JP4907396B2 - Single crystal manufacturing method - Google Patents

Description

  The present invention relates to a method for producing a single crystal, and more particularly to a method for producing a single crystal by the Czochralski (CZ) method.

  A so-called Czochralski method (CZ) method is known as a method for producing a single crystal, for example, a silicon single crystal. In this method, a raw material lump is accommodated in a crucible installed in a chamber, and a heater is heated at a high temperature to use the raw material in the crucible as a melt. Then, a seed crystal is deposited on the surface of the raw material melt, and a silicon single crystal having a desired diameter and quality is grown below the pulled seed crystal.

  When a single crystal is grown by the CZ method, a phenomenon may occur in which the single crystal undergoes dislocation during the growth. In dislocation formation in the initial stage of single crystal growth, dislocation-free single crystal growth can be attempted again by remelting the single crystal. However, in this case, time loss due to remelting of the single crystal, increase in electric power cost and labor cost, etc. cause an increase in manufacturing cost, which is not preferable. Further, when dislocations occur in the later stage of growth, the re-melting increases the manufacturing cost. For this reason, it is possible to continue the growth with dislocations without melting the single crystal. In this case, as a matter of course, the dislocation portion cannot be shipped as a product. Therefore, a manufacturing method that prevents the dislocation of the single crystal as much as possible and stably grows the single crystal with no dislocations is desired.

There are several possible causes for the dislocation of the single crystal. For example, thermal stress caused by the internal temperature difference of the single crystal, presence of foreign matter in the raw material melt in the crucible, and the like. The foreign material present in the raw material melt is mixed when the raw material is charged into the crucible, the inner surface of the quartz crucible is deteriorated and peeled off, the mixed foreign material in the single crystal manufacturing apparatus, or the raw material. The thing etc. which remain | survived without being excluded while being generated by evaporation from the melt surface can be considered.
Countermeasures for dislocations resulting from the disorder of the crystal structure due to thermal stress are being promoted by optimizing the production conditions of the single crystal, particularly the thermal environment.
Various techniques have also been proposed to prevent dislocation caused by foreign matter. For example, Patent Document 1 discloses a technique in which a heat insulating material is provided around a radiation shield so that SiO foreign matter generated by evaporation from a raw material melt surface is attached to a position where it does not enter the crucible. Patent Document 2 discloses a technique for preventing the generation of foreign matter due to a radiation shield or a quartz crucible by optimizing the pressure in the chamber of the single crystal manufacturing apparatus.
JP-A-5-294784 Japanese Patent No. 3787452

  However, the conventionally proposed technique for preventing dislocation caused by the foreign material is focused on suppressing the generation of the foreign material and the falling of the foreign material into the crucible. However, it is difficult to completely suppress the generation of foreign matter and the fall of foreign matter into the crucible. And once the dislocation due to the foreign matter occurs, there is a high possibility that the dislocation occurs again due to the same foreign matter even if remelting is performed.

  The present invention has been made in view of the above circumstances. The object of the present invention is to prevent dislocation of a single crystal by removing the foreign matter even if the foreign matter falls into the crucible. An object of the present invention is to provide a method for producing a single crystal that can improve the productivity of crystals and reduce the production cost.

The method for producing a single crystal according to the first aspect of the present invention is a method for producing a single crystal by a Czochralski (CZ) method, comprising melting a raw material filled in a crucible into a raw material melt, and the raw material A step of pulling a single crystal from the melt, and a step of flowing an inert gas on the surface of the raw material melt between the step of melting the raw material into a raw material melt and the step of pulling the single crystal It is provided, in the step of flowing the inert gas, the raw material melt surface, the flow velocity of the inert gas toward the crucible periphery from the crucible center, and 8m / sec 12m / sec, the non In the step of flowing active gas, the height of the portion where the raw material melt surface is in contact with the crucible inner wall is higher than the height of the portion where the raw material melt surface is in contact with the crucible inner wall in the step of pulling up the single crystal. 2mm or higher And controlling the rotational speed of the crucible.

