JP5036735B2 - Silica glass crucible for pulling silicon single crystal and manufacturing method thereof - Google Patents

Description

  The present invention relates to a quartz glass crucible for pulling a silicon single crystal and a method for manufacturing the same, and more particularly to optical characteristics of the quartz glass crucible.

  A quartz glass crucible is used for manufacturing a silicon single crystal. In the Czochralski method (CZ method), polysilicon is heated and melted in a quartz glass crucible, the seed crystal is immersed in this silicon melt, and the seed crystal is gradually pulled up while rotating the crucible to grow a single crystal. Let In order to produce a high-purity silicon single crystal for semiconductor devices, it is required that the silicon single crystal is not contaminated by the elution of impurities contained in the quartz glass crucible, and the quartz glass crucible must have sufficient heat resistance. It is.

  The raw material of the quartz glass crucible includes natural quartz and synthetic quartz. Generally, natural quartz is lower in purity than synthetic quartz but has excellent heat resistance, and synthetic quartz is inferior in heat resistance but higher in purity than natural quartz. Therefore, the outer layer of the crucible is made of natural quartz to increase the strength of the crucible at high temperatures, while the inner layer of the crucible that contacts the silicon melt is made of synthetic quartz to prevent impurities from entering. A quartz glass crucible having a structure is generally used (see Patent Document 1). In addition, in order to control the amount of dissolved oxygen in the silicon melt, we also propose a quartz glass crucible in which the inner surface of the straight body of the crucible is made of synthetic quartz and the natural quartz that forms the outer layer is exposed at the bottom of the crucible. Has been. (See Patent Document 2).

  By the way, due to the recent increase in the size of silicon ingots, the weight of silicon loaded in the crucible has increased, and bubbles contained in the silicon melt are difficult to escape from the silicon melt. The problem that a bubble defect (also referred to as a void or an air pocket) is formed in the crystal due to the bubbles being taken into the silicon single crystal has become conspicuous. The cause of the cavity defect is considered to be argon (Ar) gas adhering to the inner surface of the quartz glass crucible or silicon monoxide (SiO) gas generated by the reaction between the quartz glass crucible and the silicon melt. Cavity defects caused by bubbles are generally spherical, and the size (diameter) occupies most of 300 to 500 μm. However, small cavity defects of 150 μm or less and very large cavity defects of 1 mm or more may be formed. is there. As described above, the cavity defect due to the bubbles has characteristics that are clearly different from the Grown-in defect such as COP (Crystal Originated Particle). At present, it is not possible to non-destructively inspect for the presence of such a cavity defect, but it can only be detected by cutting the wafer from the ingot, and the cavity defect is a hole that penetrates or does not penetrate through the surface or inside of the wafer (pin hole). Appears as

  In recent years, the influence of pinholes in a wafer on the latest highly integrated semiconductor devices has been extremely large. The effect of pinholes varies depending on the size, number, location, and type of semiconductor device, but pinholes are very large compared to COPs. It cannot be formed at all. In particular, when the number of pinholes in the wafer is large, the yield is remarkably lowered, and the wafer itself must be discarded. Therefore, it is necessary to make the probability that pinholes are included in the wafer as close to zero as possible.

  In order to solve this problem, for example, Patent Documents 3 and 4 propose a method of adjusting the furnace pressure during the melting of polysilicon. Patent Document 5 proposes a method of starting the growth of a silicon single crystal after applying vibration to the crucible to reduce bubbles adhering to the inner surface of the crucible.

JP-A-1-261293 JP 2002-284596 A JP-A-5-9097 JP 2000-169287 A JP 2007-210803 A

  However, in order to produce a high-quality silicon single crystal free from void defects caused by bubbles, the environment for preventing the generation of bubbles in the crucible as described above and the process for removing bubbles alone are not sufficient. It is not sufficient, and the crucible itself is required to have the property of not generating bubbles.

  The present invention solves the above-described problems, and an object of the present invention is to provide a quartz glass crucible for pulling up a silicon single crystal capable of preventing generation of cavity defects due to air bubbles being taken into the silicon single crystal. .

