WO2005035838A1 - Procede et appareil pour la production de monocristal, et monocristal - Google Patents

Procede et appareil pour la production de monocristal, et monocristal Download PDF

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Publication number
WO2005035838A1
WO2005035838A1 PCT/JP2004/014726 JP2004014726W WO2005035838A1 WO 2005035838 A1 WO2005035838 A1 WO 2005035838A1 JP 2004014726 W JP2004014726 W JP 2004014726W WO 2005035838 A1 WO2005035838 A1 WO 2005035838A1
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Prior art keywords
single crystal
cooling cylinder
forced cooling
producing
raw material
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PCT/JP2004/014726
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English (en)
Japanese (ja)
Inventor
Tatsuo Mori
Kouji Mizuishi
Izumi Fusegawa
Hirotoshi Yamagishi
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Shin-Etsu Handotai Co., Ltd.
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Application filed by Shin-Etsu Handotai Co., Ltd. filed Critical Shin-Etsu Handotai Co., Ltd.
Publication of WO2005035838A1 publication Critical patent/WO2005035838A1/fr

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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
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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

Definitions

  • the present invention relates to a single crystal manufacturing method and a single crystal manufacturing apparatus used for manufacturing a silicon single crystal by the Czochralski method and the like.
  • a single crystal used as a substrate of a semiconductor device includes, for example, a silicon single crystal and the like, and is mainly manufactured by a Czochralski method (hereinafter abbreviated as CZ method).
  • CZ method Czochralski method
  • FPD FloW Pattern Defect
  • COP Crystal Originated Particle
  • an OSF Oxidation Induced Stacking Fault
  • the OSF ring shrinks to the center of the wafer and disappears.
  • LSEPD Large Secco Etch Pit Defect
  • LFPD Large Flow Pattern Defect
  • a Cu deposition defect region there is a region where defects detected by the Cu deposition process are remarkably generated (hereinafter referred to as a Cu deposition defect region) in a part of the Nv region where oxygen precipitation is likely to occur after the thermal oxidation process. It has been found that this causes deterioration of electric characteristics such as breakdown voltage characteristics of the oxide film.
  • the concentration at which these grown-in defects are introduced into the single crystal depends on the pulling speed V (mmZmin) of the silicon single crystal when pulling the silicon single crystal by the CZ method, and the bow I near the crystal growth interface. It is known that the relationship with the crystal temperature gradient G (° C / mm) depends on the VZG force.
  • V pulling speed
  • the pulling speed of the single crystal must be 0.5 mmZmin or less to pull up the crystal straight body, and the single crystal in the V region When pulling, the pulling speed must be significantly lower than the general pulling speed of 1.0 mmZmin.
  • the pulling speed at the end of the growth of the single crystal straight body portion has an influence on the pulling speed and the pulling time of the single crystal in the rounding step performed thereafter to form the single crystal tail. Therefore, as described above, when the pulling speed at the end of the growth of the straight body part is low, the pulling speed in the rounding process is also low, and the pulling time is further prolonged. There has been a problem in that the manufacturing cost has risen due to the reduction.
  • a rectifying cooling cylinder with a dual structure of powerful internal cooling cylinders is provided, and the heat generated in the internal cooling cylinders is transferred to the outside by the external cooling cylinders, thereby suppressing the rise in temperature of the internal cooling cylinders and cooling efficiency of crystals.
  • a cooling medium such as water to cool a growing single crystal more effectively has been disclosed.
  • a cooling duct through which a liquid refrigerant flows is passed through a main chamber, and a cooling duct made of a material having a high thermal conductivity such as silver is placed under the cooling duct.
  • a member is provided, and the heat released from the crystal surface is quickly transferred to the outside to effectively cool the single crystal.
  • a cooling cylinder formed of copper or a metal having higher thermal conductivity than copper is provided at least in the vicinity of the crystal growth interface so as to surround the single crystal being pulled.
  • a single crystal growing apparatus that grows a single crystal while arranging and passing a cooling medium through the cooling cylinder to forcibly cool the vicinity of a crystal growth interface.
  • an object of the present invention is to provide an effect of cooling a single crystal when producing a single crystal by raising the raw material melt power by the CZ method.
  • the single crystal being pulled over the raw material melt is surrounded.