The method for producing a single crystal according to the second aspect of the present invention is a method for producing a single crystal by a Czochralski (CZ) method, wherein a raw material filled in a crucible is melted to form a raw material melt, and the raw material A step of pulling the single crystal from the melt, and when the single crystal has undergone dislocation, the step of re-melting the single crystal and the melting of the raw material after the re-melting when the re-melting is completed. In the step of flowing an inert gas on the liquid surface and the step of flowing the inert gas, a step of pulling a single crystal from the remelted raw material melt is provided, and in the step of flowing the inert gas, The remelting in the step of flowing the inert gas at a flow rate of the inert gas from the center of the crucible toward the outer periphery of the crucible on the surface of the raw material melt after remelting is 8 m / second or more and 12 m / second or less. The surface of the subsequent raw material melt contacts the inner wall of the crucible The height of the portion is 2 mm or more higher than the height of the portion where the surface of the raw material melt after remelting is in contact with the inner wall of the crucible in the step of pulling the single crystal from the raw material melt after remelting. The number of revolutions of the crucible is controlled .

  According to the present invention, even if foreign matter falls into the crucible, it is possible to prevent the dislocation of the single crystal by removing the foreign matter, improve the productivity of the single crystal, and reduce the manufacturing cost. It becomes possible to provide the manufacturing method of the single crystal.

As a result of continual investigation, the inventors have optimized the gas flow conditions of the inert gas flowing in the single crystal production apparatus in the single crystal growth process, so that the foreign substances existing in the raw material melt can be reduced. In particular, it has been found that foreign substances floating on the surface of the raw material melt can be removed, and the present invention has been completed based on this finding.
Hereinafter, embodiments of a method for producing a single crystal according to the present invention will be described with reference to the accompanying drawings by taking silicon as a single crystal as an example.

[First embodiment]
The method for producing a silicon single crystal according to the present embodiment is a method for producing a silicon single crystal by the CZ method. During the step of pulling up the single crystal, the center of the crucible of the inert gas flowing on the surface of the raw material melt in the crucible The flow rate from 4 m / second to 12 m / second is directed to the outer periphery of the crucible.

  Hereinafter, the manufacturing method of the silicon single crystal of the present embodiment will be described with reference to FIGS.

First, with reference to FIG. 1, one aspect of the configuration of a silicon single crystal manufacturing apparatus that can be used in this embodiment will be briefly described.
FIG. 1 shows a schematic longitudinal section of a silicon single crystal manufacturing apparatus that can be used in the present embodiment.
A silicon single crystal manufacturing apparatus 100 shown in FIG. 1 includes crucibles 101 and 103 filled with solid polycrystalline silicon as a raw material, and a main heater 107 for heating and melting the solid polycrystalline silicon to form a silicon melt 105. The lower heater 109 is stored in the chamber 111. A pulling mechanism 141 for pulling up the grown silicon single crystal 150 is provided above the chamber 111.
A pulling wire 129 is unwound from a pulling mechanism 141 attached to the upper portion of the chamber 111, and a seed holder (not shown) for mounting a seed crystal is connected to the tip of the pulling wire 129.

The crucibles 101 and 103 are composed of a quartz crucible 101 that directly accommodates the silicon melt 105 on the inside and a carbon crucible 103 for supporting the quartz crucible 101 on the outside. The crucibles 101 and 103 are supported by a crucible shaft 113 that can be rotated up and down by a rotational drive function (not shown) attached to the lower part of the silicon single crystal manufacturing apparatus.
A main heater 107 and a lower heater 109 are disposed so as to surround the crucibles 101 and 103, and the heat from the main heater 107 is prevented from being directly radiated to the chamber 111 outside the main heater 107. A first heat insulating material 115 and a second heat insulating material 117 are provided so as to surround the main heater 107. In addition, a third heat insulating material 119 and a fourth heat insulating material 121 for preventing heat from the silicon melt 105 and the crucibles 101 and 103 from being directly radiated to the chamber 111 are provided. A radiation shield 125 is provided between the silicon melt 105, the crucibles 101, 103 and the silicon single crystal 150 so that the heat from the silicon melt 105 and the crucibles 101, 103 is not pulled up and hinders the cooling of the silicon single crystal 150. ing. In addition, about the material of the heat insulating materials 115 and 117, it is desirable to use the thing especially excellent in heat retention property, and the shaping | molding heat insulating material is normally used. As the material of the heat insulating materials 119 and 121, for example, a molded heat insulating material, carbon, or a material whose surface is covered with silicon carbide is used. The radiation shield 125 plays the role of adjusting the radiant heat. For example, a metal such as molybdenum, tungsten, or tantalum, carbon, carbon whose surface is covered with silicon carbide, and a molded heat insulating material are installed inside these. Used.

