WO2024079934A1

WO2024079934A1 - Single crystal pulling device and single crystal pulling method

Info

Publication number: WO2024079934A1
Application number: PCT/JP2023/020633
Authority: WO
Inventors: 寛之坪田; 智紀佐々木
Original assignee: グローバルウェーハズ・ジャパン株式会社
Priority date: 2022-10-13
Filing date: 2023-06-02
Publication date: 2024-04-18
Also published as: TW202415817A; JP2024057807A

Abstract

The present invention precisely controls a gap that is the distance between the bottom end of a radiation shield and molten silicon when pulling a silicon single crystal by means of the Czochralski method, and grows a silicon single crystal. The present invention comprises: a raising/lowering driving unit 15 that raises and lowers a crucible 3; a heater 4 that heats the crucible; a cylindrical radiation shield 7 that is disposed above molten silicon M formed in the crucible and surrounds the periphery a single crystal C that is pulled upward; a translucent pin member 8 that is disposed to a terraced surface located at the front end of the radiation shield and penetrates the radiation shield such that the bottom part of the pin member is located on the molten liquid-side and the top part is located on the radiation shield inner circumference-side; a brightness detection portion 17 that detects the brightness of the pin member; and a controller 11 that, when the detected brightness of the pin member exceeds a prescribed threshold, determines that the bottom end of the pin member has come into contact with the molten silicon and stops the raising of the crucible.

Description

Single crystal pulling apparatus and method

The present invention relates to a single crystal pulling device and a single crystal pulling method, and in particular to a single crystal pulling device and a single crystal pulling method for pulling silicon single crystals by the Czochralski method.

In growing silicon single crystals by the Czochralski method (CZ method), as shown in FIG. 5 , a quartz crucible 51 installed in a chamber 50 is filled with polysilicon as a raw material, and the polysilicon is heated and melted by a heater 52 provided around the quartz crucible 51 to obtain a silicon melt M.
Thereafter, a seed crystal P (seed) attached to a seed chuck is immersed in the silicon melt M, and a single crystal C is grown inside the radiation shield 53 by lifting the seed chuck while rotating the seed chuck and the quartz crucible 51 in the same or opposite directions.

In the growth of silicon single crystals by the Czochralski method, defect-free single crystals are required, but the manufacturing conditions under which defect-free single crystals can be produced are extremely narrow, including the ratio of the pulling rate to the temperature gradient.
The temperature gradient is the temperature change per unit length in the height direction of the single crystal near the solid-liquid interface, and the pulling speed is the speed at which the single crystal is pulled up. When the pulling speed is V and the temperature gradient is G, the defects formed during the production of the single crystal change sensitively depending on the ratio (V/G) of the pulling speed V to the temperature gradient G. For example, when the ratio (V/G) of the pulling speed V to the temperature gradient G is too large, vacancy type defects (void defects) are formed, and conversely, when the ratio (V/G) of the pulling speed V to the temperature gradient G is too small, interstitial Si type defects (dislocation loops) are formed.

Therefore, to obtain single crystals of stable quality, it is necessary to control the ratio of the pulling speed V to the temperature gradient G (V/G) with high precision. Since the pulling speed V can be precisely controlled mechanically, a common method for producing single crystals is to control the pulling speed V to be constant in order to achieve both stable crystal quality and planned production.

However, the quality of the crystal may vary along the length of the crystal simply by controlling the pulling speed V to be constant, because the temperature gradient G is not constant but fluctuates during the pulling process.
The distance (called the gap) between the bottom end of the radiation shield and the silicon melt surface is a factor that greatly affects the control to keep the temperature gradient G constant. During single crystal pulling, it is important to precisely control this gap to a constant value.

There is a conventional gap setting method, for example, disclosed in Patent Document 1. In this method, a rod-shaped pin 60 is attached to the lower end 53a of a radiation shield 53, which is surrounded by a dashed circle in Figure 5, as shown in Figure 6(a), and the crucible 51 is raised. Then, as shown in Figure 6(b), a fusion ring 70 that occurs around the pin 60 when the pin 60 comes into contact with the silicon melt M is detected by a CCD camera or the like, and the initial gap is set based on this.

