WO2021095324A1 - Procédé de production d'un monocristal de silicium - Google Patents

Procédé de production d'un monocristal de silicium Download PDF

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Publication number
WO2021095324A1
WO2021095324A1 PCT/JP2020/032354 JP2020032354W WO2021095324A1 WO 2021095324 A1 WO2021095324 A1 WO 2021095324A1 JP 2020032354 W JP2020032354 W JP 2020032354W WO 2021095324 A1 WO2021095324 A1 WO 2021095324A1
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single crystal
crucible
quartz glass
oxygen concentration
crystal
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PCT/JP2020/032354
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English (en)
Japanese (ja)
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尚 松村
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グローバルウェーハズ・ジャパン株式会社
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Priority to CN202080078286.9A priority Critical patent/CN114616361B/zh
Priority to DE112020005532.9T priority patent/DE112020005532T5/de
Publication of WO2021095324A1 publication Critical patent/WO2021095324A1/fr

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10Crucibles or containers for supporting the melt
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Definitions

  • the present invention relates to a method for producing a silicon single crystal by the Czochralski method (CZ method), and relates to a method for producing a silicon single crystal capable of producing a silicon single crystal having a uniform oxygen concentration in the crystal length direction.
  • CZ method Czochralski method
  • polysilicon as a raw material is filled in a quartz glass crucible 51 installed in a chamber 50 as shown in FIG. 8, and a heater 52 provided around the quartz glass crucible 51 is used for poly.
  • the seed crystal (seed) P attached to the seed chuck is immersed in the silicon melt M, and the seed chuck and the quartz glass crucible 51 are placed in the same direction or in the opposite direction. This is done by pulling up the seed chuck while rotating it to.
  • the seed crystal P is brought into contact with the silicon melt M to dissolve the tip of the seed crystal P, and then necking is performed.
  • Necking is an indispensable step for removing dislocations generated in a silicon single crystal due to a thermal shock generated by contact between the seed crystal P and the silicon melt M.
  • the neck portion P1 is formed by this necking. Further, the neck portion P1 is required to have a diameter of about 5 mm and a length of 30 to 40 mm or more in the case of a crystal having a diameter of 300 mm, for example.
  • the steps after the start of pulling include a step of forming a shoulder portion C1 that spreads the crystal to the diameter of the straight body portion after the end of necking, a step of forming a straight body portion C2 that grows a single crystal to be a product, and a process of forming the straight body portion.
  • a step of forming a tail portion (not shown) is performed in which the diameter of the single crystal after the step is gradually reduced.
  • the oxygen contained in the quartz glass crucible 51 dissolves in the silicon melt M and reacts with the silicon melt M to form SiOx. Become. Most of this SiOx evaporates from the free surface of the melt and is discharged together with the inert gas (Ar or the like) introduced into the single crystal pulling device.
  • the oxygen incorporated into the silicon single crystal has an effect of suppressing heavy metal gettering and slip dislocations due to oxygen precipitates in the semiconductor device manufacturing process. ..
  • the oxygen precipitate is present in the active layer in the process of manufacturing a semiconductor device, there is a risk that the electrical characteristics will be adversely affected. Therefore, it is required to manufacture a wafer having an appropriate oxygen concentration according to the type of semiconductor device.
  • the upper part of the straight body that grew in the early stage of pulling has a large amount of silicon melted in the quartz glass crucible, and the contact area between the inner wall surface of the crucible and the silicon melt is large, so the amount of oxygen eluted from the quartz glass crucible. It is pulled up in a state where there are many. As the single crystal is pulled up, the amount of silicon melt in the crucible decreases, so the contact area between the inner wall surface of the crucible and the silicon melt becomes smaller, and oxygen from the quartz glass crucible to the silicon melt becomes smaller. The amount of elution decreases.
  • the oxygen concentration in the silicon melt was not stable, and the oxygen concentration distribution in the growth direction of the single crystal tended to be non-uniform (for example, the oxygen concentration was higher in the upper part and lower in the lower part).