The chamber 111 is made of a metal having excellent heat resistance and thermal conductivity, such as stainless steel, and is water-cooled through a cooling pipe (not shown).
Further, a sub chamber 127 for holding and taking out the silicon single crystal 150 pulled up from the silicon melt 105 is provided at the upper portion of the chamber 111 through a gate valve (not shown). The upper end of the sub-chamber is sealed with a top plate 147, and a lid (not shown) of the sub-chamber 127 that makes it possible to take out the pulled silicon single crystal 150 is provided on the upper side surface of the sub-chamber.

  The single crystal manufacturing apparatus 100 is provided with a supply pipe 501 for supplying an inert gas to the chamber 111 and a discharge pipe 505 for discharging the inert gas supplied into the chamber 111. The supply pipe 501 has one end connected to the side surface of the sub-chamber 127 and the other end connected to a tank (not shown) that stores an inert gas. The supply pipe is provided with a first flow rate adjustment valve 502 for adjusting the flow rate of the inert gas. The discharge pipe 505 has one end connected to the lower surface of the chamber 111 and the other end connected to a vacuum pump (not shown). The discharge pipe 505 is provided with a second flow rate adjustment valve 506 that adjusts the discharge amount of the inert gas.

  Next, the silicon single crystal manufacturing method of the present embodiment using the single crystal manufacturing apparatus 100 will be specifically described.

  First, as shown in FIG. 2, the solid polycrystalline silicon raw material 155 is put into the quartz crucible 101. Then, the silicon single crystal manufacturing apparatus 100 opens the gate valve 135 (not shown) and keeps the lid (not shown) provided on the upper side surface of the sub chamber 127 closed.

  Next, after the inside of the chamber 111 and the sub chamber 127 is replaced with an inert gas, the supply pipe 501 is maintained at a low pressure in a state where an inert gas such as argon (Ar) gas is supplied. Thereafter, by heating the heaters 107 and 109, the solid polycrystalline silicon raw material 155 previously charged in the quartz crucible 101 is melted to obtain a silicon melt.

Next, as shown in FIG. 3, the gate valve 135 is closed, and the chamber 111 and the sub-chamber 127 are shut off. Thereby, the sub chamber 127 is returned to normal pressure in a state where the inside of the chamber 111 is maintained in an inert atmosphere and oxidation of the silicon melt 105 is prevented. Thereafter, the lid (not shown) of the sub chamber 127 is opened, and the seed crystal 131 is suspended from the lower end of the wire 129. After the seed crystal 131 is suspended from the lower end of the wire 129, the lid (not shown) of the sub chamber 127 is closed, and the sub chamber 127 is sealed.
Thereafter, the subchamber 127 is depressurized, and the subchamber 127 is filled with an inert atmosphere such as argon gas. Next, the gate valve 135 is opened, and the chamber 111 and the sub-chamber 127 are communicated. In this state, since the seed crystal 131 is located immediately above the silicon melt 105, it is preheated by the radiant heat of the silicon melt 105.

  Next, as shown in FIG. 1, the pulling device 141 is driven, the seed crystal 131 suspended from the lower end of the wire 129 is lowered, and at least a part of the seed crystal 131 is immersed in the silicon melt 105. Then, while pulling up the seed crystal 131, a neck portion 152 whose crystal diameter is once narrowed is formed. After dislocations are removed, the neck portion 152 is expanded to a desired crystal diameter, and a silicon single crystal 150 is gradually grown downward.

Here, when pulling up the single crystal 150, the first flow rate adjustment valve 502 is opened, and an inert gas such as argon gas is supplied into the chamber 111 from a storage tank (not shown) via the supply pipe 501. To supply. Then, the inert gas supplied into the chamber 111 moves down between the side surface of the silicon single crystal 150 and the radiation shield 125 and moves down the surface of the silicon melt 105 in the crucible from the crucible center toward the outer periphery of the crucible. Flowing. Then, the inert gas passes between the wall of the quartz crucible 103 and the radiation shield 125 and is discharged from the discharge pipe 505 to the outside of the chamber 111.
At this time, the maximum flow rate of the present embodiment is to control and maintain the flow rate of the inert gas flowing on the surface of the silicon melt 105 from the center of the crucible toward the outer periphery of the crucible so as to be 4 m / second or more and 12 m / second or less. It is a feature.
The flow rate of the inert gas is controlled and maintained by adjusting the inert gas supply / discharge amount by the first and second flow rate adjusting valves 502 and 506, adjusting the pressure inside the chamber 111, the radiation shield 125 and silicon. It is possible to adjust the distance on the surface of the melt 105 or the like.