  Another object of the present invention is to provide a method for producing a quartz glass crucible capable of producing a high-quality silicon single crystal free from void defects caused by bubbles.

  As a result of intensive studies to solve the above problems, the present inventor has found that the temperature at the bottom of the crucible is greatly involved in the generation of SiO gas by the reaction between the quartz glass crucible and the silicon melt. In other words, the higher the temperature at the bottom of the crucible, the more active the reaction between the quartz constituting the crucible and the silicon melt and the easier generation of SiO gas. I found out that I can do it.

  The present invention has been made on the basis of such technical knowledge, the quartz glass crucible for pulling a silicon single crystal according to the present invention is a quartz glass crucible for pulling a silicon single crystal having a straight body part and a bottom part, The infrared transmittance of a region within a certain range from the center of the bottom is higher than the infrared transmittance of the straight body, the infrared transmittance of the bottom is 50 to 80%, and the difference in infrared transmittance between the bottom and the straight body Is 10 to 30%.

  The method for producing a quartz glass crucible for pulling a silicon single crystal according to the present invention includes a step of depositing quartz powder on the inner surface of a rotating mold, and a step of forming a quartz glass crucible by melting the quartz powder. The step of forming the quartz glass crucible includes a step of sucking the gas inside the quartz powder, and the step of sucking the gas makes the gas suction time at the bottom longer than that of the straight body, or the gas at the bottom And a step of controlling the infrared transmittance of the bottom portion to be higher than the infrared transmittance of the straight barrel portion by increasing the suction pressure of the straight barrel portion.

  According to the present invention, since the infrared transmittance having a large thermal action and a strong transmission power is increased at the bottom of the crucible, generation of SiO gas bubbles can be suppressed. In particular, the infrared transmittance of the crucible is 50 to 80%, and the difference in infrared transmittance between the bottom portion of the crucible and the straight body portion is 10 to 30%, so that the production yield of the silicon single crystal is not lowered. The cooling effect at the bottom of the crucible can be ensured. Therefore, it is possible to prevent the occurrence of cavity defects due to the incorporation of SiO gas bubbles into the silicon single crystal.

In the present invention, it is preferable that the region within a certain range from the center of the bottom of the crucible having a high infrared transmittance includes a projection surface of a silicon single crystal. If a bubble of SiO gas is generated in a region corresponding to the projection surface of the silicon single crystal, it is taken into the silicon single crystal with a very high probability. However, if the infrared transmittance is high on the projection surface of the silicon single crystal, bubbles are generated. It is because it can prevent reliably. In particular, the diameter of the area within a predetermined range from the center of the crucible bottom is preferably 0.45R is ₀ or more 0.8 R ₀ or less with respect to the crucible diameter _{R 0.} If the region having a high infrared transmittance satisfies the above conditions with respect to the crucible diameter, the generation of bubbles can be reliably prevented without lowering the yield of the single crystal due to insufficient heat resistance.

  Thus, according to the present invention, quartz glass that can prevent the generation of cavity defects due to the incorporation of SiO gas bubbles into the silicon single crystal and can produce a high-quality silicon single crystal. A crucible can be provided.

  In addition, according to the present invention, it is possible to provide a method for producing a quartz glass crucible capable of producing a high-quality silicon single crystal having no cavity defect.

  Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

  FIG. 1 is a schematic sectional view showing the structure of a quartz glass crucible for pulling a silicon single crystal according to a preferred embodiment of the present invention.

  As shown in FIG. 1, the quartz glass crucible 10 according to the present embodiment has a two-layer structure, and has an opaque quartz glass layer 11 constituting an outer layer of the crucible and a transparent quartz glass layer 12 constituting an inner layer of the crucible. ing.