JP 2011-57464 A

However, as disclosed in Patent Document 1, when the tip of the pin 60 provided at the lower end of the radiation shield 53 comes into contact with the silicon melt M, the fusion ring 70 is very small and occurs above the liquid surface, making it difficult to detect accurately and sometimes resulting in erroneous detection. This can lead to a risk of low accuracy in setting the initial gap, which can lead to poor accuracy in controlling the gap during single crystal pulling, resulting in a problem of a low yield of high-quality defect-free single crystals.

The present invention was made in light of the above circumstances, and aims to provide a single crystal pulling device and a single crystal pulling method that can grow silicon single crystals by precisely controlling the gap between the bottom end of the radiation shield and the silicon melt when pulling silicon single crystals using the Czochralski method.

The single crystal pulling device according to the present invention, which has been made to solve the above problems, is a single crystal pulling device that pulls a single crystal by the Czochralski method from a silicon melt contained in a crucible in a chamber, and is equipped with a lifting drive unit that lifts and lowers the crucible, a heater that heats the crucible, a cylindrical radiation shield that is arranged above the silicon melt formed in the crucible and surrounds the single crystal to be pulled, a light-transmitting pin member that is arranged on the terrace surface located at the tip side of the radiation shield, penetrating the radiation shield so that its lower part is on the melt side and its upper part is on the inner circumference side of the radiation shield, a brightness detection unit that detects the brightness of the pin member, and a controller that controls the lifting drive unit, and the controller is characterized in that it lifts the crucible using the lifting drive unit and causes the brightness detection unit to detect the brightness of the pin member, and when the detected brightness of the pin member exceeds a predetermined threshold value, it determines that the lower end of the pin member has come into contact with the silicon melt and stops the lifting of the crucible using the lifting drive unit.

Furthermore, after stopping the raising of the crucible by the lifting drive unit, it is desirable for the controller to lower the crucible by the lifting drive unit a distance obtained by subtracting the known length from the lower end of the radiation shield to the tip of the pin member from the desired value of the gap from the lower end of the radiation shield to the silicon melt.
Moreover, it is preferable that the predetermined threshold value of the brightness is a value obtained by adding a value of 25% or more of a reference brightness to a reference brightness in a state where the pin member is not in contact with the silicon melt.
Alternatively, the predetermined brightness threshold value is preferably a value obtained by adding a value that is 50% or more of a reference brightness when the pin member is not in contact with the silicon melt.

According to this configuration, in setting the initial gap between the lower end of the radiation shield and the silicon melt surface before the start of pulling the single crystal, the crucible is raised, and when the pin members provided at the lower end of the radiation shield come into contact with the silicon melt and the luminance of the pin members changes significantly, the raising of the crucible is stopped. Here, the luminance is detected by detecting the luminance of the pin members, not the luminance on the liquid surface, so that there is little risk of erroneous detection and accurate detection results can be obtained.
Then, the crucible is lowered by a height obtained by subtracting the known length of the pin member from the desired gap value, thereby making it possible to set the initial gap with high accuracy.
As a result, the gap can be controlled with high precision in the subsequent single crystal pulling process, making it possible to pull a high-quality defect-free single crystal.

The single crystal pulling method according to the present invention, which has been made to solve the above problems, is a method for pulling a single crystal by the Czochralski method from a silicon melt contained in a crucible in a chamber, and is characterized by comprising the steps of: before pulling the single crystal, raising the crucible and detecting the brightness of a light-transmitting pin member that is placed above the silicon melt formed in the crucible and extends downward from the lower end of a cylindrical radiation shield that surrounds the single crystal to be pulled; and, when the brightness exceeds a predetermined threshold value, determining that the lower end of the pin member has come into contact with the silicon melt and stopping the raising of the crucible.

In addition, it is desirable to include a step of determining that the lower end of the pin member has come into contact with the silicon melt when the brightness exceeds a predetermined threshold value, and after the step of stopping the raising of the crucible, lowering the crucible a distance obtained by subtracting a known length from the lower end of the radiation shield of the pin member to the tip of the pin from a desired value of the gap from the lower end of the radiation shield to the silicon melt.
Moreover, it is preferable that the predetermined threshold value of the brightness is a value obtained by adding a value of 25% or more of a reference brightness to a reference brightness in a state where the pin member is not in contact with the silicon melt.
Alternatively, the predetermined brightness threshold value is preferably a value obtained by adding a value that is 50% or more of a reference brightness when the pin member is not in contact with the silicon melt.

