TW201800625A - Single crystal silicon manufacturing method - Google Patents

Abstract

A single crystal silicon manufacturing method using Czochralski method can prevent crystal tortuosity and reduction of single crystallization ratio due to separation from molten liquid, and restrain epitaxial defects when the single crystal silicon is used as substrate materials of epitaxial silicon wafers. The single crystal silicon manufacturing method includes: a body growth step wherein a body 3c with a crystal diameter maintained constant is grown; and a tail growth step wherein a tail 3d with a crystal diameter decreased slowly is grown. A water cooling body 18 is used to cool the single crystal silicon 3 pulled up from the silicon molten liquid. The cooling body 18 is disposed above the lower end 17b, and at the inner side of a heat shelter 17 which is disposed above a quartz crucible 11. In the tail growth step, from the beginning to the end of the growth of the tail 3d, the single crystal silicon 3d is pulled up at a pulling-up speed equal to the pulling-up speed at the time when the growth of the body is end.

Description

Method for manufacturing single crystal silicon

The present invention relates to a method of manufacturing single-crystal silicon using the Tchaisky method (hereinafter referred to as the CZ method), and particularly to a method of cultivating the tail of a single-crystal silicon rod.

As a substrate material for semiconductor devices, epitaxial silicon wafers are widely used. An epitaxial silicon wafer is a product formed by forming an epitaxial layer on the surface of a monolithic silicon substrate. Because of the high crystal integrity, a high-quality and highly reliable semiconductor device can be manufactured.

The single crystal silicon used as the substrate material of the epitaxial silicon wafer is mostly manufactured by the CZ method. In the CZ method, raw materials such as polycrystalline silicon are filled into a quartz crucible, and the silicon raw materials are heated and melted in the chamber. Next, the seed crystal attached to the lower end of the pull-up shaft is lowered from above the quartz crucible to contact the silicon melt, and the seed crystal is slowly raised while rotating the seed crystal and the crucible, thereby growing under the seed crystal Large diameter single crystal.

As a method of manufacturing epitaxial silicon wafers, for example, Patent Document 1 discloses that when pulling up a single crystal silicon rod, the temperature range of 1030 to 920 ° C during the pulling up is cooled at a rate of 1.0 ° C / min or more, and then In the temperature range of 920 ~ 720 ℃, after the single crystal silicon is cultivated at a cooling rate of 0.5 ℃ / min or more, it is cut out from the single crystal Epitaxial layer is formed on the surface of the wafer. The temperature range (1030 ~ 920 ℃) where the core of OSF (Oxygen induced Stacking Fault) is easy to grow quickly is reduced to a very small size, thereby suppressing the generation of epitaxial defects caused by OSF .

In the pull-up step of the single crystal, a necking step to narrow the crystal value by the punching method to make the single crystal non-displacement, a shoulder cultivating step to gradually increase the crystal diameter, while maintaining the crystal diameter at Continue to grow the body growth step of the crystal at a certain value, and gradually reduce the diameter of the crystal to form the tail growth step of the conical tail. Among them, the tail rearing step is to prevent the thermal equilibrium collapse between the melt and the single crystal existing at the crystal growth interface and give the crystal a sharp thermal shock, resulting in the occurrence of quality abnormalities such as sliding dislocation or abnormal oxygen analysis. Steps necessary to separate the single crystal from the melt.

Regarding the tail rearing step, for example, Patent Document 2 describes that the pulling speed of the tip cone (tail) of the ingot is maintained at the same speed as the second half of the body (body) of the ingot A relatively constant speed, and if necessary, will increase the power (heat) supplied to the heater, or reduce the crystal rotation speed or crucible rotation speed to produce a single crystal silicon rod with a uniform thermal history.

Advanced technical literature

Patent Document 1: Japanese Patent Laid-Open No. 2010-30856

Patent Document 2: Japanese Patent Laid-Open No. 10-95698

In Patent Document 1, a single crystal pulling device equipped with a water cooling body is used, Controlling the pull-up speed during crystallization of the single crystal The temperature change in the direction of the pull-up axis of the single crystal after crystallization. However, the part used as the substrate material of epitaxial silicon wafers is the body part (straight body part) whose crystal diameter is kept constant, and the tail part is not used as a wafer product. Therefore, although Patent Document 1 describes the cooling conditions of the body, it does not describe the specific pulling conditions such as the pulling speed of the tail portion, the heater power, and the rotation speed of the single crystal.

In the rearing of the tail, it is common practice to accelerate the pulling speed of the single crystal and gradually narrow the crystal diameter. This is because the tail can be simply narrowed by increasing the pulling speed of the single crystal, and the shortening of the tail incubation time will reduce the manufacturing cost. In addition, as mentioned above, the tail is a part that does not become a wafer product, and increasing the pulling speed to lower the crystal quality of the tail itself will not cause any problems. For this reason, in the past, in the general tail growing step, the control of increasing the pulling speed of the single crystal is performed, and even in Patent Document 1, the condition that the tail is easily narrowed is adopted.