The opaque quartz glass layer 11 is an amorphous silica glass layer containing a large number of minute bubbles, and is provided over the entire length of the crucible from the straight body portion 10A to the bottom portion 10B. Natural quartz is preferably used as a raw material for the opaque quartz glass layer 11. Since natural quartz has a higher viscosity at high temperatures than synthetic quartz, the heat resistance of the entire crucible can be increased. Natural quartz is cheaper than synthetic quartz and is advantageous in terms of cost. The opaque quartz glass layer 11 is not necessarily made entirely of natural quartz, and the raw material in the vicinity of the boundary with the transparent quartz glass layer 12 may be synthetic quartz. The bubble content of the opaque quartz glass layer 11 is preferably 0.7 to 2%, and the average diameter of the bubbles is preferably about 100 μm. Here, the bubble content is defined as the ratio (W ₂ / W ₁ ) of the bubble occupation area (W ₂ ) to the unit area (W ₁ ).

  The transparent quartz glass layer 12 is an amorphous silica glass layer substantially free of bubbles, and is provided over the entire length of the crucible from the straight body portion 10A to the bottom portion 10B. According to the transparent quartz glass layer 12, it is possible to prevent an increase in the number of quartz pieces to be peeled off, and to increase the silicon single crystal yield. It is preferable to use synthetic quartz as a raw material for the transparent quartz glass layer 12. When synthetic quartz is used for the inner layer of the crucible, the elution of impurities into the silicon melt can be prevented, and the silicon single crystal yield can be increased. The transparent quartz glass layer 12 does not necessarily need to be made of natural quartz as a whole, and the raw material in the vicinity of the boundary with the transparent quartz glass layer 12 may be natural quartz. Here, “substantially free of bubbles” means that the bubble content is 0.1% or less and the average diameter of the bubbles is 100 μm or less.

  The crucible straight body 10A is a cylindrical portion parallel to the central axis (Z-axis) of the crucible, and extends substantially directly from the opening of the crucible. However, the straight body portion 10A does not need to be completely parallel to the Z axis, and may be inclined so as to gradually spread toward the opening. Further, the straight body portion 10A may be linear or may be gently curved.

  The bottom portion 10B of the crucible is a substantially disc-shaped portion including an intersection with the Z axis of the crucible, and a curved portion 10C is formed between the bottom portion 10B and the straight body portion 10A. The shape of the crucible bottom 10B may be a so-called round bottom or a flat bottom. Further, the curvature and angle of the bending portion 10C can be arbitrarily set. When the crucible bottom portion 10B has a round bottom, the bottom portion 10B also has an appropriate curvature, so that the difference in curvature between the bottom portion 10B and the curved portion 10C is very small compared to the flat bottom. When the crucible bottom portion 10B is a flat bottom, the bottom portion 10B has a flat or extremely gentle curved surface, and the curvature of the curved portion 10C is very large. The bottom portion 10B is defined as a region where the tangential inclination angle of the crucible wall surface with respect to the XY plane orthogonal to the Z axis is 30 degrees or less.

  In a region within a certain range from the center of the bottom 10B of the crucible, a region (high transmittance region) having a higher infrared transmittance than the surroundings is provided. The high transmittance region 10X serves to suppress the temperature rise of the bottom 10B and prevent the generation of SiO gas. When the temperature of the inner surface of the crucible rises, SiO gas is generated by the reaction between the crucible and the silicon melt. However, since the infrared transmittance of the bottom portion 10B is high and the heat easily escapes, the temperature rise of the bottom portion 10B is suppressed. Accordingly, generation of SiO gas (bumping phenomenon) due to a rapid reaction with the silicon melt can be prevented, and SiO gas generated from the bottom 10B during pulling of the silicon single crystal can be suppressed.

  The transparent quartz glass layer 12 is a transparent layer substantially free of bubbles, whereas the opaque quartz glass layer 11 is an opaque layer containing a large number of minute bubbles. The rate is very low compared to the transparent quartz glass layer 12. Therefore, the infrared transmittance of the crucible bottom 10B is dominated by the opaque quartz glass layer 11, but the infrared transmittance of the transparent quartz glass layer 12 cannot be ignored. In order to increase the infrared transmittance of the bottom portion 10B, the ratio of the thickness of the opaque quartz glass layer 11 and the transparent quartz glass layer 12 in the bottom portion 10B may be changed, or the opaque quartz glass layer 11 in the bottom portion 10B. You may carry out by making the bubble content rate of low. Such infrared transmittance can be controlled by changing the evacuation time and pressure in the arc melting step. Furthermore, it may be performed by adjusting the particle size of the quartz powder as a raw material.