  • the oxygen concentration in the crystal growing axis direction in order to improve the yield, it has been desired to control the oxygen concentration in the crystal growing axis direction to be uniform.
  • Patent Document 1 Japanese Patent Laid-Open No. 6-56571
  • an inverted truncated cone-shaped or cylindrical heat shielding jig is arranged above the silicon melt, and the silicon melt surface and the heat shield cure are provided.
  • a method of controlling the oxygen concentration of a single crystal by adjusting the gap with the lower end of the jig is disclosed.
  • the melt surface is cooled by the inert gas supplied to the melt surface from above the heat shielding jig, and the heat radiated from the crucible to the melt surface is shielded.
  • the degree can be accurately controlled, and as a result, the diffusion evaporation of oxygen in the melt can be controlled, and the amount of oxygen supplied to the single crystal can be controlled.
  • Patent Document 2 (Republished WO2001 / 063027) discloses that the oxygen concentration is controlled by changing the flow rate and pressure of the inert gas flowing into the furnace according to the amount of pulling up. According to the method disclosed in Patent Document 2, the amount of oxygen evaporating as an oxide from the surface of the melt near the crystal growth interface can be easily adjusted by changing the flow rate or pressure of the inert gas in the furnace. The amount of oxygen contained in the silicon melt can be easily controlled.
  • Patent Documents 1 and 2 can make the crystal oxygen concentration in the crystal growth axis direction uniform, but have the following problems. Specifically, in the method disclosed in Patent Document 1, the temperature of the silicon melt surface changes due to the gap between the silicon melt surface and the heat shielding jig, and the temperature distribution in the crystal height direction changes. Since it changes, it affects the formation of crystal defects such as void-like defects (COP) and oxygen precipitates (BMD), and there is a problem that the distribution of crystal defects becomes non-uniform.
  • COP void-like defects
  • BMD oxygen precipitates
  • the amount of SiO gas evaporated from the melt is adjusted by the flow rate and pressure of the inert gas, and when the flow rate of the inert gas is large, the gas is exhausted. There is a problem that a vacuum pump having high exhaust performance is required for the pump, which increases the cost. On the other hand, when the flow rate of the inert gas is small, there is a problem that the dirt in the furnace is not exhausted and the single crystallization rate is lowered.
  • the present inventor does not use a heat shield jig as in the method disclosed in Patent Document 1, but uses the flow rate and pressure of the inert gas from the melt as in the method disclosed in Patent Document 2.
  • the amount of evaporation of SiO gas in the above was not adjusted, and a new method was examined.
  • the crystal growth of the silicon single crystal to be pulled up by adjusting the ratio t / T of the thickness t of the transparent inner layer to the wall thickness T of the quartz glass crucible along the height direction of the quartz glass crucible. It has been found that the oxygen concentration in the axial direction can be controlled, and the present invention has been completed.
  • An object of the present invention is to provide a method for producing a silicon single crystal capable of producing a silicon single crystal having a more uniform oxygen concentration distribution.
  • the method for producing a silicon single crystal according to the present invention uses a quartz glass turret having an opaque outer layer and a transparent inner layer from a silicon melt contained in the quartz glass rug.
  • the quartz glass crucible is divided into a plurality of regions from the upper part to the lower part of the side wall of the quartz glass crucible, and the ratio t / T of the thickness t of the transparent inner layer to the thickness T of the side wall of the quartz glass crucible.
  • the adjustment is made for each of the plurality of regions.
  • the ratio t / T of the thickness t of the transparent inner layer to the thickness T of the side wall of the quartz glass crucible is in the range of more than 0.05 and less than 0.8.
  • the ratio t of the thickness t of the transparent inner layer to the wall thickness T of the quartz glass crucible along the height direction of the quartz glass crucible is adjusted.
  • silicon single having a more uniform oxygen concentration distribution in the silicon crystal length direction.
  • a method for producing a silicon single crystal capable of producing a crystal can be obtained.
  • FIG. 1 is a cross-sectional view of a single crystal pulling device in which the method for producing a silicon single crystal according to the present invention is carried out.