  • a forced cooling cylinder having a thermal conductivity of 300 WZm'K or more and a material force is installed, and a cooling medium is supplied to the forced cooling cylinder to pull up the single crystal while cooling the single crystal.
  • a method for producing a single crystal characterized in that the thermal stress generated during the cooling is controlled to be equal to or lower than the yield stress of the forced cooling cylinder.
  • a forced cooling cylinder made of a material having a thermal conductivity of 300 WZm'K or more, for example, copper, oxygen-free copper, gold, or silver is installed on the raw material melt, and the cooling medium is supplied to the forced cooling cylinder.
  • the thermal stress generated in the forced cooling cylinder to be equal to or lower than the yield stress of the forced cooling cylinder when pulling while supplying and cooling the single crystal, the single crystal is effectively cooled by the forced cooling cylinder. It is possible to pull up a single crystal of the desired quality with high productivity without plastic deformation of the forced cooling cylinder and metal contamination while cooling at a high speed in the desired defect area. It can be manufactured stably and with high safety.
  • the forced cooling cylinder also has a copper force.
  • the forced cooling cylinder also has an oxygen-free copper force.
  • the forced cooling cylinder is made of copper, especially oxygen-free copper, the thermal conductivity is high, so that the heat absorbed by the forced cooling cylinder can be quickly transmitted to the cooling medium. Therefore, a high cooling effect can be stably obtained. Also, these metals are mechanical Because of its high strength and excellent heat resistance, it can withstand high temperatures in the chamber sufficiently, does not easily deform or deteriorate, and can be used safely for a long time.
  • Oxygen-free copper is generally copper whose purity is higher than that of copper containing impurities such as cuprous oxide, which is about 9.96% or more, and whose oxygen content is lOppm or less. Say.
  • the forced cooling cylinder is subjected to a surface treatment so that the emissivity of the surface of the cooling cylinder becomes 0.2 or more and 1.0 or less to control thermal stress generated in the forced cooling cylinder.
  • the forced cooling cylinder is preferably subjected to surface treatment using nickel plating, nickel spraying, chromia spraying, titania spraying, alumina spraying, or yttria spraying.
  • the forced cooling cylinder is generated during pulling of the single crystal. Since it is possible to easily control the thermal stress to be applied to be equal to or lower than the yield stress of the forced cooling cylinder, it is possible to stably produce a single crystal without plastically deforming the forced cooling cylinder. Also, in this case, by using nickel plating, nickel spraying, chromia spraying, titania spraying, alumina spraying, or Italy spraying, the surface treatment of the forced cooling cylinder can be easily performed, and the heat transfer characteristics can be improved. More desirable.
  • the thermal stress generated in the forced cooling cylinder can also be reduced by changing the thickness and the Z or length of the heat conducting section while the cooling medium in the forced cooling cylinder does not circulate. Since it is possible to easily control the stress to be equal to or less than the stress, it is possible to stably produce a single crystal without plastically deforming the forced cooling cylinder.
  • the temperature of the forefront portion of the forced cooling cylinder on the raw material melt side can be set to 200 ° C. or less.
  • the temperature of the leading end of the forced cooling cylinder on the side of the raw material melt can be reduced to 200 ° C. or less during the pulling of the single crystal, whereby the single crystal can be grown at high speed.
  • the forced cooling cylinder is not plastically deformed during the pulling of the single crystal, and metal contamination of the single crystal can be reliably prevented. Can be manufactured.
  • the temperature gradient of the heat conducting portion can be set to 1 l ° C / cm or less while the cooling medium in the forced cooling cylinder does not flow.
  • the thermal stress generated in the forced cooling cylinder can be extremely reduced.
  • the single crystal can be grown extremely stably and with high safety without causing plastic deformation, and can withstand the production of the single crystal for a long time.
  • a single crystal manufactured by the method for manufacturing a single crystal is provided.
  • the single crystal manufactured according to the present invention is a single crystal manufactured at high cost and low cost as compared with the conventional single crystal, and has a desired defect region and is extremely high in quality without metal contamination. Of a single crystal.
  • an apparatus for producing a single crystal by pulling it from the raw material melt by the Czochralski method at least a crucible containing the raw material melt and a heater for heating the raw material melt
  • a forced cooling cylinder for cooling the single crystal being pulled a main chamber for storing the crucible, a heater, and a forced cooling cylinder, and a pulling chamber for containing the single crystal pulled from the raw material melt.