However, in the tail rearing step, if the speed of pulling up the single crystal is increased, there is a risk of the crystal bending or the single crystal suddenly separating from the melt and causing the single crystal to be misaligned.

Patent Document 2 discloses that the pulling speed of the tail is maintained at a relatively constant speed that is the same as the pulling speed of the second half of the body. Keeping the pulling speed of the tail part controlled like this, at first glance, the whole body of the single crystal will have a certain cooling rate and residence time.

However, if the tail pull-up speed is set to the same speed as the body, the pull-up speed of the single crystal will become slower than the conventional tail growth step, so the single crystal silicon pulled up from the silicon melt stays at OSF nucleation time in the temperature field It will actually become longer, risking increased misalignment defects.

In addition, in the tail rearing step, the crystal diameter gradually decreases. As shown in FIG. 8, the distance D between the heat shield 17 and the single crystal silicon 3 becomes larger, and the heat from the silicon melt 2 etc. is shown by the white arrow The ground diffuses upward, and the surroundings of the crystallized single crystal silicon 3 increase in temperature. In such an environment, when the tail portion 3d of the single crystal silicon 3 is slowly pulled up at the same pulling speed as the body portion 3c, the influence of the increase in temperature around the single crystal silicon 3 changes greatly. In other words, the time for the single crystal silicon 3 pulled up from the silicon melt 2 to stay in the OSF nucleus formation temperature region becomes longer, and the epitaxial defects increase.

In addition, unlike the case where the body portion 3c is pulled up, the crystal diameter of the tail portion 3d is reduced, and the state of pulling up the crystal changes from time to time, so it is easy to be displaced. In addition, in the tail rearing step, the amount of melt in the crucible is small, and the bottom of the crucible holds the melt. Therefore, the state of the melt in the crucible changes with time as the tail 3d is pulled up, and misalignment is likely to occur. Therefore, when the tail portion 3d is pulled up at the same speed as the body portion 3c, there is a problem that the time until the end of the tail portion 3d is pulled up becomes long, and the risk of misalignment of the tail portion 3d increases.

Therefore, an object of the present invention is to provide a method for manufacturing single crystal silicon, which can prevent the use of a substrate material as an epitaxial silicon wafer while preventing the reduction of the single crystal rate caused by crystal bending or separation from the melt The occurrence of epitaxial defects at the time.

In order to solve the above-mentioned problems, the method for manufacturing single-crystal silicon of the present invention uses the Tchaikovsky method of pulling single-crystal silicon from the silicon melt in a quartz crucible to manufacture single-crystal silicon, including: a body growing step, The rearing crystal diameter maintains a certain body; the rearing step is to rearwardly reduce the rearward diameter of the crystal, wherein a water cooling body is used to cool the single crystal silicon pulled from the silicon melt, the water cooling body is arranged In the tail rearing step, which is higher than the lower end of the heat shield arranged above the quartz crucible and inside the heat shield, from the start of the rear of the tail to the end, the end of the rear of the body is used The single-crystal silicon is pulled up at the same pull-up speed at the same time.

In the tail rearing step, the crystal diameter gradually decreases so that the lateral gap between the heat shield and the single crystal gradually becomes larger, the heat shielded by the heat shield diffuses upward, and the single crystal silicon becomes difficult to be cooled. In addition, in the tail rearing step, in order to avoid the contact between the heat shield and the crucible and stop the rise of the quartz crucible, the lowering of the melt surface will gradually widen the gap between the heat shield and the melt surface. Radiant heat is more likely to spread upward. Therefore, the crystal quality of the body near the tail is affected by heat and becomes different from the crystal quality of the upper side. That is, the residence time in the temperature range of 1020 to 980 ° C becomes longer, forming a slow cooling state, and forming crystals containing large OSF nuclei that are prone to epitaxial defects.

However, according to the present invention, since the water-cooling body is provided around the pull-up path above the heat shield, it is possible to shorten the stay of a crystallized single-crystal silicon in the OSF formation temperature range without increasing the pull-up speed of the single crystal Period. Therefore, it is possible to manufacture a single crystal silicon, which can prevent the reduction of the single crystallization rate caused by the warpage of the crystal or the separation of the crystal from the melt, and can suppress the occurrence of epitaxial defects during the formation of the epitaxial layer.

In the tail rearing step, in the tail rearing step, the body of the single crystal silicon is preferably passed through the temperature range of 1020 ° C to 980 ° C within 15 minutes. In this way, the single-crystal silicon pulled up from the silicon melt quickly passes through the OSF core formation temperature region, whereby the size of the single-crystal silicon OSF core can be reduced. Therefore, in the single crystal When an epitaxial layer is formed on the surface of a silicon wafer cut from a silicon rod, epitaxial defects caused by OSF can be suppressed.

In the method for manufacturing single crystal silicon of the present invention, the power of the heater for heating the silicon melt is gradually increased from the beginning to the end of the rearing of the tail, and the power of the heater is set to It is preferable that the power of the heater is 1.1 times or more and 1.5 times or less at the start of rearing the tail. According to such a method, tail shrinkage can be realized while preventing the crystal from bending or separating the single crystal from the silicon melt.

