WO2019124073A1

WO2019124073A1 - Recharging tube, raw material feeding device, single crystal pulling up device, usage of recharging tube, recharging method, and single crystal pulling up method

Info

Publication number: WO2019124073A1
Application number: PCT/JP2018/044699
Authority: WO
Inventors: 飯田　哲広; 信明溝上; 孝岩本
Original assignee: 株式会社Sumco
Priority date: 2017-12-20
Filing date: 2018-12-05
Publication date: 2019-06-27
Also published as: CN111465723B; TW201928130A; JP2019112238A; JP7135315B2; CN111465723A; TWI720354B

Abstract

A cylindrical recharging tube 10, which can be used in the growth of a single crystal by Czochralski method, and which is used in a raw material feeding device for additionally charging or recharging a granular massive solid raw material S1 into a raw material molten liquid S2 in a crucible 3. The recharging tube 10 is provided with: multiple split tubes 10A and 10B which are split in the axis direction when the solid raw material is filled; and a connection unit 11 which can connect the split tubes one above the other when the solid raw material is charged into the crucible. It becomes possible to prevent the decrease in the life of the recharging tube, and it also becomes possible to reduce the occurrence of dislocation.

Description

Recharge Tube, Raw Material Supply Device, Single Crystal Pulling Device, Method of Using Recharge Tube, Recharge Method, Single Crystal Pull Method

The present invention relates to a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a charge method and a single crystal pulling method, and in particular, a technique suitable for adding or recharging solid materials in single crystal pulling by CZ method. About.
Priority is claimed on Japanese Patent Application No. 2017-244437, filed Dec. 20, 2017, the content of which is incorporated herein by reference.

Usually, in growing a silicon single crystal by the CZ method (Czochralski method), solid polycrystalline silicon introduced as initial charge into a crucible is heated and melted by a heater surrounding the crucible. Then, when the raw material melt is formed in the crucible, while rotating the crucible in a fixed direction, the seed crystal held on the crucible is lowered to be immersed in the raw material melt in the crucible. Thereafter, by raising the seed crystal while rotating the seed crystal in a predetermined direction, a cylindrical silicon single crystal is pulled and grown below the seed crystal.

As solid materials to be introduced into the crucible as initial charge, polycrystalline silicon of various shapes such as rod shape, massive, or granular is used, and each is supplied singly or as a composite to melt a silicon single crystal. It becomes the raw material of the liquid.

In such growth of silicon single crystal by the CZ method, when the solid raw material initially charged in the crucible is melted, the apparent volume after melting decreases, so the raw material melt obtained relative to the volume of the crucible Insufficient quantity. If single crystals are grown in such a state, productivity is forced to decrease due to the shortage of the raw material melt amount.

In order to avoid the decrease in productivity due to the above reasons, it is necessary to replenish the shortage of the raw material melt to secure a desired melt amount, and after the initial charge to the crucible, the solid raw material is additionally supplied An "additional charge" is being performed as a technology.

That is, in the “additional charge”, a technology for increasing the amount of raw material melt in the crucible by melting the solid raw material initially charged in the crucible and then additionally charging the solid raw material to the formed raw material melt. It is. By applying this "additional charge", the volume of the crucible to be used can be effectively utilized, and the productivity in silicon single crystal growth can be improved.

Furthermore, in the growth of silicon single crystals by the CZ method, a technique of supplying a solid material called "recharge" is also performed. Specifically, after growing and pulling up the first single crystal, a solid raw material of an amount corresponding to the decrease due to pulling up of the raw material melt is additionally charged to the residual melt in the crucible.

In other words, by recharging, a predetermined amount of raw material melt is re-formed in the crucible, and pulling up of the single crystal is repeated to increase the number of pulled crystals per crucible. Therefore, by adopting "recharge", the cost can be reduced by efficient use of the crucible, and the productivity can be improved and the growth cost of the silicon single crystal can be reduced as in the "additional charge" described above.

The raw material supply by “additional charge” and “recharge” is performed by using a raw material supply apparatus having a recharge pipe inserted from the pull chamber above the crucible into the pulling furnace, and solidifying the granular solid raw material into the raw material melt in the crucible It is known how to add to.

At this time, when adding the solid raw material, the crucible is damaged, or splashing of the raw material melt causes droplets of the raw material melt to adhere to the parts in the chamber, thereby shortening the life of the parts. May adversely affect the growth of single crystals. In order to solve such problems, various proposals have been made regarding "additional charge" and "recharge" as described in the patent documents.

JP 2003-020295 A JP, 2005-001977, A JP 2007-217224 A

However, in recent years, there has been a demand to increase the amount of recharge due to factors such as increasing the diameter of the single crystal to be pulled up, increasing the pulling length, or improving the efficiency of operation.
In order to meet this requirement, the recharge tube is inserted from the pull chamber side, so there is a limit to increasing its thickness. Therefore, although the length of the recharge pipe is to be increased, simply when the length of the recharge pipe is increased, the following problems occur.

The recharge tube is made of a softer material than polycrystalline silicon as an additional material, such as quartz, to prevent contamination. For this reason, if the length of the recharge pipe is increased, the falling lump of raw material silicon hits when charging the raw material into the recharge pipe, and the inner surface of the recharge pipe is damaged and worn away, and minute pieces such as quartz generated at this time Is mixed into the molten material, causing dislocations.
If the length of the recharge tube is increased, the material to be charged into the recharge tube may fall at a falling distance when the material is loaded, so that there is a problem that the dislocationization due to the small pieces such as quartz due to wear is further increased. .

In addition, if the inner surface of the recharging tube is damaged when massive raw material silicon hits during filling of the material, there is a possibility that the recharging tube may be damaged due to a temperature difference between the inside of the chamber during recharging and the time of filling. Therefore, in view of this strength reduction, the use of the recharge pipe has been limited a predetermined number of times.
However, if the length of the recharge pipe is increased, the material to be charged into the recharge pipe is dropped at the time of filling the material, and the falling distance of the material to be charged is increased. There was a problem that time and the number of times of use could be extremely reduced.

Furthermore, as a measure against the strength reduction due to the occurrence of such a scratch in the recharge tube, it is necessary to carry out a repair (regeneration) step for eliminating the scratch caused by heating and melting the inner surface of the recharge tube. As the length of the tube increases, the number of repairs necessarily increases.
The heating in the repair process may cause distortion in the entire recharge tube, so if the deformation is within the allowable range, it can be used after the repair process. However, if the recharge tube is elongated and the drop distance at the time of raw material filling is increased and the flaw generated is formed large and deeply at an accelerated rate, the heating amount required for repair also increases. As a result, the amount of deformation increases, and the life of the final recharge tube (usable time until discarding / usable number of times) decreases.
At the same time, along with the lengthening of the recharge pipe, the amount of heating in the repair process increases, and the amount of deformation also increases, and the life of the final recharge pipe (usable time until discarding, usable number of times) Will decrease.

In addition, although the recharge pipe cleans the inner surface each time after the completion of the recharge, this work efficiency is significantly reduced if the length of the recharge pipe is increased. Or, there was a possibility that the cleaning was insufficient, resulting in the formation of dislocations or the deterioration of the crystal properties.

The present invention has been made in view of the above circumstances, and aims to achieve the following objects.
1. To simultaneously realize an increase in the amount of charge in the recharge pipe and a reduction in the life of the recharge pipe.
2. At the same time, reduce the occurrence of dislocations.
3. At the same time, to prevent the deterioration of the work required to recharge.
4. Also, prevent the deterioration of crystal quality.

The recharge pipe of the present invention is a cylindrical recharge pipe in a raw material supply apparatus which is used to grow a single crystal by the Czochralski method, and additionally charges or recharges the granular solid raw material to the raw material melt in the crucible. ,
A plurality of divided tubes which are divided in the axial direction when filling the solid material;
A connecting portion connecting the divided tubes up and down when the solid material is introduced into the crucible;
The above problem is solved by having the
In the split pipe of the present invention, in the split pipe, the inner diameter of the upper end of the split pipe at the lower position when connected is equal to the inner diameter of the lower end of the split pipe at the upper position, or the lower end of the split pipe at the upper position It can be set larger than the inner diameter of.
In the recharge pipe of the present invention, the upper end inner diameter of the divided pipe may be set equal to the lower end inner diameter or larger than the lower end inner diameter.
In the recharge pipe of the present invention, the connecting portion may be provided with a flange portion extending outward in the radial direction, and a fastening portion for fastening the flange portion may be provided.
According to the recharge pipe of the present invention, the lower end of the divided pipe, which is the upper position, can be fitted to the upper end of the divided pipe, which is the lower position at the time of connection.
In the recharge pipe of the present invention, the connection portion may be connected by abutting the upper end surface and the lower end surface of the divided pipe.
In the recharge pipe of the present invention, a buffer member may be provided on the surface where the upper divided pipe and the lower divided pipe are in contact with each other in the connection portion.
The inner diameter of the buffer member may be set equal to the inner diameter of the lower end of the divided pipe at the upper position, or larger than the inner diameter of the lower end of the divided pipe at the upper position.
In the recharge pipe of the present invention, the divided pipe may be made of quartz, and the buffer member may be made of a material having flexibility and containing carbon.
The raw material supply apparatus according to the present invention is a raw material supply apparatus which is used to grow a single crystal by the Czochralski method, and additionally charges or recharges the granular solid raw material to the raw material melt in the crucible,
Any of the above-mentioned recharge tubes,
A conical bottom lid removably attached to the lower open end of the recharge tube;
A lifting means for suspending the recharging pipe and the bottom cover so as to be able to move up and down and opening the lower opening end of the recharging pipe so that the solid raw material can be charged into the raw material melt in the crucible;
Can be equipped.
The single crystal pulling apparatus of the present invention is a single crystal pulling apparatus for growing a single crystal from a raw material melt by the Czochralski method,
The above-mentioned raw material supply device,
A furnace body provided with the crucible inside;
And a heat shield for shielding radiant heat to the single crystal grown from the raw material melt at the upper position of the crucible inside the furnace body as a cylindrical shape having a diameter-reduced diameter at the lower end. ,
At the time of additional charging or recharging, the recharge tube is inserted from above into the inside of the heat shield, and the lower end of the recharge tube is positioned above the lower end of the heat shield, and in this state the inside of the crucible The solid material can be charged into the raw material melt.
In the single crystal pulling apparatus of the present invention, when the solid raw material is charged into the raw material melt in the crucible, the connecting portion can be set at a position higher than the lower end position of the heat shield.
In the single crystal pulling apparatus according to the present invention, when charging the solid material into the recharge pipe outside the furnace body,
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion It can have an inclined support that supports as it can be connected to.
The method of using the recharge tube of the present invention is
It is a usage method of the recharge pipe as described in any of the above,
By filling the solid material, only the divided pipe whose inner surface is damaged can be replaced to a predetermined state.
According to the method of using the recharge tube of the present invention, the divided tube may be replaced when the filling of the solid raw material causes a flaw of the inner surface to have a permeability of less than 70% as compared with the condition without flaws. it can.
According to the method of using the recharge tube of the present invention, the inner surface of the split tube which has been damaged and replaced can be heated and regenerated.
The method of using the recharge pipe according to the present invention can prevent reuse when the deformation of the divided pipe regenerated by heating exceeds a predetermined amount.
The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion The solid material can be further charged in connection with
The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
The inclined support supports the divided pipe mounted with the bottom lid at the lower end by the inclined support, and the divided pipe erected along with the filling of the solid material is erected in the vertical direction side, and the connection portion Thus, the divided pipe can be connected to the upper side to further charge the solid material.
The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
After additionally charging or recharging the raw material melt in the crucible,
The inclined support supports the plurality of connected divided tubes and can be inclined to separate the divided tubes by the connecting portion.
According to the single crystal pulling method of the present invention, the raw material melt in the crucible is additionally charged or recharged by the above-described recharge method.
A single crystal can be grown from the raw material melt.