According to the present invention, when pulling silicon single crystals using the Czochralski method, the gap between the bottom end of the radiation shield and the silicon melt can be precisely controlled to grow the silicon single crystal.

FIG. 1 is a cross-sectional view showing an example of a single crystal pulling apparatus according to the present invention. FIG. 2 is a schematic cross-sectional view showing an enlarged portion of the single crystal pulling apparatus shown in FIG. FIG. 3 is a flow chart showing an example of the method for pulling a single crystal according to the present invention. FIG. 4 is a graph showing the results of the examples. FIG. 5 is a cross-sectional view of a conventional single crystal pulling apparatus. 6(a) and 6(b) are enlarged views of a portion of FIG. 5 for explaining a fusion ring that occurs when a pin provided at the lower end of the radiation shield comes into contact with the silicon melt.

The following describes the single crystal pulling device and single crystal pulling method according to the present invention with reference to the drawings. However, this embodiment is described as an example of the present invention, and the present invention is not limited to this.

Figure 1 is a cross-sectional view showing an example of a single crystal pulling apparatus according to the present invention. This single crystal pulling apparatus 1 has a furnace body 10 formed by stacking a pull chamber 10b on top of a cylindrical main chamber 10a, and is equipped with a carbon crucible (or graphite crucible) 2 that is provided in this furnace body 10 so as to be rotatable about a vertical axis and movable up and down, and a quartz glass crucible 3 (hereinafter simply referred to as crucible 3) held by the carbon crucible 2. This crucible 3 is rotatable about a vertical axis together with the rotation of the carbon crucible 2.

Further, below the carbon crucible 2, there are provided a rotation drive unit 14 such as a rotation motor for rotating the carbon crucible 2 around a vertical axis, and an elevation drive unit 15 for moving the carbon crucible 2 up and down.
The rotation drive unit 14 is connected to a rotation drive control unit 14a, and the elevation drive unit 15 is connected to an elevation drive control unit 15a.

The single crystal pulling apparatus 1 also includes a heater 4 of a resistance heating type or a high-frequency induction heating type for heating and melting the semiconductor raw material (raw polysilicon) placed in the crucible 3 to form a silicon melt M.
The single crystal pulling apparatus 1 also includes a pulling mechanism 9 that winds up the wire 6 and pulls up the grown single crystal C. A seed crystal P is attached to the tip of the wire 6 of the pulling mechanism 9. A rotation drive control unit 9a that controls the rotation drive of the pulling mechanism 9 is connected to the pulling mechanism 9.

In addition, a radiation shield 7 is disposed above the silicon melt M formed in the crucible 3 to surround the single crystal C. This radiation shield 7 is formed with openings at the top and bottom, and serves to block excess radiant heat from the side heaters 4, the silicon melt M, etc., to the single crystal C being grown, and to straighten the gas flow in the furnace.
2, the radiation shield 7 has a tapered portion 7b that narrows in diameter (downward) from an upper opening 7a toward the silicon melt M, and a ring-shaped terrace portion 7c that extends horizontally inward from the lower end of the tapered portion 7b. The single crystal is pulled up so as to pass through a lower opening 7d formed on the inner edge of the terrace portion 7c and the upper opening 7a.

The radial length (width) of the terrace portion 7c is set to, for example, 10 mm or more and 150 mm or less so that reflection of the silicon melt M and stray light do not reach the vicinity 7c1 of the lower end of the tapered portion 7b. The terrace portion 7c is provided with a light-transmitting quartz pin 8 (pin member) extending downward as shown in the figure. That is, the quartz pin 8 is disposed on the terrace portion 7c (terrace surface) located on the tip side of the radiation shield 7, penetrating the radiation shield 7 so that its lower portion is located on the melt M side and its upper portion is located on the inner peripheral side of the radiation shield 7.
The quartz pin 8 is provided by inserting the straight body portion 8a from above downward into a hole 7c1 formed in the terrace portion 7c in accordance with the diameter of the straight body portion 8a, and engaging the head portion 8b with the terrace portion 7c. The length L of the quartz pin 8 from the lower end 7d of the radiation shield 7 to the pin tip 8a1 is, for example, 15 mm.