  • the forced cooling cylinder has a thermal conductivity of 300 WZm'K or more, and the thermal stress generated in the forced cooling cylinder when pulling up the single crystal is not more than the yield stress of the forced cooling cylinder.
  • the material having a thermal conductivity of 300 WZm'K or more includes, for example, copper, oxygen-free copper, gold, silver, and the like.
  • the forced cooling cylinder also has a copper force, and it is particularly preferable that the forced cooling cylinder force is an oxygen-free copper force.
  • the forced cooling cylinder force is an oxygen-free copper force.
  • the forced cooling cylinder has been subjected to a surface treatment so that the emissivity of the surface is 0.2 or more and 1.0 or less.
  • the thermal stress generated in the forced cooling cylinder during single crystal growth is reduced. Since the yield stress can be controlled to be equal to or less than the yield stress, the apparatus can stably produce a single crystal without plastically deforming the forced cooling cylinder.
  • the forced cooling cylinder extends to the heat-removing section through which the cooling medium flows, and extends toward the raw material melt from the heat-removing section, so that the cooling medium does not flow. It is also preferable that the heat-removing part and the heat-conducting part are formed of a body, which also acts as a heat-conducting part.
  • the single crystal can be rapidly cooled in the vicinity of the crystal growth interface during pulling of the single crystal, and the single crystal can be rapidly cooled from the crystal growth interface. As the distance increases, the cooling effect of the single crystal is further enhanced, so that a configuration having excellent crystal cooling ability can be obtained.
  • the heat removal part and the heat conduction part are integrated, a desired cooling atmosphere can be continuously and stably formed in the crystal growth axis direction. In some cases, it is possible to avoid the concentration of thermal stress, especially at the joint. Therefore, the single crystal during growth can be efficiently cooled, and a single crystal manufacturing apparatus capable of manufacturing a single crystal having a desired defect region at high speed and very stably can be obtained.
  • the forced cooling cylinder may have a tapered shape in which the thickness of the heat conduction portion decreases toward the raw material melt, or the thickness of the heat conduction portion may be uniform and the thickness of the heat removal portion may be reduced. It is preferable to have a thin fin shape.
  • the forced cooling cylinder has a tapered shape or a fin shape, it is possible to increase the space extending to the tip of the forced cooling cylinder.
  • a heat insulating member or the like can be easily installed at the end of the cylinder without obstructing the growth of the single crystal, and the radiant heat of the raw material melt can be effectively shielded.
  • the thickness of the distal end of the heat conduction part of the forced cooling cylinder is 50% or more of the thickness of the heat removal part.
  • the thickness of the tip of the heat conducting portion of the forced cooling cylinder is 50% or more of the thickness of the heat removing portion, a high cooling effect can be maintained, and thus the single crystal can be formed in a desired defect region.
  • a cooling atmosphere capable of growing the water can be easily and stably formed.
  • the single crystal can be effectively cooled by the forced cooling cylinder by the CZ method and pulled up at a desired defect region at a high speed. It is possible to produce a high-quality single crystal having a desired defect region without deformation or metal contamination, with high stability, high productivity, and high safety. .
  • FIG. 1 is a schematic configuration diagram showing one example of an apparatus for producing a single crystal of the present invention.
  • FIG. 2 is a schematic configuration diagram schematically showing a shape of a forced cooling cylinder installed in the apparatus for producing a single crystal of the present invention.
  • FIG. 3 is a graph showing the relationship between the surface emissivity of a forced cooling cylinder and the temperature at the tip of a heat conducting part.
  • FIG. 4 is a graph showing the relationship between the surface emissivity of a forced cooling cylinder and the thermal stress generated in the forced cooling cylinder.
  • FIG. 5 is a graph showing the relationship between the thickness of the tip portion of the heat conducting portion of the forced cooling cylinder and the temperature of the tip portion of the heat conducting portion.
  • FIG. 6 is a graph showing the relationship between the length of the heat conducting portion of the forced cooling cylinder and the temperature at the tip of the heat conducting portion.
  • FIG. 7 is an explanatory diagram showing a relationship between VZG and crystal defect distribution.
  • FIG. 8 is a graph showing the result of a simulation analysis of the relationship between the thermal conductivity of the forced cooling cylinder and the crystal temperature gradient at the center of the single crystal.