The recharge pipe of the present invention is a cylindrical recharge pipe in a raw material supply apparatus which is used to grow a single crystal by the Czochralski method, and additionally charges or recharges the granular solid raw material to the raw material melt in the crucible. ,
A plurality of divided tubes which are divided in the axial direction when filling the solid material;
A connecting portion connecting the divided tubes up and down when the solid material is introduced into the crucible;
Have. As a result, when the solid raw material is charged, the recharge pipe can be divided in the axial direction to fill the divided pipe with a short axial dimension. Thereby, even if the filling amount of the solid raw material is the same, the distance in which the solid raw material to be filled falls is short compared to the non-divided recharge tube. Therefore, it is possible to reduce the impact on the surface of the recharge tube at the time of filling, and to reduce the occurrence of scratches on the surface of the recharge tube.

This makes it possible to prevent the generation of fine powder from the recharge tube made of quartz or the like, and to suppress the occurrence of dislocation formation. At the same time, after filling the solid material to the vicinity of the upper end in the axial direction, the next divided pipe is connected by the connecting portion, and the solid material is charged to recharge the solid material without increasing the falling distance of the solid material. It is possible to significantly increase the total filling volume.

Moreover, according to the above configuration, it is possible to selectively replace only the divided pipe which is largely deteriorated in the inner surface state due to the falling of the solid material. Thereby, it becomes possible to make the replacement time of each divided pipe different according to the progress degree of the inner surface deterioration state.

For example, in the recharge pipe divided into two, the replacement time of the upper position can be made longer than the replacement time of the divided pipe at the lower position. Alternatively, in the recharge pipe divided into three parts, only the lower position is exchanged in a short cycle, and the divided pipes in the upper and middle positions are exchanged at the connection position, and the exchange timings are made approximately the same. It becomes possible to set and the like.

Furthermore, even when the inner surface of the pipe is cleaned after completion of the recharge, the pipe length is short, so it has high handling properties, and it is possible to reduce the burden on workers and shorten the working time.
At the same time, it is possible to reduce the deterioration rate of the inner surface state caused by the falling of the forming material. For this reason, the life itself to the regeneration process of the recharge tube can be increased to increase the usable number of recharges. In addition, it is possible to reduce the number of times of the regeneration process and to increase the life due to the deformation in the regeneration process.

Here, in the present invention, the term "recharge" means to additionally charge or recharge the raw material melt in the crucible.

In the split pipe of the present invention, in the split pipe, the inner diameter of the upper end of the split pipe at the lower position when connected is equal to the inner diameter of the lower end of the split pipe at the upper position, or the lower end of the split pipe at the upper position It is set larger than the inner diameter of. As a result, the divided pipe at the lower position at the time of connection does not protrude inward (center side) from the divided pipe at the upper position in plan view. For this reason, the solid raw material to be charged does not directly collide with the upper end of the divided pipe which is the lower position. Thereby, a flaw can be made in the vicinity of the upper end of the divided pipe which is the lower position. Alternatively, cracking or chipping occurs near the upper end of the divided pipe which is the lower position, and generation of impurities resulting therefrom can be prevented. For this reason, it is possible to realize the prevention of the occurrence of dislocation and the prevention of the deterioration of the crystal characteristics.

In the recharge pipe of the present invention, the upper end inner diameter of the divided pipe is set equal to the lower end inner diameter or larger than the lower end inner diameter. Thus, for example, the inner diameter of the divided pipe is reduced from the upper end toward the lower end, or in the cylindrical divided pipe, the inner diameter is reduced toward the lower end only near the lower end. be able to.

In the recharge pipe of the present invention, the connecting portion is provided with a flange portion extending radially outward, and a fastening portion for fastening the flange portion is provided. Thus, in the connecting portion, the upper and lower divided tubes are arranged so that the axial directions coincide with each other, and the flange located near the upper end of the divided tube at the lower position and the flange located near the lower end of the divided tube at the upper position Let the parts face each other. And it becomes possible to connect easily by fastening these flange parts in a parallel state from the up-and-down direction or from the radial outside by fastening parts.

In the recharge pipe of the present invention, the lower end of the divided pipe, which is the upper position, is fitted to the upper end of the divided pipe, which is the lower position at the time of connection. As a result, the lower end of the divided pipe, which is the upper position, is inserted into the upper end of the divided pipe, which is the lower position at the time of connection, and it is possible to easily connect only by fitting them.

In the recharge pipe of the present invention, the connection portion is connected by butting the upper end face and the lower end face of the divided pipe. As a result, the upper end surface and the lower end surface of the divided pipe come into contact with each other, and it becomes possible to seal the vicinity of the connection portion of the connected divided pipe. As a result, it is possible to move the recharge tube to a predetermined recharge position while maintaining the state in which the inside and the outside of the recharge tube are separated in the single crystal pulling apparatus at the time of recharge.
Furthermore, when the upper end surface and the lower end surface of the divided pipe do not contact each other in the connecting portion, the upper end outer peripheral surface and the lower end inner peripheral surface are in contact with each other to seal the vicinity of the connecting portion of the divided pipe. Is also possible.

In the recharge pipe according to the present invention, a buffer member is provided on the surface where the upper divided pipe and the lower divided pipe are in contact with each other in the connection portion. As a result, the connecting divided tubes made of quartz or the like having rigidity do not come in direct contact with each other and can be connected via the flexible buffer member to easily seal the vicinity of the connecting portion. At the same time, it is possible to prevent the occurrence of problems such as breakage caused by direct contact between the connected divided pipes made of quartz or the like.

In the recharge pipe of the present invention, the inner diameter of the buffer member is set equal to the inner diameter of the lower end of the divided pipe at the upper position, or larger than the inner diameter of the lower end of the divided pipe at the upper position. Thus, the solid material to be filled does not directly collide with the buffer member because the buffer member is hidden in the divided pipe at the upper position. As a result, the generation of impurities caused by the buffer member can be prevented, so that it is possible to prevent the deterioration of crystal characteristics such as an increase in carbon concentration due to the mixing of the buffer member containing carbon, for example. .

In the recharge pipe of the present invention, the divided pipe is made of quartz, and the buffer member is made of a material having flexibility and containing carbon. Thereby, even when the divided pipes are deformed, the deformation can be absorbed to easily seal the vicinity of the connection portion. At the same time, it is possible to prevent the occurrence of problems such as breakage caused by direct contact between the connected divided pipes made of quartz or the like.

The raw material supply apparatus according to the present invention is a raw material supply apparatus which is used to grow a single crystal by the Czochralski method, and additionally charges or recharges the granular solid raw material to the raw material melt in the crucible,
Any of the above-mentioned recharge tubes,
A conical bottom lid removably attached to the lower open end of the recharge tube;
A lifting means for suspending the recharging pipe and the bottom cover so as to be able to move up and down and opening the lower opening end of the recharging pipe so that the solid raw material can be charged into the raw material melt in the crucible;
Equipped with As a result, in the recharge pipe capable of increasing the amount of recharging, the occurrence of damage due to solid raw material contact is reduced, the occurrence of dislocation is reduced, the number of usable recharge pipes is increased, and the replacement time of each divided pipe is controlled. It is possible to improve work efficiency.

At the same time, the axial length of the split tube can be shortened. In addition, the distance to which the solid material to be filled falls is also shortened with respect to the bottom lid and the pulling means located inside the recharge pipe. As a result, it is possible to reduce the impact on the bottom lid and the pulling means at the time of filling, and to reduce the generation of impurities resulting from the bottom lid and the pulling means.

The single crystal pulling apparatus of the present invention is a single crystal pulling apparatus for growing a single crystal from a raw material melt by the Czochralski method,
The above-mentioned raw material supply device,
A furnace body provided with the crucible inside;
And a heat shield for shielding radiant heat to the single crystal grown from the raw material melt at the upper position of the crucible inside the furnace body as a cylindrical shape having a diameter-reduced diameter at the lower end. ,
At the time of additional charging or recharging, the recharge tube is inserted from above into the inside of the heat shield, and the lower end of the recharge tube is positioned above the lower end of the heat shield, and in this state the inside of the crucible The solid material is charged into the raw material melt. As a result, in the recharge pipe which can increase the recharge amount, the occurrence of damage due to contact with the solid material is reduced. In addition, the generation of impurities due to the bottom lid and pulling means is reduced, the occurrence of dislocations is reduced, the deterioration of the crystal characteristics of the single crystal to be pulled up is prevented, and the number of usable recharge tubes is increased. It becomes possible to control the replacement time and improve the work efficiency.

In the single crystal pulling apparatus of the present invention, when the solid raw material is charged into the raw material melt in the crucible, the connecting portion is set at a position higher than the lower end position of the heat shield. Thereby, the bad influence resulting from the high temperature from the heat | fever of the raw material melt solution with respect to the fastening part and buffer member in a connection part or a heater can be reduced. At the same time, it is possible to reduce adverse effects such as deformation due to high temperature from the heat of the raw material melt and the heater with respect to the divided tubes other than the lowermost position.

In the single crystal pulling apparatus according to the present invention, when charging the solid material into the recharge pipe outside the furnace body,
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion And an inclined support that supports as connectable to the With this configuration, when the filling operation is performed, first, the divided pipe at the lowermost position where the bottom cover is mounted is supported (placed) in an inclined state on the inclined support. Then, the divided tube is filled with the solid material. Then, when the solid raw material is filled up to the vicinity of the upper end of the divided pipe which is the lowermost position, the next divided pipe is connected by the connecting portion. Furthermore, solid material can be filled in the connected divided pipe. Moreover, during this filling operation, the inclination angle of the divided pipe can be changed between the inclined state and the erected state regardless of the connected state of the divided pipe, so that the workability of the filling operation can be improved. In addition, it is possible to adjust the angle so as to reduce the impact of the solid raw material to be filled coming into contact with the recharging pipe or the like. Furthermore, when charging is completed, it is also easy to set up so that the axial direction of the recharge pipe is vertical so that it can be lifted in the vertical direction in order to perform recharging.

The method of using the recharge tube of the present invention is
It is a usage method of the recharge pipe as described in any of the above,
Only the divided pipe whose inner surface is damaged to a predetermined state is replaced by the filling of the solid material. As a result, it is possible to selectively replace only the divided pipe which is largely deteriorated in the inner surface state due to the falling of the solid material. As a result, the life of the recharge tube is extended by changing the replacement time of each divided tube according to the progress degree of the inner surface degradation state, and the increase in the recharge amount, the reduction of occurrence of dislocation and the prevention of the crystal quality deterioration It is possible to simultaneously achieve cost reduction.

