TWI720354B - Recharge tube, raw material supply device single crystal pulling device, recharge tube using method, recharge method, single crystal pulling method - Google Patents

Abstract

The present invention seeks to prevent a reduction in the life of a recharge tube and to reduce the occurrence of dislocation. A raw material supply device is used for the cultivation of a single crystal in the Czochralski process, and a pellet-shaped solid raw material S1 is additionally charged or recharged into raw material melt S2 in the crucible 3 of the raw material supply device. The raw material supply device has a cylindrical recharge tube 10. The recharge tube 10 has a plurality of divided tubes 10A and 10b that are divided in the axial direction when the solid raw material is filled, and a connecting portion 11 that connects the divided tubes vertically when the solid raw material is thrown in the crucible.

Description

Recharging tube, raw material supply device, single crystal pulling device, using method of recharging pipe, recharging method, single crystal pulling method

The present invention relates to a refilling 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, and particularly relates to suitable use for the CZ method The technology of adding or recharging the solid raw material of single crystal pulling.

Generally speaking, in the growth of single crystal silicon by the CZ (Czochralski) method, the solid polycrystalline silicon put into the crucible as an initial charge is heated and melted by the heater surrounding the crucible. Then, when a raw material melt is formed in the crucible, while rotating the crucible in a certain direction, the seed crystals held on the crucible are lowered and immersed in the raw material melt in the crucible. After that, by rotating the seed crystal in a predetermined direction, the seed crystal is raised, and the column-shaped single crystal silicon is raised below the seed crystal.

The solid raw material put into the crucible as the initial charge will use various shapes of polycrystalline silicon such as rods, blocks, or granules. Each of them will be supplied individually or in combination to form a molten liquid for growing monocrystalline silicon. Raw materials.

In the cultivation of single crystal silicon using the CZ method, when the solid raw material refilled in the crucible initially melts, the volume of the melted appearance is reduced. Therefore, compared with the volume of the crucible, the obtained raw material melt will be insufficient . If a single crystal is grown in this state, the productivity cannot be avoided due to the insufficient amount of raw material melt.

In order to avoid the decrease in productivity caused by the above-mentioned reasons, it is necessary to replenish the insufficient raw material melt to ensure the desired amount of melt. After the initial refilling of the crucible, the technology for additional supply of solid raw materials will be "additional charging". ".

That is, "additional charging" is a technique in which the solid raw material initially charged in the crucible is melted, and then the solid raw material is added to the formed raw material melt, thereby increasing the amount of raw material melt in the crucible. By applying this "additional charge", the volume of the crucible used can be effectively utilized, and the productivity in the growth of single crystal silicon can be improved.

In addition, in the cultivation of single crystal silicon using the CZ method, a technique of supplying solid raw materials called "refilling" is implemented. Specifically, it is a technique in which after the initial single crystal is grown and pulled up, the amount of solid raw material corresponding to the reduced amount of the raw material melt is added 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 single crystals are repeatedly pulled up, increasing the number of crystal pulls per crucible. Therefore, by adopting "recharging", it is expected that the crucible can be used efficiently to reduce costs, and at the same time, as with the aforementioned "additional charging", productivity can be improved and the cost of growing single crystal silicon can be reduced.

Using "additional charging" or "recharging" of raw material supply, there is a known method to use a raw material supply device with a recharge tube, which is inserted into the pulling furnace from the pulling chamber above the crucible , And then add the granular solid raw material into the raw material melt in the crucible.

At this time, with the additional input of solid raw materials, the crucible will be damaged, the raw material melt splashes, the raw material melt will adhere to the components in the chamber, and the life of the components will be shortened, which will have many undesirable effects on the growth of single crystals. . In order to solve these problems, as described in the patent literature, various proposals regarding "additional charging" or "recharging" have been proposed.

[Advanced Technical Literature] [Patent Document 1] JP 2003-020295 A [Patent Document 2] JP 2005-001977 A [Patent Document 3] JP 2007-217224 A

However, in recent years, due to the increase in the diameter of the pulled single crystal, the increase in the length of the pull, or the efficiency of the work, there is a demand for increasing the refill amount. Under strong conditions to meet this requirement, the refill tube will be inserted from the side of the pull-up chamber, so there is a limit to increasing this thickness. Therefore, the length of the refill tube is increased, but when the length of the refill tube is simply increased, the following problems occur.