In the tail rearing step, in the tail rearing step, it is better to raise the quartz crucible to keep the interval between the heat shield and the silicon melt constant. Until the end of the rearing step, the quartz crucible is continuously raised to keep the height of the melt surface constant, thereby suppressing the influence of radiant heat from the quartz crucible and suppressing the expansion of the OSF nucleation temperature range.

In the tail rearing step, the rotation speed of the quartz crucible or the single crystal silicon is preferably kept constant, and it is also preferable to apply a magnetic field to the silicon melt. In this tail rearing step, the amount of melt in the quartz crucible is small, and in order to hold the melt at the bottom of the crucible, the melt is easily affected by the change in the rotation speed of the quartz crucible, and the state of the melt will be unstable. Keeping the rotation speed constant, you can try to stabilize the melt state, which can reduce the risk of dislocation of single crystal silicon. Similarly, by maintaining a constant rotation speed of the single crystal silicon, or by applying a magnetic field to the silicon melt, an attempt can be made to stabilize the melt state in the rearing step, which can reduce the risk of dislocation of the single crystal silicon . In addition, the rotation speed of the quartz crucible and single crystal silicon may be substantially constant, and the variation of ± 2 rpm is within the allowable range.

According to the present invention, it is possible to provide a method for manufacturing single-crystal silicon, which can prevent the reduction of the single-crystallization rate caused by crystal bending or separation from the melt, and at the same time suppress the use of the substrate material as an epitaxial silicon wafer The occurrence of epitaxial defects.

1A, 1B‧‧‧Single crystal manufacturing equipment

2‧‧‧Silver melt

3‧‧‧Single crystal silicon

3a‧‧‧Neck

3b‧‧‧Shoulder

3c‧‧‧Body

3d‧‧‧tail

10‧‧‧ chamber

10a‧‧‧Main chamber

10b‧‧‧traction chamber

10c‧‧‧Gas inlet

10d‧‧‧gas outlet

10e‧‧‧ observation window

11‧‧‧Quartz crucible

12‧‧‧Carrier

13‧‧‧rotation axis

14‧‧‧Rotary shaft drive mechanism

15‧‧‧heater

16‧‧‧Insulation

17‧‧‧ Cover

17a‧‧‧Opening

17b‧‧‧lower

17i‧‧‧Inside

18‧‧‧Water cooling body

19‧‧‧Single crystal pulling wire

20‧‧‧coil winding mechanism

21‧‧‧ magnetic field generating device

22‧‧‧CCD camera

23‧‧‧Image Processing Department

24‧‧‧Control Department

FIG. 1 is a side cross-sectional view schematically showing the structure of a single crystal manufacturing apparatus according to a first embodiment of the present invention.

FIG. 2 is a flowchart illustrating a method for manufacturing single crystal silicon according to an embodiment of the present invention.

Figure 3 is a schematic cross-sectional view showing the shape of a single crystal silicon rod.

Fig. 4 is a schematic cross-sectional view showing the state of pulling up of the single crystal in the tail growing step.

Fig. 5 is a sequence diagram showing the change of the pulling speed of the single crystal and the heater power.

FIG. 6 is a side cross-sectional view schematically showing the structure of a single crystal manufacturing apparatus according to a second embodiment of the present invention.

Fig. 7 is a graph showing the relationship between the pulling position of a single crystal and the passage time of the single crystal's OSF nucleation temperature range (1020 to 980 ° C).

Figure 8 is used to explain the conventional problems in the rearing step.

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

FIG. 1 is a side cross-sectional view schematically showing the structure of a single crystal manufacturing apparatus according to a first embodiment of the present invention.

As shown in FIG. 1, the single crystal manufacturing apparatus 1A includes: a chamber 10; a quartz crucible 11 that holds a silicon melt 2 in the chamber 10; a carrier 12 made of graphite that holds a quartz crucible 11; a rotating shaft 13, Support carrier 12; rotating shaft drive mechanism 14, which rotates and lifts the rotating shaft 13; heater 15, which is arranged around the carrier 12; heat insulation material 16, which is arranged along the inner surface of the chamber 10 outside the heating side 15 ; The heat shield 17 is arranged above the quartz crucible 11; the water-cooled body 18, which is arranged above the lower end of the heat shield 17 inside the heat shield; the wire 19 for pulling up the single crystal, is located above the quartz crucible 11 Is arranged coaxially with the rotating shaft 13; the winding mechanism 20 is arranged above the chamber 10.

Further, the single crystal manufacturing apparatus 1A includes: a magnetic field generating device 21 arranged outside the chamber 10; a CCD camera 22, which shoots inside the chamber 10; an image processing section 23, which processes images shot by the CCD camera 22; a control section 24, based on The output of the image processing unit 23 controls the shaft drive mechanism 14, the heater 15, and the winding mechanism 20.