The single crystal pulling device 1 also includes an optical diameter measuring sensor (diameter measuring device) 16, such as a CCD camera, for measuring the diameter of the single crystal being grown. A small observation window 10a1 is provided on the top surface of the main chamber 10a, and the positional change of the crystal end (position indicated by the dashed arrow) at the solid-liquid interface can be detected from outside this small window 10a1.

The single crystal pulling apparatus 1 also includes a brightness detector 17 such as a CCD camera for measuring the brightness of the head 8b of the quartz pin 8 provided at the lower end of the radiation shield 7. This brightness detector 17 is arranged to measure the brightness of the head 8b of the quartz pin 8 arranged on the upper surface of the terrace portion 7c of the radiation shield 7 as shown in FIG. 2. A small window 10a2 separate from the small window 10a1 is provided on the upper surface of the main chamber 10a, and changes in the brightness of the head 8b of the quartz pin 8 are detected from outside this small window 10a2.

In this embodiment, the reason for detecting the change in brightness of the head 8b of the quartz pin 8 in this manner is to set the initial gap between the lower end 7d of the radiation shield 7 and the melt surface with high precision. The method for setting this initial gap will be described in detail later, but when the tip 8a1 of the quartz pin 8 comes into contact with the silicon melt M, light passes through the quartz pin 8, causing the head 8b of the quartz pin 8 to shine with a higher brightness. This change in brightness is detected by the brightness detector 17.
The reason why the head 8b of the quartz pin 8 shines with high brightness is due to the following principle. The silicon melt M is orange in color and is considerably brighter than the surrounding environment in the furnace. When the transparent quartz pin 8 comes into contact with the silicon melt M, a ring is formed around the quartz pin 8 due to surface tension, and the ring captures more visible light emitted from the silicon melt M than before contact. The quartz pin 8 is transparent, and the visible light is transmitted to the head of the quartz pin 8 with almost no reflection or absorption, causing it to shine with high brightness.

The single crystal pulling device 1 also includes a controller 11 having a storage device 11a and an arithmetic and control device 11b, and the rotation drive control unit 14a, the lift drive control unit 15a, the rotation drive control unit 9a, the diameter measurement sensor 16, and the brightness detector 17 are each connected to the arithmetic and control device 11b.

In the single crystal pulling apparatus 1 thus constructed, when a single crystal C having a diameter of, for example, 300 mm is grown, pulling is performed as follows.
That is, first, raw polysilicon (for example, 460 kg) is loaded into the crucible 3, and a crystal growing process is started based on the program stored in the storage device 11a of the controller 11.

First, a predetermined atmosphere (mainly an inert gas such as argon gas) is created inside the furnace body 10. For example, a furnace atmosphere with an internal furnace pressure of 65 torr and an argon gas flow rate of 90 l/min is created.
Then, while the crucible 3 is rotated in a predetermined direction at a predetermined rotation speed (rpm), the raw material polysilicon loaded in the crucible 3 is melted by heating with the heater 4 to become silicon melt M (step S1 in FIG. 3).

The pulling conditions are adjusted using parameters such as the initial power supply to the heater 4 and the pulling speed, and the seed crystal P starts to rotate around its axis at a predetermined rotation speed. The rotation direction is opposite to that of the crucible 3.
When the liquid level of the silicon melt M has stabilized, under the control of the controller 11, the lift drive unit 15 is driven via the lift drive control unit 15a to raise the height of the crucible 3 by an inching (small movement) operation, for example, in increments of 0.05 mm (step S2 in Figure 3).
During this time, the controller 11 monitors the change in luminance of the head 8b of the quartz pin 8 by the luminance detector 17 (step S3 in FIG. 3). In this embodiment, the controller 11 stores in advance the maximum luminance after the quartz pin 8 comes into contact with the silicon melt M as 100%. The luminance (reference luminance) before the quartz pin 8 comes into contact with the silicon melt M is, for example, 40%.

