JP2010155726A - Method for growing single crystal and single crystal grown by the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To control the oxygen concentration to be uniform and optimum over the whole length of a single crystal and to grow a single crystal free from grown-in defects. <P>SOLUTION: A melt 15 is stored in a crucible 13 accommodated in a chamber 12, 19, and then a single crystal 11 is grown by dipping a seed crystal 22 into the melt 15 and pulling the seed crystal 22. Further, the outer peripheral surface of the single crystal 11 being grown is shielded from the irradiation with radiant heat from a heater 17 by a heat shielding body 28 which is provided at an upper part above the surface of the melt 15 to surround the peripheral surface of the single crystal 11. When the top part of the single crystal 11 is grown, the gap GP between the surface of the melt 15 and the lower end of the heat shielding body 28 is adjusted to 20-60 mm, and when the bottom part of the single crystal 11 is grown, the gap GP is adjusted to 40-80 mm larger than the gap GP during growth of the top part. Thereby, the difference of oxygen concentrations in the top part and the bottom part in the single crystal 11 is controlled to be within ±1.0 ppma. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a method for growing a single crystal such as a silicon single crystal having no grow-in defect (Grown-in defect) by the Czochralski method (hereinafter referred to as CZ method), and a single crystal grown by the method. It is.

  With the recent high integration of semiconductor devices, the design rules are further miniaturized, and minute defects on the silicon wafer as a material have a great influence on the device yield. Thus, when a wafer is produced by slicing the pulled single crystal along a plane perpendicular to the axis, it is necessary to produce a wafer having no glow-in defect over the entire surface of the wafer. Therefore, when the temperature gradient in the axial direction in the vicinity of the solid-liquid interface when pulling the single crystal is G (° C./mm) and the pulling speed is V (mm / min), V / G is constant. It is important to set the pulling speed over the entire length and control the pulling speed to be set. Further, it is necessary to satisfy the specification that the silicon single crystal has no glow-in defect and at the same time contains a predetermined concentration of oxygen in the single crystal.

On the other hand, when growing a single crystal by pulling up from the raw material melt in the chamber by the CZ method, the pulling speed when growing the straight body portion of the single crystal is expressed as V (mm / min), and near the solid-liquid interface. When the crystal temperature gradient in the pulling axis direction is represented by G (° C./mm), the crystal is obtained by changing the distance between the melt surface of the raw material melt and the shielding member disposed opposite to the raw material melt surface in the chamber. A method for manufacturing a single crystal is disclosed in which the temperature gradient G is controlled to control V / G so that a single crystal having a desired defect region can be grown (see, for example, Patent Document 1). In this method for producing a single crystal, when the single crystal is grown by the CZ method, the crystal temperature gradient G can be controlled by changing the distance between the raw material melt surface and the heat shield member. V / G can be controlled without conversion to a single crystal, and a single crystal having a desired defect region can be manufactured efficiently in a short time. Further, if the single crystal can be efficiently manufactured in this way, the productivity in manufacturing the single crystal can be improved and the manufacturing cost can be reduced. Furthermore, by controlling the V / G by changing the distance between the melt surface and the heat shield member in this way, the V / G can be controlled with high accuracy and at the same time, the diameter control of the single crystal by the pulling speed can be enhanced. Since it can be performed stably with high accuracy, a high-quality single crystal having a desired crystal quality and crystal diameter can be stably manufactured with a high yield.
JP-A-2005-15290 (Claim 1, paragraph [0016])

  However, in the conventional method for producing a single crystal shown in Patent Document 1, as shown in FIG. 2 of Patent Document 1, when the first half of the straight body of the single crystal is pulled up, the melt surface and the shielding member are By gradually decreasing the distance and gradually increasing it, and when raising the latter half of the single crystal straight body part, by gradually reducing the distance between the melt surface and the shielding member, the crystal temperature gradient G is controlled, and the pulling speed V is increased. Although V / G is controlled without reducing the speed, if the distance between the melt surface and the shielding member is changed as described above, the oxygen concentration in the single crystal greatly changes depending on the position in the pulling direction, There was a problem that a single crystal having a uniform oxygen concentration in the pulling direction could not be obtained.