In order to prevent contamination, the refill tube is made of a material softer than the additional raw material polysilicon, such as quartz. Therefore, when the length of the recharging pipe becomes longer and the material is filled into the recharging pipe, the falling lumps of raw material silicon will collide and damage the inner surface of the recharging pipe. At this time, small fragments such as quartz are mixed and melted. Raw materials, and form the cause of dislocation. When the length of the refill tube becomes longer, the distance that the raw material filled in the refill tube falls during the filling of the raw material becomes longer, so there is a problem of further increase in misalignment due to small fragments such as quartz caused by abrasion. .

In addition, when the inner surface of the refill tube is damaged by collision with the massive raw material silicon during the material filling, the temperature difference between the chamber during the refill and the filling time may cause the refill tube to be damaged. Therefore, it is generally expected to reduce the strength and limit the use of the refill tube by a predetermined number of times. However, when the length of the refilling tube becomes longer, the falling distance of the raw material filled in the refilling tube during the filling of the raw material will become longer. Therefore, the formation of damage will become larger and deeper at an accelerated rate. This solves the problem that the usable time and the usable times of the refill tube are extremely reduced.

In addition, as a countermeasure to prevent the damage of the refill tube from causing a decrease in strength, it is necessary to perform a repair (regeneration) step, heating and melting the inner surface of the refill tube to eliminate the damage. However, as the length of the refill tube becomes longer, the number of repairs will inevitably increase. The heating in the repairing step may cause the entire refill tube to be twisted. Therefore, if the deformation is within the allowable range, it can still be used after the repair process, but when the refill tube becomes longer, the falling distance of the raw material during filling becomes longer. If the damage caused becomes larger and deeper at an accelerated rate, the amount of heating required for repair will also increase, resulting in an increase in the amount of deformation, and the life of the final refill tube (the usable time until disposal, the number of usable times) cut back. At the same time, along with the lengthening of the refill tube, the amount of heating in the repair step increases, and the amount of deformation increases, and the life of the final refill tube (the usable time until discarding, the number of usable times) is reduced.

In addition, the inner surface of the recharging pipe is cleaned after each recharging, but as the length of the recharging pipe becomes longer, this workability will be significantly reduced. Or, insufficient cleaning may result in dislocation or deterioration of crystal properties.

In view of the above-mentioned problems, the present invention aims to achieve the following objects. 1. At the same time, realize the increase of the filling volume of the refilling tube and prevent the life of the refilling tube from being reduced; 2. At the same time, strive to reduce the occurrence of misalignment; 3. At the same time, prevent the workability of loading from decreasing; 4. Also, prevent Decrease in crystal quality.