  • the present inventors have solved the above-mentioned conventional problems and can pull up a single crystal at a desired defect region at a high speed.
  • the thermal stress generated in the forced cooling cylinder when pulling up while cooling the single crystal should be controlled to be equal to or lower than the yield stress of the forced cooling cylinder.
  • the present inventors have found that it is sufficient to complete the present invention.
  • FIG. 1 is a schematic configuration diagram illustrating an example of a single crystal manufacturing apparatus of the present invention
  • FIG. 2 is a schematic diagram illustrating a shape of a forced cooling cylinder installed in the single crystal manufacturing apparatus of the present invention. It is a schematic diagram.
  • the apparatus 20 for producing a single crystal of the present invention shown in FIG. 1 includes crucibles 5 and 6 containing a raw material melt, for example, a polycrystalline silicon melt 4, and a heater for heating and melting the polycrystalline silicon raw material. 7.
  • a forced cooling cylinder 11 for cooling the single crystal 3 being pulled is housed in the main chamber 1.
  • a pulling chamber 2 for accommodating and removing the grown single crystal 3 is connected to the upper part of the main chamber 1, and the single crystal 3 is pulled above the pulling chamber 2.
  • a pulling mechanism (not shown) for pulling while rotating with the wire 16 is provided.
  • the crucible is composed of a quartz crucible 5 for directly containing the raw material melt 4 inside, and a graphite crucible 6 for supporting the quartz crucible 5 on the outside.
  • the crucibles 5 and 6 are supported on a crucible rotation shaft 19 that can rotate and move up and down by a rotation drive mechanism (not shown) attached to the lower part of the single crystal manufacturing apparatus 20.
  • a rotation drive mechanism (not shown) attached to the lower part of the single crystal manufacturing apparatus 20.
  • the melt is rotated in the direction opposite to the rotation of the single crystal and the melt is pulled as the single crystal 3 is pulled up. Raise crucibles 5 and 6 by the reduced amount.
  • the heater 7 is arranged so as to surround the crucibles 5 and 6. Outside the heater 7, the heat from the heater 7 is prevented from being directly radiated to the main chamber 1.
  • a heat insulation member 8 is provided so as to surround the periphery of the heater.
  • an inert gas such as an argon gas is provided through the gas inlet 10 provided in the upper part of the pulling chamber 2 for the purpose of discharging the reaction gas generated in the furnace outside the furnace. The gas is introduced, passes through the upper part of the single crystal 3 being pulled and the upper part of the raw material melt 4, and is discharged from the gas outlet 9.
  • the main chamber 1 and the pull-up chamber 2 are made of a metal having excellent heat resistance and rigidity such as stainless steel, and the walls of the chambers 1 and 2 have a double structure, and a cooling medium such as water is returned to the gap between the chambers.
  • a cooling medium such as water
  • the forced cooling cylinder 11 installed on the raw material melt 4 so as to surround the single crystal 3 has a cylindrical or conical shape, and a cooling medium is introduced from a cooling medium inlet 12.
  • the forced cooling cylinder 11 has a structure in which the single crystal is forcibly cooled by supplying a cooling medium to the forced cooling cylinder 11.
  • the cooling medium to be supplied to the forced cooling cylinder 11 it is preferable to use water from the viewpoints of ease of handling, cost, etc., in addition to the power cooling characteristics that can use the liquid or gas conventionally used as the cooling medium. It is. Further, by adjusting the flow rate and temperature of the cooling medium flowing into these cooling cylinders as needed, the heat removal amount of the forced cooling cylinder can be controlled.
  • the forced cooling cylinder 11 In such a single crystal manufacturing apparatus 20 of the present invention, the forced cooling cylinder 11 However, the material strength becomes 300 WZm'K or more, and the thermal stress generated in the forced cooling cylinder 11 when pulling a single crystal is equal to or lower than the yield stress of the forced cooling cylinder 11.
  • the thermal conductivity of the forced cooling cylinder 11 is less than 300 WZm′K
  • the heat absorbed in the cooling cylinder does not flow quickly to the cooling medium, so that a sufficient cooling effect cannot be obtained and the single crystal
  • the productivity is lowered in the manufacture of the semiconductor device, and it is difficult to form a desired cooling atmosphere, so that it may not be possible to pull up a single crystal in a desired defect region.