An object of the present invention is to provide a method for growing a single crystal that can be controlled to a uniform and optimal oxygen concentration over the entire length of the single crystal and that can grow a single crystal free from glow-in defects.
Another object of the present invention is to provide a single crystal having a uniform and optimal oxygen concentration distribution over the entire length and free from glow-in defects.

  There are various control factors for controlling the oxygen concentration in the single crystal. For example, the rotational speed of a single crystal, the rotational speed of a crucible, the flow rate of an inert gas (such as argon gas) in the chamber, the pressure in the chamber, the position of the silicon melt in the chamber, and the like can be mentioned. However, since the conditions for pulling a single crystal free of glow-in defects are limited, there is a limit to the control of oxygen concentration. Therefore, while controlling the oxygen concentration in the single crystal, the oxygen concentration was also optimized by growing it to an optimal gap depending on the pulling site of the single crystal to grow a single crystal without glow-in defects. It came to make this invention that a single crystal without a grow-in defect can be grown.

  According to the first aspect of the present invention, the melt is stored in a crucible housed in a chamber, a seed crystal is immersed in the melt and pulled up to grow a single crystal, and further provided above the melt surface. This is an improvement of the method for growing a silicon single crystal in which the thermal shield surrounds the outer peripheral surface of the growing single crystal and shields the irradiation of the radiant heat to the outer peripheral surface of the single crystal by the heater. The characteristic configuration is that the gap between the melt surface and the lower end of the heat shield is adjusted to 25 to 60 mm when growing the top portion of the single crystal, and the gap when growing the bottom portion of the single crystal is adjusted to the top portion of the single crystal. The gap is adjusted to 40 to 80 mm, which is larger than the gap at the time of growth, and the difference in oxygen concentration between the top portion and the bottom portion in the single crystal is within ± 1.0 ppma.

  The invention according to claim 2 is the invention according to claim 1, wherein the flow rate of the inert gas flowing through the gap during the growth of the top portion of the single crystal is adjusted to 1.0 to 4.3 mm / second, and the single crystal The flow rate of the inert gas flowing through the gap at the time of growing the bottom portion is adjusted to 0.3 to 1.7 mm / second, which is slower than the flow rate of the inert gas flowing through the gap at the time of growing the top portion of the single crystal. .

  The invention according to claim 3 is the invention according to claim 1 or 2, wherein the pressure in the chamber at the time of growing the top portion of the single crystal is adjusted to 2500 to 4500 Pa, and at the time of growing the bottom portion of the single crystal The pressure in the chamber is adjusted to 4000 to 7000 Pa higher than the pressure in the chamber at the time of growing the top portion of the single crystal.

  The invention according to claim 4 is a single crystal grown by the method according to any one of claims 1 to 3 and having a difference in oxygen concentration between the top portion and the bottom portion of ± 1.0 ppma or less.

  In the invention according to claim 1, the gap at the time of growing the top part is adjusted to 25 to 60 mm, the gap at the time of growing the bottom part is adjusted to 40 to 80 mm larger than the gap at the time of growing the top part, and the top part in the single crystal Since the difference in oxygen concentration between the bottom portion and the bottom portion is ± 1.0 ppma or less, the portion of the single crystal straight body portion where the difference in oxygen concentration is ± 1.0 ppma can be increased to 80% or more. As a result, it is possible to control the oxygen concentration uniformly and optimally over the entire length of the single crystal, and to grow a single crystal free from glow-in defects.

  In the invention which concerns on Claim 2, the flow rate of the inert gas which flows through the gap at the time of top part growth is adjusted to 1.0-4.3 mm / sec, and the flow rate of the inert gas which flows through the gap at the time of bottom part growth is the top Since it was adjusted to 0.3 to 1.7 mm / second, which is slower than the flow rate of the inert gas flowing through the gap at the time of part growth, an effect that the oxygen concentration distribution can be made uniform over the entire length of the single crystal can be obtained.

  In the invention according to claim 3, the pressure in the chamber at the time of growing the top portion is adjusted to 2500 to 4500 Pa, and the pressure in the chamber at the time of growing the bottom portion is adjusted to 4000 to 7000 Pa higher than the pressure in the chamber at the time of growing the top portion. Furthermore, the effect that the oxygen concentration distribution can be made uniform over the entire length of the single crystal can be obtained.