In order to solve the above-mentioned problems, the recharging tube of the present invention is used for the growth of single crystals of the Tchaikrasky method, which is used for the additional charging of granular solid raw materials or the raw material melt in the crucible. The cylindrical refill tube in the raw material supply device in the raw material supply device includes: a plurality of divided tubes that are divided in the axial direction when the solid raw material is filled; and a connection part that will be used when the solid raw material is put into the crucible The dividing pipe is connected up and down. In the refill tube of the present invention, in the split tube, the inner diameter of the upper end of the split tube located at the lower position during connection can be set to be equal to or greater than the inner diameter of the lower end of the split tube located at the upper position. The lower end of the split tube has a large inner diameter. In the refilling pipe of the present invention, the inner diameter of the upper end of the divided pipe is set to be equal to the inner diameter of the lower end, or larger than the inner diameter of the lower end. In the refill tube of the present invention, the connecting portion can be provided with a flange portion extending to the outside in the radial direction, and a locking portion that locks this flange portion. In the refill tube of the present invention, in the connecting portion, the upper end of the divided pipe located at the lower position during the connection can be fitted with the lower end of the divided pipe located at the upper position. In the refill tube of the present invention, the connecting portion can be connected to the upper end surface and the lower end surface of the divided tube. In the refill tube of the present invention, a buffer member can be provided on the connecting portion on the surface where the upper divided tube and the lower divided tube are in contact. In the refill tube of the present invention, the inner diameter of the buffer member can be set to be equal to the lower end inner diameter of the divided pipe located at the upper side, or larger than the lower end inner diameter of the divided pipe located at the upper side. In the refill tube of the present invention, the dividing tube can be composed of quartz, and the buffer member can be composed of a material containing carbon having flexibility. The raw material supply device of the present invention is a raw material supply device used for the growth of single crystals of the Tchaikovsky method, which additionally charges granular solid raw materials or recharges them into the raw material melt in the crucible, It can include: any one of the above-mentioned recharging pipes; a conical bottom cover detachably installed at the lower open end of the recharging pipe; and a lifting means capable of suspending the recharging pipe The tube and the bottom cover are raised and lowered, and the lower open end of the recharging tube can be opened, and the solid raw material can be poured into the raw material melt in the crucible. The single crystal pulling device of the present invention is to grow single crystals from the raw material melt by the Tchaikovsky method, and includes: the above-mentioned raw material supply device; a furnace body with the crucible inside; and a heat shielding body in the furnace The inner circumference of the body is located above the crucible, and it is a cylindrical shape with a reduced inner circumference at the lower end, which is used to shield the radiant heat from the single crystal grown from the raw material melt. When additional charging or recharging is performed, the The recharging tube is inserted into the inner side of the heat shield from above, and the lower end of the recharging pipe is positioned below the lower end of the heat shield. In this state, the solid raw material is poured into the crucible Melt. In the single crystal pulling device of the present invention, when the solid raw material is dropped into the raw material melt in the crucible, the connecting portion can be set at a position higher than the lower end of the heat shield. In the single crystal pulling device of the present invention, when filling the solid raw material into the recharging tube, there is an inclined support platform on the outside of the furnace body, wherein the inclined support platform is installed with the splitting of the bottom cover at the lower end The tube is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is supported so that the upper side can be connected by the connecting portion. The method of using the refill tube of the present invention is the method of using the refill tube as described in any one of items 1 to 9 in the scope of the patent application, including: only replacing the inner surface of the tube due to the filling of the solid raw material. The split tube in a given state. The method of using the refill tube of the present invention is only in a state where there is no damage, because the filling of the solid raw material damages the inner surface If the transmittance is lower than 70%, replace the split tube. The method of using the refill tube of the present invention includes heating the inner surface of the divided tube that has been replaced due to damage to regenerate it. In the method of using the refill tube of the present invention, when the deformation of the split tube regenerated by heating exceeds a predetermined amount, it is no longer used. The recharging method of the present invention is a method of additionally charging or recharging the raw material melt in the crucible in the above-mentioned single crystal pulling device, including: tilting the dividing pipe with the bottom cover installed at the lower end And support and erect the divided tube inclined with the filling of the solid raw material on the vertical side, connect the divided tube to the upper side by the connecting portion, and then fill the solid raw material. The recharging method of the present invention is a method of additionally charging or recharging the raw material melt in the crucible in the above-mentioned single crystal pull-up device, including: through the inclined support table, the lower end is installed with the The divided tube of the bottom cover is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is connected to the upper side by the connecting portion, and then the solid raw material is filled . The recharging method of the present invention is the method of adding or recharging the raw material melt in the crucible in the above-mentioned single crystal pulling device, including: adding or recharging in the crucible After the raw material is melted, the inclination support table supports the connected plural divided pipes, makes them inclined, and separates the divided pipes by the connecting portion. The single crystal pulling method of the present invention uses the above-mentioned recharging method. After additional charging or recharging of the raw material melt in the crucible, the single crystal is grown from the raw material melt.

The recharging tube of the present invention is a raw material supply device used for the growth of single crystals of the Tchaikrasky method, and additional charging of granular solid raw materials or recharging raw materials into the raw material melt in the crucible The inner cylindrical recharging tube includes: a plurality of divided tubes divided in the axial direction when the solid raw material is filled; and a connecting part that connects the divided tubes up and down when the solid raw material is put into the crucible . Thereby, when filling the solid raw material, it is possible to fill the split tube having a shorter size in the axial direction after the refill tube is divided in the axial direction. Thereby, even if the filling amount of the solid raw material is the same, the falling distance of the filled solid raw material becomes shorter than that of a refill tube without division. Therefore, it is possible to reduce the impact on the inner surface of the refill tube during filling, and reduce the occurrence of damage to the inner surface of the refill tube.

This prevents the generation of fine powder from the refill tube, which is regarded as quartz or the like, and can suppress the occurrence of dislocation. At the same time, after filling the solid material to the vicinity of the upper end in the axial direction, connect the next divided pipe by the connecting part, and then fill the solid material, which can greatly increase the solid material to be recharged without increasing the falling distance of the solid material. The full filling amount of the raw material.