The chamber 10 is composed of a main chamber 10a and an elongated cylindrical traction chamber 10b connected to the upper opening of the main chamber 10a. The quartz crucible 11, the carrier 12, the heater 15 and the heat shield 17 are provided in the main chamber 10a. The traction chamber 10b is provided with a gas introduction port 10c for introducing inactive gas (rinsing gas) such as argon gas into the chamber 10, and a gas discharge port 10d for discharging the inactive gas is provided in the lower part of the main chamber 10a. In addition, an observation window 10e is provided on the upper portion of the main chamber 10a, and the growth state of the single crystal silicon 3 can be observed through the observation 10e.

The quartz crucible 11 is a quartz glass container having a cylindrical side wall portion and a curved bottom. In order to maintain the shape of the quartz crucible 11 softened by heating, the carrier 12 is held so as to cover the quartz crucible 11 so as to cover the quartz crucible 11. The quartz crucible 11 and the carrier 12 constitute a support in the chamber 10 A double-structure crucible of silicon melt.

The carrier 12 is fixed to the upper end portion of the rotating shaft 13 extending in the vertical direction. In addition, the lower end portion of the rotating shaft 13 penetrates the center of the bottom of the chamber 10 and is connected to the rotating shaft drive mechanism 14 provided outside the chamber 10. The carrier 12, the rotating shaft 13 and the rotating shaft drive mechanism 14 constitute a rotating mechanism and a lifting mechanism of the quartz crucible 11.

The heater 15 is used to melt the silicon raw material filled in the quartz crucible 11 to produce the silicon melt 2. The heater 15 is an impedance heating heater made of carbon, and is provided so as to surround the quartz crucible 11 in the carrier 12. In addition, the outside of the heater 15 is surrounded by the heat insulating material 16, whereby the heat retention in the chamber 10 is improved.

The heat shield 17 is provided to suppress the temperature fluctuation of the silicon melt 2, form an appropriate hot zone near the solid-liquid interface, and prevent radiant heat from the heater 15 and the quartz crucible 11 from heating the single crystal silicon 3. The heat shield 17 is a graphite member that covers the area above the silicon melt 2 except for the path through which the single crystal silicon 3 is pulled up, and has a reverse cone trapezoid whose diameter decreases from above to below.

In the center of the lower end of the heat shield 17, a circular opening 17 a larger than the diameter of the single crystal silicon 3 is formed to ensure the pulling path of the single crystal silicon 3. As shown in the figure, the single crystal silicon 3 is pulled upward through the opening 17a. The diameter of the opening 17a of the heat shield 17 is smaller than the diameter of the quartz crucible 11, and the lower end of the heat shield 17 is located inside the quartz crucible 11, so even if the upper edge of the quartz crucible 11 is raised to be more than the lower end of the heat shield 17 Even above, the heat shield 17 does not interfere with the quartz crucible 11.

As the single crystal silicon 3 grows, the amount of molten metal in the quartz crucible 11 decreases, but by raising the quartz crucible 11 the gap (gap ΔG) between the molten surface and the heat shield 17 is kept constant, and the silicon can be suppressed The temperature of the melt 2 changes, and the flow velocity of the gas flowing near the melt surface (flushing gas induction path) can be maintained Certainly, the evaporation amount of the dopant from the silicon melt 2 is controlled. Therefore, the stability of the crystal defect distribution, oxygen concentration distribution, and resistivity distribution of the single crystal in the direction of the pull-up axis can be improved.

Inside the heat shield 17 above the lower end 17 b of the heat shield 17, a water cooling body 18 is arranged. Like the heat shield 17 and the like, the water cooling body 18 is provided so as to surround the pulling path of the single crystal silicon 3. The water-cooled body 18 is composed of a metal having good thermal conductivity, such as copper, iron, stainless steel (SUS), and molybdenum. It is preferable that the cooling water can be circulated inside to maintain the surface temperature in the range of normal temperature to 200 ° C. The details will be described later, but by including this water-cooling body 18, the cooling of a crystallized single crystal silicon 3 can be promoted.

Above the quartz crucible 11, a wire 19 as a pull-up shaft of the single crystal silicon 3 and a wire winding mechanism 20 for winding the wire 19 are provided. The wire winding mechanism 20 has a function of rotating the wire 19 together with the single crystal. The wire winding mechanism 20 is arranged above the traction chamber 10b, the wire 19 extends downward from the wire winding mechanism 20 through the traction chamber 10b, and the front end portion of the wire 19 reaches the internal space of the main chamber 10a. Fig. 1 shows the state in which the single crystal silicon 3 during the breeding is suspended on the wire 19. When the single crystal is pulled up, the seed crystal is immersed in the silicon melt 2. While the quartz crucible 11 and the seed crystal are respectively rotated, the wire 19 is slowly pulled up, thereby growing the single crystal.

