when the conical valve 22 is in contact with the solidified surface A, and the solid raw material can be more smoothly reduced by lowering the stone root. Is filled.
  • the entire surface of the residual melt in the quartz tube 11a is taken out of the silicon single crystal manufacturing apparatus 10 from the grown silicon single crystal, and the lithium tube 20 holding the solid raw material is removed.
  • the solidification is achieved by reducing the heating power of the heat source to about 50% of the power (melting power) at the time of melting the raw material while being taken into the silicon single crystal manufacturing apparatus 10.
  • the heating power is increased to the melting power at once after the entire surface of the residual melt has solidified, thereby preventing excessive solidification.
  • damage to the inner surface of the stone crucible 11a can be reduced, and the phenomenon that dislocations are generated in the single crystal due to the peeled quartz chips and polycrystallized can be reduced. By this operation, a dislocation-free single crystal can be manufactured safely and efficiently.
  • the recharge tube wire 27 is wound up, the conical valve 22 is accommodated in the lower end of the quartz tube 21, and the recharge tube 20 can be taken out.
  • 100 kg of polycrystalline raw material is charged into a 22 inch (55.88 cm) diameter quartz truss 11a, and the heating power (melting power) of the heater is set to 150 kW to produce the polycrystalline raw material.
  • a silicon single crystal having a diameter of 8 inches (20.34 cm) and a mass of 80 kg was grown and taken out of the silicon single crystal manufacturing apparatus 10.
  • the recycle tube 20 holding the nugget-like raw material 40 kg is taken into the silicon single crystal manufacturing apparatus 10, and the flange portion 28 of the recharge tube 20 is placed on the support ring 12 d and stopped. During this operation, the heating power (solidification power) of the heater was reduced to 90 kW.
  • the surface of the residual melt solidifies, and immediately after almost the entire surface has solidified, heating The power was increased to the melting power.
  • the quartz root 11a since the quartz root 11a is located below, the quartz root 11a is raised to bring the solidified surface A into contact with the conical valve 22 of the recharge pipe 20, and the solidified surface A and the cone are formed.
  • the load on the suspended recharge tube wire 27 is loosened, and the nugget-like material in the recharge tube 20 is solidified on the surface A by lowering the quartz tube 11 a. Gradually put in.
  • the recharge tube wire 27 is wound up, the conical valve 22 is accommodated in the lower end of the quartz tube 21, and the recharge tube 20 is moved from the silicon single crystal manufacturing apparatus 10. I took it out.
  • the recharge tube 20 holding the nugget-like raw material 40 kg is introduced into the silicon single crystal manufacturing equipment 10 again, and the unmelted raw material is filled with the nugget-like raw material in the same manner as described above. The same amount of 10 O kg of raw material was used.
  • Example and Comparative Example 1 From the results of Example and Comparative Example 1, the surface of the residual melt solidified, and almost the entire surface was solidified. Immediately after the heating, the heating power was increased to the melting power, which shows that dislocation-free silicon single crystals can be produced safely and efficiently.
  • the nugget-like raw material penetrates through the solidified surface A to disperse the melt, and the water droplets scattered on the upper part of the inner surface of the quartz root 11a may adhere and solidify.
  • the solidified part becomes small projections, and silicon oxide evaporating from the surface of the molten metal precipitates, and becomes oxide debris, falls on the surface of the molten metal, and drifts on the surface of the melt to form a silicon single crystal growing. It is considered that the silicon single crystal was attached and turned into dislocations.
  • Example and Comparative Example 2 From the results of Example and Comparative Example 2, no dislocation was caused by gradually charging the nugget-like raw material in the recharge tube 20 onto the solidified surface A while the solidified surface A was in contact with the conical valve 22. It can be seen that the silicon single crystal can be safely and efficiently produced.
  • a solid raw material when filling a solid raw material into a quartz tube 11a in which a silicon single crystal is grown and a silicon melt is reduced, a solid raw material is placed in a recycle tube 20.
  • the quartz tube 11a can be smoothly filled with the solid raw material by taking the recycle tube 20 into the silicon single crystal manufacturing apparatus 10 and taking it out easily. Thus, a plurality of silicon single crystals can be grown from one quartz root.
  • the present invention is not limited to the above embodiment.
  • the above embodiment is an exemplification, and is substantially the same as the technical idea described in the claims of the present invention. Anything having the structure and exhibiting the same function and effect is included in the technical scope of the present invention.
  • the present invention can be applied to, for example, the MCZ method. That is, it is needless to say that the method is also effective in the MCZ method, and the diameter, length, and the like of the quartz tube 21 can be selected at any time, and the present invention is not limited to this.
  • the present invention it is possible to easily take in and take out a recharge pipe into a single crystal apparatus without attaching the conventional raw material supply apparatus, and furthermore, to feed a nugget raw material smoothly and efficiently into a crucible, Further, it is possible to provide a recharge tube capable of preventing contamination of the filled polycrystalline material. Therefore, a supply rate suitable for recharging is realized, and single-crystal productivity can be improved by performing recharging smoothly and efficiently in a short time, and a recharge tube for inexpensive solid polycrystalline raw material and its recharge A method for producing a single crystal capable of safely and efficiently producing a dislocation-free single crystal using a tube can be provided. Therefore, the solid polycrystalline raw material recharge tube of the present invention and the method for producing a single crystal using the same are particularly suitable for producing a single crystal using the solid polycrystalline raw material.