For example, in the divided divided recharge pipe, the replacement time of the divided pipe at the lower position where the solid material may contact more even when the divided pipe at the upper position is filled, the replacement time of the divided pipe at the upper position It can be made shorter and the split tube at the lower position can be replaced quickly. Alternatively, in the recharge tube divided into three and having the same shape, prepare a split tube more than the number required for the initial recharge amount in the connected state, and the lower position where the pain gets worse first and the replacement state takes place Only the split tubes of can be replaced in a short cycle. Furthermore, the frequency of replacement of the middle divided pipe can be reduced compared to the lower divided pipe. Further, the frequency of replacement of the divided pipe at the upper position can be reduced compared to the divided pipe at the middle position. Furthermore, it is possible to extend the life as a recharge pipe, such as setting the replacement time to almost the same degree by using the connection positions in the divided pipes at the upper, middle, and lower positions in turn, and using them in sequence. Become.

According to the method of using the recharge tube of the present invention, the divided tube is replaced when there is a portion with a transmittance of less than 70% due to the scratch of the inner surface caused by the filling of the solid material compared to the condition without the scratch. . As a result, it is possible to selectively replace only the divided pipe having a large inner surface state deterioration. If the transmission rate is lower than 70%, the divided pipes are not suitable because the strength is reduced. Also, in the portion where the transmittance is less than 70%, the portion having the largest area can be a region of about 10 cm square. Alternatively, three to four regions each having a size of about 5 cm square can be formed in a portion where the transmittance is less than 70%.
As a result, the strength of the recharge tube can be ensured, the occurrence of dislocation can be prevented, and the deterioration of crystal quality can be prevented.

The method of using the recharge tube of the present invention heats and regenerates the inner surface of the split tube which has been damaged and replaced. Thereby, the replaced divided pipe can be made reusable. As a result, it is possible to reuse the divided pipe in a state of maintaining strength and preventing dislocation in a non-scratched state to extend the life and achieve cost reduction.

The method of using the recharge pipe according to the present invention does not reuse when the deformation of the divided pipe regenerated by heating exceeds a predetermined amount. In this way, it is possible to secure the safety in the recharge by using only the divided pipe which can maintain the sealing at the connection portion.

The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion And the solid material is further charged. Thereby, it is possible to perform single crystal pulling by adding or recharging the raw material increased by the recharge pipe in a state where generation of dislocation is suppressed and quality deterioration such as fluctuation of carbon concentration is suppressed in the pulling crystal. It becomes.

The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
The inclined support supports the divided pipe mounted with the bottom lid at the lower end by the inclined support, and the divided pipe erected along with the filling of the solid material is erected in the vertical direction side, and the connection portion Thus, the dividing pipe is connected to the upper side to further charge the solid material. As a result, the inclination angle is controlled between the inclined state and the erected state in the vertical direction, and the solid raw material can be charged into the recharging pipe, thereby improving the work efficiency and the safety in the raw material filling step. And improve the crystal quality.

The recharging method of the present invention is, in the single crystal pulling apparatus described above, a method of additionally charging or recharging the raw material melt in the crucible,
After additionally charging or recharging the raw material melt in the crucible,
The inclined support supports the connected plurality of divided pipes, and the divided pipes are separated by the connection portion by being inclined. As a result, it is possible to improve the work efficiency to the next recharging step after the recharging step, and to reduce the manufacturing cost of the single crystal.

According to the single crystal pulling method of the present invention, the raw material melt in the crucible is additionally charged or recharged by the above-described recharge method.
A single crystal is grown from the raw material melt. As a result, the amount of recharging can be increased, the reduction in crystal quality can be prevented, the occurrence of dislocation can be suppressed, the working efficiency can be improved, and the manufacturing cost can be reduced to perform single crystal pulling.

According to the present invention, the increase of the filling amount in the recharge tube and the prevention of the life decrease of the recharge tube are realized simultaneously, and at the same time, the occurrence of dislocation is reduced, the workability for the recharge is prevented, and the crystal quality is reduced. It is possible to achieve the effect that the drop can be prevented.

It is a front sectional view showing a 1st embodiment of a recharge pipe used for a materials feeding device concerning the present invention. It is an exploded perspective view showing a 1st embodiment of a recharge pipe concerning the present invention. It is an expanded sectional view showing the connection part of the division pipe in a 1st embodiment of the recharge pipe concerning the present invention. It is an expansion right sectional view showing the lower end side in a 1st embodiment of the recharge pipe used for the materials feeding device concerning the present invention. It is a plane sectional view showing a 1st embodiment of a recharge pipe used for a materials feeding device concerning the present invention. It is an enlarged front view showing the upper end side of the state where rise of the recharge pipe in the first embodiment of the recharge pipe used for the raw material supply device according to the present invention is stopped. It is an enlarged front view showing the upper end side in the state where the metal shaft on the upper end side in the first embodiment of the recharge pipe used in the raw material supply device according to the present invention is further lowered to open the bottom lid. It is a top view which shows the metal upper member used on the upper end side in 1st Embodiment of the recharge pipe used for the raw material supply apparatus which concerns on this invention. It is a schematic diagram which shows the filling process to the division pipe in 1st Embodiment of the recharge method which concerns on this invention. It is a schematic diagram which shows the filling process to the division pipe in 1st Embodiment of the recharge method which concerns on this invention. It is a schematic diagram which shows the filling process to the conventional recharge pipe. It is a flowchart which shows 1st Embodiment of the recharge method which concerns on this invention. It is a schematic diagram which shows 1st Embodiment of the single-crystal pulling apparatus which has arrange | positioned the raw material supply apparatus which concerns on this invention. It is a schematic diagram which shows 1st Embodiment of the single-crystal pulling apparatus which has arrange | positioned the raw material supply apparatus which concerns on this invention. It is a schematic diagram which shows the inclination support stand in 2nd Embodiment of the single crystal pulling apparatus which concerns on this invention. It is a schematic diagram which shows the inclination support stand in 2nd Embodiment of the single crystal pulling apparatus which concerns on this invention. It is a schematic diagram which shows the inclination support stand in 2nd Embodiment of the single crystal pulling apparatus which concerns on this invention. It is a schematic diagram which shows the inclination support stand in 2nd Embodiment of the single crystal pulling apparatus which concerns on this invention. It is a schematic cross section which shows 3rd Embodiment of the recharge pipe | tube which concerns on this invention. It is an expanded sectional view showing a divided pipe connection part in a 3rd embodiment of a recharge pipe concerning the present invention. It is an exploded perspective view showing a 3rd embodiment of a recharge pipe concerning the present invention. It is a schematic diagram which shows the raw material supply apparatus in 3rd Embodiment of the single crystal pulling apparatus which concerns on this invention. It is a schematic cross section which shows the division pipe connection part in 4th Embodiment of the recharge pipe which concerns on this invention. It is a schematic diagram in 5th Embodiment of the recharge pipe | tube which concerns on this invention. It is a schematic diagram in 6th Embodiment of the recharge pipe | tube which concerns on this invention. It is a schematic diagram in 7th Embodiment of the recharge pipe | tube which concerns on this invention.

S1: Solid raw material S2: Raw material melt 1: Main chamber 2: Pull chamber 2a: Drive mechanism (pulling up means)
3 Crucible 4 Support shaft 4A Susceptor 5 Heater 6 Insulation material 7 Pull-up shaft (pull-up means)
8 ... Suspension jig (lifting means)
9 Upper flange portion 9a Metal flange 10 Recharge pipe 10A Lower divided pipe (divided pipe)
10Aa ... upper end 10Ab ... lower end 10B ... upper divided pipe (divided pipe)
10Ba: upper end portion 10Bb: lower end portion 10C: upper additional split pipe (split pipe)
10D ... inside split tube (split tube)
11 ...

connection part

11a, 11b, 1m, 11n ... flange part 11c ... connection hole 11d ... bolt and nut (fastening part)

11e Buffer member

11g Mating groove

11h Mating groove 12 Heat shield 13 Gate valve 14 Bottom lid 15 Metal shaft (pulling up means)
16 ... Protective pipe (lifting means)
16a: Sliding protective tube 16b: Coating protective tube 16c: Fixed plate portion 16f: Fixed inclined plate 18: Hanger 19: Metal washer 20: Metal upper member 21: Long screw 30: Tilted support base 31: Support portion 32: Support truck portion 33: Wheel 34: Tilting stand 35: Tilting support portion 35a: Horizontal axis 36: Base portion 36a: Tilting portion 37, 38: Axis 39: Tilting drive portion

Hereinafter, a first embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a recharge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
FIG. 1 is a front sectional view showing a recharge pipe in the present embodiment. FIG. 2 is an exploded perspective view showing the recharge pipe in the present embodiment. FIG. 3 is an enlarged cross-sectional view showing a connection portion in the recharge pipe in the present embodiment. In the figure, reference numeral 10 is a recharge pipe.

The recharge tube 10 according to the present embodiment, as described later, constitutes a raw material supply device that recharges a single crystal pulling apparatus according to the CZ method (Czochralski method).
As shown in FIGS. 1 to 3, the recharge tube 10 according to the present embodiment has a cylindrical shape made of quartz, and the solid raw material is charged therein.

As shown in FIGS. 1 and 2, the recharge pipe 10 is divided into two in the vertical direction, which is the axial direction in the present embodiment, and the lower divided pipe (divided pipe) 10A and the upper divided pipe (divided pipe) 10B It consists of
The lower divided pipe 10A and the upper divided pipe 10B are set to have substantially the same inner diameter, and the upper end of the lower divided pipe 10A and the lower end of the upper divided pipe 10B can be connected by the connecting portion 11.

As the connection portion 11, as shown in FIGS. 2 to 3, a flange portion 11a at the upper end of the lower divided pipe 10A and a flange portion 11b at the lower end of the upper divided pipe 10B are provided. The connecting portion 11 is provided with a plurality of connecting

holes

11c and 11c circumferentially separated from each other in the flange portion 11a and the flange portion 11b, and bolts and nuts 11d and 11d as fastening portions for fastening these. Be As the connection part 11, the buffer member 11e pinched by the flange part 11a and the flange part 11b is provided.

As shown in FIGS. 2 to 3, a plurality of connection holes 11c are arranged at substantially equal intervals in the circumferential direction in the flange portion 11a and the flange portion 11b. In the present embodiment, six connection holes 11 c are provided, but the number is not limited to this number.

As shown in FIG. 3, the bolts and nuts 11d and 11d are made of metal that is resistant to high temperatures in the single crystal pulling apparatus, and further, to prevent release of minute objects and the like that cause dislocation or the like. For example, it is a set of a bolt and a nut subjected to surface treatment and the like. Specifically, it can be made of SUS (stainless steel) or the like when heat resistance is not required so much, or molybdenum or the like when high temperature resistance is required. Further, the nut 11 d is a double nut.