When the flow rate of the inert gas on the surface of the silicon melt is increased, the surface of the silicon melt is pushed by the inert gas flow to generate convection from the central region of the quartz crucible toward the inner wall of the quartz crucible. If there is a foreign substance floating on the surface of the silicon melt, the foreign substance is driven to the outer periphery of the silicon melt surface by this convection and cannot approach the single crystal growth region at the center of the quartz crucible. Accordingly, it is possible to prevent the occurrence of dislocations in the silicon single crystal due to the foreign matters floating on the surface of the silicon melt adhering to the growing single crystal.
Here, the flow rate of the inert gas on the surface of the silicon melt means the flow rate of the inert gas in the vicinity of the surface that can directly affect the convection of the surface layer of the silicon melt. For example, the flow rate of the inert gas at the lower end of the radiation shield that does not directly affect the convection of the silicon melt surface layer does not fall within the range of the flow rate of the inert gas on the surface of the silicon melt.

At this time, if the flow rate of the inert gas passing through the surface of the silicon melt is too slow, foreign matters floating on the surface of the silicon melt cannot be effectively removed. Therefore, as described above, the flow rate of the inert gas is desirably 4 m / second or more. In addition, if the flow rate of the inert gas is too high, it becomes difficult to control the convection of the silicon melt in order to satisfy the standards such as the impurity and oxygen concentration of the silicon single crystal. In addition, an inert gas having a too high flow rate vibrates the silicon melt surface vigorously, which may make it difficult to grow a single crystal. Therefore, as described above, the flow rate of the inert gas is desirably 12 m / second or less.
In order to further stabilize the single crystal growth, the flow rate of the inert gas is more preferably 8 m / second or less.

  Thereafter, the silicon single crystal 150 having a desired diameter and length is pulled up by pulling the wire 129 at a predetermined speed as the silicon single crystal 150 grows while maintaining the flow rate of the inert gas.

  Then, the grown silicon single crystal 150 is raised to the subchamber 127 as shown in FIG. Then, the gate valve 135 is closed, and the chamber 111 and the sub-chamber 127 are shut off. Thereafter, the inside of the chamber 111 is maintained in an inert atmosphere, and the sub-chamber 127 is returned to normal pressure in a state where oxidation of the silicon melt 105 is prevented. Thereafter, the lid of the sub chamber 127 is opened, and the silicon single crystal 150 is taken out. In this way, the manufacturing process of the silicon single crystal 150 is completed.

  According to the present embodiment, even when foreign matter is generated in the chamber and falls into the silicon melt, the foreign matter floating on the surface of the silicon melt is effectively eliminated to grow the single crystal. The rate of dislocation can be reduced. Therefore, it is possible to provide a method for manufacturing a single crystal that can improve the productivity of the single crystal and reduce the manufacturing cost.

[Second Embodiment]
The method for producing a silicon single crystal according to the present embodiment is a method for producing a silicon single crystal by a CZ method, and a step of melting a raw material filled in a crucible into a raw material melt, and pulling the single crystal from the raw material melt A step of flowing an inert gas on the surface of the raw material melt is provided between the steps, and the outer periphery of the crucible from the crucible center of the inert gas flowing on the surface of the raw material melt in the crucible during the flow of the inert gas. The flow velocity toward is set to 8 m / second or more and 12 m / second or less.

Hereinafter, a method for manufacturing a silicon single crystal according to the present embodiment will be described with reference to FIGS.
Note that the single crystal manufacturing apparatus used in the present embodiment is the same as that in the first embodiment, and a description thereof will be omitted.
In addition, the solid polycrystalline silicon raw material is charged into the quartz crucible and the silicon raw material is melted to form a silicon melt, which is the same as that of the first embodiment described with reference to FIGS. is there.