In addition, with the above-mentioned structure, it is possible to selectively replace only the large split pipe whose inner surface is cracked due to the drop of the solid raw material. Thereby, the replacement time of each split pipe can be changed according to the degree of progress of the internal cracking state.

For example, in a refill tube divided into two, the replacement time of the upper position can be lengthened with respect to the replacement time of the divided tube at the lower position. Or, in the three-divided refill tube, only the lower position is replaced in a shorter cycle, and by exchanging the connection positions of the upper and middle positions of the divided tube, the replacement time can be set to almost the same degree .

In addition, when the inner surface of the tube is cleaned after the refilling is completed, the tube length is relatively short, so it has high handling properties, which can reduce the burden on the operator and shorten the working time. At the same time, it can reduce the deterioration rate of the inner surface state caused by the falling of the solid material, so it can increase the life of the refill tube until the regeneration process, increase the number of refills that can be used, and reduce the number of regeneration processes. Increase the life span that will be affected by the deformation of the regeneration process.

Here, the recharging in the present invention refers to additional charging or recharging of the raw material melt in the crucible.

In the refill tube of the present invention, the split tube is set to have the upper end inner diameter of the split tube located at the lower side when connected, which is the same as the lower end inner diameter of the split tube located at the upper side, or is larger than the inner diameter of the lower end of the split tube at the upper side. The lower end of the dividing tube has a large inner diameter. As a result, the split tube located at the lower position during connection will not protrude further inward (center side) than the split tube located at the upper side when viewed in a plane, so the filled solid material will not directly collide with the split tube located at the lower side. The upper end of the tube. With this, the occurrence of scars near the upper end of the divided pipe located at the lower side, or the occurrence of cracks or defects in the divided pipe located at the lower side, can be prevented from generating impurities. Therefore, prevention of dislocation and deterioration of crystal characteristics can be achieved.

In the refill tube of the present invention, the inner diameter of the upper end of the divided tube can be set equal to the inner diameter of the lower end or larger than the inner diameter of the lower end. Thereby, for example, the divided pipe has a structure in which the inner diameter is reduced from the upper end to the lower end, or in a cylindrical divided pipe, a structure in which the inner diameter is reduced toward the lower end only in the vicinity of the lower end can be formed.

In the refill tube of the present invention, the connecting portion can be provided with a flange portion extending to the outside in the radial direction, and a locking portion that locks this flange portion. Thereby, in the connecting portion, the upper and lower divided pipes are arranged in a state in which their axial directions are aligned, so that the flange near the upper end of the divided pipe at the lower position and the flange near the lower end of the divided pipe at the upper position are aligned. Facing each other, the flanges in the parallel state are locked from the up-down direction or from the outside in the radial direction by the locking portion, so that they can be easily connected.

In the refill tube of the present invention, in the connecting portion, the upper end of the divided pipe located at the lower position during the connection can be fitted with the lower end of the divided pipe located at the upper position. Thereby, at the time of connection, the lower end of the divided pipe located at the upper side is inserted into the upper end of the divided pipe located at the lower side, and the connection can be easily connected only by fitting it.

In the refill tube of the present invention, the connecting portion is connected by the upper end surface and the lower end surface of the divided tube. Thereby, the upper end surface and the lower end surface of the divided pipe contact each other, and the vicinity of the connection part of the connected divided pipe can be sealed. Thereby, in the single crystal pulling device during recharging, the inside and the outside of the recharging tube are maintained in a separated state, and the recharging pipe can be moved to a predetermined recharging position. Moreover, when the upper end surface and the lower end surface of the divided pipe are not in contact with each other in the connecting portion, the upper end outer peripheral surface and the lower end inner peripheral surface are brought into contact with each other to seal the vicinity of the connecting portion of the divided pipe.

In the refill tube of the present invention, the connecting portion is provided with a buffer member on the surface where the upper divided tube and the lower divided tube are in contact. Thereby, the divided pipes made of rigid quartz or the like that are connected to each other do not directly contact, and can be connected by a flexible buffer member, and the vicinity of the connection portion can be easily sealed. At the same time, it is possible to prevent defects such as breakage caused by direct contact between divided pipes made of quartz and the like connected to each other.