Further, a metal member 11f is provided between the bolt / nut 11d and the connection hole 11c on the lower surface of the flange portion 11a and the upper surface of the flange portion 11b, and the flange portion 11a, the flange portion 11b, and the bolt Direct contact with the nut 11 d is prevented.

The buffer member 11 e contacts the upper surface of the flange portion 11 a and the lower surface of the flange portion 11 b as shown in FIGS. 1 and 3. The buffer member 11 e is in the form of a thin, flexible ring. This is to prevent direct contact between the upper surface of the flange portion 11a fastened by the bolt and nut 11d and the lower surface of the flange portion 11b, and to absorb deformation between them. Specifically, the buffer member 11 e can be made of a heat-resistant resin that is resistant to high temperatures in the single crystal pulling apparatus. Alternatively, the buffer member 11 e may include or consist of flexible carbon. Further, as the buffer member 11e, a fluorine resin such as Teflon (registered trademark), a carbon fiber non-woven fabric, or the like is applied.

The outer diameter of the buffer member 11e is not particularly limited, but the inner diameter is larger than the inner diameter of the lower end of the upper divided pipe 10B. In other words, when viewed from the upper side, it is set so as not to protrude inside the recharge pipe 10 more than the lower end of the upper divided pipe 10B. Further, the thickness dimension of the buffer member 11e is not particularly limited as long as it can follow the deformation of the lower divided pipe 10A and the upper divided pipe 10B at the time of fastening by the fastening portion and the sealing of these connecting portions 11 can be maintained. .

Furthermore, when the plane accuracy is high enough that the upper end surface of the lower divided pipe 10A and the lower end surface of the upper divided pipe 10B can butt seal each other, the buffer member 11e may not be provided.

At the upper end of the upper divided pipe 10B, as shown in FIGS. 1 to 2, the upper flange portion 9 is set such that its outer dimensions are larger than the outer diameters of the

flange portions

11a and 11b. It is done.

FIG. 4 is an enlarged front sectional view showing the lower end side of the recharge pipe in the present embodiment. FIG. 5 is a plan sectional view showing the lower end side of the recharge pipe in the present embodiment.
As shown in FIG. 4, the lower end of the lower divided pipe 10A has a conical bottom lid 14 detachably attached to the recharge pipe.
The bottom cover 14 is connected to a metal shaft (pulling up means) 15 penetrating the inside of the recharge pipe 10 from the top.

As shown in FIG. 4, the metal shaft 15 penetrates the recharge pipe 10 and is protected by a protective pipe (pulling-up means) 16 in order to prevent direct contact with the solid raw material inside. The protective tube 16 is composed of a coated protective tube 16b directly covering the metal shaft 15, and a sliding protective tube 16a in which the coated protective tube 16b is slidably inserted. The protective tube 16 prevents the metal shaft 15 from coming into direct contact with the solid raw material, and ensures a stable operating state without causing the metal shaft 15 to shift.

The sliding protection tube 16a is fixed to the recharge tube 10 by a fixing plate portion 16c, as shown in FIGS. The sliding protective tube 16a is vertically disposed. The sliding protective tube 16 a is disposed at an axial center position of the recharge tube 10. The fixed plate portion 16c is a plate. The fixed plate portion 16c is disposed in the vertical direction, which is the axial direction of the recharge tube 10 and the sliding protection tube 16a. The fixed plate portion 16 c extends from the inner surface of the recharge tube 10 to the recharge tube 10 in the radial direction of the recharge tube 10.

The fixed plate portion 16c is connected by the lower divided pipe 10A and the upper divided pipe 10B, and the metal shaft 15 is in the axial direction with respect to the coated protective pipe 16b and the sliding protective pipe 16a which are separated in the vicinity of the connecting portion 11. It penetrates in a continuous state.

Therefore, the metal shaft 15 passing through the recharging pipe 10 is not only prevented from being contaminated with the solid raw material by the covering protection pipe 16b directly covering the same, but also by the action of the sliding protection pipe 16a. It does not shift from the center position.

In addition, since the fixed plate portion 16c is located in the radial direction of the recharge pipe 10, when the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11, they should be arranged to be substantially flush. Good.
Thereby, the metal shaft 15 can vertically suspend the recharge tube 10 at the center position of the crucible, and can uniformly supply the solid material into the melt in the crucible.

FIG. 6 is an enlarged front view showing the upper end side of the state where the descent of the recharge pipe in the present embodiment is stopped. FIG. 7 is an enlarged front view showing the upper end side of a state in which the metal shaft is further lowered on the upper end side of the recharge pipe in the present embodiment to open the bottom lid. FIG. 8 is a plan view showing a metal upper member used on the upper end side of the recharge pipe in the present embodiment.

In the raw material supply device, lifting and lowering means is also provided to the recharge pipe 10 in synchronization with the lifting and lowering of the metal shaft 15. In the raw material supply device, the conical bottom lid 14 is inserted into the lower opening end to lift the recharging pipe 10 in synchronization with the lifting timing by the lifting means (pulling up means) provided on the recharging pipe 10 ing. By synchronizing the elevation timing, not only elevation of the metal shaft 15 but also elevation of the recharge tube 10 can be stabilized.

In the raw material supply apparatus, as shown in FIGS. 6 to 7, a metal (stainless steel or the like) washer 19 is provided on the metal shaft 15 as a lifting and lowering means (lifting means) of the recharge pipe 10. The sliding protection pipe 16a is disposed at the center position of the recharge pipe 10, and the metal shaft is moved up and down in the inside thereof. A metal washer 19 is attached to a predetermined height position of the metal shaft 15. Furthermore, as the lifting means by the metal washer 19, a dedicated hanger 18 equipped to suspend the recharging tube 10 uniformly is used.

Elevation timing by adjusting the fixing position of the metal washer 19 so that the timing to lift the recharge tube 10 by inserting the conical bottom lid 14 into the lower opening end and the timing to lift the recharge tube 10 coincide with each other. Can be synchronized. Thereby, according to the raising and lowering of the metal shaft 15, the raising and lowering of the recharge pipe 10 can be further stabilized.

The metal upper member 20 is made of the same material as the bolt and nut 11 d and is attached to the upper portion of the recharge pipe 10.
A metal flange 9a can be provided as a hooking member.

The metal flange 9a is provided with a through hole 20a at a predetermined position in the circumferential direction of the metal upper member 20 described above, and is fixed to the metal upper member 20 of the recharge pipe 10 by tightening the long screw 21 with nuts. Structure. In this case, the height adjustment of the metal flange 9 a is performed by the tightening length of the long screw 21 so as to adjust the lowering stop height of the recharge pipe 10.

FIG. 9 is a process chart showing a method of filling the recharge pipe in the present embodiment. FIG. 10 is a process chart showing a method of filling the recharge pipe in the present embodiment. FIG. 11 is a process diagram showing a filling method in the conventional recharging tube. FIG. 12 is a flowchart showing the recharging method in the present embodiment.

As shown in FIG. 12, the recharging method according to the present embodiment includes, as shown in FIG. 12, a recharging amount setting step S01, a coupling length setting step S02, a cleaning step S03, a lowermost divided pipe setting step S04, an inclination step S05, and a raw material. Filling step S06, recharge amount determination step S07, divided pipe setting step S08, connection step S09, erecting step S10, recharge step S11, division step S12, recharge number counting step S13, recharge number determination step It can have S14, tube penetration visual observation process S15, exchange process S16, cleaning process S17, regeneration treatment process S20, deformation amount determination process S21, and discard process S22.

In the recharging method according to this embodiment, the amount of solid raw material S1 to be additionally charged or recharged to the crucible is set as a recharging amount setting step S01 shown in FIG. Then, as the coupling length setting step S02 shown in FIG. 12, the number of couplings of the divided pipes in the recharge pipe 10 is determined so as to have a volume capable of charging the solid raw material S1 of the amount set in the recharge amount setting step S01.

At this time, in consideration of the falling distance of the solid raw material S1 described later and the damage to the inner surface of the recharge pipe 10, the length (the number of connected pipes) of the divided pipe is set. In the present embodiment, since the recharge pipe 10 is divided into two parts, the lower divided pipe 10A and the upper divided pipe 10B, it is set whether to connect the upper divided pipe 10B.

Then, after cleaning the inner surface of the divided pipe to be used as the cleaning step S03 shown in FIG. 12, the lower divided pipe 10A is not connected to the upper divided pipe 10B as the lowermost divided pipe setting step S04 shown in FIG. Prepare in a separated state. Then, the bottom lid 14 is inserted into the lower open end of the lower divided pipe 10A to be in a closed state, and the lower end of the metal shaft 15 penetrating the protective tube 16 is attached to the bottom lid 14 in a filling ready state.

Next, as shown in FIG. 9, as the raw material filling step S06 shown in FIG. 12 with the lower divided pipe 10A supported in the inclined state at the predetermined angle as the inclination step S05 shown in FIG. The lower divided pipe 10A is filled.
At this time, although the solid raw material S1 hits the inner wall surface of the lower divided pipe 10A, the falling distance of the solid raw material S1 is shorter than that of the conventional non-divided recharge pipe 100 shown in FIG. Less damage to the wall.

Subsequently, it is determined whether the solid raw material S1 of the quantity set by recharge amount setting process S01 was filled as recharge amount determination process S07 shown in FIG. Then, when the amount of the solid raw material S1 is insufficient, the upper divided pipe 10B is set at the upper position of the lower divided pipe 10A in the divided pipe setting step S08 shown in FIG. Then, in the connecting step S09 shown in FIG. 12, the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11. At this time, also in the upper divided pipe 10B, the metal shaft 15 is made to penetrate the protective pipe 16.

Next, as shown in FIG. 10, as the raw material filling step S06 shown in FIG. 12, the solid raw material S1 is filled in the upper divided pipe 10B following the lower divided pipe 10A.
At this time, since the lower divided pipe 10A is filled with the solid raw material S1, the input solid raw material S1 falls and hits the inner wall surface of the upper divided pipe 10B, but the inner wall surface of the lower divided pipe 10A There is no impact from falling. Therefore, compared with the conventional non-divided recharge tube 100 shown in FIG. 11, since the falling distance of the solid raw material S1 is short, damage to the inner wall surface of the upper divided tube 10B can be reduced.

Subsequently, it is determined whether the solid raw material S1 of the quantity set by recharge amount setting process S01 was filled as recharge amount determination process S07 shown in FIG. Then, when the solid raw material S1 reaches the set amount, erecting is performed so that the axis line of the recharge pipe 10 is in the vertical direction as the erecting step S10 shown in FIG.

FIG. 13 is a cross-sectional view showing the entire configuration of a single crystal pulling apparatus in which the raw material supply apparatus of the present embodiment is disposed. FIG. 14 shows a state in which the solid raw material is being charged into the raw material solution in the crucible.

The single crystal pulling apparatus in this embodiment is a furnace body for pulling a single crystal by the CZ method, and as shown in FIGS. 13 and 14, it comprises a main chamber 1 and a pull chamber 2 as a furnace main body, and further a gate valve 13 Have. The pull chamber 2 has a cylindrical shape smaller in diameter than the main chamber 1, and is disposed on the same central axis as the main chamber 1 at the top via the gate valve 13.