The upper part of the traction chamber 10b is provided with a gas inlet 10c for introducing inactive gas into the chamber 10, and the bottom of the main chamber 10a is provided with a gas discharge port 10d for discharging inert gas in the chamber 10. The inert gas is introduced into the chamber 10 from the gas introduction port 10c, and the introduction amount is controlled by a valve. In addition, the inert gas in the sealed chamber 10 is exhausted from the outside of the chamber 10 through the gas discharge port 10d, so the SiO gas or CO gas generated in the chamber 10 can be recovered and the chamber is maintained Clean room 10. Although not shown, the vacuum pump is connected to the gas discharge port 10d through a pipe, and the flow rate is controlled by a valve while sucking the inert gas in the chamber 10 by the vacuum pump, thereby keeping the chamber 10 at a certain decompressed state .

The magnetic field generating device 21 applies a horizontal magnetic field or a vertical magnetic field to the silicon melt 2. By applying a magnetic field to the silicon melt 2, it is possible to suppress the convection of the melt in the direction orthogonal to the lines of magnetic force. Therefore, the elution of oxygen from the quartz crucible 11 can be suppressed, and the oxygen concentration in the single crystal silicon can be reduced.

The upper part of the main chamber 10a is provided with an observation window 10e to observe the inside, and the CCD camera 22 is provided outside the observation window 10e. In the step of pulling up the single crystal, the CCD camera 22 captures an image of the interface between the single crystal silicon 3 and the silicon melt 2 that can be seen through the opening 17 a of the heat shield 17 from the observation window 10 e. The CCD camera 22 is connected to the image processing unit 23, and the captured image is processed by the image processing unit, and the processing result is used in the control unit 24 to control the pull-up conditions.

The second part is a flowchart illustrating a method for manufacturing single crystal silicon according to an embodiment of the present invention. FIG. 3 is a schematic cross-sectional view showing the shape of a single crystal silicon rod.

As shown in FIGS. 2 and 3, in the production of the single crystal silicon 3, the silicon raw material in the quartz crucible 11 is heated to produce a silicon melt 2 (step S11). After that, the seed crystal attached to the tip of the wire 19 is lowered and brought into contact with the silicon melt (step S12).

Next, a single crystal pulling step is carried out, and the seed crystal is slowly pulled up while maintaining contact with the silicon melt 2 to form a single crystal. In the pulling-up step of the single crystal, a necking step (step S13) is sequentially performed to form a neck 3a with a narrowed crystal diameter for dislocation-free; a shoulder growing step (step S14) is formed to obtain a predetermined diameter Shoulder 3b with increasing crystal diameter; body growing step (step S15), forming body 3c with a constant crystal diameter; tail growing step (part Play S16) to form a tail 3d whose crystal diameter gradually decreases. When the single crystal is finally separated from the melt surface, the tail rearing step ends. Through the above steps, the single crystal silicon rod 3 having the neck 3a, the shoulder 3b, the body 3c, and the tail 3d in order from the upper end to the lower end of the single crystal is completed.

In the single crystal pulling step, in order to control the diameter of the single crystal silicon 3 and the liquid surface position of the silicon melt 2, a CCD camera is used to capture the image of the interface between the single crystal silicon 3 and the silicon melt 2, and the solid state is calculated from the captured image. The diameter of the single crystal at the liquid interface and the gap (gap ΔG) between the melt surface and the heat shield 17. The control unit 24 controls the pulling conditions such as the pulling speed of the wire 19 and the power of the heater 15 so that the diameter of the single crystal silicon 3 becomes the target diameter. In addition, the control unit 24 controls the height position of the quartz crucible 11 so that the distance between the melt surface and the heat shield 17 is kept constant.

Fig. 4 is a schematic cross-sectional view showing the state of pulling up of the single crystal in the tail growing step.

As shown in FIG. 4, in order to separate the single crystal silicon 3 from the silicon melt 2 in a state of no misalignment, the crystal diameter will gradually become smaller as the pull-up progresses in the tail rearing step, so the heat shield 17 and The interval D between the stand-alone 3 gradually widens. Therefore, the width of the heat dissipation path from the silicon melt 2 toward the upper side becomes larger, the heat is easily diffused upward from the lower end 17b of the heat shield 17, and the temperature of the space above becomes the lower end 17b of the heat shield 17 high. Thereby, the upper part of the heat shield 17 is heated, the heat shield 17 itself becomes a heat source, and a single crystal 3 after crystallization is heated. In this state, the single crystal silicon 3 becomes unable to quickly pass through the temperature range of 1020 to 980 ° C where the OSF nucleus is easily formed in the single crystal (OSF nucleus formation temperature range), when the pulling speed of the single crystal 3 is slowed down It becomes more difficult.

However, in the present embodiment, because of the heat shield 17 The water cooling body 18 is provided above the end 17b and inside 17i of the heat shield 17 to reduce the temperature in the high-temperature region after passing through the opening of the lower end 17b of the heat shield 17 and to narrow the crystal growth in the temperature region of 1020 to 980 ° C The width of the direction. Therefore, even if the pulling speed of the single crystal silicon 3 becomes slower than conventional knowledge, the time for the single crystal silicon 3 to stay in the temperature range of 1020 to 980 ° C can be shortened, and the temperature can be quickly formed by the OSF core In the field, the size of the OSF core in the single crystal is extremely reduced.