Next, as shown in FIG. 5, in a state where the silicon raw material is melted, the first flow rate adjustment valve 502 is opened and, for example, argon gas or the like is discharged from a storage tank (not shown) via the supply pipe 501. An active gas is supplied into the chamber 111. Then, the inert gas supplied into the chamber 111 descends through the inside of the radiation shield 125 and flows on the surface of the silicon melt 105 in the quartz crucible 101 from the center of the quartz crucible 101 toward the outer periphery. Then, the inert gas passes between the wall of the quartz crucible 101 and the radiation shield 125 and is discharged out of the chamber 111 from the discharge pipe 505.
At this time, the maximum flow rate of the present embodiment is that the flow rate of the inert gas flowing on the surface of the silicon melt 105 from the center of the quartz crucible 101 toward the outer periphery is controlled to 8 m / second or more and 12 m / second or less and maintained for a certain time. It is a feature.
The flow rate of the inert gas is controlled and maintained by adjusting the inert gas supply / discharge amount by the first and second flow rate adjusting valves 502 and 506, adjusting the pressure inside the chamber 111, the radiation shield 125 and silicon. It can be performed by adjusting the distance on the surface of the melt 105, as in the first embodiment.

Thereafter, the seed crystal 131 is suspended as shown in FIG. 3, and the silicon single crystal 150 is grown while pulling up the seed crystal 131 as shown in FIG. 1, as in the first embodiment. is there.
However, unlike the first embodiment, the flow rate of the inert gas is set to be about 2 m / second.
Then, the grown silicon single crystal 150 is lifted and taken out as shown in FIG. 4 to complete the manufacturing process of the silicon single crystal 150.

In the first embodiment, a method for producing a silicon single crystal has been described in which foreign matter floating on the surface of the silicon melt is effectively eliminated by increasing the flow rate of the inert gas during pulling the single crystal. However, depending on the pulling conditions, it may be difficult to increase the flow rate of the inert gas during pulling the single crystal in order to achieve the desired single crystal quality.
In the present embodiment, the flow rate of the inert gas during pulling of the single crystal is optimized in order to realize other single crystal qualities without considering the foreign substance removal effect.
Then, after the silicon raw material is melted, prior to pulling the single crystal, an inert gas having a high flow rate is passed over the surface of the silicon melt to remove foreign matters on the surface of the silicon melt. That is, by flowing an inert gas having a high flow velocity over the surface of the melt, foreign matters floating on the surface of the silicon melt are strongly driven to the outer peripheral portion of the melt surface, and as a result, are attached to and trapped on the inner wall of the quartz crucible. Once the foreign matter adhered to the inner wall of the quartz crucible is difficult to peel off from the inner surface of the quartz crucible, the reoccurrence of floating foreign matters can be suppressed. In this way, by eliminating foreign matters floating on the surface of the silicon melt and then starting the subsequent single crystal pulling, it is possible to suppress dislocation caused by the floating foreign matters.

  In this embodiment, before the single crystal is pulled, an inert gas of 8 m / second or more and 12 m / second or less is allowed to flow on the surface of the raw material melt, so that floating foreign matters on at least the outer peripheral portion of the silicon melt surface. Is expected to be attached and captured on the inner wall of the quartz crucible. However, if the flow rate of the inert gas is slower than 8 m / second, it is not preferable because the suspended foreign matter may not be sufficiently pushed to the inner wall of the quartz crucible. Also, if the speed is faster than 12 m / sec, the silicon melt surface vibrates violently due to the high-speed inert gas flowing on the silicon melt surface, and as a result, the contact point between the quartz crucible inner wall and the silicon melt surface also fluctuates up and down. To fluctuate. When this happens, suspended foreign matter once attached to and trapped on the inner wall of the quartz crucible may be dissociated from the inner wall of the quartz crucible again when the quartz crucible inner wall and the silicon melt surface contact with each other in the vertical vibration. This is not preferable because the effect of removing the floating foreign matter is not sufficiently exhibited.

[Third embodiment]
Since the silicon single crystal manufacturing method of this embodiment is the same as that of the second embodiment except that the present invention is applied when the dislocation-converted silicon single crystal is once melted, description thereof is omitted.

When the pulled silicon single crystal is dislocated, it is assumed that the cause of the dislocation is a floating foreign material in the silicon melt. In this case, even if the single crystal is pulled after remelting, there is a high possibility that dislocations will occur due to the same foreign matter again.
Therefore, the present embodiment is characterized in that a step of flowing an inert gas is provided in the second embodiment as described with reference to FIG. 5 after remelting the dislocated silicon single crystal. And Thereafter, pulling of the silicon single crystal is continued from the re-melted silicon melt as in the second embodiment.