In the refill tube of the present invention, the inner diameter of the buffer member is set to be equal to or larger than the lower end inner diameter of the divided pipe located at the upper side. Thereby, the buffer member is hidden in the divided pipe located at the upper side, and the filled solid material does not directly collide with the buffer member. With this, it is possible to prevent the occurrence of impurities caused by the buffer member, and it is possible to prevent deterioration of crystal characteristics such as an increase in carbon concentration due to mixing of a buffer member considered to contain carbon, for example.

In the refill tube of the present invention, the split tube is composed of quartz, and the buffer member is composed of a material containing carbon with flexibility. Thereby, even if the two divided pipes are deformed, the deformation can be absorbed and the vicinity of the connecting portion can be easily sealed. At the same time, it is possible to prevent defects such as breakage caused by direct contact between divided pipes made of quartz or the like connected to each other.

The raw material supply device of the present invention is a raw material supply device used for the growth of single crystals of the Tchaikovsky method, which additionally charges granular solid raw materials or recharges them into the raw material melt in the crucible, It includes: the refilling tube described in any of the above; a conical bottom cover detachably installed at the lower open end of the refilling tube; and a lifting means capable of suspending the refilling tube and the refilling tube. The bottom cover is raised and lowered, and the lower open end of the recharging tube can be opened, and the solid raw material can be poured into the raw material melt in the crucible. As a result, in the refill tube that can increase the amount of refill, it is possible to reduce damage caused by contact with solid raw materials, reduce the occurrence of misalignment, increase the number of times the refill tube can be used, and suppress the failure of each divided tube. Change the time and improve work efficiency.

At the same time, when shortening the axial length of the split tube, the bottom cover or the lifting means located inside the refilling tube can also shorten the distance of the solid material to be filled and reduce the impact on the bottom cover or the lifting means during filling. , Reduce the generation of impurities caused by the bottom cover or lifting means.

The single crystal pulling device of the present invention is to grow single crystals from the raw material melt by the Tchaikovsky method, and includes: the above-mentioned raw material supply device; a furnace body with the crucible inside; and a heat shielding body in the furnace The inner circumference of the body is located above the crucible, and it is a cylindrical shape with a reduced inner circumference at the lower end, which is used to shield the radiant heat from the single crystal grown from the raw material melt. When additional charging or recharging is performed, the The recharging tube is inserted into the inner side of the heat shield from above, and the lower end of the recharging pipe is positioned below the lower end of the heat shield. In this state, the solid raw material is poured into the crucible Melt. As a result, in the refill tube that can increase the refill volume, it is possible to reduce the damage caused by the collision of solid raw materials, reduce the generation of impurities caused by the bottom cover or the lifting means, reduce the generation of dislocation, and prevent the single crystal being pulled up. Deterioration of the crystallization characteristics of the tube, increase the number of times the refill tube can be used, control the replacement time of each split tube, and improve work efficiency.

In the single crystal pulling device of the present invention, when the solid raw material is dropped into the raw material melt in the crucible, the connecting portion is set at a position higher than the lower end of the heat shield. Thereby, it is possible to reduce the undesirable influence of the high temperature of the heat from the raw material melt or the heater on the locking portion of the connecting portion or the cushioning member. At the same time, it is also possible to adversely affect the divided pipes located other than the lowermost position due to the deformation caused by the raw material melt or the heat of the heater.

In the single crystal pull-up device of the present invention, when filling the solid raw material into the recharging tube on the outer side of the furnace body, there is an inclined support platform, wherein the inclined support platform is such that the lower end of the bottom cover is installed with the division The tube is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is supported so that the upper side can be connected by the connecting portion. Thereby, the inclined support table can be tilted to support (place) the divided pipe at the lowermost position with the bottom cover installed, and then fill the solid raw material into the divided pipe, when it is filled to the lowermost position. In the vicinity of the upper end of the divided pipe at the position, the next divided pipe is connected by the connecting part, and then the solid material is filled. Moreover, in this filling operation, regardless of the connection state of the divided pipes, the inclination angle of the divided pipes can be changed to switch between the inclined state and the upright state, so the workability of the filling operation can be improved, and the angle can be adjusted to make the filling The contact impact of the solid raw material on the refilling tube is reduced. In addition, at the end of filling, in order to perform refilling, the refill tube can be erected so that the axial direction of the refill tube is in the vertical direction and is easily suspended in the vertical direction.