  In the invention according to claim 4, since the difference in oxygen concentration between the top portion and the bottom portion of the single crystal is ± 1.0 ppma or less, the difference in oxygen concentration in the straight body portion of the single crystal is ± 1.0 ppma. Some parts can be increased to 80% or more. As a result, it is possible to obtain a single crystal having a uniform and optimal oxygen concentration distribution over the entire length of the single crystal and having no glow-in defects.

  Next, the best mode for carrying out the present invention will be described with reference to the drawings. As shown in FIG. 1, an apparatus for growing a silicon single crystal 11 includes a main chamber 12 that is configured to be evacuated inside, and a crucible 13 provided in the center of the chamber 12. The main chamber 12 is a cylindrical vacuum container. The crucible 13 includes a bottomed cylindrical inner layer container 13 a formed of quartz and storing the silicon melt 15, and a bottomed cylindrical outer layer container 13 b formed of graphite and fitted to the outside of the inner layer container 13 a. It consists of. The upper end of the shaft 14 is connected to the bottom of the outer layer container 13 b, and a crucible driving means 16 that rotates the crucible 13 through the shaft 14 and moves up and down is provided at the lower end of the shaft 14. Further, the outer peripheral surface of the crucible 13 is surrounded by a cylindrical heater 17 at a predetermined interval from the outer peripheral surface of the crucible 13, and the outer peripheral surface of the heater 17 is predetermined from the outer peripheral surface of the heater 17 by a cylindrical heat retaining cylinder 18. Surrounded at intervals.

  On the other hand, a cylindrical pull chamber 19 having a smaller diameter than the main chamber 12 is connected to the upper end of the main chamber 12 so as to communicate with the inside. In addition, a pulling shaft 21 is suspended in the main chamber 12 through a pull chamber 19 so that the pulling shaft 21 can rotate and move up and down. A seed crystal 22 is detachably mounted on the seed chuck 23 at the lower end of the pulling rod 21. After immersing the lower end of the seed crystal 22 in the silicon melt 15, the seed crystal 22 and the crucible 13 are rotated and raised to pull up the silicon single crystal 11 from the lower end of the seed crystal 22 and grow it. Composed.

  An inert gas consisting only of argon gas flows through the main chamber 12. The inert gas is introduced into the pull chamber 19 through the gas supply pipe 26 connected to the side wall of the pull chamber 19, and is discharged out of the main chamber 12 through the gas discharge pipe 27 connected to the lower wall of the main chamber 12. Configured to be The gas supply pipe 26 is provided with a first flow rate adjustment valve 26a, and the gas discharge pipe 27 is provided with a second flow rate adjustment valve 27a. A heat shield 28 is provided in the main chamber 12 to block the irradiation of the radiant heat of the heater 17 to the outer peripheral surface of the silicon single crystal 11 and to rectify the inert gas. The heat shield 28 has a truncated cone-like cylinder that gradually decreases in diameter as it goes downward and surrounds the outer peripheral surface of the silicon single crystal 11 pulled up from the silicon melt 15 at a predetermined interval from the outer peripheral surface. 28a and a flange portion 28b that is connected to the upper edge of the cylindrical body 28a and projects outward in a substantially horizontal direction. A heat insulating material is provided inside each of the cylindrical portion 28a and the flange portion 28b, and the periphery thereof is covered with carbon. Further, the heat shield 28 is configured such that the flange 28b is placed on the heat retaining cylinder 18 via the ring plate 28c so that the lower edge of the cylinder 28a extends upward from the surface of the silicon melt 15 with a predetermined gap GP. It is fixed in the main chamber 12 so as to be positioned. By adjusting the first and second flow rate adjusting valves 26a and 27a, the pressure in the chamber (the main chamber 12 and the pull chamber 19) flows through the gap GP between the surface of the silicon melt 15 and the lower end of the heat shield 28. The flow rate of the inert gas can be adjusted.