  • FIG. 2 is a cross-sectional view of a quartz glass crucible included in the single crystal pulling device of FIG.
  • FIG. 3 is a partially enlarged cross-sectional view of the quartz glass crucible of FIG.
  • FIG. 4 is a flow showing a flow of a method for producing a silicon single crystal according to the present invention.
  • 5 (a), (b), and (c) are cross-sectional views showing the relationship between the amount of silicon melt and the crucible, which changes with crystal pulling.
  • FIG. 6 is a graph showing the results of Example (Experiment 1).
  • FIG. 7 is a graph showing the results of Example (Experiment 2).
  • FIG. 8 is a cross-sectional view for explaining a process of pulling up a silicon single crystal by the Czochralski method.
  • FIG. 1 is a cross-sectional view of a single crystal pulling device in which the method for producing a silicon single crystal according to the present invention is carried out.
  • FIG. 2 is a cross-sectional view of a quartz glass crucible included in the single crystal pulling device of FIG.
  • the single crystal pulling device 1 includes a furnace body 10 formed by superimposing a pull chamber 10b on a cylindrical main chamber 10a, and is provided in the furnace body 10 so as to be rotatable and elevating around a vertical axis.
  • It includes a carbon susceptor (or graphite susceptor) 2 and a quartz glass crucible 3 (hereinafter, simply referred to as a crucible 3) held by the carbon susceptor 2.
  • the crucible 3 can rotate around a vertical axis as the carbon susceptor 2 rotates.
  • the crucible 3 is formed, for example, with a bottom portion 31 having a diameter of 800 mm and having a predetermined curvature, a corner portion 32 formed around the bottom portion 31 and having a predetermined curvature, and a straight body portion extending upward from the corner portion 32. It has 33 and. A crucible opening (upper end opening) is formed at the upper end of the straight body portion 33.
  • the crucible 3 has a two-layer structure consisting of an opaque outer layer 3A (opaque layer) and a transparent inner layer 3B (transparent layer).
  • the opaque outer layer 3A is made of natural raw material quartz glass
  • the transparent inner layer 3B is made of, for example, high-purity synthetic raw material quartz glass.
  • opaque means a state in which a large number of bubbles (pores) are contained in the quartz glass and the quartz glass is apparently cloudy.
  • the natural raw material quartz glass means silica glass produced by melting a natural material such as crystal
  • the synthetic raw material quartz glass means, for example, a synthetic raw material synthesized by hydrolysis of silicon alkoxide is melted. It means the silica glass to be manufactured.
  • a quartz glass crucible in which the ratio t / T of the thickness t of the transparent inner layer to the wall thickness T of the quartz glass crucible is adjusted (set) in the crucible height direction is used.
  • the oxygen concentration in the silicon melt is not stable, and the oxygen concentration distribution in the growth direction of the single crystal tends to be non-uniform.
  • the non-uniformity depends on the magnetic field strength, magnetic field center position, inert gas flow rate and furnace pressure, quartz glass crucible 3, rotation, single crystal rotation, etc. It is influenced by the parameters.
  • the tendency of the oxygen concentration distribution in which the pulled single crystal becomes non-uniform (for example, the distribution in which the oxygen concentration in the upper part of the crystal is higher than that in the lower part) is grasped in advance. Then, the ratio t / T is adjusted based on the ratio.
  • the tendency of the oxygen concentration distribution is such that the oxygen concentration in the upper part of the crystal is higher than that in the lower part will be described as an example.
  • the crucible upper portion 33A, the crucible middle portion 33B, and the crucible lower portion 33C have a crucible wall thickness (opaque outer layer 3A and opaque).
  • the ratio t / T of the thickness t of the transparent inner layer 3B to T) T which is the total thickness of the inner layer 3B, is set to be greater than 0.05 and less than 0.8.
  • the ratio t / T is set from a small value to a large value from the upper 33A to the lower 33C.
  • the ratio t / T of the thickness t of the transparent inner layer 3B to the crucible wall thickness T is set to 0.10, and the ratio t / T of the intermediate portion 33B is set to 0.3.