The gate valve 13 is provided to operate the interior of the main chamber 1 and the interior of the pull chamber 2 so as to be able to communicate or shut off, and the diameter of communication provided in the gate valve 13 is smaller than that of the pull chamber 2.

A crucible 3 is disposed at the center of the main chamber 1. The crucible 3 has a double structure in which an inner quartz crucible 3a and an outer graphite crucible 3b are combined, and is supported via a susceptor 4A on a support shaft 4 called pedestal. The support shaft 4 drives the crucible 3 so as to be vertically movable in the axial direction and rotatable in the circumferential direction.

The heater 5 is disposed to surround the crucible 3. Further outside the heater 5, a heat insulating material 6 is disposed along the inner surface of the main chamber 1. On the upper side of the crucible 3, a heat shield 12 is provided around the heater 5 and the heat of the molten raw material melt S2 in the crucible 3. The heat shield 12 is cylindrical or in the shape of an inverted truncated cone or the like, and the lower end thereof is located near the upper side of the raw material melt S2.

The solid raw material introduced into the crucible 3 as an initial charge is melted by the heating of the heater 5 to form a raw material melt S2. After melting the initially charged solid material, an additional charge is performed to replenish the shortage of the material melt S2 in the crucible 3 and secure a desired amount of melt.

For this reason, the pull-up shaft 7 is suspended in the pull chamber 2, and the recharge pipe 10 used for the raw material supply device of the present embodiment is suspended. At this time, the recharge tube 10 filled with the solid raw material S1 is positioned above the crucible 3 in which the raw material melt S2 is formed via the suspension jig 8 connected to the lower end of the pulling shaft 7. The pull-up shaft 7 is rotationally driven and vertically driven by a drive mechanism 2 a provided at the top of the pull chamber 2.
The pulling up shaft 7, the hanging jig 8, the drive mechanism 2a, the metal flange 9a, etc. constitute a pulling up means.

In the single crystal pulling apparatus according to the present embodiment, as the recharging step S11 shown in FIG. 12, the solid material S1 is recharged using a material feeding device provided with the recharge pipe 10.

Recharge is performed after melting of the solid material initially charged in the crucible 3 is finished, as shown in FIG. When the additional charge is performed, the recharge pipe 10 filled with the solid raw material S1 is placed above the crucible 3 on which the raw material melt S2 is formed via the suspension jig 8 connected to the lower end of the pulling shaft 7. Position on
The raw material melt S2 in the crucible 3 is in an insufficient state with respect to the crucible volume because the solid raw material initially charged in the crucible 3 is limited as compared to the volume of the crucible.

The melting pipe 10 is lowered to such an extent that melting of the initially charged solid material in the crucible 3 is almost completed and the unmelted solid material is in a floating island state.
At this time, as shown in FIG. 13, the metal flange 9 a abuts on a predetermined height position, for example, a small diameter portion provided on the gate valve 13, and the descent only of the recharge pipe 10 is stopped.

Here, as shown in FIGS. 13 and 14, the length of the lower divided pipe 10A is set such that the connecting portion 11 is positioned above the lower end position of the heat shield 12. As a result, the connecting portion 11 is shielded from the heat radiated from the raw material melt S2 or the heat radiated from the heater 5. Therefore, the temperature of the connecting portion 11 does not rise to the same extent as the raw material melt S2.

On the other hand, there is no hindrance to the descent of the conical bottom lid 14 connected to the metal shaft 15, and when the pulling up shaft 7 is further lowered from that position, the bottom lid 14 is opened as shown in FIG. The granular solid material S1 in the recharge pipe 10 falls by its own weight and is supplied to the raw material melt S2.

At this time, as shown in FIG. 14, the metal shaft 15 penetrating the recharge pipe 10 directly covers the sliding protection pipe 16 a fixed on the inner surface of the recharge pipe 10 and the metal shaft 15 for sliding protection. It is protected by the covering protection tube 16b inserted in the tube 16a. For this reason, it is possible to prevent the contamination of the solid raw material S1 and at the same time eliminate the deviation from the central axis of the metal shaft 15, and uniformly supply the solid raw material S1 into the crucible 3 in the circumferential direction.

When charging of the solid raw material S1 is completed, the recharge pipe 10 is pulled up and taken out of the pull chamber 2.
Here, when the raw material melt amount in the crucible 3 does not reach the target value, the charging of the solid raw material S1 can also be repeated using the recharge pipe 10 again. However, in the present embodiment, since the recharging amount is set in the recharging amount setting step S01, a sufficient amount of solid raw material S1 can be input. For this reason, it is not necessary to repeat injection | pouring of solid raw material S1.

When the additional charge is completed and the raw material melt S2 in the crucible 3 reaches the target amount, the suspension jig 8 connected to the lower end of the pulling shaft 7 is replaced with a seed crystal, and the process proceeds to a single crystal growth process. .

Although the work procedure of the additional charge has been described above, the solid raw material S1 of an amount commensurate with the reduction of the raw material melt is grown in the crucible 3 after growing the first single crystal by the same work procedure also in the recharge. The raw material melt S2 remaining in the
Recharge means, as described above, an additional charge which is carried out after introducing the initial raw material into the crucible 3 and melting, and a recharge when continuously processing after pulling up a single crystal. In both the additional charge and the recharge, the solid raw material S1 is additionally charged while the raw material melt S2 is in the crucible 3.

When the recharging step S11 is completed, the recharging pipe 10 is divided into a lower divided pipe 10A and an upper divided pipe 10B in a dividing step S12 shown in FIG.
Next, as the recharge number counting step S13 shown in FIG. 12, the number of recharges used up to now is counted for each divided pipe.

Next, as the number-of-recharges determination step S14 shown in FIG. 12, if it is determined that the number of recharges counted in the number-of-recharges count step S13 does not exceed the predetermined number, the divided tubes are reused. Therefore, the upper divided pipe 10B is sent to the cleaning step S17 shown in FIG. 12, and the lower divided pipe 10A is sent to the cleaning step S03 shown in FIG.

Here, the number of reusable rechargings is about 40 to 50, and a predetermined number of times for the lower divided tube 10A and a predetermined number of times for the upper divided tube 10B are set in advance for each of the divided tubes. This is a process by which the damage by the falling impact of the solid material S1 is different because the falling distance of the solid material S1 is different when the length dimension of the lower divided pipe 10A and the upper divided pipe 10B is different. .

Next, in the tube penetration visual check step S15 shown in FIG. 12, damage due to the drop impact of the solid raw material S1 is visually determined for each divided tube.
At this time, by replacing only the divided pipe whose inner surface is damaged to a predetermined state by the filling of the solid raw material S1, selectively replacing only the divided pipe having large internal state deterioration due to the falling of the solid raw material S1. It becomes possible.

As a reference for replacement in the tube transmission visual check step S15, the lower split tube 10A and / or the upper split tube 10B are replaced when a portion that becomes turbid and visible compared to a non-used and flawless state is generated Can be set to This visible white turbidity part can be made into the part to which the transmittance | permeability fell below 70% by the flaw of the inner surface produced by filling of solid raw material S1.

In particular, in the portion where the transmittance is less than 70%, the portion having the largest area can be a region of about 10 cm square. Alternatively, it is suitable that three to four areas each having a diameter of about 5 cm square be formed in a portion where the transmittance is less than 70%.

If it is determined in the tube penetration visual confirmation step S15 that the white turbid region does not reach the reference, the divided tubes are separately sent for reuse. The upper divided pipe 10B is sent to the cleaning step S17 shown in FIG. Further, the lower divided pipe 10A is sent to the washing step S03 shown in FIG.

In addition, it is also possible to implement only one of the number-of-recharges determination step S14 and the pipe permeation visual confirmation step S15. Alternatively, the number-of-recharges determination step S14 can be performed after the tube penetration visual check step S15.

When it is determined in the pipe permeation visual check step S15 that the white turbid region has reached the standard, the divided pipe is replaced as the replacement step S16 shown in FIG. 12, and the regeneration processing step S20 shown in FIG. 12 is performed.
In the regeneration processing step S20, the inner surface of the split pipe replaced with a flaw is subjected to heating and melting processing to eliminate the flaw and to make it transparent for regeneration, thereby making the replaced split pipe reusable.

Here, in the regeneration process step S20, the axial length of the lower divided pipe 10A and the upper divided pipe 10B can be set shorter than in the conventional non-divided recharge pipe 100 shown in FIG. And the deformation caused by the regeneration process can be reduced.

After the completion of the regeneration processing step S20, when it is determined that the deformation caused by the regeneration processing exceeds the predetermined amount as the deformation amount determination step S21 shown in FIG. 12, the divided pipe is excluded as the discarding step S22 shown in FIG. Discard Further, in the deformation amount determination step S21, when it is determined that the deformation caused by the regeneration processing did not exceed the predetermined amount, the divided pipes are distinguished and reused. For this purpose, the upper divided pipe 10B is sent to the cleaning step S17 shown in FIG. Further, the lower divided pipe 10A is sent to the cleaning step S03 shown in FIG.

Thus, the recharge method in the present embodiment is completed.

According to the raw material supply apparatus having the recharge pipe 10 in the present embodiment, and the recharge method using the single crystal pulling apparatus, even if the filling amount of the solid raw material S1 is the same, compared to the recharge pipe 100 which is not divided. The distance over which the solid raw material S1 to be filled falls can be reduced. For this reason, it is possible to reduce the impact on the inner surface of the recharge tube 10 at the time of filling, and to reduce the occurrence of flaws on the inner surface of the recharge tube 10.

Thereby, the usable life of the recharge pipe 10 can be extended even if the filling amount of the solid raw material S1 to be recharged is greatly increased. In addition, it is possible to improve the safety and prevent the occurrence of dislocation by changing the replacement times of the divided

pipes

10A and 10B according to the progress degree of the inner surface deterioration state.

Furthermore, it is possible to prevent the deterioration of the sealed state of the recharge pipe 10 by providing the buffer member 11e and judging that the divided

pipes

10A and 10B are to be regenerated. In addition, the efficiency of the raw material supply operation can be achieved.

Hereinafter, a second embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a recharge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
FIG. 15 is a schematic view showing the inclined support in the lowermost divided pipe setting step S04 according to the present embodiment. FIG. 16 is a schematic view showing the tilt support in the tilt step S05 and the raw material charging step S06 of the present embodiment. FIG. 17 is a schematic view showing the inclined support in the divided pipe setting step S08 and the raw material filling step S06 of the present embodiment. FIG. 18 is a schematic view showing the inclined support in the erecting step S10 and the recharging step S11 of the present embodiment.

The present embodiment differs from the first embodiment described above in the point of the inclined support 30. The other corresponding components are denoted by the same reference numerals and the description thereof will be omitted.

In the present embodiment, an inclined support for supporting the recharge pipe 10 in each step such as the lowermost divided pipe setting step S04, the tilting step S05, the raw material charging step S06, the divided pipe setting step S08, the connecting step S09, and the standing step S10. A platform 30 can be used.