  A method for growing the silicon single crystal 11 using the apparatus configured as described above will be described. First, after depressurizing the chamber (the main chamber 12 and the pull chamber 19), an inert gas (argon gas) is introduced into the chamber, and the pressure in the chamber, that is, when the top portion of the silicon single crystal 11 described later is grown. An inert gas atmosphere in which the pressure in the chamber was reduced to 2500 to 4500 Pa, preferably 2500 to 4000 Pa, and the crystal raw material in the crucible 13 was dissolved by the heater 17. Next, while the pulling shaft 21 is on the same axis as the axis of the shaft 14 and is rotated at a predetermined speed in the direction opposite to the rotation direction of the shaft 14, the seed crystal 22 attached to the seed chuck 23 is lowered and its tip is moved. The part is positioned immediately above the surface of the silicon melt 15. In this state, the gap GP between the surface of the silicon melt 15 and the lower end of the heat shield 28, that is, the gap GP between the surface of the silicon melt 15 and the lower end of the heat shield 28 at the time of growth of the top portion described later of the silicon single crystal 11 is 25. After the crucible 13 is lowered by the crucible driving means 16 so as to be ˜60 mm, preferably 25 to 50 mm, the flow rate of the inert gas flowing through the gap GP, that is, the gap at the time of growing the top portion of the silicon single crystal 11 which will be described later Is set to 1.0 to 4.3 mm / sec, preferably 2.0 to 4.3 mm / sec. The flow rate of the inert gas flowing through the gap GP is a value measured at the inner peripheral portion of the lower end of the cylindrical body 28a of the heat shielding member 28.

  The grown silicon single crystal 11 has a top portion, a middle portion, and a bottom portion. When the length of the straight body portion of the pulled silicon single crystal 11 is 100%, the top portion of the silicon single crystal 11 is a conical portion whose diameter gradually increases when the seed crystal 22 is pulled up from the silicon melt 15. , The part consisting of the upper straight body part from the time when the straight body part starts to be pulled up to the time when the straight body part is pulled up from 0% to 33.3%, and the bottom part is the straight part A portion composed of a lower straight body portion between the time when the body portion is pulled up 66.7% and the time when the straight body portion is raised 100%, and an inverted conical portion that is continuous with the lower straight body portion and gradually decreases in diameter. . Moreover, a middle part means the straight body part between an upper straight body part and a lower straight body part.

  Here, the reason why the pressure in the chamber at the time of growing the top portion of the silicon single crystal 11 is limited to the range of 2500 to 4500 Pa cannot be achieved with a vacuum pump having a vacuum capacity that is normally used at less than 2500 Pa, and exceeds 4500 Pa. This is because the oxygen concentration in the silicon single crystal 11 becomes high. The reason why the gap GP when growing the top portion of the silicon single crystal 11 is limited to the range of 25 to 80 mm is that when the gap GP is set, the heat shield 28 is too close to the surface of the silicon melt 15 if it is less than 25 mm. This is because the lower end of the body 28 may come into contact with the silicon melt 15, and if it exceeds 80 mm, the temperature gradient in the axial direction of the silicon single crystal 11 near the solid-liquid interface will decrease. Furthermore, the flow rate of the inert gas flowing through the gap GP during the growth of the top portion of the silicon single crystal 11 is limited to the range of 1.0 to 4.3 mm / second. This is because if the oxygen concentration of the silicon becomes high and exceeds 4.3 mm / sec, the flow rate is too high and the silicon single crystal 11 is easily dislocated.

  In this state, the crucible 13 is rotated at a predetermined rotational speed, and while pulling the seed crystal 22 immersed in the silicon melt 15 while rotating the seed crystal 22 at a predetermined rotational speed in a direction opposite to the crucible 13, The silicon single crystal 11 is grown from the silicon melt 15 and the conical portion and the upper straight body portion are grown through the neck portion. The pulling speed of the silicon single crystal 11 at this time is set to 0.3 to 5.0 mm / min, preferably 0.3 to 2.0 mm / min. Here, the pulling speed of the silicon single crystal 11 is limited to the range of 0.3 to 5.0 mm / min because if the pulling speed is less than 0.3 mm / min, the pulling speed is too low and the productivity of the silicon single crystal 11 is poor. This is because if it exceeds 5.0 mm / min, the pulling speed is too high and the silicon single crystal 11 is easily dislocated.