  • the ratio t / T of the lower 33C is set to 0.6.
  • the ratio t / T is 0.05 or less (when the thickness of the transparent inner layer 3B is too thin), all the transparent inner layer 3B is melted during crystal growth, and the opaque outer layer 3A containing bubbles is a silicon melt. It is exposed on the M side, and there is a risk that minute quartz particles will come off. In that case, there is a risk that the particles will reach the surface of the melt and the dislocation rate will increase, or that air bubbles will be incorporated into the crystal to form air pockets.
  • the ratio t / T is 0.8 or more (when the thickness of the transparent inner layer 3B is too thick), the uniform diffusion of heat by the opaque outer layer 3A becomes insufficient, making temperature control difficult, or the product. There are drawbacks such as high price.
  • the ratio t / T is specified as described above because the heat transfer coefficient of the opaque outer layer 3A and the transparent inner layer 3B is different. Since the opaque outer layer 3A contains a large amount of air bubbles, heat is uniformly diffused to obtain a uniform temperature distribution. On the other hand, the transparent inner layer 3B has a high thermal conductivity, and it is difficult to control the temperature.
  • the ratio t / T of the transparent inner layer 3B to the wall thickness T of the crucible 3 is small, the opaque outer layer 3A that uniformly diffuses heat becomes thick, and it is not necessary to heat the crucible 3 more than necessary. Since the inner surface temperature can be lowered, the amount of quartz dissolved in the silicon melt M can be reduced. On the other hand, when the ratio t / T of the transparent inner layer 3B to the wall thickness T of the crucible 3 is large, the heat conduction is large, so that the inner surface temperature of the crucible becomes high, the amount of quartz dissolved increases, and the silicon melt M The amount of quartz dissolved in the material can be increased.
  • the ratio t / T of the upper part 33A, the middle part 33B, and the lower part 33C of the crucible in which the silicon melt surface M1 that most affects the crystal oxygen concentration moves in order is, as an example, quartz glass.
  • a rotary drive unit 14 such as a rotary motor that rotates the carbon susceptor 2 around a vertical axis, and an elevating drive unit 15 that moves the carbon susceptor 2 up and down.
  • the rotation drive control unit 14a is connected to the rotation drive unit 14, and the lift drive control unit 15a is connected to the lift drive unit 15.
  • the single crystal pulling device 1 includes a side heater 4 by resistance heating that melts the semiconductor raw material (raw polysilicon) loaded in the crucible 3 into a silicon melt M (hereinafter, simply referred to as melt M). It is provided with a pulling mechanism 9 that winds up the wire 6 and pulls up the single crystal C to be grown. A seed crystal P is attached to the tip of the wire 6 of the pulling mechanism 9.
  • a heater drive control unit 4a for controlling the amount of power supplied is connected to the side heater 4, and a rotation drive control unit 9a for controlling the rotation drive thereof is connected to the pulling mechanism 9.
  • an electromagnetic coil 8 for applying a magnetic field is installed outside the furnace body 2. When a predetermined current is applied to the magnetic field application electromagnetic coil 8, a horizontal magnetic field having a predetermined strength is applied to the silicon melt M in the crucible 3.
  • An electromagnetic coil control unit 8a that controls the operation of the electromagnetic coil 8 for applying a magnetic field is connected to the electromagnetic coil 8.
  • the MCZ method Magnetic field applied CZ method in which a magnetic field is applied into the melt M to grow a single crystal is carried out, thereby controlling the convection of the silicon melt M and causing the single crystal. It is designed to stabilize the crystallization.
  • a radiation shield 7 surrounding the circumference of the single crystal C is arranged above the melt M formed in the crucible 3.
  • the radiant shield 7 has openings formed at the upper and lower portions, shields excess radiant heat from the side heater 4 and the melt M, etc. with respect to the growing single crystal C, and rectifies the gas flow in the furnace. ..
  • the gap between the lower end of the radiation shield 7 and the surface of the molten liquid is controlled so as to maintain a constant distance according to the desired characteristics of the single crystal to be grown.