  The infrared transmittance of the high transmittance region 10X needs to be 50 to 80%. If the infrared transmittance of the high transmittance region 10X is less than 50%, the cooling effect of the crucible bottom 10B is insufficient, and if it exceeds 80%, it becomes difficult to control the melt temperature when the amount of silicon melt decreases. This is because the yield is lowered due to the disturbance of oxygen and the inability to control the oxygen concentration. Furthermore, the difference in infrared transmittance between the high transmittance region 10X and the other regions needs to be 10 to 30%. If the difference in infrared transmittance between the crucible bottom 10B and the crucible straight body 10A is less than 10%, it is difficult to create a temperature difference between the crucible straight body 10A and the crucible bottom 10B, and if the difference in infrared transmittance exceeds 30%, the crucible straight This is because the temperature difference between the body portion 10A and the crucible bottom portion 10B becomes large, making it difficult to control the temperature at the time of pulling up the silicon single crystal, leading to a decrease in yield due to crystal disorder.

  Note that the difference in infrared transmittance refers to a difference when the infrared transmittance is 100% as a reference. Therefore, when the infrared transmittance of the high transmittance region 10X is 50%, the infrared transmittance of other regions is 20 to 40%, and when the infrared transmittance of the high transmittance region 10X is 80%. In other regions, the infrared transmittance is 50 to 70%.

  On the other hand, the infrared transmittance of the straight barrel portion 10A and the curved portion 10C of the quartz glass crucible 10 is lower than that of the bottom portion 10B. Therefore, although the straight body portion 10A and the curved portion 10C become high temperature and SiO gas is likely to be generated, the possibility that SiO gas bubbles generated from the straight body portion 10A and the curved portion 10C are taken into the silicon single crystal is extremely low. . This is because the rising speed of the SiO gas in the silicon melt is 30 to 60 cm / sec, whereas the convection speed of the silicon melt is only a few mm / sec, and the generated SiO gas bubbles are caused to flow by convection. This is because it rises almost vertically in the silicon melt.

  Accordingly, the low infrared transmittance of the straight body portion 10A and the curved portion 10C does not cause a cavity defect. Rather, when the infrared transmittance of the straight body portion 10A and the curved portion 10C is increased in the same manner as the bottom portion 10B, it is difficult to control the temperature of the silicon melt, which is the original purpose, and the cause of lowering the silicon single crystal yield It becomes. From such a viewpoint, in the present embodiment, the infrared transmittance of the straight body portion 10A and the curved portion 10C is set low. However, in the present invention, it is not essential to set the infrared transmittance of both the straight body portion 10A and the curved portion 10C to be low, and it is sufficient to set at least the infrared transmittance of the straight body portion 10A.

  Although not particularly limited, the thickness of the crucible is preferably about 8 to 30 mm. The thickness of the crucible may be uniform or may be formed so as to gradually increase from the bottom center toward the outside. Further, the thickness of the straight body portion 10A and the bottom portion 10B may be different.

  On the other hand, the thickness of the transparent quartz glass layer 12 is preferably 1.0 mm or more. In the pulling of the silicon single crystal, the inner surface of the crucible usually melts by about 0.3 to 1.0 mm. However, when the transparent quartz glass layer 12 is less than 1.0 mm, the melting damage occurs during the pulling of the silicon single crystal. This is because the opaque quartz glass layer 11 may be exposed. The thickness of the transparent quartz glass layer 12 may be uniform, or may be formed so as to gradually increase from the bottom center toward the outside.

  FIG. 2 is a schematic cross-sectional view showing the positional relationship between the quartz glass crucible and the silicon single crystal.