As shown in FIGS. 15 to 18, the inclined support 30 includes a support carriage 32 having a support 31 for supporting the recharge tube 10, and an incline 34 having an inclined support 35 for tilting the support carriage 32. , And an inclination drive unit 39 which inclines the inclination platform 34.

The support portion 31 is erected on one side of the substantially flat support carriage portion 32 as shown in FIGS. 15 to 18 so as to be able to support the divided

tubes

10A and 10B at the time of inclination,

Wheels

33 and 33 are provided on the lower side of the carriage portion 32 so as to be movable.

The inclined base 34, which is substantially flat, is connected to a base 36 disposed on a floor surface or the like so as to be rotatable around a horizontal axis 35a.
An inclined support portion 35 provided upright on the upper side of the horizontal shaft 35 a to be inclined is connected to the inclined table 34.

On the back side of the inclined support portion 35, an inclined drive portion 39 whose both ends are rotatably connected by the

axis

37, 38 parallel to the horizontal axis 35a with respect to the base 36 located outside the inclined table 34. Is provided.

The inclination drive part 39 consists of an air cylinder, an oil cylinder, a ball screw etc., for example, and is made into the drive part which can change the extension. The tilt drive unit 39 is configured to be able to rotate the tilt platform 34 from the horizontal position around the horizontal axis 35 a and drive the tilt platform 34 to the tilt position by the extension change of the tilt drive unit 39. Further, the tilt drive portion 39 is configured to be able to drive the tilt support portion 35 from the vertical position around the horizontal axis 35 a to drive it to the tilt position.

By driving the tilt drive unit 39, the support carriage 32 placed on the tilt table 34 follows and turns from the horizontal position around the horizontal axis 35a to the tilt position and also the support unit 31. From the vertical position, it can be driven to an inclined position by rotating around the horizontal axis 35a.

At the same time, the tilt drive portion 39 charges the support tube portion 32 and the recharge tube 10 mounted on and supported by the support portion 31 and the recharge tube 10 in the state of being turned to the tilt position and in the tilt position. The weight of the solid raw material S1 can be supported.

The base portion 36 is provided with an inclined portion 36a at the end opposite to the horizontal shaft 35a of the inclined table 34, and there is no step so that the support carriage 32 can travel from the upper surface to the floor surface of the inclined table 34. It is arranged.

As shown in FIG. 15, in the state where the tilt drive unit 39 is extended, the tilt stand 30 in this embodiment has the tilt stand 34 and the support carriage 32 in the horizontal position, and the tilt support 35 and the support 31 are vertical. It will be in the state of the position.

Then, in the lowermost divided pipe setting step S04, the bottom cover 14 is inserted into the lower opening end of the lower divided pipe 10A to be in a closed state. Further, in the lower divided pipe 10A, the lower end of the metal shaft 15 penetrating the protective pipe 16 is attached to the bottom cover 14 to be in a filling ready state. The lower divided pipe 10A in this state is mounted on the support carriage 32 such that the axis of the lower divided pipe 10A is in the vertical direction.

Next, in the tilting step S05, the tilt drive unit 39 is driven to be reduced, and as shown in FIG. 16, the tilt stand 34 is rotated from the horizontal position around the horizontal axis 35a to drive it to the tilt position. Further, the tilt support portion 35 is rotated from the vertical position around the horizontal shaft 35a to drive it to the tilt position.

As a result, the support carriage portion 32 is made to follow and is rotated from the horizontal position around the horizontal axis 35a and driven to the inclined position. Further, the support portion 31 is made to follow and is rotated from the vertical position around the horizontal axis 35 a to drive it to the inclined position. As described above, by driving the support carriage portion 32 and the support portion 31 respectively, the lower divided pipe 10A is supported in a state of being inclined at a predetermined angle.

Next, in the raw material filling step S06, the solid raw material S1 is filled in the lower divided pipe 10A.

Further, as shown in FIG. 17, the upper divided pipe 10B is set at the upper position of the lower divided pipe 10A in the divided pipe setting step S08. Then, in the connecting step S09, the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11. At this time, the tilt drive portion 39 is driven to be extended, and the support carriage portion 32 is rotated from the tilt position around the horizontal axis 35 a to drive it to the horizontal position. Further, the support portion 31 is rotated from the inclined position around the horizontal shaft 35a to drive it to the vertical position. By driving the support carriage portion 32 and the support portion 31 in this manner, as shown in FIG. 15, the lower divided pipe 10A is supported so that the axis thereof is in the vertical direction. In this state, the bolt / nut 11 d as a fastening portion is fastened in the connecting portion 11.
Furthermore, in the upper divided pipe 10B as well, the metal shaft 15 is penetrated through the protective pipe 16.

Next, in the raw material charging step S06, the solid raw material S1 is charged into the upper divided pipe 10B connected to the lower divided pipe 10A. At this time, the tilt drive portion 39 is driven to be reduced, and the support carriage portion 32 is rotated from the horizontal position around the horizontal axis 35 a to drive it to the tilt position. Further, the support portion 31 is rotated from the vertical position around the horizontal shaft 35a to drive it to the inclined position. Thus, by driving the support carriage portion 32 and the support portion 31 respectively, as shown in FIG. 17, the connected recharge tube 10 is supported so that the axis thereof is in the inclined direction. Thereafter, the solid raw material S1 is filled in the upper divided pipe 10B.

When the raw material filling step S06 is completed, the tilt drive unit 39 is driven to extend, and the tilt table 34 is rotated from the tilt position around the horizontal axis 35a to drive it to the horizontal position. Further, the tilt support portion 35 is rotated from the tilt position around the horizontal shaft 35a to drive it to the vertical position.

As a result, the support carriage portion 32 is rotated from the inclined position around the horizontal shaft 35a and driven to the horizontal position. Further, the support portion 31 is rotated from the inclined position around the horizontal shaft 35a to drive it to the vertical position. By driving the support carriage portion 32 and the support portion 31 respectively, the recharge tube 10 is supported in a filling state in which the axis line thereof is in the vertical direction.

In this state, as shown in FIG. 18, the support carriage portion 32 is smoothly transported from the tilt table 34 via the tilt portion 36a. Thus, the recharge tube 10 filled with the solid material S1 placed on the support carriage portion 32 is transported to the vicinity of the single crystal pulling furnace. Then, the metal shaft 15 is connected to the lower end of the lifting shaft 7 by the suspension jig 8 and is lifted by the drive mechanism 2a.

Next, the recharge pipe 10 is positioned above the crucible 3 on which the raw material melt S2 is formed, and the solid raw material S1 is recharged using a raw material supply device equipped with the recharge pipe 10 as a recharge step S11.

When the recharging tube 10 is finished, the recharging tube 10 is placed on the support carriage portion 32 and the support carriage portion 32 is transported to the tilt table 34. Then, the tilt drive unit 39 is driven to be reduced, and the support carriage unit 32 is rotated from the horizontal position around the horizontal axis 35 a to drive it to the tilt position. Further, the support portion 31 is rotated from the vertical position around the horizontal shaft 35a to drive it to the inclined position. Thus, by driving the support carriage portion 32 and the support portion 31 respectively, the connected recharging tube 10 is supported so that the axis thereof is in the inclined direction. Thereafter, the connecting portion 11 is separated to separate the lower divided pipe 10A and the upper divided pipe 10B.

According to the present embodiment, by using the inclined support 30, it is possible to efficiently and safely perform the process of filling the recharge pipe 10 for dividing and connecting the divided

pipes

10A and 10B.
Furthermore, the inclined support 30 makes it possible to adjust the angle so as to reduce the impact that the solid raw material S1 to be filled abuts on the recharge tube 10 and the like.

Hereinafter, a third embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a recharge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
The present embodiment differs from the above-described first or second embodiment in that it relates to the upper additional divided pipe 10C. The other corresponding components are denoted by the same reference numerals, and the description thereof will be omitted.

FIG. 19 is a schematic positive cross-sectional view showing the recharge pipe in the raw material supply device of the present embodiment. FIG. 20 is an enlarged cross-sectional view showing the connection portion of the present embodiment. FIG. 21 is an exploded perspective view showing the recharge pipe of the present embodiment. FIG. 22 is a front sectional view showing a point crystal pulling apparatus of the present embodiment.

As shown in FIGS. 19 to 21, in the recharge pipe 10 of the present embodiment, the amount of the solid raw material S1 to be charged by adding and extending the upper additional divided pipe (division pipe) 10C above the upper divided pipe 10B It will increase.

The upper additional divided pipe 10C has a substantially cylindrical shape as shown in FIGS. 19 to 21 and does not have the

flange portions

11a and 11b as the connecting portion 11 like the lower divided pipe 10A and the upper divided pipe 10B. Instead, the lower end of the upper additional divided pipe 10C can be fitted to the upper end of the upper divided pipe 10B. When the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the inner surfaces thereof are set to be flush with each other in the vertical direction.
In the drawings, the present embodiment shows a state in which the buffer member 11 e is not used.

At the lower end of the upper additional divided pipe 10C, as shown in FIGS. 19 to 21, a fitting groove 11h is circumferentially provided at the outer peripheral position as the connecting portion 11. Further, at the lower end of the upper additional divided pipe 10C, a corresponding fitting groove 11g is circumferentially provided as the connecting portion 11 at the upper end inner peripheral position of the upper divided pipe 10B. Thus, when the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the fitting groove 11h fits into the upper end of the upper divided pipe 10B. At the same time, the fitting groove 11g supports the lower end of the upper additional divided pipe 10C. At this time, the inner circumferential surface located on the radially outer side of the fitting groove 11g is in a state of being substantially in contact with the outer circumferential surface located on the radially inner side of the fitting groove 11h.

In the height direction of the fitting groove 11h and the fitting groove 11g, the fitting groove 11h can be made equal to or larger than the side wall thickness of the upper divided pipe 10B, and the fitting groove 11g can be made longer than the fitting groove 11h. .

Further, the protective pipe 16 in the upper additional divided pipe 10C extends in the vertical direction (axial direction) at the axial center of the upper additional divided pipe 10C, similarly to the lower divided pipe 10A and the upper divided pipe 10B. However, in the upper additional divided pipe 10C, the lower end of the protective pipe 16 is supported by a configuration different from the plate-like fixed plate portion 16c extending in the radial direction from the inner surface of the recharge pipe 10 to the axial center thereof. In the upper additional divided pipe 10C, the lower end of the protective pipe 16 is supported by a fixed inclined plate 16f provided diametrically at the lower end of the upper additional divided pipe 10C.

Further, the upper end of the protective pipe 16 in the upper divided pipe 10B is continuous with the lower end of the protective pipe 16 of the upper additional divided pipe 10C without any gap. Further, the lower end of the protective pipe 16 in the upper divided pipe 10B is continuous with the upper end of the protective pipe 16 of the lower divided pipe 10A without a gap. By these, it can prevent that solid raw material S1 to be thrown in is caught in the connection part of the protective tube 16, and causing trouble in raw material injection. The state in which the respective protective tubes 16 are continuous can be in such a degree that the solid raw material S1 does not get caught on this connection portion even if they are in contact with each other or are separated from each other.