  According to the present embodiment, even when pulling after remelting due to dislocation due to floating foreign matter in the silicon melt, the floating foreign matter causing the dislocation is effectively removed. In addition, it is possible to prevent dislocation of the pulled single crystal.

[Fourth embodiment]
In the silicon single crystal manufacturing method of the present embodiment, the height of the portion where the surface of the raw material melt is in contact with the inner wall of the crucible in the step of flowing an inert gas at a high flow rate is the raw material melt in the step of pulling up the single crystal. Except for controlling the number of rotations of the crucible so that the surface is higher than the height of the portion in contact with the inner wall of the crucible, the description is omitted because it is the same as in the second embodiment.

  When the crucible rotational speed is increased in a state where the silicon melt is present in the quartz crucible, the silicon melt also starts to rotate so as to follow the quartz crucible rotational speed. As a result, centrifugal force is generated in the silicon melt, and the surface shape of the silicon melt has an inclination. In other words, the slope of the silicon melt surface becomes higher as it goes to the outer peripheral portion of the silicon melt surface. The inclination of the silicon melt surface tends to be promoted as the rotational speed of the quartz crucible is increased. The greatest feature of the present embodiment is that this phenomenon is used to improve the effect of removing floating foreign substances.

In the present embodiment, in the inert gas supply step before the silicon single crystal pulling step shown in FIG. 5 described in the second embodiment, the rotation of the quartz crucible is changed to the silicon single crystal pulling step shown in FIG. The speed will be higher than the expected speed. Then, the height of the portion of the silicon melt surface in contact with the inner wall of the quartz crucible is controlled to be higher than that in the silicon single crystal pulling step shown in FIG. Thereby, floating foreign substances in the silicon melt are attached to and captured on the inner wall surface of the quartz crucible.
Thereafter, the rotation speed of the quartz crucible is reduced, and the silicon single crystal 150 is pulled up as described in FIGS. 3, 1, and 5 in the second embodiment.

  Here, in the present embodiment, the height of the portion where the silicon melt surface is in contact with the inner wall of the quartz crucible when pulling the silicon single crystal is lower than the inert gas supply step before the silicon single crystal 150 pulling step. It has become. As the silicon single crystal 150 is pulled up, the silicon melt is consumed, and naturally the height of the portion where the surface of the silicon melt contacts the inner wall of the quartz crucible decreases. For this reason, during the pulling of the silicon single crystal 150, the position of the portion where the silicon melt surface is in contact with the inner wall of the quartz crucible is decreasing. Therefore, during the pulling of the silicon single crystal 150, the surface of the silicon melt does not come into contact with the suspended foreign matter adhered to or trapped on the inner wall of the quartz crucible. Absent. Therefore, according to the present embodiment, it is possible to eliminate the possibility of dislocation due to separation / regeneration of floating foreign matters. Therefore, it is possible to further reduce the dislocation rate due to floating foreign matters.

In the present embodiment, the difference in height between the step of flowing an inert gas at a high flow rate and the step of pulling up the single crystal is 2 mm or more at the portion where the surface of the raw material melt contacts the inner wall of the crucible. Is desirable. This is because the contact position between the silicon melt and the quartz crucible inner wall slightly varies with time depending on the wettability of the quartz crucible inner wall and the silicon melt, crystal growth conditions, and the like, from the viewpoint of securing a margin.
Further, in the present embodiment, the method for adding the control of the height of the portion where the surface of the raw material melt contacts the inner wall of the crucible is added to the second embodiment, but the third embodiment is described. In addition, by applying similar control, in addition to the operation and effect of the third embodiment, it is possible to obtain the same operation and effect as the present embodiment.

The embodiments of the present invention have been described above with reference to specific examples. In the description of the embodiment, the single crystal manufacturing apparatus, the manufacturing method of the single crystal, etc. are omitted for the parts that are not directly required for the description of the present invention, but the required single crystal manufacturing apparatus, Elements related to the method of manufacturing a single crystal can be appropriately selected and used.
For example, in the embodiments, a silicon single crystal has been described as an example. However, a single crystal to be grown is not necessarily limited to a silicon single crystal. For example, germanium (Ge), indium phosphide (InP), and other single crystals. It doesn't matter.
In the embodiment, argon gas is described as an example of the inert gas. However, the inert gas is not necessarily limited to argon gas, and helium gas, krypton gas, and other inert gases may be applied. Is also possible.
In addition, any single crystal manufacturing method that includes the elements of the present invention and can be appropriately modified by those skilled in the art is included in the scope of the present invention.