The shape of the high transmittance region 10X of the crucible bottom 10B viewed from the Z-axis direction is a circle centered on the intersection with the Z-axis, and its diameter R ₁ is ₁ of the diameter R _S of the silicon single crystal 21 to be pulled up. More preferably, it is 5 times or more and 1.8 times or less. If it is less than 1.5 times, the temperature of the projection surface of the silicon single crystal diameter Rs cannot be lowered sufficiently, so that the suppression of SiO gas is insufficient, and if it exceeds 1.8 times, the silicon melt is reduced. This is because it becomes difficult to control the pulling temperature, which leads to a decrease in yield due to crystal disorder.

The diameter R _S of the silicon single crystal 21 is not uniquely determined from the shape and size of the quartz glass crucible 10, but greatly depends on the diameter R ₀ of the quartz glass crucible 10. If the crucible diameter R ₀ is too small relative to the silicon single crystal diameter R _S , it becomes difficult to control the crystal quality such as oxygen concentration and oxygen in-plane distribution of the single crystal. This is because it is necessary to increase the cost. Therefore, the diameter _{R S} of the silicon single crystal _21, it is customary to set to 0.45R ₀ ~0.8R 0.

Considering such points, the diameter R ₁ of the high transmittance region 10X of the crucible bottom 10B is 0.45R ₀ or more and 0.8R ₀ or less with respect to the diameter R ₀ of the quartz glass crucible 10. preferable. When the diameter R ₁ of the high transmittance region 10X of the crucible bottom portion 10B is smaller than 0.45R ₀ , the temperature of the projection surface 21S of the silicon single crystal 21 cannot be lowered sufficiently, and the transparent quartz glass layer 12 This is because the generated SiO gas bubbles are more likely to be taken into the silicon single crystal 21. On the other hand, when the diameter R ₁ of the high transmission region 10X of the crucible bottom part 10B is greater than 0.8 R _0, although it is possible to reliably cover the projection plane 21S of the silicon single crystal 21, less silicon melt This is because it becomes difficult to control the pulling temperature when it becomes, causing a decrease in the yield of the silicon single crystal.

Specifically described diameter _{R 1} of the high transmission region 10X of the crucible bottom part 10B, for example, in the case of the quartz glass crucible having a diameter of 32 inches (diameter _{R 0} ≒ 800mm), high transmittance region formed in the bottom portion 10B of the crucible The lower limit of the 10X diameter R ₁ is 0.45 R ₀ = 360 mm, and the upper limit is 0.8 R ₀ = 640 mm. Usually, a 32-inch crucible is used for pulling up a silicon single crystal having a diameter of about 300 mm. In this case, the diameter R ₁ of the high transmittance region 10X is preferably 450 mm or more and 540 mm or less, but this value is 360 to 640 mm. It is within the above range. Thus, if the diameter R ₁ of the high transmittance region 10X of the crucible bottom portion 10B is 0.45R ₀ or more and 0.8R ₀ or less, the single crystal yield is hardly reduced, and the silicon single crystal being pulled up can be formed. Generation | occurrence | production of the bubble of SiO gas which may be taken in can be suppressed effectively.

  As described above, the bubbles of the SiO gas rise almost vertically, but the bubbles generated outside the projection surface 21S of the silicon single crystal 21 being pulled up (outside the high transmittance region 10X) are horizontal for some reason. As a result, the silicon single crystal 21 may be taken in. However, since the position of such bubbles is near the outer periphery of the silicon single crystal 21 and the vicinity of the outer periphery of the silicon single crystal 21 is ground as an unnecessary portion later, there is no problem even if bubbles are taken in.

  As described above, according to the quartz glass crucible 10 of the present embodiment, since the infrared high transmittance region 10X is formed on the crucible bottom 10B, it is possible to suppress the temperature rise at the crucible bottom. Therefore, SiO gas generated from the bottom of the crucible during the pulling process of the silicon single crystal can be suppressed, and the generation of cavity defects in the silicon single crystal can be prevented.

  Next, a method for manufacturing the quartz glass crucible 10 will be described with reference to the flowchart of FIG.

  The quartz glass crucible 10 can be manufactured by a rotational mold method. In the rotary mold method, natural quartz powder is deposited on the inner surface of the rotating carbon mold with a predetermined thickness (step S11), and then synthetic quartz powder is deposited on the inner surface of the layer made of natural quartz powder with a predetermined thickness. (Step S12).