  • the single crystal pulling device 1 includes a computer 11 having a storage device 11a and an arithmetic control device 11b, and includes a rotation drive control unit 14a, an elevating drive control unit 15a, an electromagnetic coil control unit 8a, and a rotation drive control unit 9a. Are connected to the arithmetic control device 11b, respectively.
  • the single crystal pulling device 1 configured in this way, for example, when growing a single crystal C having a diameter of 300 mm, the single crystal pulling device 1 is pulled as follows. That is, first, the raw material polysilicon (for example, 350 kg) is loaded into the crucible 3, and the crystal growth step is started based on the program stored in the storage device 11a of the computer 11.
  • the raw material polysilicon for example, 350 kg
  • the polysilicon is melted by heating by the side heater 4 to form a melt M (step S1 in FIG. 4).
  • a predetermined current is passed through the magnetic field application electromagnetic coil 8, and a horizontal magnetic field is started to be applied into the melt M at a magnetic flux density (for example, 2500 Gauss) set in the range of 1000 to 4000 Gauss (step of FIG. 4).
  • a magnetic flux density for example, 2500 Gauss
  • the wire 6 is lowered, the seed crystal P is brought into contact with the melt M, the tip portion of the seed crystal P is melted, and then necking is performed and the neck portion P1 is started to be formed (step S3 in FIG. 4).
  • the pulling conditions are adjusted with the power supplied to the side heater 4, the pulling speed, the magnetic field application strength, and the like as parameters, and the seeds are seeded at a predetermined rotation speed in the direction opposite to the rotation direction of the rutsubo 3.
  • the crystal P starts rotating.
  • the crystal diameter is gradually increased to form the shoulder portion C1 (step S4 in FIG. 4), and the process proceeds to the step of forming the straight body portion C2 to be the product portion (step S5 in FIG. 4).
  • the oxygen concentration in the single crystal grown from the silicon melt M into which the oxygen eluted from the crucible 3 is introduced is, for example, the magnetic field strength, the magnetic field center position, the flow rate of the inert gas, the furnace pressure, and the quartz glass crucible. Parameters such as rotation of 3 and rotation of a single crystal have an effect.
  • the crystal growth axis is adjusted by adjusting the ratio t / T of the thickness t of the transparent inner layer 3B to the crucible wall thickness T in the height direction of the crucible 3. Control the crystal oxygen concentration in the direction.
  • the growth axis direction of the single crystal C raised by the above parameters such as the magnetic field strength, the magnetic field center position, the flow rate of the inert gas and the pressure inside the furnace, the rotation of the base quartz glass crucible 3, and the rotation of the single crystal.
  • the tendency of the oxygen concentration is recorded in the storage device 11a as data in advance, the ratio t / T in the quartz glass crucible 3 is determined accordingly, and the crucible based on the ratio t / T is manufactured and used.
  • the silicon melt surface M1 is located at the upper portion 33A of the crucible as shown in FIG. 5 (a).
  • the amount of oxygen taken into the single crystal C is most affected by the oxygen concentration in the melt M near the silicon melt surface M1.
  • the amount of silicon melt is large and the contact area with the inner surface of the crucible is large, so that the oxygen concentration in the melt is high as a whole.
  • the ratio t / T of the thickness t of the transparent inner layer 3B to the wall thickness T is set as small as 0.08, for example. That is, since the transparent inner layer 3B is formed to be thin, the opaque outer layer 3A is thick, whereby heat is diffused and made uniform. As a result, the temperature of the inner surface of the crucible is lowered, and the amount of quartz dissolved in the silicon melt M from the crucible 3 is suppressed.
  • the transparent inner layer 3B with respect to the crucible wall thickness T The ratio t / T of the thickness t is set to, for example, 0.3.
  • the inner layer 3B is thick, the amount of quartz dissolved in the crucible 3 into the silicon melt M increases.
  • the ratio t / T of t is set as high as 0.6, for example.