  Examples of the present invention will be described below, but the present invention is not limited by these examples.

表１から明らかなように、ガス流速を速くしていくにつれて無転位化率が上昇する傾向が見られる。そして、４ｍ／秒以上では、ほぼ一定となった。無転位化率が１００％に達しないのは、浮遊異物以外の有転位化要因が関与しているためと考えられる。 Example 1
A silicon single crystal having a diameter of 200 mm was grown using the method for manufacturing a silicon single crystal described in the first embodiment. The solid polycrystalline silicon charged into the quartz crucible was 150 kg.
Then, adjust the supply amount of argon gas, which is an inert gas, the pressure inside the chamber, the distance between the radiation shield and the surface of the silicon melt, and adjust the distance from the crucible center to the outer periphery of the crucible on the surface of the silicon melt during the single crystal pulling process. The flowing argon gas flow rate was changed. Under each condition, the silicon single crystal was pulled a total of 10 times, and the dislocation-free rate was examined.
Here, the dislocation-free rate is 100% when the silicon single crystal growth is completed without dislocation. When dislocations are generated during the growth of the silicon single crystal, the length of the dislocation-free portion of the silicon single crystal (= the length of the complete dislocation-free crystal portion excluding the dislocation portion and the dislocation portion of the dislocation from the grown silicon crystal) ) Is divided by the single crystal length when the dislocation-free rate is 100% (single crystal length to be pulled), and is expressed as a percentage. The results are shown in Table 1. The numerical value of the dislocation-free rate in Table 1 shows an average value of 10 times.

As is apparent from Table 1, there is a tendency for the dislocation-free rate to increase as the gas flow rate is increased. And it became almost constant at 4 m / sec or more. The reason why the dislocation-free rate does not reach 100% is considered to be because dislocation factors other than floating foreign matters are involved.

表２から明らかなように、単結晶引上げ工程の、ガス流速を速くしていくにつれて無転位化率が上昇する傾向が見られる。そして、８ｍ／秒未満では無転位化率が低下していく傾向がある。これは、アルゴンガスの流速が不十分であった為、浮遊異物が石英ルツボ内壁に完全に付着・捕獲されず、シリコン融液表面に残留してしまったことによると推測される。もっとも、シリコン単結晶の引上げ工程のアルゴンガス流速の３倍以上、すなわち、６ｍ/秒以上の領域では、実施例１の２ｍ／秒の条件と比較すると、本実施例の場合の有転位化防止効果が有意に認められると判断できる。 (Example 2)
A silicon single crystal was grown using the method for manufacturing a silicon single crystal described in the second embodiment. The silicon single crystal manufacturing apparatus used was the same as in Example 1.
After melting the solid polycrystalline silicon in the quartz crucible to form a silicon melt, before the step of pulling up the silicon single crystal, argon gas, which is an inert gas, is supplied and held in that state for 5 minutes, Thereafter, the silicon single crystal pulling step was performed with the argon flow rate lowered to 2 m / sec.
When an inert gas is flowed before the step of pulling up the silicon single crystal, the contact position between the silicon melt surface and the inner wall of the quartz crucible is approximately the same as the contact position in the subsequent step of pulling the silicon single crystal. Thus, the rotation speed of the quartz crucible was controlled.
Then, the argon gas flow rate from the center of the crucible to the outer periphery of the crucible before the step of pulling up the silicon single crystal is adjusted by adjusting the supply amount of argon gas, the pressure inside the chamber, the distance between the radiation shield and the silicon melt surface. Changed. Under each condition, the silicon single crystal was pulled a total of 10 times, and the dislocation-free rate was examined. The results are shown in Table 2.

As is apparent from Table 2, there is a tendency for the dislocation-free rate to increase as the gas flow rate is increased in the single crystal pulling step. And if it is less than 8 m / sec, there exists a tendency for a dislocation-free rate to fall. This is presumably due to the fact that the flow rate of argon gas was insufficient, so that the suspended foreign matter was not completely attached and trapped on the inner wall of the quartz crucible and remained on the surface of the silicon melt. However, in the region of 3 times or more of the argon gas flow rate in the pulling process of the silicon single crystal, that is, 6 m / second or more, compared with the condition of 2 m / second of Example 1, prevention of dislocation in the case of this example. It can be judged that the effect is significantly recognized.