FIG. 5 is a sequence diagram showing the pull-up speed of the single crystal silicon 3 and the power change of the heater 15.

As shown in FIG. 5, the pulling speed of the single crystal silicon 3 is controlled to a certain value from the body portion 3c to the tail portion 3d. However, a certain pull-up speed in the tail rearing step means that the rate of change relative to the pull-up speed at the beginning of the tail rearing step is within ± 3%.

In the conventional general tail rearing step, the pull-up speed is faster than the body rearing step, and the power of the heater 15 is supplementarily increased, thereby narrowing the crystal diameter. However, in this embodiment, the pull-up speed is not changed, and only the power of the heater is changed to achieve tail shrinkage. In this way, by keeping the pull-up speed constant from the start to the end of the rearing of the tail 3d, it is possible to prevent the occurrence of dislocation of the single crystal caused by the crystal bending or separation from the melt.

When the pull-up speed of the tail portion 3d is the same as the pull-up speed of the body portion 3c, although the control of the narrowing of the tail portion becomes difficult, it is difficult to solidify the silicon melt 2 by strengthening the power of the heater 15 This situation can make tailing easier. When the power of the heater 15 is increased, the influence of its radiant heat becomes stronger. If there is no water cooling body 18, the OSF nucleus as described above at 1020 to 980 ° C The temperature range will change wide. However, as described above, the provision of the water cooling body 18 can narrow the OSF nuclei formation temperature range, and can shorten the time (residence time) for the crystalline silicon 3 to pass through the OSF nuclei formation temperature range.

As described above, the power of the heater 15 in the tail rearing step will be greater than the power of the heater 15 at the end of the body rearing step. In particular, the power of the heater 15 gradually increases at the beginning of the tail rearing step, and the power of the tail 15 at the end of the rear rearing is preferably 1.1 to 1.5 times the power at the beginning of the rear rearing. In this way, gradually increase the power of the heater 15 in the tail rearing step, and the power of the heater 15 at the end of the rear rearing is within the range of 1.1 to 1.5 times at the start of rearing, whereby even the tail 3d When the pull-up speed is the same as that of the body 3c, tail shrinkage can be achieved, and the crystal can be prevented from bending or dislocation.

Even in the tail rearing step, it is better to gradually raise the quartz crucible 11 to maintain the liquid level of the silicon melt 2 constant. In order to improve the single crystallization rate, the conventional technique reduces the residual amount of the silicon melt 2 in the quartz crucible 11 as much as possible, and then starts the tail incubation step. If 11, the quartz crucible 11 may interfere with the heat shield 17. Therefore, it is necessary to stop raising the quartz crucible 11 at the beginning or in the middle of the tail rearing step, and the lowering of the melt surface causes the interval between the melt surface and the heat shield 17 to become wider, and the single crystal silicon 3 becomes more vulnerable to The influence of the radiant heat of the quartz crucible 11 causes a problem that the OSF nucleation temperature range becomes larger.

However, in this embodiment, the tail incubation step is started before the silicon melt 2 is fully consumed, and the quartz crucible 11 is raised until the end of the tail incubation step to keep the height position of the melt surface constant, thereby suppressing The influence of the radiant heat of the crucible 11 can suppress the increase in the OSF nucleation temperature range.

The diameter of the crystal gradually decreases during the rearing of the tail, and the crystal pull-up state changes from moment to moment. Therefore, the stand-alone 3 is easily misaligned. However, when the pull-up speed in tail rearing is slowed down to be slower than conventional knowledge, the tail rearing step time becomes longer, which increases the risk of misalignment. In order to reduce the risk of misalignment as much as possible under such conditions, it is preferable to maintain the rotation speed of the single crystal silicon 3 and the quartz crucible 11 in the tail rearing step. These rotation speeds may be the same as or different from those in the body growing step. With this, the convection of the silicon melt 2 in the quartz crucible 11 can be stabilized, and the melt temperature can be stabilized.

Even in the tail rearing step, it is preferable to operate the magnetic field generating device 21 and apply a horizontal magnetic field and a vertical magnetic field to the silicon melt 2. By doing so, the convection of the silicon melt 2 in the quartz crucible 11 can be more stabilized. The tail 3d of the monocrystalline silicon 3 is a part that is not used as a product, and the commercialized area is the body 3c. Therefore, in the tail rearing step S16, there is no need to apply a magnetic field to control the crystals such as the oxygen concentration level and its surface distribution. quality. In the tail rearing step S16, in order not to reduce the quality of the body 3c of the single crystal silicon 3 reared so far, it is important to quickly separate from the silicon melt 2. However, when a magnetic field is applied during tail growth, the convection of the silicon melt 2 in the quartz crucible 11 can be stabilized, and the melt temperature can be stabilized, thereby preventing the crystal from bending or dislocation.