  • the amount of the silicon melt in the crucible is further reduced to a small amount, the oxygen concentration in the silicon melt is low, but the transparent inner layer 3B is formed thicker in the lower part 33C of the crucible. , The thermal conductivity is high. As a result, the temperature of the inner surface of the crucible rises, and the amount of quartz dissolved in the silicon melt from the crucible 3 increases.
  • the process proceeds to the final tail portion step (step S6 in FIG. 2).
  • the contact area between the lower end of the crystal and the melt M is gradually reduced, the single crystal C and the melt M are separated, and a silicon single crystal is produced.
  • the ratio t / T of the thickness t of the transparent inner layer to the wall thickness T of the quartz glass crucible is adjusted along the height direction of the quartz glass crucible.
  • the oxygen concentration in the crystal growth axis direction of the silicon single crystal can be brought close to a desired value and made uniform.
  • the cost can be suppressed as compared with the configuration of the conventional general single crystal pulling device.
  • the temperature of the silicon melt surface can be controlled to be kept constant, it is possible to prevent the distribution of crystal defects from becoming non-uniform.
  • the ratio t / T of the thickness t of the transparent inner layer 3B to the crucible wall thickness T is set to 0.08, 0.3, 0.6, but the magnetic field is shown.
  • the ratio t / T can be appropriately changed by changing parameters such as strength, magnetic field center position, flow rate and furnace pressure of inert gas, rotation of quartz glass crucible, and rotation of single crystal.
  • the quartz glass crucible 3 is divided into three regions (33A, 33B, 33C) in the height direction, and the ratio t / T is set in each region.
  • the ratio t / T is set.
  • the number of the regions is not limited and can be set as appropriate.
  • the ratio t / T may be gradually changed in the height direction of the quartz glass crucible 3.
  • the quartz glass crucible 3 has a two-layer structure of an opaque outer layer 3A and a transparent inner layer 3B, but the present invention is not limited to the structure, and if the inner layer is a transparent layer, the layer can be formed. The number is not limited.
  • a method using a heat shielding jig as in the method disclosed in Patent Document 1 and a method using a flow rate and pressure of an inert gas as in the method disclosed in Patent Document 2 are used to melt the liquid.
  • a method of adjusting the amount of evaporation of SiO gas from the gas may be used together.
  • Experiment 1 by changing the ratio t / T of the thickness t of the transparent inner layer to the crucible wall thickness T in the crucible height direction, how is the oxygen concentration distribution in the pulling direction of the pulled silicon single crystal? We verified whether it would affect it.
  • the ratio t / T of the thickness t of the transparent inner layer 3B to the crucible wall thickness T shown in FIG. 3 was set as shown in Table 1 in Example 1, Example 2, and Comparative Example 1.
  • the ratio t / T of the quartz crucible was set under the condition of the pulling device in which the oxygen concentration in the upper part of the pulled single crystal tended to be higher than the oxygen concentration in the lower part.
  • the ratio t / T of the quartz crucible was set under the condition of the pulling device in which the oxygen concentration in the upper part of the pulled single crystal tended to be higher than the oxygen concentration in the lower part.
  • Example 1 As shown in the graph of FIG. 6, in Example 1, the oxygen concentration at the initial stage of crystal pulling was suppressed, and a single crystal having a low oxygen concentration and a uniform oxygen concentration in the crystal growth axis direction was obtained. Further, as shown in Table 1, the variation in oxygen concentration was suppressed to 14%. Further, in Example 2, the oxygen concentration in the late stage of crystal pulling was improved, and a single crystal having a high oxygen concentration and a uniform oxygen concentration in the crystal growth axis direction was obtained. Further, as shown in Table 1, the variation in oxygen concentration was suppressed to 13%. Further, in Comparative Example 1, a single crystal having a higher oxygen concentration was obtained in the upper part of the crystal. Further, as shown in Table 1, the variation in oxygen concentration was as large as 30%. From the results of this experiment 1, it was confirmed that according to the present invention, the oxygen concentration can be controlled more uniformly in the crystal growth axis direction, and the variation in oxygen concentration can be suppressed within 20%.