  Next, when the middle part of the silicon single crystal 11 is grown, the gap GP is gradually increased to 40 to 80 mm, preferably 40 to 70 mm, and the flow rate of the inert gas flowing through the gap GP is gradually increased. The pressure in the chamber is adjusted to 0.3 to 1.7 mm / second, preferably 0.3 to 1.5 mm / second, and the pressure in the chamber is gradually increased to 4000 to 7000 Pa, preferably 4000 to 6500 Pa. Then, the bottom portion (lower straight body portion and inverted conical portion) of the silicon single crystal 11 is grown with the changed gap GP, the flow rate of the inert gas, and the pressure in the chamber. Thereby, the gap GP when the bottom portion of the silicon single crystal 11 is grown is larger by 10 to 55 mm, preferably 10 to 40 mm than the gap GP when the top portion of the silicon single crystal 11 is grown. Further, the flow rate of the inert gas flowing through the gap GP when the bottom portion of the silicon single crystal 11 is grown is 0.7 to 4 than the flow rate of the inert gas flowing through the gap GP when the top portion of the silicon single crystal 11 is grown. .3 mm / sec, preferably 0.7 to 4.0 mm / sec. Furthermore, the pressure in the chamber when the bottom portion of the silicon single crystal 11 is grown is higher by 1500 to 4500 Pa, preferably 1500 to 4000 Pa than the pressure in the chamber when the top portion of the silicon single crystal 11 is grown. Here, the gap GP at the time of growing the bottom portion of the silicon single crystal 11 is limited to the range of 40 to 80 mm. If the gap GP is less than 40 mm, the control range of the flow rate of the inert gas is narrowed and the flow rate of the inert gas is decreased. This is because if the thickness exceeds 80 mm, the temperature gradient in the axial direction of the single crystal 11 near the solid-liquid interface becomes too small. The flow rate of the inert gas flowing through the gap GP during the growth of the bottom portion of the silicon single crystal 11 is limited to the range of 0.3 to 1.7 mm / second. This is because the flow rate is too small and vapor (steam) from the silicon melt 15 may rise, and if it exceeds 1.7 mm / second, it becomes disadvantageous to make the oxygen concentration in the silicon single crystal 11 uniform. Furthermore, the pressure in the chamber at the time of growing the bottom portion of the silicon single crystal 11 is limited to the range of 4000 to 7000 Pa. If the pressure is less than 4000 Pa, the oxygen concentration is lower than the top portion of the silicon single crystal 11 and exceeds 7000 Pa. This is because the oxygen concentration in the silicon single crystal 11 becomes high. The changing speed of the gap GP is 0.01 to 0.1 mm / min, and the gap GP is set by the pulling length of the silicon single crystal 11.

  In the silicon single crystal 11 grown in this way, the difference in oxygen concentration between the top portion and the bottom portion in the silicon single crystal 11 is ± 1.0 ppma or less. The portion where the difference in concentration is ± 1.0 ppma can be increased to 80% or more. As a result, it is possible to control the oxygen concentration to be uniform and optimal over the entire length of the silicon single crystal 11 and to grow the silicon single crystal 11 having no glow-in defect.

  In this embodiment, a silicon melt is used as the melt, and a silicon single crystal is used as the single crystal. However, a GaAs melt and a GaAs single crystal, an InP melt and an InP single crystal, a ZnS melt and a ZnS single crystal are used. A crystal, or a ZnSe melt and a ZnSe single crystal may be used.