FIG. 6 is a side cross-sectional view schematically showing the structure of a single crystal manufacturing apparatus according to a second embodiment of the present invention.

As shown in FIG. 6, the single crystal manufacturing apparatus 1B is characterized in that the water-cooled body 18 is composed of a cylindrical member much longer than the first embodiment, from the upper end of the main chamber (the lower end of the traction chamber) The position extends downward until the inner side 17i of the heat shield 17 surrounded by a dotted line in the figure. That is, the water-cooled body 18 is set to cover the pulling path of the monocrystalline silicon 3 as long as possible.

In this embodiment, the inner side 17i of the heat shield 17 above the lower end 17b of the heat shield 17 has the water-cooling body 18, so the temperature in the high-temperature area after passing through the opening of the lower end 17b of the heat shield 17 can be reduced. The width of the crystal growth direction in the temperature range of 1020 to 980 ° C can be narrowed. Therefore, even if the pulling speed of the single crystal silicon 3 is slower than conventional knowledge, the time for the single crystal silicon 3 to stay in the temperature range of 1020 to 980 ° C can be shortened, and it can pass through the OSF core formation field more quickly, extremely Reduce the size of the OSF core in the single crystal.

As described above, in the method for manufacturing single crystal silicon of this embodiment, the water-cooling body 18 is disposed inside the heat-shielding body 17 above the lower end 17b of the heat-shielding body 17, and the water-cooling body 18 is cooled and crystallized in the tail rearing step. Single crystal silicon 3, and use the same speed as the body 3c to pull up the tail 3d, so in the tail incubation step S16 can prevent the crystal bending or separation from the melt, while producing an OSF core (cause of epitaxial defects ) Very few high-quality single crystal silicon.

The above has described a preferred embodiment of the present invention, but the present invention is not limited to this, and various changes can be made within a range not departing from the gist of the present invention, and of course these changes are also included in the scope of the present invention.

[Example]

The difference between the pull-up speed in the tail rearing step and the presence or absence of the water-cooled body 18 was evaluated, and the occurrence of the single crystallization rate and epitaxial defects. Using the single crystal manufacturing apparatus 1A shown in FIG. 1, samples 1 to 6 of a single crystal silicon rod having a diameter of 300 mm were pulled up. At this time, the pull-up speed of the body was set to 1.0 mm / min, and the single crystal was pulled up while raising the quartz crucible, so that the melt surface and the lower end of the heat shield were not only grown in the body but also in the tail. The interval is also maintained constant.

In samples 1 and 2, the tail 3d was pulled up faster than the body 3c (1.1 times). In addition, in samples 3 and 4, the pulling speed of the tail 3d was made equal to the body 3c, and in samples 5 and 6, the pulling speed of the tail 3d was made slower (0.9 times) than the body 3c. In addition, in samples 1, 3, and 5, a single crystal manufacturing apparatus 1A with the water cooling body 18 removed was used, and in samples 2, 4, and 6, a single crystal manufacturing apparatus 1A with the water cooling body 18 grounded was used.

Next, the samples 1 to 6 of the obtained single crystal silicon rods were processed to produce a silicon wafer (polished wafer) with a thickness of 775 μm. A 4 μm epitaxial layer was formed on the surface of the silicon wafer to produce samples corresponding to samples 1 to 6 Epitaxial silicon wafer. Then, the number of epitaxial defects of each epitaxial silicon wafer is measured by a particle counter.

Table 1 is a table showing the results of evaluation experiments on the single crystallization rate and epitaxial defects of samples 1 to 6.

As shown in Table 1, in the sample 1 manufactured without using the water-cooled body 18 and the pulling-up speed of the tail portion 3d is higher than that of the body portion 3c, separation of the tail portion 3d from the silicon melt occurs, and the single crystallization rate deteriorates. In addition, in the sample 2 manufactured using a water-cooled body and the tail part 3d is pulled faster than the body part 3c, the tail part 3d is separated from the silicon melt, and the single crystallization rate deteriorates. Therefore, the occurrence of epitaxial defects in these samples 1 and 2 cannot be evaluated.

The water-cooling body 18 is not used and the pulling speed of the tail 3d and the body 3c etc. In the sample 3 produced by Su, the single crystallization rate is more than 75%, and the number of epitaxial defects is 5 ~ 10 / wf. In the sample 4 produced using the water-cooled body 18 and the tail 3d is pulled up at the same speed as the body 3c, the single crystallization rate is more than 75%, and the number of epitaxial defects is less than 5 / wf, which is very small. It can be confirmed that the quality standards for epitaxial defects are met.

In the samples 5 and 6, the tail 3d was pulled up at a slower speed than the body 3c, regardless of whether the water-cooled body 18 was used, there was a high single crystallization rate of more than 75%, but there were more than 10 epitaxial defects / wf.

From the above results, it can be confirmed that in the sample 4 manufactured using the water-cooled body 18 and the pull-up speed of the tail portion 3d and the body portion 3c at a constant speed, the quality of both the single crystallization rate and the epitaxial defects can be satisfied.