When the liquid level M1 of the silicon melt M comes into contact with the tip 8a1 of the quartz pin 8 at the lower end of the radiation shield 7 due to the rise of the crucible 3, the brightness of the head 8b of the quartz pin 8 rises above a predetermined threshold value (step S4 in FIG. 3).
The controller 11 detects this with the brightness detector 17 and controls the lifting drive unit 15 to stop the lifting operation of the crucible 3 (step S5 in FIG. 3). Specifically, the controller 11 determines that the quartz pins 8 at the lower end of the radiation shield 7 have come into contact with the silicon melt M when the change in brightness detected by the brightness detector 17 exceeds a predetermined threshold. For example, the predetermined threshold of brightness is a value obtained by adding, when the maximum brightness after the quartz pins 8 have come into contact with the silicon melt M is taken as 100%, to a reference brightness (here, 40%) in a state in which the quartz pins 8 are not in contact with the silicon melt M, for example, 25% or more (or 50% or more) of the reference brightness (here, 40%).

The controller 11 lowers the crucible 3 by the lift driver 15 by a dimension H obtained by subtracting the length L of the quartz pin 8 from the desired gap value G (step S6 in FIG. 3). This allows the initial gap value to be set with high precision.
In addition, since the height position of the fixed radiation shield 7 is known, the height position of the silicon melt surface M1 after the gap is set (initial liquid level height) can be easily obtained. The controller 11 stores this initial liquid level height (step S7 in FIG. 3).

Next, the wire 6 is lowered to bring the seed crystal P into contact with the silicon melt M, and after the tip of the seed crystal P is melted, necking is performed to form a neck portion P1 (step S8 in FIG. 3).
Then, the crystal diameter gradually expands to form a shoulder portion C1 (step S9 in FIG. 3).
The controller 11 also controls the lift drive control unit 15a to drive and control the lift drive unit 15, keeps the pulling speed constant at, for example, 0.55 mm/min, and proceeds to the process of forming the straight body portion C2 that will become the product part (step S10 in Figure 3).

During the formation of this straight body portion C2, the controller 11 determines the solidification rate of the silicon single crystal using the measurement results of the measurement sensor 16, and calculates the height position and gap of the silicon melt surface M1 at that time based on this solidification rate and the initial height of the silicon melt surface M1 (step S11 in Figure 3).
Then, it is determined whether the variation in the measured dimension of the gap is within ±0.1 mm (step S12 in FIG. 3), and if it is not, the lifting device control unit 15a is controlled to adjust the height position of the crucible 3 by the lifting drive unit 15 so that the condition is satisfied (step S13 in FIG. 3). During the pulling process, control is performed so that the condition of step S12 is satisfied, and the single crystal pulling process proceeds.

When the body portion C2 is formed to a predetermined length (step S14 in FIG. 3), the process proceeds to the final tail portion process (step S15 in FIG. 3). In this tail portion process, the contact area between the bottom end of the crystal and the silicon melt M gradually decreases, and the single crystal C and the silicon melt M are separated, producing a silicon single crystal.

As described above, according to this embodiment, in setting the initial gap between the lower end of the radiation shield and the silicon melt surface before starting to pull the single crystal, the crucible 3 is raised by an inching motion, and the raising of the crucible 3 is stopped when the luminance of the quartz pins 8 provided at the lower end of the radiation shield 7 changes significantly when the quartz pins 8 come into contact with the silicon melt M. Here, the luminance is detected by detecting the luminance of the quartz pins 8, rather than the luminance on the liquid surface M1, so that there is little risk of erroneous detection and accurate detection results can be obtained.
Then, the crucible 3 is lowered by a height H obtained by subtracting the known length L of the quartz pin 8 from the desired gap value, whereby the initial gap can be set with high accuracy.
As a result, the gap can be controlled with high precision in the subsequent single crystal pulling process, making it possible to pull a high quality single crystal.

In the above embodiment, in the gap control during the pulling of the single crystal, the height position detection of the silicon melt surface M1 is calculated based on the solidification rate of the single crystal, but the present invention is not limited to this. For example, as disclosed in JP 2008-189522 A, the reflection of a laser beam irradiated on the silicon melt surface may be detected by a CCD camera, and the detected image signal may be subjected to image processing to determine the silicon melt surface height.
Furthermore, in the above embodiment, the pulling speed is constant, but the pulling speed may not be constant but may be variable.