Two fixed inclined plates 16f are provided symmetrically about the axis of the upper additional divided pipe 10C such that the widthwise end is positioned at the axis of the upper additional divided pipe 10C. Here, each fixed inclined plate 16f has an inclination in the width direction. The fixed inclined plate 16f is disposed such that the inclination angle in the width direction is lowered radially outward from the center of the upper additional divided pipe 10C axis. Further, the fixed inclined plate 16f has a through hole penetrating in the vertical direction at the center position of the upper additional divided pipe 10C axis. Here, the periphery of the through hole of the fixed inclined plate 16 f is connected to the lower end of the protective tube 16.

At the lower end of the upper additional divided pipe 10C, a portion located radially outward of the widthwise end of the fixed inclined plate 16f which is lowered is a lower opening. When the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the lower opening of the lower end of the upper additional divided pipe 10C can communicate the inside of the upper additional divided pipe 10C with the upper divided pipe 10B.

The two fixed inclined plates 16f are joined together at their widthwise ends, which are raised from each other, to form a ridge. The ridge line of the fixed inclined plate 16f has a length equal to the diameter of the upper additional divided pipe 10C. Further, the longitudinal direction end portions of the two fixed inclined plates 16f are formed in a mountain shape. In addition, a notch is formed at the lower end of the upper additional divided pipe 10C. Both ends in the longitudinal direction of the fixed inclined plate 16 f and the lower end of the upper additional divided pipe 10 C are connected. The chevron shape at the end of the fixed inclined plate 16f and the cutout shape of the lower end of the upper additional divided pipe 10C correspond to each other.

When the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the upper end of the protective pipe 16 of the upper divided pipe 10B is positioned at the lower side of the two fixed inclined plates 16f formed in a mountain shape. Thus, the metal shaft 15 can be communicated and supported.

As a result, the axial length dimension of the recharge tube 10 is increased. At the same time, in the upper additional divided pipe 10C, the upper divided pipe 10B, and the lower divided pipe 10A, the metal shaft 15 is continuous in the axial direction with respect to the respective protective pipes 16 at the axial center position of the recharge pipe 10. It is supposed to penetrate.

Also in the present embodiment, as the raw material charging step S06, the solid raw material S1 is filled in the lower divided pipe 10A. Then, in the divided pipe setting step S08, the upper divided pipe 10B is set at the upper position of the lower divided pipe 10A. Then, in the connecting step S09, the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11. Then, in the raw material filling step S06, the solid raw material S1 is filled in the upper divided pipe 10B. Then, as the recharge amount determination step S07, it is determined whether the solid raw material S1 of the amount set in the recharge amount setting step S01 has been charged.

Thereafter, the upper additional divided pipe 10C is placed on the upper divided pipe 10B in the divided pipe setting step S08.
In the present embodiment, only the metal shaft 15 is made to penetrate the protective pipe 16 in the coupling step S09, and it is not necessary to fasten the bolt / nut 11d which is the fastening portion.

Furthermore, solid raw material S1 is filled in the upper additional divided pipe 10C as raw material charging step S06, and erected so that the axis line of the recharge pipe 10 is in the vertical direction as rising step S10.
Next, as shown in FIG. 22, the lumped solid raw material S1 in the recharge tube 10 is dropped by its own weight, with the suspension jig 8 positioned above the crucible 3 on which the raw material melt S2 is formed. , Feed to the raw material melt S2.

In the present embodiment, the recharge amount can be increased by the upper additional divided pipe 10C.
Furthermore, by reducing the number of times of recharging, the required time for the recharging step can be shortened and the production efficiency can be improved.

Hereinafter, a fourth embodiment of a recharging tube, a raw material supply device, a single crystal pulling device, a method of using the recharging tube, a recharging method, and a single crystal pulling method according to the present invention will be described based on the drawings.
The present embodiment differs from the third embodiment described above in the connection point, and the other corresponding components are denoted by the same reference numerals and the description thereof will be omitted.
FIG. 23 is an enlarged cross-sectional view showing the connection portion in the recharge pipe of the present embodiment.

In the recharge pipe 10 of the present embodiment, as shown in FIG. 23, the fitting groove 11h is not provided circumferentially at the outer peripheral position at the lower end of the upper additional divided pipe 10C. At the same time, a fitting groove 11g having a radial dimension substantially the same as the thickness dimension of the lower end of the upper additional divided pipe 10C is circumferentially provided at the upper inner peripheral position of the upper divided pipe 10B.

For this reason, the enlarged diameter part 11j diameter-expanded by the part corresponding to the fitting groove 11g radially outward is provided in the upper end outer periphery of upper part divided pipe 10B. Further, the axial dimension of the enlarged diameter portion 11j, that is, the length by which the lower additional divided pipe 10C is fitted into the fitting groove 11g, may be made longer than in the third embodiment in which the fitting groove 11h is provided. it can.

Specifically, in the height direction of the enlarged diameter portion 11j and the fitting groove 11g, the enlarged diameter portion 11j is 1/6 or more of the outer diameter of the upper divided pipe 10B main body, and the fitting groove 11g is the enlarged diameter portion It can be longer than 11j.

Thereby, in the recharge pipe 10 of the present embodiment, the upper additional divided pipe 10C can be mounted on the upper divided pipe 10B in a state where the stability is increased.
Furthermore, instead of the upper additional divided pipe 10C, it becomes possible to place a divided pipe such as the lower divided pipe 10A having no flange portion at its lower end on the upper divided pipe 10B.

In addition, a thin ring-shaped buffer member 11e is used so that the upper end surface of the upper divided pipe 10B and the lower end surface of the upper additional divided pipe 10C do not come in direct contact with each other. It is possible to use a buffer member 11e.

Hereinafter, a fifth embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a recharge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
The present embodiment differs from the above-described first to fourth embodiments in terms of the inner diameter of the divided tube, and the corresponding components other than this are denoted by the same reference numerals and the description thereof will be omitted.
FIG. 24 is a front sectional view showing the recharge pipe of the present embodiment.

As shown in FIG. 23, the recharge pipe 10 of the present embodiment is set so that the inner diameter of the lower end portion 10Ab of the lower divided pipe 10A is smaller than that of the upper end portion 10Aa of the lower divided pipe 10A. Similarly, the inner diameter of the lower end portion 10Bb of the upper divided pipe 10B is set smaller than the upper end portion 10Ba of the upper divided pipe 10B.

Accordingly, the inner surface of each of the upper divided pipe 10B and the lower divided pipe 10A has an inverted truncated cone shape and the diameter is reduced from the upper end to the lower end. Further, the thickness of each of the upper divided pipe 10B and the lower divided pipe 10A increases from the upper end to the lower end.

Further, the inner diameter of the upper end portion 10Aa of the lower divided pipe 10A is set to be smaller than that of the lower end portion 10Bb of the upper divided pipe 10B, and viewed from the upper side, the upper portion divided pipe 10B is recharged more than the lower end. It is set so that it does not stick out to the pipe 10 inside.

In the recharge pipe 10 of the present embodiment, when viewed from above, the buffer member 11e is hidden by the lower end portion 10Bb of the upper divided pipe 10B, and the solid raw material S1 to be filled does not directly collide with the buffer member 11e. As a result, the generation of impurities resulting from the buffer member 11 e can be prevented, so that it is possible to prevent the deterioration of crystal characteristics such as carbon concentration fluctuation caused by, for example, the mixing of the buffer member 11 e made carbon.

Further, when viewed from above, the upper end portion 10Aa of the lower divided pipe 10A is hidden by the lower end portion 10Bb of the upper divided pipe 10B, and the solid raw material S1 to be filled directly collides with the upper end portion 10Aa of the lower divided pipe 10A. I have not. Thereby, it is possible to prevent the occurrence of cracking, chipping or the like in the upper end portion 10Aa of the lower divided pipe 10A. Furthermore, since the lower end portion 10Ab and the lower end portion 10Bb of the divided

pipes

10A and 10B are thick, it is possible to improve the strength of the lower end portion 10Ab and the lower end portion 10Bb and to reduce the occurrence of deformation in the regenerating process.

Hereinafter, a sixth embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a recharge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
The present embodiment differs from the first to fifth embodiments described above in the point of the ratio of the axial length of the split tube, and the corresponding components other than this are denoted by the same reference numerals and explanations thereof I omit it.
FIG. 25 is a front sectional view showing the recharge pipe of the present embodiment.

As shown in FIG. 25, in the recharge pipe 10 of the present embodiment, the axial length of the lower divided pipe 10A is set to be larger than that of the upper divided pipe 10B.
Thereby, the amount of recharge can be increased. At the same time, by setting the height position of the connecting portion 11 upward, the distance between the raw material melt S2 and the heater 5 in the crucible 3 and the connecting portion 11 can be increased. Thereby, it becomes possible to reduce the influence of the high temperature on the connecting portion 11 in the recharging step S11.

In addition, the axial length of the lower divided pipe 10A can be made substantially the same as that of the conventional recharge pipe 100 shown in FIG. In this case, by connecting and using the upper divided pipe 10B, it is possible to increase the amount of charge once. As a result, it is possible to increase the number of times the recharge tube 10 can be used.

Hereinafter, a seventh embodiment of a recharge tube, a raw material supply apparatus, a single crystal pulling apparatus, a method of using the recharge tube, a charge method, and a single crystal pulling method according to the present invention will be described based on the drawings.
The present embodiment differs from the first to fifth embodiments described above in the number of divisions of the recharge tube, that is, in terms of the number of connections of the divided tubes, and the same reference numerals are given to the other corresponding components. The explanation is omitted.
FIG. 26 is a front sectional view showing the recharge pipe of the present embodiment.

The recharge pipe 10 according to the present embodiment is divided into three in the vertical direction, and as shown in FIG. 26, the middle divided pipe (divided pipe) 10D is between the lower divided pipe 10A and the upper divided pipe 10B. Provided.

The middle divided pipe 10D is set to have substantially the same inner diameter as the lower divided pipe 10A and the upper divided pipe 10B. Further, the upper end of the lower divided pipe 10A and the lower end of the middle divided pipe 10D are connectable by the connecting portion 11, respectively. Further, the upper end of the middle divided pipe 10D and the lower end of the upper divided pipe 10B can be connected by the connecting portion 11.

Similar to the lower divided pipe 10A and the upper divided pipe 10B, the connecting portion 11 is provided with a flange 11n at the upper end of the middle divided pipe 10D and a flange 11m at the lower end of the middle divided pipe (divided pipe) 10D. Be The connecting portion 11 is provided with a plurality of connecting

holes

11c and 11c circumferentially separated from each other in the flange portion 11n and the flange portion 11m, and bolts and nuts 11d and 11d as fastening portions for fastening these. Be In the present embodiment, the buffer member 11 e is not used, but may be provided.

In the present embodiment, the middle divided pipe 10D is set at the upper position of the lower divided pipe 10A in the divided pipe setting step S08. Then, in the connecting step S09, the connecting portion 11 connects the flange portion 11a of the lower divided pipe 10A and the flange portion 11m of the middle divided pipe 10D by the fastening portion.
Further, in the divided pipe setting step S08, the upper divided pipe 10B is set at the upper position of the middle divided pipe 10D. Then, in the connecting step S09, the flange portion 11n of the middle divided pipe 10D and the flange portion 11b of the upper divided pipe 10B are connected by the fastening portion.