  • the relationship between the thermal conductivity of the forced cooling cylinder and the crystal temperature gradient at the center of the single crystal to be grown was calculated using the comprehensive heat transfer analysis software FEMAG (F. Dupret et al .; Int. J. Heat Mass Transfer , 33, 1849 (1990)).
  • a forced cooling cylinder having a thermal conductivity of 300 WZm′K or more is used as the forced cooling cylinder.
  • Examples of the material of such a forced cooling cylinder 11 include copper, oxygen-free copper, and gold.
  • the thermal conductivity of copper is about 400 WZm'K, and if the forced cooling cylinder 11 is made to have a material strength of 300 WZm * K or more, radiant heat from the single crystal during pulling can be reduced. Since it can be absorbed by the forced cooling cylinder and quickly transferred to the cooling medium and transferred to the outside, a very excellent cooling effect can be obtained, and a single crystal can be grown in a desired defect region. Preferably, a cooling atmosphere can be easily formed.
  • the thermal conductivity of oxygen-free copper is as high as about 400 WZm'K.By using a forced cooling cylinder that has a very high oxygen-free copper power, the radiant heat of single crystal power can be efficiently transferred to the outside of the chamber, resulting in an excellent heat removal effect. Can be obtained stably. Furthermore, these metals have high mechanical strength and high heat resistance, so they can withstand high temperatures in the chamber sufficiently and can be used safely for a long time. Further, in the present invention, the forced cooling cylinder 11 is controlled so that the thermal stress generated in the forced cooling cylinder when pulling a single crystal is equal to or lower than the yield stress of the forced cooling cylinder 11. For example, if the forced cooling cylinder 11 is oxygen-free copper power, since the yield stress of the oxygen-free copper is about 4.
  • the thermal stress generated in the forced cooling cylinder can be easily confirmed by performing an experiment or the like in advance.
  • the surface treatment is performed on the forced cooling cylinder to perform the surface treatment. Adjusting the emissivity of the surface of the cooling cylinder, or changing the thickness, Z or length of the heat conducting part of the forced cooling cylinder, raises the forced cooling cylinder installed in the single crystal manufacturing equipment while pulling the single crystal. It is possible to make sure that the thermal stress generated at the time is not more than the yield stress of the forced cooling cylinder.
  • the forced cooling cylinder 11 installed in the single crystal manufacturing apparatus 20 of the present invention includes, as shown in FIG. 2 (a), for example, a heat removal section in which a flow channel 13 for flowing a cooling medium is formed. 14 and a heat conducting part 15 extending from the heat removing part 14 to the raw material melt side and through which the cooling medium does not flow. Further, the heat removing part 14 and the heat conducting part 15 are integrally formed. If the forced cooling cylinder 11 is thus composed of the heat removal part 14 and the heat conduction part 15, the single crystal can be rapidly cooled near the crystal growth interface, and the cooling effect of the single crystal further increases as the distance from the crystal growth interface increases. It will have an excellent crystal cooling capacity of being higher.
  • the heat removal part and the heat conduction part are formed in a body, it is possible to continuously and stably form a desired cooling atmosphere in the crystal growth axis direction, and to join with a forced cooling cylinder. If there is a joint, it is possible to avoid the concentration of thermal stress particularly occurring at the joint.
  • the forced cooling cylinder has, for example, a tapered shape in which the thickness of the heat conducting portion 15 decreases toward the raw material melt as shown in FIG. 2 (b), or as shown in FIG. 2 (c).
  • a fin shape in which the thickness of the heat conducting portion is uniform and smaller than the thickness of the heat removing portion.
  • a heat insulating member (not shown) can be easily installed at the tip of the cooling / cooling cylinder without obstructing the growth of the single crystal, and the radiant heat of the raw material melt power can be effectively shielded. It becomes.
  • the thickness of the distal end of the heat conduction part of the forced cooling cylinder is 50% or more of the thickness of the heat removal part, so that the forced cooling cylinder has a high cooling effect. Can be.
  • the single crystal manufacturing apparatus 20 in which the forced cooling cylinder 11 having a thermal conductivity of 300 WZm * K or more and having a material strength of not less than the raw material melt 4 is used.
  • a silicon melt obtained by melting polycrystalline silicon is stored as a raw material melt 4 in a quartz crucible 5, and a seed crystal 17 fixed in a seed holder 18 is immersed in the silicon melt 4 in the quartz crucible 5.