Next, examples of the present invention will be described in detail together with comparative examples.
<Example 1>
A silicon single crystal having a diameter of 200 mm was grown using a growth apparatus shown in FIG. 1 by a heat transfer analysis simulation using a computer. Specifically, first, the inside of the chamber (the main chamber 12 and the pull chamber 19) is decompressed, and then an argon gas (inert gas) is introduced to create an inert gas atmosphere in which the inside of the chamber is decompressed to 2600 Pa. The raw material was melted by the heater 17. Next, the crucible 13 is rotated at a speed of 10 rpm, and the seed crystal 22 attached to the seed chuck 23 is lowered while rotating the pulling shaft 21 at a speed of 10 rpm in the direction opposite to the direction of rotation of the crucible 13, and the tip portion thereof. Was positioned immediately above the surface of the silicon melt 15. In this state, after the crucible 13 is lowered by the crucible driving means 16 so that the gap GP between the silicon melt 15 and the lower end of the heat shield 28 becomes 50 mm, the flow rate of the inert gas flowing through the gap GP is 1.3 mm / The first and second flow rate adjusting valves 26a and 27a were adjusted so as to be seconds. In this state, the seed crystal 22 was immersed in the surface of the silicon melt 15 to grow a top portion (cone portion and upper straight body portion) through the neck portion of the silicon single crystal 11. Next, when the middle portion of the silicon single crystal 11 is grown, the gap GP is gradually increased to 70 mm, and the flow rate of the inert gas flowing through the gap GP is gradually decreased to 0.5 mm / The pressure in the chamber is further increased to 7000 Pa by gradually increasing the pressure in the chamber, and the bottom portion of the silicon single crystal 11 (the lower straight body portion and the lower body portion) is adjusted with the changed gap GP, the flow rate of the inert gas, and the pressure in the chamber. The inverted cone was nurtured. As a result, the gap GP is increased by 20 mm when the bottom portion of the silicon single crystal 11 is grown, the flow rate of the inert gas flowing through the gap GP is decreased by 0.8 mm / second, and the pressure in the chamber is increased by 4400 Pa. It was. The changing speed of the gap GP was 0.1 mm / min. Note that changes in the gap GP, the flow rate of the inert gas, and the pressure in the chamber with respect to the change in the pulling length of the silicon single crystal 11 are shown in FIGS.

<Comparative Example 1>
When the middle part of the silicon single crystal is grown, the bottom part (lower straight body part and inverted conical part) is grown without changing the gap, the flow rate of the inert gas, and the pressure in the chamber as in Example 1 above. A silicon single crystal was grown in the same manner as in Example 1 except that.
<Comparative example 2>
Although the gap and the flow rate of the inert gas were not changed during the growth of the middle part of the silicon single crystal, the bottom part (lower) was changed by increasing only the pressure in the chamber to 7000 Pa. A silicon single crystal was grown in the same manner as in Example 1 except that the straight body portion and the reverse cone portion were grown.
<Comparative Example 3>
Before the silicon single crystal is grown, the gap is set to 50 mm (the same gap as in the top portion growth in Example 1), and the flow rate of the inert gas is 0.5 mm / second (in the bottom portion growth in Example 1). Except that the top part, the middle part and the bottom part of the silicon single crystal were grown by setting the pressure in the chamber to 7000 Pa (same pressure as in the bottom part growth of Example 1). Grown a silicon single crystal in the same manner as in Example 1.
<Comparative example 4>
Before the silicon single crystal is grown, the gap is set to 70 mm (the same gap as in the bottom portion growth in Example 1), and the flow rate of the inert gas is 0.5 mm / second (in the bottom portion growth in Example 1). Except that the top part, the middle part and the bottom part of the silicon single crystal were grown by setting the pressure in the chamber to 7000 Pa (same pressure as in the bottom part growth of Example 1). Grown a silicon single crystal in the same manner as in Example 1.

<Comparative test 1 and evaluation>
A change in pulling speed with respect to a change in pulling length of the silicon single crystal of Example 1 and Comparative Examples 1 to 4, a region having no glow-in defect in the pulling direction and the radial direction of the silicon single crystal with respect to the pulling length change of the silicon single crystal The change in the ingot pulling speed (defect-free margin) and the change in oxygen concentration in the silicon single crystal with respect to the pulling length change in the silicon single crystal were measured. The results are shown in FIGS.

  In Comparative Example 1, the pulling rate was relatively high at 0.7 mm / min and a large defect-free margin could be secured, but the oxygen concentration in the silicon single crystal gradually decreased from 13 ppma to 8 ppma (FIG. 4). Then, although the oxygen concentration in the silicon single crystal became almost constant over the entire length of 13 to 10 ppma, the pulling rate gradually decreased from 0.7 mm / min to 0.65 mm / min when growing the bottom portion, and the defect-free margin was reduced. It gradually became smaller (FIG. 5). In Comparative Example 3, the pulling rate is relatively low at 0.65 mm / min, the defect-free margin is narrow, and the oxygen concentration in the silicon single crystal varies in the pulling direction of the silicon single crystal (FIG. 6). In No. 4, the pulling rate was relatively high at 0.7 mm / min, and a wide defect-free margin could be secured, but the oxygen concentration in the silicon single crystal varied in the pulling direction of the silicon single crystal (FIG. 7). On the other hand, in Example 1, the pulling rate was relatively high at 0.7 mm / min and a large defect-free margin could be secured, and the oxygen concentration in the silicon single crystal was almost constant over the entire length of 12 to 10 ppma ( FIG. 3).