In addition, in the above embodiment, an example was described in which one quartz pin 8 is provided at the lower end of the radiation shield 7, but in addition to the quartz pin 8, a quartz pin shorter than this quartz pin 8 may also be provided at the lower end of the radiation shield 7.
In this case, during control of pulling up the single crystal, the crucible 3 is controlled to rise as the silicon melt M decreases, but in order to prevent contact between the radiation shield 7 body and the silicon melt M, if a short pin comes into contact with the silicon melt M, the rising of the crucible 3 may be stopped or the crucible 3 may be controlled to be lowered.

In addition, in the above embodiment, the quartz pin 8 is composed of a straight body portion 8a having a constant diameter and a disk-shaped head portion 8b having a diameter larger than that of the straight body portion 8a, but the present invention is not limited to this form.
For example, the lower diameter may be smaller than the upper diameter (the upper diameter may be larger than the lower diameter). In other words, when the surface area per length of the head 8b above the radiation shield 7 (second region above the radiation shield 7) of the quartz pin 8 is larger than that of the straight body portion 8a below the radiation shield 7 (first region below the radiation shield 7), it becomes easier to detect the luminance by the luminance detector 17 (when the surface area of the head 8b is too small, the head 8b becomes more susceptible to the effects of disturbances, etc., and the measurement accuracy decreases).

The single crystal pulling device and single crystal pulling method according to the present invention will be further explained based on examples.

(Experiment 1)
In experiment 1, in the single crystal pulling apparatus shown in Fig. 1, 460 kg of silicon raw material was filled into a quartz crucible having a diameter of 32 inches to form a silicon melt. After the silicon melt was melted in the crucible, the crucible was raised to verify whether there was a change in brightness when the silicon melt came into contact with the quartz pin provided at the lower end of the radiation shield.
The crucible was raised in increments of 0.05 mm by inching, and the luminance at that time was detected.

The results of Experiment 1 are shown in the graph of Figure 4. In the graph of Figure 4, the left vertical axis represents the crucible fluctuation (mm) relative to the reference value (0 mm), and the right vertical axis represents the brightness (%). Note that the brightness (%) on the vertical axis is set to 100% as the maximum brightness after the quartz pin contacted the silicon melt.
As shown in the graph in Fig. 4, the brightness increased significantly when the crucible was raised by +0.4 mm. This position was visually confirmed to be the position where the silicon melt came into contact with the quartz pin provided at the bottom end of the radiation shield. In other words, it was confirmed that the brightness increased significantly when the silicon melt came into contact with the quartz pin provided at the bottom end of the radiation shield.
Furthermore, from the graph in Figure 4, it was confirmed that the threshold value for the controller to determine contact between the quartz pin and the silicon melt is preferably a brightness of 50% or more (a value obtained by adding 25% of the reference brightness (40%) to the reference brightness of 40% before the quartz pin comes into contact with the silicon melt) at which there is almost no possibility of picking up external disturbances and making an erroneous determination, and more preferably, 60% or more (a value obtained by adding 50% of the reference brightness (40%) to the reference brightness of 40% before the quartz pin comes into contact with the silicon melt).

(Experiment 2)
Example 1
Ten silicon single crystals were actually pulled in Experiment 2. In Example 1, similarly to Experiment 1, 460 kg of silicon raw material was filled in a quartz crucible having a diameter of 32 inches to form a silicon melt.
According to the present embodiment, a quartz pin was provided at the lower end of the radiation shield, and an initial gap between the radiation shield and the melt surface was set to 50 mm.
The furnace environment was created by setting the furnace pressure at 50 torr and flowing argon gas at a flow rate of 100 l/min.
Then, the crucible rotation speed was set to 1 rpm, the crystal rotation speed was set to 7 rpm (opposite to the crucible rotation direction), and the single crystal was grown at a pulling speed of 0.6 mm/min with a target crystal diameter of 305 to 310 mm. During pulling, the gap between the radiation shield and the melt surface was controlled to be 50 mm±0.1 mm.

In this Example 1, 10 single crystals were pulled to be defect-free. To evaluate the defect-free region, the V-rich side, where void defects exist, was checked for the presence or absence of clusters using 50 overlapping maps of LPD (Light Point Defect) evaluation, and the presence or absence of COP (Crystal Originated Particle) was determined.

The I-rich side was judged for the presence or absence of a B-band region, which is a region where oxygen precipitates are likely to occur by the Cu decoration method. A defect-free crystal was defined as a crystal that had neither COPs nor a B-band region.
The results of Example 1 are shown in Table 1. As shown in Table 1, the evaluation of 10 single crystals confirmed that all 10 were defect-free crystals over their entire length.