  • the silicon single crystal 3 having a substantially cylindrical shape can be grown stably at a high speed by gently pulling while rotating through a seed drawing, and is generated in the forced cooling cylinder 11 when the single crystal is pulled. Thermal stress can be controlled to be equal to or lower than the yield stress.
  • the thermal stress generated in the forced cooling cylinder is controlled in advance by performing an experiment or the like, for example, by performing surface treatment on the forced cooling cylinder to adjust the emissivity of the cooling cylinder surface, or It can be easily performed by changing the thickness, Z or length of the heat conduction part of the forced cooling cylinder.
  • the surface emissivity was set as the forced cooling cylinder 11 of the single crystal manufacturing apparatus 20 shown in FIG.
  • the pulling of the single crystal was performed using several types of forced cooling cylinders, and the change in temperature at the tip of the heat conducting part in the forced cooling cylinder 11 and the change in thermal stress generated in the forced cooling cylinder were observed. An experiment was conducted to investigate.
  • the heat conduction part as shown in Fig. 2 (a) has the same thickness (60mm) as the heat removal part, and the length of the heat conduction part is 20cm.
  • Acid-free with a reduced shape Prepare a forced cooling cylinder that also has a copper power, and perform nickel plating, titanium spraying, or chromia spraying on the surface of this forced cooling cylinder to set the surface emissivity to 0.25, 0.5, or 0.8, respectively. Then, a single crystal with a diameter of 300 mm was pulled up, and the temperature at the tip of the heat conducting part and the thermal stress generated in the forced cooling cylinder were measured.
  • FIG 3 is a graph showing the relationship between the emissivity of the forced cooling cylinder surface obtained by measuring the temperature at the tip of the heat conducting part and the temperature at the tip of the heat conducting part.
  • a graph showing the relationship between the emissivity of the cooling cylinder surface obtained by measuring the thermal stress generated in the cylinder and the thermal stress generated in the forced cooling cylinder is shown.
  • the forced cooling cylinder 11 of the single crystal manufacturing apparatus 20 has a fin shape as shown in FIG. 2 (c), the thickness of the heat removal part is 33 mm, the length of the heat conduction part is 10 cm,
  • three types of forced cooling cylinders were prepared, with the thickness of the heat conducting part being 10 mm, 19 mm, and 33 mm, respectively.
  • the one with a heat conducting part thickness of 33 mm has the shape shown in Fig. 2 (a). Become).
  • all of these forced cooling cylinders prepared in Experiment 2 were subjected to surface treatment by chromia spraying so that the surface emissivity was 0.8.
  • a forced cooling cylinder a single crystal with a diameter of 200 mm was pulled, and the temperature at the tip of the heat conducting part was measured at that time.
  • Figure 5 shows the measurement results.
  • the forced cooling cylinder 11 has a tapered shape as shown in FIG. 2 (b) in which the thickness of the heat conducting portion gradually decreases, and the thickness of the heat removing portion is 33 mm.
  • Three types of forced cooling cylinders were prepared, with the length of the heat conducting part being 10 cm and the thickness of the tip of the heat conducting part being 10 mm, 19 mm, and 33 mm, respectively (the thickness of the tip of the heat conducting part was 33 mm Figure 2 (a) Having the shape of These forced cooling cylinders were subjected to surface treatment by chromia spraying in the same manner as described above so that the surface emissivity was 0.8. Using such a forced cooling cylinder, a single crystal with a diameter of 200 mm was pulled, and the temperature at the tip of the heat conducting part was measured at that time. The measurement results are also shown in FIG.
  • the thickness of the heat conducting portion is changed to change the thickness of the forced cooling cylinder during pulling the single crystal. It has been found that the temperature at the tip can be changed. In other words, by changing the thickness of the heat conducting portion of the forced cooling cylinder, the temperature of the tip portion of the heat conducting portion can be lowered, thereby making the forced cooling similar to Experiment 1 described above. Thermal stress generated in the cylinder can be controlled to be small. In addition, the forced cooling cylinder having a tapered shape was able to more effectively lower the temperature at the tip of the heat conducting portion than the forced cooling cylinder having a fin shape.
  • the forced cooling cylinder has a tapered shape or a fin shape as described above, the space that extends to the tip of the heat conducting portion can be increased. Can be easily installed without obstructing the growth of the single crystal, the radiation heat from the raw material melt can be effectively shielded, and the cooling effect of the single crystal can be enhanced.