Next, under the conditions of the above sample 4, it is simulated how the distance between the melt surface and the heat shield 17 affects the temperature change in the crystal growth direction of the single crystal.

Figure 7 shows the relationship between the pull-up position of the single crystal and the passage time of the single crystal's OSF nucleation temperature range (1020 to 980 ° C range). In FIG. 7, the horizontal axis represents the distance from the bottom of the single crystal (the lower end of the tail 3d), and the vertical axis represents the passage time in the OSF nucleation temperature range.

As shown in FIG. 7, under the condition that the gap (gap ΔG) between the melt surface and the heat shield 17 is enlarged, that is, relative to the decrease of the melt surface, the rise of the quartz crucible 11 is not controlled to change the melt surface and When the interval between the heat shields 17 is kept constant, it can be seen that the passing time of the OSF nucleus formation temperature range of the bottom single crystal becomes longer as the pulling position is closer to the bottom. When the pull-up speed of the tail 3d is constant, the passage time of the OSF nucleus formation temperature range becomes longer, indicating that the pull-up position is closer The bottom OSF nucleus formation temperature range expands toward the pull-up axis.

On the other hand, if the distance between the melt surface and the heat shield 17 is kept constant, it can be seen that even if the pull-up position is close to the lower end of the tail 3d, the passage time of the single crystal OSF nucleus formation temperature range does not become so long. From the above results, it can be confirmed that by maintaining a constant distance between the melt surface and the heat shield 17 during the tail rearing step, the expansion of the OSF nucleation temperature range can be suppressed.

Next, the influence of the difference in the output of the heater 15 in the tail rearing step on the quality of the single crystal was evaluated. When the powers of the heater 15 at the beginning and the end of tail rearing were set to CkW and DkW, respectively, the heater power ratio D / C was changed in the range of 0.9 to 1.8 in the evaluation experiment. The other pull-up conditions are the same as the evaluation experiments of the single crystallization rate and epitaxial defects described above.

Table 2 shows the results of evaluation experiments showing the crystal growth conditions caused by different heater power ratios.

As shown in Table 2, when the heater power ratio D / C is less than 1.1, the tail will not shrink. Also, when the heater power ratio exceeds 1.5, crystal bending occurs, and the tail 3d cannot be organized into a beautiful cone shape. On the other hand, when the heater power ratio D / C is in the range of 1.1 to 1.5, the tail can be shrunk, and the tail can be bred 3d.

From the above results, the heater power ratio D / C at the end of tail rearing relative to the beginning of tail rearing satisfies 1.1 to 1.5, and the power of the heater during tail rearing is always larger than that at the beginning of tail rearing. In this case, a beautifully shaped tail can be bred without crystal bending or single crystal separation from the silicon melt.

2‧‧‧Silver melt

3‧‧‧Single crystal silicon

3c‧‧‧Body

3d‧‧‧tail

11‧‧‧Quartz crucible

12‧‧‧Carrier

15‧‧‧heater

17‧‧‧ Cover

17b‧‧‧The lower end of the cover

17i‧‧‧Inside of the cover

18‧‧‧Water cooling body

D‧‧‧Interval

Claims (7)

A method for manufacturing single-crystal silicon, which uses the Tchaikovsky method of pulling single-crystal silicon from the silicon melt in a quartz crucible to manufacture single-crystal silicon. Tail rearing step, rearing the tail with gradually decreasing crystal diameter, wherein a water-cooled body is used to cool the single-crystal silicon pulled up from the silicon melt, the water-cooled body is arranged in a heat shield above the quartz crucible The lower end of the upper part and the inner side of the heat shield, in the tail rearing step, from the beginning of the rearing of the tail to the end, use the same pulling speed as the end of the rearing of the body to pull up The single crystal silicon. The method for manufacturing single crystal silicon as described in item 1 of the patent application scope, wherein in the tail rearing step, the body of the single crystal silicon is passed through a temperature range of 1020 ° C to 980 ° C within 15 minutes. The method for manufacturing single crystal silicon as described in item 1 or 2 of the patent application, wherein the power of the heater that heats the silicon melt is gradually increased from the beginning to the end of the rearing of the tail to breed the tail The power of the heater at the end is set to be 1.1 times or more and 1.5 times or less the power of the heater at the start of rearing the tail. The method for manufacturing single crystal silicon as described in item 1 or 2 of the patent application range, wherein in the tail rearing step, the quartz crucible is raised to maintain a constant interval between the heat shield and the silicon melt. The method for manufacturing single crystal silicon as described in item 1 or 2 of the patent application scope, wherein in the tail rearing step, the rotation speed of the quartz crucible is maintained constant. The method for manufacturing single crystal silicon as described in item 1 or 2 of the patent application range, wherein the rotation speed of the single crystal silicon is maintained constant during the tail rearing step. The method for manufacturing single crystal silicon as described in item 1 or 2 of the patent application scope, wherein in the tail rearing step, a magnetic field is applied to the silicon melt.