In the present embodiment, since the recharging pipe 10 is divided into three in the vertical direction, the falling distance of the solid raw material S1 in the raw material charging step S06 can be further shortened. Thereby, the damage to the inner wall surface in each divided

pipe

10A, 10B, 10D in raw material filling process S06 may be less.
Further, it is possible to connect a plurality of middle side divided pipes 10D between the lower divided pipe 10A and the upper divided pipe 10B, and it becomes easy to increase to a desired amount of recharge. This makes it possible to reduce the number of recharges with respect to the amount of recharge.

In the present invention, it is possible to appropriately combine and use each configuration in each embodiment described above, or to adopt a state in which only a specific configuration is not adopted.

Hereinafter, examples according to the present invention will be described.

In a silicon single crystal pulling apparatus having a diameter of 300 mm, recharging was carried out using a quartz tube having a diameter of about 300 mm and a length of 1.8 m in the axial direction as a recharging tube used for recharging. This is referred to as Experimental Example 1.

Similarly, as a recharging tube, recharging was performed using a quartz tube having an axial length of 1.5 m on the lower side and 0.3 m on the upper side. This is referred to as Experimental Example 2.

Similarly, as a recharging tube, recharging was performed using a quartz tube having an axial length of 0.9 m on the lower side and 0.9 m on the upper side. This is referred to as Experimental Example 3.

Similarly, as a recharging tube, recharging was performed using a quartz tube whose axial length is divided into three parts of 0.6 m on the lower side, 0.6 m on the middle side, and 0.6 m on the upper side. This is referred to as Experimental Example 4.

The inner surface of the recharge tube of Experimental Example 1 became cloudy due to a flaw or the like caused by the drop of the solid material, and the number of recharges when it was determined that visual regeneration was necessary was used as the reference frequency.

In Experimental Example 2, the number of times the regeneration process was required similarly for the lower divided pipe among the recharge pipes was 1.21 times the reference number.
Further, the number of times the regeneration process was required for the upper divided pipe was 2.29 times the reference number.

In Experimental Example 3, the number of times the regeneration process was required similarly for the lower divided pipe among the recharge pipes was 1.45 times the reference number.
In addition, the number of times the regeneration process was required similarly for the upper divided pipe was 1.49 times the reference number.

In Experimental Example 4, the number of times the regeneration process was similarly required for the lower divided pipe among the recharge pipes was 1.90 times the reference number.
Further, the number of times the regeneration process was required for the middle divided pipe was 2.05 times the reference number.
Further, the number of times the regeneration process was required similarly for the upper divided pipe was 2.15 times the reference number.

In each of the experimental examples, each divided tube was reused even after the regeneration treatment, and the regeneration treatment was performed a plurality of times.

In the recharge tube of the experimental example 1, the deformation amount which seems to be caused by heating in a plurality of regeneration processes exceeds the reference value, and the total number of recharges up to that point when it is determined that it can not be used any more It is the standard life.

In Experimental Example 2, the number of times when it was determined that the lower divided pipe among the recharge pipes was similarly discarded was 1.10 times the reference life.
In addition, the number of times that the upper divided pipe was judged to be discarded similarly was 1.51 times the reference life.

In Experimental Example 3, the number of times when it was determined that the lower divided pipe among the recharge pipes was similarly discarded was 1.15 times the reference life.
In addition, the number of times that the upper divided pipe was judged to be discarded similarly was 1.37 times the reference life.

In Experimental Example 4, the number of times when it was determined that the lower divided pipe among the recharge pipes was similarly discarded was 1.25 times the reference life.
In addition, the number of times when it was determined that the middle divided pipe was similarly discarded was 1.40 times the reference life.
In addition, the number of times when it was determined that the upper divided pipe was similarly discarded was 1.49 times the reference life.
In addition, the above-mentioned frequency | count each employ | adopts the average value at the time of using to the last life in about 3 recharge pipe | tubes, respectively.

Furthermore, with respect to the initial production cost of each divided tube in each experimental example, the ratio of the increase in the number of times the regeneration process is required and the cost changed from the increase in deformation resistance life are calculated. The sum of costs was calculated as the total cost in the recharge tube of the experimental example.

In the recharge pipe of Experimental Example 1, the initial manufacturing cost was 10, the reprocessing cost was 1, the deformation resistance cost was 1, and the total cost when used up to the final life was 10.

On the other hand, in Experimental Example 2, similarly to the lower divided pipe among the recharge pipes, the initial production cost was 9 and the cost was 6.76.
Also, similarly for the upper divided pipe, the initial manufacturing cost was 3, and the cost was 0.87.
In the recharge pipe of Experimental Example 2, the total cost when used up to the final life was 7.63.

In Experimental Example 3, similarly to the lower divided pipe among the recharge pipes, the initial production cost was 6 and the cost was 3.60.
Also, similarly for the upper divided pipe, the initial manufacturing cost was 6, and the cost was 2.94.
In the recharge pipe of Experimental Example 3, the total cost when used up to the final life was 6.54.

In Experimental Example 4, the initial production cost was 5 and the cost was 2.11 for the lower divided pipe among the recharge pipes.
In addition, the initial production cost was 5 and the cost was 1.74 similarly for the middle divided pipe.
Also, similarly for the upper divided pipe, the initial manufacturing cost was 5 and the cost was 1.56.
In the recharge pipe of Experimental Example 3, the total cost when used up to the final life was 5.41.

From these results, it can be understood that the number of usable times can be extended by using the axially divided recharge tube, and as a result, the cost of the recharge can be reduced.

Furthermore, when the number of times of use in the recharge tube of Experimental Example 1 increases, the number of dislocations that can be considered to be generated due to the fine quartz powder from the inner surface of the recharge tube is significantly reduced in Experimental Examples 2 to 4. I was able to confirm.

Further, in Experimental Examples 2 to 4, it was also confirmed that the purchase of fragments of the buffer member did not occur because no abnormality in the carbon concentration occurred.

Claims

A cylindrical recharging pipe in a raw material supply apparatus which is used for growing a single crystal by the Czochralski method and additionally charges or recharges a bulky solid raw material to a raw material melt in a crucible,
A plurality of divided tubes which are divided in the axial direction when filling the solid material;
A connecting portion connecting the divided tubes up and down when the solid material is introduced into the crucible;
A recharge tube characterized by having.
In the divided pipe, the inner diameter of the upper end of the divided pipe at the lower position at the time of connection is set equal to the inner diameter of the lower end of the divided pipe at the upper position or larger than the inner diameter of the lower end of the divided pipe at the upper position The recharge tube according to claim 1, characterized in that:
The recharge tube according to claim 1, wherein the upper end inner diameter of the divided tube is set equal to the lower end inner diameter or larger than the lower end inner diameter.
The said connection part is provided with the flange part extended to radial direction outer side, The fastening part which fastens this flange part is provided, The recharge pipe | tube of Claim 1 characterized by the above-mentioned.
The recharge pipe according to claim 1, wherein the lower end of the divided pipe which is the upper position is fitted to the upper end of the divided pipe which is the lower position at the time of connection in the connecting portion.
The recharge pipe according to claim 1, wherein the connection portion is connected such that the upper end surface and the lower end surface of the divided pipe are butted.
The recharge pipe according to claim 5, wherein a shock absorbing member is provided on a surface where the upper divided pipe and the lower divided pipe are in contact with each other.
8. The recharge according to claim 7, wherein the inner diameter of the buffer member is set equal to the inner diameter of the lower end of the divided pipe at the upper position, or larger than the inner diameter of the lower end of the divided pipe at the upper position. tube.
The recharge tube according to claim 7, wherein the divided tube is made of quartz, and the buffer member is made of a flexible material containing carbon.
A raw material supply apparatus which is used to grow a single crystal by the Czochralski method, and additionally charges or recharges the granular solid raw material to the raw material melt in the crucible,
A recharge pipe according to any one of claims 1 to 9,
A conical bottom lid removably attached to the lower open end of the recharge tube;
A lifting means for suspending the recharging pipe and the bottom cover so as to be able to move up and down and opening the lower opening end of the recharging pipe so that the solid raw material can be charged into the raw material melt in the crucible;
The raw material supply apparatus characterized by having.
A single crystal pulling apparatus for growing a single crystal from a raw material melt by the Czochralski method, comprising:
A raw material supply apparatus according to claim 10;
A furnace body provided with the crucible inside;
And a heat shield for shielding radiant heat to the single crystal grown from the raw material melt at the upper position of the crucible inside the furnace body as a cylindrical shape having a diameter-reduced diameter at the lower end. ,
At the time of additional charging or recharging, the recharge tube is inserted from above into the inside of the heat shield, and the lower end of the recharge tube is positioned above the lower end of the heat shield, and in this state the inside of the crucible A single crystal pulling apparatus characterized by charging the solid material into the raw material melt.
12. The single crystal pulling according to claim 11, wherein when the solid raw material is charged into the raw material melt in the crucible, the connecting portion is set at a position higher than the lower end position of the heat shield. apparatus.
When charging the solid material into the recharging pipe outside the furnace body,
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion 12. The single crystal pulling apparatus according to claim 11, further comprising: an inclined support supported as being connectable to the first.
A method of using the recharge tube according to any one of claims 1 to 9,
A method of using a recharge pipe, comprising replacing only the divided pipe whose inner surface is damaged to a predetermined state by the filling of the solid material.
15. The recharge tube according to claim 14, wherein the divided tube is replaced when the filling of the solid material causes a flaw of the inner surface to have a permeability of less than 70% as compared with the condition without a scratch. How to use
The method according to claim 14, wherein the inner surface of the split pipe replaced with a scratch is heated and regenerated.
The method of using a recharge pipe according to claim 16, wherein when the deformation of the divided pipe regenerated by heating exceeds a predetermined amount, it is not reused.
The single crystal pulling apparatus according to claim 11, wherein the raw material melt in the crucible is additionally charged or recharged.
The divided pipe mounted with the bottom cover at the lower end is supported by being inclined, and the divided pipe inclined along with the filling of the solid material is erected in the vertical direction side, and the divided pipe is upside by the connecting portion And charging the solid material.
The single crystal pulling apparatus according to claim 13, wherein the raw material melt in the crucible is additionally charged or recharged.
The inclined support supports the divided pipe mounted with the bottom lid at the lower end by the inclined support, and the divided pipe erected along with the filling of the solid material is erected in the vertical direction side, and the connection portion The split tube is connected to the upper side by the above to further charge the solid material.
The single crystal pulling apparatus according to claim 13, wherein the raw material melt in the crucible is additionally charged or recharged.
After additionally charging or recharging the raw material melt in the crucible,
A method of recharging comprising: supporting the plurality of connected divided tubes by the inclined support and separating the divided tubes by the connecting portion by inclining the divided tubes.
A method according to claim 18, after the raw material melt in the crucible is additionally charged or recharged,
A single crystal pulling method characterized in that a single crystal is grown from the raw material melt.