(Comparative Example 1)
In Comparative Example 1, an attempt was made to pull a defect-free crystal using a gap matching method using a mirror image gap. The mirror image gap was calculated from the difference between the actual image of the radiation shield and the edge of the shield as its mirror image reflected on the melt surface, detected using the same CCD camera as that used to detect the brightness of the quartz pin.
The results of Comparative Example 1 are shown in Table 1 together with the results of Example 1. As a result of pulling 10 single crystals, I-defects were detected over the entire length of two of the crystals by wafer evaluation using the Cu decoration method. Also, DSOD and LPD crowding modes were observed in parts of the two crystals.

The results of Example 1 confirmed that the present invention reduces gap variation and increases the yield of defect-free crystals.

1 Single crystal block 3 Quartz glass crucible 4 Side heater 6 Wire 7 Radiation shield 8 Quartz pin (pin member)
C Silicon single crystal M Silicon melt M1 Melt surface C Silicon single crystal C2 Body part

Claims

A single crystal pulling apparatus for pulling a single crystal by the Czochralski method from a silicon melt contained in a crucible in a chamber, comprising:
the crucible is provided with an elevation drive unit for raising and lowering the crucible, a heater for heating the crucible, a cylindrical radiation shield disposed above the silicon melt formed in the crucible and surrounding the single crystal to be pulled, optically transparent pin members disposed on a terrace surface located at a tip side of the radiation shield, penetrating the radiation shield with a lower portion positioned on the melt side and an upper portion positioned on an inner peripheral side of the radiation shield, a brightness detection unit for detecting the brightness of the pin members, and a controller for controlling the elevation drive unit,
The controller causes the lifting drive unit to lift the crucible while causing the brightness detection unit to detect the brightness of the pin member, and when the detected brightness of the pin member exceeds a predetermined threshold, determines that the lower end of the pin member has come into contact with the silicon melt, and stops the lifting of the crucible by the lifting drive unit.
From a state in which the lifting of the crucible by the lifting drive unit is stopped,
The controller:
2. The single crystal pulling apparatus according to claim 1, wherein the crucible is lowered by the lifting drive unit by a distance obtained by subtracting a known length from the lower end of the radiation shield to the tip of the pin in the pin member from a desired value of a gap from the lower end of the radiation shield to the silicon melt.
The single crystal pulling apparatus described in claim 1, characterized in that the predetermined brightness threshold is a value obtained by adding a value of 25% or more of the reference brightness to the reference brightness when the pin member is not in contact with the silicon melt.
The single crystal pulling apparatus described in claim 1, characterized in that the predetermined brightness threshold is a value obtained by adding a value of 50% or more of the reference brightness to the reference brightness when the pin member is not in contact with the silicon melt.
A method for pulling a single crystal by the Czochralski method from a silicon melt contained in a crucible in a chamber, comprising the steps of:
Before pulling a single crystal,
The crucible is raised,
detecting the brightness of an optically transparent pin member extending downward from a lower end of a cylindrical radiation shield that is disposed above the silicon melt formed in the crucible and surrounds the single crystal being pulled;
determining that the lower end of the pin member has come into contact with the silicon melt when the brightness exceeds a predetermined threshold value, and stopping the ascent of the crucible;
A method for pulling a single crystal comprising the steps of:
When the brightness exceeds a predetermined threshold value, it is determined that the lower end of the pin member has come into contact with the silicon melt, and after stopping the ascent of the crucible,
lowering the crucible by a distance obtained by subtracting a known length of the pin member from the lower end of the radiation shield to the tip of the pin from a desired gap from the lower end of the radiation shield to the silicon melt;
6. The method for pulling a single crystal according to claim 5, further comprising:
The method for pulling a single crystal, as described in claim 5, characterized in that the predetermined brightness threshold is a value obtained by adding a value of 25% or more of the reference brightness to the reference brightness when the pin member is not in contact with the silicon melt.
The method for pulling a single crystal, as described in claim 5, characterized in that the predetermined brightness threshold is a value obtained by adding a value of 50% or more of the reference brightness to the reference brightness when the pin member is not in contact with the silicon melt.