  Thereafter, arc discharge is performed from the inside of the mold, and the entire inner surface of the quartz powder is heated and melted to 1720 ° C. or higher (step S13). Simultaneously with this heating, pressure is reduced from the mold side, the gas inside the quartz is sucked to the outer layer side through the vent provided in the mold, and exhausted to the outside through the vent, thereby partially removing bubbles on the inner surface of the crucible. Then, the transparent quartz glass layer 12 substantially free of bubbles is formed (step S14). Thereafter, the decompression is stopped at the straight body portion and the curved portion, and further, heating is continued to leave bubbles, thereby forming the opaque quartz glass layer 11 including a large number of minute bubbles (step S15).

  In this embodiment, in order to form the high transmittance region 10X of the crucible bottom portion 10B, the decompression is stopped at the straight barrel portion 10A and the curved portion 10C, but the decompression is continued at the crucible bottom portion 10B, and the opaque quartz glass layer 11 In step S15, a region with few bubbles is formed. Alternatively, at the time of the first decompression, the pressure at the time of decompression is relatively low in the straight body portion 10A and the curved portion 10C, and the pressure at the time of decompression at the bottom portion 10B is relatively high, thereby increasing the infrared transmittance of the bottom portion 10B. May be raised. Thereby, it is possible to form the high transmittance region 10X with less bubbles than the surroundings and high transparency. As described above, a quartz glass crucible including the opaque quartz glass layer 11 constituting the outer layer and the transparent quartz glass layer 12 constituting the inner layer is completed.

  The quartz glass crucible 10 can also be manufactured by a so-called thermal spraying method. Specifically, natural quartz powder that is a raw material for the opaque quartz glass layer 11 is deposited on the entire inner surface of the carbon mold with a predetermined thickness, and arc discharge is performed from the inside of the mold, whereby 1720 natural quartz powder is obtained. The opaque quartz glass layer 11 is formed by heating and melting at a temperature equal to or higher than 0 ° C. Thereafter, a synthetic quartz powder is arc sprayed on the inner surface of the opaque quartz glass layer 11 to form a transparent quartz glass layer 12, thereby completing a quartz glass crucible.

  The preferred embodiments of the present invention have been described above. However, the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the spirit of the present invention. Needless to say, these are also included in the present invention.

  For example, in the above embodiment, a quartz glass crucible using natural quartz powder and synthetic quartz powder as an example has been described as an example. However, the present invention can also be applied to a quartz glass crucible using only natural quartz powder as a raw material. is there.

Example samples A1 to A4 and comparative example samples B1 to B4 of quartz glass crucibles having the same structure as the quartz glass crucible 10 shown in FIG. 1 and having different infrared transmittances at the bottom of the crucible and the straight barrel part were prepared. The infrared transmittance of each sample is as follows. An infrared power meter with a heat receiving area of 1 cm ² is installed at a position 30 cm from an infrared lamp having a wavelength of 0.5 to 3.5 μm and a peak wavelength of 1.0 μm, and the sample is placed immediately before the heat receiving surface. The amount of heat received by infrared rays was measured, and the amount of heat received measured without inserting the crucible piece was calculated as 100%. The size of each crucible sample A1 to A4, B1 to B4 is 32 inches in diameter (diameter 800 mm), the height of the crucible is 500 mm, and the thickness from the inner surface to the outer surface of the crucible is 17 mm straight copper, 25 mm curved, bottom 14 mm. Further, the diameter R ₁ of the high transmittance region 10X was set to 500 mm.

  Next, after 400 kg of polysilicon fragments are filled in the quartz glass crucible samples A1 to A4 and B1 to B4, the quartz glass crucible is loaded into a single crystal pulling apparatus, and the polysilicon in the crucible is melted in the furnace. The silicon single crystal ingot having a diameter of about 320 mm was pulled up.