  • the heat conducting part as shown in FIG. 2A has the same thickness (60 mm) as the heat removing part, and the length of the heat conducting part is 0, 5, and 5, respectively.
  • Such a forced cooling cylinder is fixed to the single crystal manufacturing apparatus 20 so that the distance between the heat removal part of the forced cooling cylinder and the surface of the raw material melt is constant, and a single crystal having a diameter of 300 mm is pulled up. At that time, the temperature of the tip part of the heat conducting part was measured.
  • Figure 6 shows the measurement results.
  • the thermal stress generated in the forced cooling cylinder during pulling of the single crystal can be adjusted by applying a surface treatment to the forced cooling cylinder to adjust the emissivity of the cooling cylinder surface, It can be easily adjusted by changing the thickness and Z or length of the heat conducting part of the forced cooling cylinder.
  • the emissivity of the surface of the cooling cylinder is 0.2 or more and 1.0 or less, particularly 0.2 or less. It is preferable to apply a surface treatment to the forced cooling cylinder so as to be 0.5 or less. In this way, by performing surface treatment so that the emissivity of the surface of the forced cooling cylinder becomes 0.2 or more and 1.0 or less, the thermal stress generated in the forced cooling cylinder is reduced to the yield stress of the forced cooling cylinder or less.
  • the surface treatment of the forced cooling cylinder can be easily performed by using nickel plating, nickel spraying, chromia spraying, titer spraying, alumina spraying, or yttria spraying. More desirable in raising.
  • the thermal stress generated in the forced cooling cylinder When controlling the thermal stress generated in the forced cooling cylinder by changing the thickness, Z or length of the heat conducting portion of the forced cooling cylinder, an experiment or the like is performed in advance, and the forced cooling is performed.
  • the thermal stress generated in the forced cooling cylinder during pulling the single crystal becomes less than the yield stress of the forced cooling cylinder So that it can be easily controlled.
  • the length of the heat conducting portion is preferably at least 5 cm or more in consideration of the cooling effect of the forced cooling cylinder, and in consideration of safety, the forced cooling cylinder is made of a single crystal. It is preferable that the length be less than the length that does not allow the heat conduction part to come into contact with the raw material melt when fixed to the device (depending on the device, but not more than about 30 cm). Further, regarding the thickness of the heat conducting portion, it is preferable that the thickness of the tip of the heat conducting portion of the forced cooling cylinder be 50% or more and 100% or less of the thickness of the heat removing portion. An excellent cooling effect can be obtained stably.
  • the present invention installs a forced cooling cylinder having a thermal conductivity of 300 WZm'K or more on the raw material melt, and supplies a cooling medium to the forced cooling cylinder to supply the single crystal.
  • the cold By controlling the thermal stress generated in the forced cooling cylinder to be equal to or lower than the yield stress of the forced cooling cylinder when pulling while pulling, the effect of absorbing the radiant heat in the forced cooling cylinder that is opposed to the grown crystal is enhanced. Radiant heat from the single crystal can be efficiently removed to the outside of the chamber, the desired cooling atmosphere can be easily formed around the single crystal, and plastic deformation occurs in the forced cooling cylinder. Can be reliably prevented.
  • the single-crystal growth can be maintained at a low temperature of, for example, 200 ° C. or less, at the raw material melt side end of the heat conduction portion of the forced cooling cylinder during pulling of the single crystal. It is possible to produce a single crystal having a desired quality at high speed with high productivity and very stably, and it is possible to significantly reduce costs by improving productivity. In addition, by maintaining the tip of the heat conducting portion at 200 ° C. or lower in this way, it is possible to reliably prevent metal contamination from occurring in the growing single crystal.
  • the temperature gradient of the heat conducting portion of the forced cooling cylinder during single crystal growth can be made i CZ cm or less, and further, 5.5 ° CZcm or less.
  • the thermal stress generated in the cooling can be made extremely small, and the single crystal can be grown very stably and with high safety without causing plastic deformation in the forced cooling cylinder. It can withstand the production of crystals.
  • the single crystal thus manufactured by the method for manufacturing a single crystal of the present invention becomes a single crystal manufactured at high productivity at a lower cost than the conventional single crystal and has a desired defect region. And a very high quality single crystal free of metal contamination.