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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)

Abstract

La présente invention concerne, d'une part un tube de recharge bon marché pour matériau polycristallin solide permettant d'augmenter la productivité du monocristal, et d'autre part un procédé de production de monocristal utilisant ce tuyau. Ce tube de recharge, qui est installé amovible dans le dispositif de production de monocristal disposant d'un creuset contenant le liquide fondu du cristal, est intérieurement pourvu d'un corps principal de tube de recharge sensiblement cylindrique destiné à contenir un matériau polycristallin solide, le corps principal de tube de recharge s'évasant graduellement vers l'extrémité inférieure. Le tube de recharge est en outre équipé, non seulement d'une valve conique disposée à l'extrémité inférieure du corps principal de tube de recharge, ainsi que d'un couvercle disposé amovible à l'extrémité supérieure du corps principal de tube de recharge, et d'un crochet, mais également d'un fil de tirage de tube de recharge allant du crochet à la valve conique, et enfin d'une butée permettant de positionner le tube de recharge de façon qu'il passe sensiblement par le centre du corps principal de tube de recharge.
PCT/JP2002/001796 2001-02-28 2002-02-27 Tube de recharge pour matériau polycristallin solide, et procédé de production de monocristal au moyen de ce tube WO2002068732A1 (fr)

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JP2002568821A JP4103593B2 (ja) 2001-02-28 2002-02-27 固形状多結晶原料のリチャージ管及びそれを用いた単結晶の製造方法

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JP2001055668 2001-02-28
JP2001-55668 2001-02-28

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Cited By (23)

* Cited by examiner, † Cited by third party
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WO2005007941A1 (fr) * 2003-07-18 2005-01-27 Jianzhong Yuan Appareil et procede de recharge de matiere premiere
JP2007217224A (ja) * 2006-02-16 2007-08-30 Sumco Corp 単結晶製造装置
JP2007246356A (ja) * 2006-03-17 2007-09-27 Toshiba Ceramics Co Ltd 固形状原料のリチャージ方法
US7311772B2 (en) 2004-09-21 2007-12-25 Sumco Corporation Apparatus and method for supplying raw material in Czochralski method
JP2008037745A (ja) * 2006-08-02 2008-02-21 Siltron Inc 単結晶成長装置に固体原料を供給する装置及び方法
JP2008087998A (ja) * 2006-09-29 2008-04-17 Ｓｕｍｃｏ Ｔｅｃｈｘｉｖ株式会社 原料供給装置及び原料供給方法
JP2008088001A (ja) * 2006-09-29 2008-04-17 Ｓｕｍｃｏ Ｔｅｃｈｘｉｖ株式会社 原料供給装置
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