  Thereafter, a wafer having a thickness of about 1 mm was cut out from the obtained silicon single crystal ingot with a wire saw to produce a polished wafer having a mirror-polished surface. And the pinhole incidence of this polished wafer was measured. A particle measuring device was used to measure the pinhole occurrence rate, and the number of pinholes on the surface of the polished wafer was measured. Moreover, the single crystal yield of the obtained silicon single crystal ingot was also determined. The pinhole generation rate is a value obtained by dividing the total number of pinholes contained in a large number of wafers obtained from one silicon single crystal by the number of wafers. The measurement results are shown in Table 1.

  As shown in Table 1, in Samples A1 to A4 where the infrared transmittance at the bottom of the crucible is in the range of 50 to 80%, the pinhole generation rate was 0.03%, and the single crystal yield was 90% or more. .

  On the other hand, in the sample B3 having an infrared transmittance of 40% at the bottom of the crucible, the single crystal yield was 90%, but the pinhole generation rate was greatly increased to 3.30%. Further, in sample B4 having an infrared transmittance of 85% at the bottom of the crucible, the pinhole generation rate was 0.07%, but the single crystal yield was significantly reduced to 51%.

  In addition, in sample B1 in which the infrared transmittance at the bottom of the crucible is 80% and the difference in infrared transmittance between the bottom and the straight barrel is 40%, the pinhole occurrence rate was 0.05%. The crystal yield was greatly reduced to 47%. Furthermore, in Sample B2, where the infrared transmittance at the bottom of the crucible is 70% and the difference in infrared transmittance between the bottom and the straight body is 5%, the single crystal yield was 93%, but pinholes were generated. The rate increased significantly to 2.00%. As described above, even if the infrared transmittance is in the range of 50 to 80%, if the difference in infrared transmittance between the bottom portion and the straight body portion is not in the range of 10 to 30%, a high-quality silicon single crystal is obtained. I found it impossible.

It is a schematic sectional drawing which shows the structure of the quartz glass crucible for silicon single crystal pulling by preferable embodiment of this invention. It is a schematic sectional drawing which shows the positional relationship of a quartz glass crucible and a silicon single crystal. It is a flowchart which shows the manufacturing method of the quartz glass crucible for silicon single crystal pulling by preferable embodiment of this invention.

10 quartz glass crucible 10A crucible straight body portion 10B crucible bottom portion 10C crucible curved portion 10X high transmittance region 11 opaque quartz glass layer 12 transparent quartz glass layer 21 silicon single crystal 21S silicon single crystal projection surface 22 silicon melt

Claims (4)

A quartz glass crucible for pulling a silicon single crystal having a straight body part and a bottom part,
The infrared transmittance of a region within a certain range from the center of the bottom is higher than the infrared transmittance of the straight body portion,
For infrared rays having a wavelength of 0.5 to 3.5 μm and a peak wavelength of 1.0 μm, the infrared transmittance of the bottom portion is 50 to 80%, and the difference in infrared transmittance between the bottom portion and the straight body portion is 10%. A quartz glass crucible for pulling a silicon single crystal, characterized in that it is ˜30%.   2. The quartz glass crucible for pulling a silicon single crystal according to claim 1, wherein a region within a certain range from the center of the bottom part includes at least a projection surface of the silicon single crystal. Diameter area within a predetermined range from the center of the bottom, the silicon single crystal pulling according to claim 1 or 2, characterized in that 0.45R is ₀ or more 0.8 R ₀ or less with respect to the crucible diameter R ₀ Quartz glass crucible for use. Depositing quartz powder on the inner surface of the rotating mold;
A step of forming a quartz glass crucible by melting the quartz powder,
The step of forming the quartz glass crucible includes a step of sucking a gas inside the quartz powder,
The step of sucking the gas, by the suction time of the gas at the bottom longer than the straight body portion, or be higher than the straight body portion of the suction pressure of the gas in the bottom, wavelength 0.5 A silicon single crystal pulling process including a step of controlling the infrared transmittance of the bottom portion to be higher than the infrared transmittance of the straight body portion with respect to an infrared ray of 3.5 μm and a peak wavelength of 1.0 μm Of manufacturing quartz glass crucibles for use.

Images