It is a longitudinal section lineblock diagram of an apparatus for growing a silicon single crystal of an embodiment of the present invention. (A) is a figure which shows the change of the gap with respect to the pulling length of the silicon single crystal of Example 1, (b) is a figure which shows the change of the argon gas flow rate with respect to the change of the pulling length of the silicon single crystal of Example 1. FIG. 6C is a diagram showing the change in the pressure in the chamber with respect to the change in the pulling length of the silicon single crystal of Example 1. (A) is a figure which shows the change of the pulling speed with respect to the pulling length of the silicon single crystal of Example 1, (b) is the oxygen concentration in the silicon single crystal with respect to the change of the pulling length of the silicon single crystal of Example 1. It is a figure which shows a change. (A) is a figure which shows the change of the pulling speed with respect to the pulling length of the silicon single crystal of the comparative example 1, (b) is the oxygen concentration in the silicon single crystal with respect to the pulling length of the silicon single crystal of the comparative example 1. It is a figure which shows a change. (A) is a figure which shows the change of the pulling speed with respect to the pulling length of the silicon single crystal of the comparative example 2, (b) is the oxygen concentration in the silicon single crystal with respect to the pulling length of the silicon single crystal of the comparative example 2. It is a figure which shows a change. (A) is a figure which shows the change of the pulling speed with respect to the pulling length of the silicon single crystal of the comparative example 3, (b) is the oxygen concentration in the silicon single crystal with respect to the pulling length of the silicon single crystal of the comparative example 3. It is a figure which shows a change. (A) is a figure which shows the change of the pulling speed with respect to the pulling length of the silicon single crystal of the comparative example 4, (b) is the oxygen concentration in the silicon single crystal with respect to the pulling length of the silicon single crystal of the comparative example 4. It is a figure which shows a change.

Explanation of symbols

11 Silicon single crystal 12 Main chamber (chamber)
13 Crucible 15 Silicon melt 17 Heater 19 Pull chamber (chamber)
22 Seed crystal 28 Heat shield GP gap

Claims (4)

A melt is stored in a crucible accommodated in a chamber, a seed crystal is immersed in the melt and pulled up to grow a single crystal, and a heat shield provided above the melt surface further grows the crystal. In the method for growing a silicon single crystal that surrounds the outer peripheral surface of the single crystal and shields the irradiation of radiant heat to the outer peripheral surface of the single crystal by a heater,
Adjusting the gap between the melt surface and the lower end of the heat shield at the time of growing the top part of the single crystal to 25-60 mm;
Adjusting the gap at the time of growing the bottom portion of the single crystal to 40 to 80 mm larger than the gap at the time of growing the top portion of the single crystal;
A method for growing a single crystal, wherein a difference in oxygen concentration between the top portion and the bottom portion in the single crystal is ± 1.0 ppma or less.   The flow rate of the inert gas flowing through the gap during the growth of the top portion of the single crystal is adjusted to 1.0 to 4.3 mm / second, and the flow rate of the inert gas flowing through the gap during the growth of the bottom portion of the single crystal is adjusted to The method for growing a single crystal according to claim 1, wherein the growth rate is adjusted to 0.3 to 1.7 mm / second slower than the flow rate of the inert gas flowing through the gap when growing the top portion of the single crystal.   The pressure in the chamber at the time of growing the top portion of the single crystal is adjusted to 2500 to 4500 Pa, and the pressure in the chamber at the time of growing the bottom portion of the single crystal is adjusted in the chamber at the time of growing the top portion of the single crystal. The method for growing a single crystal according to claim 1 or 2, wherein the pressure is adjusted to 4000 to 7000 Pa higher than the pressure.   A single crystal grown by the method according to any one of claims 1 to 3, wherein the difference in oxygen concentration between the top portion and the bottom portion is ± 1.0 ppma or less.

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