The method of using the refill tube of the present invention is the method of using any of the refill tubes described above, including: replacing only the divided tube whose inner surface is damaged to a predetermined state due to the filling of the solid raw material. Thereby, it is possible to selectively replace only the divided pipes whose inner surface condition is greatly deteriorated due to the falling of the solid raw material. In this way, in accordance with the progress of the inner surface deterioration state, it is possible to change the replacement time of each split tube, try to extend the life of the refill tube, increase the refill volume, reduce the occurrence of misalignment, and prevent the degradation of crystal quality. And cut costs.

For example, in a two-divided refill tube, the replacement time of the split tube at the lower position, where the raw material is more likely to collide when filling the split tube at the upper position, is shortened to that of the split tube at the upper position. The replacement period is short, and the split tube at the lower side can be replaced earlier. Or, in the refilling pipes that are divided into three and have the same shape, prepare more divided pipes than required for the initial refilling amount in the connected state, so that only the severely damaged pipes can be replaced in a shorter cycle. And the divided tube in the lower position in the replacement state, or reduce the frequency of replacement of the divided tube in the middle position compared to the divided tube in the lower position, and reduce the replacement of the divided tube in the upper position compared to the divided tube in the middle position frequency. In addition, by sequentially replacing the connection positions of the upper, middle, and lower divided pipes, the replacement period can be set to almost the same level. In addition, it is possible to try to extend the life of the refill pipe.

In the method of using the refill tube of the present invention, the split tube is replaced only when the inner surface is damaged due to the filling of the solid raw material and the transmittance is less than 70%, compared to the state without damage. . Thereby, it is possible to selectively replace only the divided pipes whose inner surface condition is greatly deteriorated. When the transmittance is lower than 70%, the strength of the split tube will decrease and become poorer. In addition, the part with a transmittance of less than 70% can have the largest area in a quadrilateral area with a side length of about 10 cm. Alternatively, the part with a transmittance of less than 70% may be formed in 3 to 4 places in a quadrilateral area with a side length of about 5 cm. Thereby, the strength of the refill tube can be ensured, the occurrence of misalignment can be prevented, and the degradation of crystal quality can be prevented.

The method of using the refill tube of the present invention further includes heating the inner surface of the divided tube that was replaced due to damage to regenerate it. Thereby, the replaced divided pipe can be reused. Thereby, the split tube can be reused in a state where there is no damage, strength is maintained, and misalignment is prevented, thereby extending the life and reducing costs.

In the method of using the refill tube of the present invention, when the deformation of the split tube regenerated by heating exceeds a predetermined amount, it is no longer used. Thereby, it is possible to use only the divided pipes that can maintain the airtightness of the connection portion, and to ensure the safety of refilling.

The recharging method of the present invention is a method of additionally charging or recharging the raw material melt in the crucible in the single crystal pull-up device described above, which includes: mounting the bottom cover on the lower end of the split The tube is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, the divided tube is connected to the upper side by the connecting portion, and the solid raw material is filled. By this, the occurrence of dislocation is suppressed, and in the pulled-up crystals, it is possible to add or reload to reload the raw material increased by the reloading tube while suppressing the quality deterioration such as the carbon concentration change, and then pull up the order. crystallization.

A recharging method of the present invention is a method of additionally charging or recharging the raw material melt in the crucible in the above-mentioned single crystal pulling device, including: using the inclined support platform to make the lower end The divided tube attached with the bottom cover is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is connected to the upper side by the connecting portion, and then filled The solid raw material. By this, the inclination angle is controlled between the inclined state and the upright state, and the refill tube can be filled with solid raw materials, in an attempt to improve the work efficiency, safety, and crystal quality in the raw material filling step.

The recharging method of the present invention is a method of additionally charging or recharging the raw material melt in the crucible in the single crystal pulling device described above, including: additional charging or recharging of the raw material melt in the crucible After the raw material in the crucible is melted, the inclination support table supports the connected plural divided pipes, is inclined, and the divided pipes are separated by the connecting portion. Thereby, the work efficiency of the next recharging step after the recharging step can be improved, and the manufacturing cost of the single crystal can be reduced.

The single crystal pulling method of the present invention uses the above-mentioned recharging method. After additional charging or recharging of the raw material melt in the crucible, the single crystal is grown from the raw material melt. Thereby, it is possible to increase the amount of refill, prevent the deterioration of crystal quality, suppress the occurrence of dislocation, improve the work efficiency, and reduce the manufacturing cost, so that the single crystal can be pulled up.