表３と表２の比較から明らかなように、実施例２に加えて、種結晶の浸漬前の、シリコン融液表面と石英ルツボ内壁との接触位置を、単結晶引上げ工程における接触位置よりも２ｍｍ上昇させることにより、実施例２より無転位化率が改善した。 Example 3
A silicon single crystal was grown using the method for manufacturing a silicon single crystal described in the fourth embodiment. The silicon single crystal manufacturing apparatus used was the same as in Example 1.
After melting the solid polycrystalline silicon in the quartz crucible to form a silicon melt, argon gas, which is an inert gas, was supplied before the single crystal pulling step, and kept in that state for 5 minutes. At this time, the rotation speed of the quartz crucible was controlled so that the contact position between the silicon melt surface and the inner wall of the quartz crucible rose by 2 mm from the contact position in the subsequent silicon single crystal pulling step. Other conditions were the same as in Example 2.
Then, similarly to Example 2, the flow rate of argon gas was changed. Under each condition, the silicon single crystal was pulled a total of 10 times, and the dislocation-free rate was examined. The results are shown in Table 3.

As is clear from the comparison between Table 3 and Table 2, in addition to Example 2, the contact position between the silicon melt surface and the inner wall of the quartz crucible before the seed crystal immersion is more than the contact position in the single crystal pulling step. By increasing by 2 mm, the dislocation-free rate was improved from that in Example 2.

The typical longitudinal section explaining the manufacturing method of the silicon single crystal of a 1st embodiment. The typical longitudinal section explaining the manufacturing method of the silicon single crystal of a 1st embodiment. The typical longitudinal section explaining the manufacturing method of the silicon single crystal of a 1st embodiment. The typical longitudinal section explaining the manufacturing method of the silicon single crystal of a 1st embodiment. The typical longitudinal section explaining the manufacturing method of the silicon single crystal of a 2nd embodiment.

Explanation of symbols

101 Quartz crucible 105 Silicon melt 111 Chamber 127 Subchamber 129 Wire 131 Seed crystal 135 Gate valve 141 Lifting mechanism 150 Silicon single crystal
155 Solid polycrystalline silicon raw material 501 Supply valve 502 First flow regulating valve 505 Discharge valve 506 Second flow regulating valve

Claims (2)

A method for producing a single crystal by the Czochralski (CZ) method,
Melting the raw material filled in the crucible into a raw material melt;
Having a step of pulling a single crystal from the raw material melt,
A step of flowing an inert gas on the surface of the raw material melt is provided between the step of melting the raw material to form a raw material melt and the step of pulling up the single crystal;
In the step of flowing the inert gas, a flow rate of the inert gas from the crucible center toward the outer periphery of the crucible on the surface of the raw material melt is set to 8 m / second or more and 12 m / second or less ,
In the flow of the inert gas, the height of the portion where the surface of the raw material melt contacts the inner wall of the crucible,
In the step of pulling up the single crystal, the number of revolutions of the crucible is controlled so that the surface of the raw material melt is 2 mm or more higher than the height of the portion in contact with the inner wall of the crucible. . A method for producing a single crystal by the Czochralski (CZ) method,
Melting the raw material filled in the crucible into a raw material melt;
Having a step of pulling a single crystal from the raw material melt,
When the single crystal is dislocated,
Remelting the single crystal;
A step of flowing an inert gas on the surface of the raw material melt after the remelting when the remelting is completed;
After the step of flowing the inert gas, a step of pulling a single crystal from the remelted raw material melt is provided,
In the step of flowing the inert gas, the flow rate of the inert gas from the crucible center toward the outer periphery of the crucible on the surface of the remelted raw material melt is 8 m / second or more and 12 m / second or less ,
In the step of flowing the inert gas, the height of the portion where the surface of the raw material melt after remelting is in contact with the inner wall of the crucible,
In the step of pulling the single crystal from the remelted raw material melt, the rotational speed of the crucible is set so that the surface of the remelted raw material melt surface is 2 mm or more higher than the height of the portion in contact with the inner wall of the crucible. A method for producing a single crystal, characterized by controlling .

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