  • Example 2 In Experiment 2, the ratio of the thickness t of the transparent inner layer to the crucible wall thickness T of the quartz crucible under the condition of the pulling device in which the oxygen concentration in the upper part of the pulled single crystal tends to be lower than the oxygen concentration in the lower part.
  • the t / T was changed in the crucible height direction, and the variation in the oxygen concentration in the height direction of the single crystal to be pulled up was verified.
  • the conditions for pulling up the single crystal are the same as in Experiment 1.
  • Table 2 shows the ratio t / T in the upper part, the middle part, and the lower part of the crucible in Examples 3, 4 and Comparative Example 2, and the variation in the oxygen concentration in the axial direction of the single crystal pulled up based on those conditions.
  • the graph of FIG. 7 shows changes in the single crystal oxygen concentration in Examples 3 and 4 and Comparative Example 2.
  • the vertical axis is the oxygen concentration ( ⁇ 10 18 / cm 3 ), and the horizontal axis is the solidification rate.
  • Example 3 In Experiment 3, the appropriate range of the ratio t / T of the thickness t of the transparent inner layer to the crucible wall thickness T was verified. Judgment as to whether or not it was appropriate was made based on the dislocation rate of the crystal and the magnitude of the amount of temperature fluctuation. Table 3 shows the ratio t / T, which is the condition in Examples 5 to 7 and Comparative Examples 3 to 6, the resulting dislocation rate of the crystal, and the amount of temperature fluctuation of the melt. In Examples 5 to 7 and Comparative Examples 3 to 6 of Experiment 3, the ratio t / T was set in order to make the oxygen concentration distribution in the pulling axis direction of the pulled single crystal uniform. Other conditions are the same as in Experiment 1.
  • Single crystal pulling device Carbon susceptor 3 Quartz glass crucible (crucible) 4 Side heater 6 Wire 7 Radiation shield 8 Electromagnetic coil for applying magnetic field 9 Pulling mechanism 10 Furnace 11 Computer 11a Storage device 11b Arithmetic control device 14 Rotation drive unit 15 Lifting drive unit C Silicon single crystal M Silicon melt C1 Shoulder C2 Straight Body

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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)
  • Glass Melting And Manufacturing (AREA)

Abstract

La présente invention concerne un procédé de production d'un monocristal de silicium, le procédé étant susceptible de produire un monocristal de silicium ayant une distribution de concentration en oxygène plus uniforme dans le sens de la longueur du cristal de silicium. Ce procédé de production d'un monocristal de silicium comprend la traction d'un monocristal de silicium à partir d'une masse fondue de silicium logée dans un creuset en verre de quartz (3) en utilisant le procédé de Czochralski et utilise un creuset en verre de quartz pour lequel le rapport t/T de l'épaisseur t de la couche interne transparente à l'épaisseur T de la paroi latérale du creuset en verre de quartz est ajusté depuis la partie supérieure vers la partie inférieure de la paroi latérale du creuset en verre de quartz, la variation dans la concentration d'oxygène dans le sens de l'axe de croissance du cristal du monocristal de silicium tiré se situe à l'intérieur de 20 %.
PCT/JP2020/032354 2019-11-11 2020-08-27 Procédé de production d'un monocristal de silicium WO2021095324A1 (fr)

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DE112020005532.9T DE112020005532T5 (de) 2019-11-11 2020-08-27 Verfahren zum Herstellen eines Silizium-Einkristalls

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WO2004106247A1 (fr) * 2003-05-30 2004-12-09 Shin-Etsu Quartz Products Co., Ltd. Creuset a verre de silice pour le montage d'un monocristal de silicium

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JP2606046B2 (ja) 1992-04-16 1997-04-30 住友金属工業株式会社 単結晶引き上げ時における単結晶酸素濃度の制御方法
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WO2004106247A1 (fr) * 2003-05-30 2004-12-09 Shin-Etsu Quartz Products Co., Ltd. Creuset a verre de silice pour le montage d'un monocristal de silicium

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