According to the present invention, it is possible to increase the filling amount of the refill tube, prevent the life of the refill tube from being reduced, and at the same time achieve reduction in the occurrence of misalignment, prevention of reduction in the workability of refilling, and reduction of crystal quality. effect.

Hereinafter, the first embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be explained based on the drawings. Figure 1 is a front cross-sectional view showing the refill tube of this embodiment. Figure 2 is an exploded perspective view showing the refill tube of this embodiment. Figure 3 is an enlarged cross-sectional view showing the connecting portion of the refill tube of this embodiment. In the figure, the symbol 10 is the refill tube.

The recharging pipe 10 of this embodiment forms a raw material supply device as described later, and recharging is performed on a single crystal pulling device using the CZ method. As shown in Figs. 1 to 3, the recharging tube 10 of this embodiment is formed into a cylindrical shape composed of quartz, and solid raw materials are filled in the cylinder.

As shown in Figures 1 to 2, the refill tube 10 is divided into two in the vertical direction of the axial direction in this embodiment, and is divided by a lower divided tube (divided tube) 10A and an upper divided tube (divided tube) 10B. composition. 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 through the connecting portion 11.

As the connecting portion 11, as shown in Figs. 2 to 3, a flange portion 11a at the upper end of the lower split pipe 10A, a lower end flange portion 11b of the upper split pipe 10B, a flange portion 11a and a flange portion 11b are provided A plurality of connecting holes 11c, 11c, screws as the locking part to lock them, nuts 11d, 11d, and a buffer member 11e clamped by the flange portion 11a and the flange portion 11b are provided in the circumferential direction of the .

As shown in FIGS. 2 to 3, the connecting hole 11c has a substantially equal interval in the circumferential direction of the flange portion 11a and the flange portion 11b, and is arranged in plural. In this embodiment, there are six connecting holes 11c, but it is not limited to this number.

The screws and nuts 11d and 11d are made of metal that is resistant to high temperatures in the single crystal pull-up device as shown in Figure 3. In order to prevent the release of fine substances that are the cause of dislocation, they are treated by, for example, surface treatment. It is composed of screws and nut groups. Specifically, SUS (stainless steel) can be used when heat resistance is not so required, or a composition such as molybdenum can be used when high temperature resistance is more required. In addition, a double nut is used for the nut 11d.

In addition, between the screw and nut 11d and the connecting hole 11c, a metal member 11f is provided on the lower surface of the flange 11a and the upper surface of the flange 11b, so that the flange portion 11a, the flange portion 11b, and the screw and nut 11d will not be in direct contact.

As shown in Figures 1 and 3, the cushioning member 11e is in contact with the upper surface of the flange portion 11a and the lower surface of the flange portion 11b, and makes the upper surface of the flange portion 11a and the flange portion locked by the screw and nut 11d The lower surface of 11b is not in direct contact, and in order to absorb the deformation between the two, a flexible, thin ring shape is used. Specifically, the cushioning member 11e is a heat-resistant resin that is resistant to high temperatures in the single crystal pull-up device, or is a carbon that has flexibility, suitable for use such as Teflon (registered trademark) fluororesin, carbon fiber non-woven fabric, etc. .

The outer diameter of the buffer member 11e is not specifically defined, but its inner diameter size will be 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 further inside the refill tube 10 than the lower end of the upper divided tube 10B. In addition, the thickness dimension of the cushioning member 11e can follow the deformation of the lower divided pipe 10A and the upper divided pipe 10b when locked by the locking portion, and is not particularly limited as long as the airtightness of the connecting portion 11 can be maintained.

In addition, when the plane accuracy is high to the extent that the upper end surface of the lower divided pipe 10A and the lower end surface of the upper divided pipe 10B can be tightly sealed, the buffer member 11e may not be provided.

At the upper end of the upper split pipe 10B, as shown in FIGS. 1 and 2, the upper flange portion 9 is set to have an outer dimension larger than the outer diameter of the flange portion 11a and the flange portion 11b.

Fig. 4 is an enlarged front cross-sectional view showing the lower end side of the recharging pipe in this embodiment, and Fig. 5 is a plan sectional view showing the lower end side of the recharging pipe in this embodiment. As shown in No. 4, the reloading pipe has a conical bottom cover 14 detachably attached to the lower open end of the lower divided pipe 10A. The bottom cover 14 is connected to a metal shaft (pull-up means) 15 that penetrates from the upper part to the inside of the refill tube 10.