  • the forced cooling cylinder is made of oxygen-free copper and has the shape shown in Fig. 2 (a), and the thermal stress generated in the forced cooling cylinder during single crystal pulling is calculated as the yield stress of the forced cooling cylinder. in a 4. as a 5KgfZmm 2 or less force to the surface of the cooling cylinder by applying a nickel plated to the surface emissivity and 0.4, also heat removing portion and the thickness of the heat conductive portion together 33 mm, thermal conduction The length of the part was set to 10 cm.
  • the present invention is not limited to the above embodiment.
  • the above embodiment is a mere example, and any one having substantially the same configuration as the technical idea described in the claims of the present invention and having the same function and effect will be described. Are also included in the technical scope of the present invention.
  • the single crystal manufacturing apparatus has been described by taking, as an example, a single crystal manufacturing apparatus by the CZ method in which a single crystal is grown without applying a magnetic field.

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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

L'invention concerne un procédé de production de monocristal par tirage vertical à partir d'une première matière fondue, selon la technique Czochralski, lequel se caractérise en ce que quand, après mise en place d'un tube de refroidissement forcé constitué d'une matière présentant une conductivité thermique de 300 W/m K ou supérieure au-dessus de la matière première fondue, de façon à entourer le monocristal-verticalement, ledit monocristal est, pendant qu'il est tiré, refroidi par le fluide de refroidissement conduit dans le tube de refroidissement forcé, la contrainte thermique générée dans le tube de refroidissement forcé est régulée de façon à ne pas dépasser la limite apparente d'élasticité du tube de refroidissement forcé. L'invention concerne également un appareil de production de monocristal. Grâce au procédé et à l'appareil de production de monocristal présentés, lors de la production d'un monocristal par tirage vertical à partir d'une matière première fondue selon la technique CZ, le refroidissement du monocristal peut se faire efficacement sans contamination métallique et également sans déformation du tube de refroidissement, et un tirage vertical du monocristal garantissant une région de défaut désirée peut être réalisé de façon stable à une vitesse élevée.
PCT/JP2004/014726 2003-10-10 2004-10-06 Procede et appareil pour la production de monocristal, et monocristal WO2005035838A1 (fr)

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JP2003351674A JP4569090B2 (ja) 2003-10-10 2003-10-10 単結晶の製造方法及び単結晶、並びに単結晶の製造装置

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JP5120337B2 (ja) * 2009-06-01 2013-01-16 株式会社Ｓｕｍｃｏ シリコン単結晶の製造方法、シリコン単結晶の温度推定方法
DE102019107929A1 (de) * 2019-03-27 2020-10-01 Pva Tepla Ag Kristallziehanlage mit einem Tiegel und einem Kühlkörper

Citations (3)

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Publication number Priority date Publication date Assignee Title
JPH0782084A (ja) * 1993-09-20 1995-03-28 Sumitomo Metal Ind Ltd 単結晶成長方法及び単結晶成長装置
WO2001057293A1 (fr) * 2000-01-31 2001-08-09 Shin-Etsu Handotai Co., Ltd. Dispositif et procede de production de monocristal et monocristal
JP2002255682A (ja) * 2001-02-28 2002-09-11 Shin Etsu Handotai Co Ltd 半導体単結晶製造装置及びそれを用いた半導体単結晶の製造方法

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JP3220542B2 (ja) * 1993-01-05 2001-10-22 ワッカー・エヌエスシーイー株式会社 半導体単結晶棒製造装置
DE19503357A1 (de) * 1995-02-02 1996-08-08 Wacker Siltronic Halbleitermat Vorrichtung zur Herstellung eines Einkristalls
JP4055362B2 (ja) * 2000-12-28 2008-03-05 信越半導体株式会社 単結晶育成方法および単結晶育成装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0782084A (ja) * 1993-09-20 1995-03-28 Sumitomo Metal Ind Ltd 単結晶成長方法及び単結晶成長装置
WO2001057293A1 (fr) * 2000-01-31 2001-08-09 Shin-Etsu Handotai Co., Ltd. Dispositif et procede de production de monocristal et monocristal
JP2002255682A (ja) * 2001-02-28 2002-09-11 Shin Etsu Handotai Co Ltd 半導体単結晶製造装置及びそれを用いた半導体単結晶の製造方法

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