As shown in FIG. 4, the metal shaft 15 penetrates the refill tube 10, and its inside is protected by a protective tube (lifting means) 16 in order to prevent direct contact with the solid raw material. The protective tube 16 is composed of a covered protective tube 16b directly covering the metal shaft 15 and a sliding protective tube 16a inserted into this covered protective tube 16b slidably. The protective tube 16 is configured to prevent the metal shaft 15 from directly contacting the solid raw material, while ensuring a stable operating state in a state where the metal shaft 15 does not deviate.

As shown in Figures 4 to 5, the sliding protection tube 16a will be extended in the radial direction from the inner surface of the refill tube 10 to the center of its axis and extending in the axial direction (vertical direction) of the sliding protection tube 16a. The fixed plate portion 16c is fixed so as to be arranged at the axial center position (vertical direction) of the refill tube 10.

The fixed plate portion 16c is connected to the lower divided pipe 10A and the upper divided pipe 10B, and the metal shaft 15 penetrates the covered protection pipe 16b and the sliding protection pipe 16a separated in the vicinity of the connection portion 11 in a continuous state in the axial direction.

Therefore, the metal shaft 15 penetrating the refill tube 10 will avoid the contamination of solid raw materials due to the directly covered protective tube 16b. Not only this, but also the sliding protection tube 16a will not cause the refill tube The center position of 10 is deviated.

In addition, since the fixed plate portion 16c is located in the radial direction of the refill pipe 10, when the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11, they may be arranged so as to form almost the same surface. Thereby, the metal shaft 15 can suspend the recharging tube 10 vertically down to the center of the crucible, and can evenly supply the solid raw material to the molten liquid in the crucible.

Fig. 6 is an enlarged front view of the upper end side showing the lowering stop state of the refill tube of this embodiment. Fig. 7 is an enlarged front view showing the upper end side of the refill tube of this embodiment, and is a state where the metal shaft is lowered and the bottom cover is opened. Fig. 8 is a plan view showing the metal upper member used on the upper end side of the refill tube of this embodiment.

In the raw material supply device, in order to synchronize with the raising and lowering of the metal shaft 15, the reloading tube 10 is also provided with a lifting means, so that the conical bottom cover 14 is inserted into the lower opening to pull up the reloading tube 10, And the lifting time point of the lifting means (the lifting means) provided in the refilling pipe 10 is synchronized. By synchronizing the lifting time point, not only the lifting of the metal shaft 15 is stabilized, but the lifting of the refilling pipe can also be stabilized.

In the raw material supply device, as shown in FIGS. 6 to 7, a metal (stainless steel, etc.) washer 19 is provided on the metal shaft 15 as a lifting means (pulling means) of the refill tube 10. The protective tube 16 is arranged at the center of the recharging tube 10, and the metal shaft 15 is raised and lowered inside the protective tube 16, and the metal washer 19 is attached to the predetermined height position of the metal shaft 15. In addition, a dedicated hanger 18 equipped for suspending the recharging pipe 10 uniformly is used for the lifting means composed of the metal gasket 19.

In order to match the time when the conical bottom cover 14 is inserted into the lower opening to pull up the refill tube 10 and the time when the refill tube 10 is pulled up, the fixing position of the metal gasket 19 can be adjusted to make the lifting Time point synchronization. Thereby, it is possible to cooperate with the raising and lowering of the metal shaft 15 to make the raising and lowering of the refill tube 10 more stable.

The metal upper member 20 is made of the same material as the screw and nut 11d, and is attached to the upper part of the refill tube 10. As the hook member, a metal flange 9a can be provided.

The metal upper member 20 is provided with a through hole 20a at a predetermined position in the circumferential direction, and the metal member 20 is fixed to the refill tube 10 by locking the long screw 21 with a through nut or the like. The structure of the metal member 20 is a metal convex缘9a. In this case, the height adjustment of the metal flange 9a can be performed by the locking length of the long screw 21 to adjust the descending stop height of the refill tube 10.

Figure 9 is a diagram showing the steps of the method of filling the refill tube in this embodiment. Figure 10 is a step diagram showing the method of filling the refill tube in this embodiment. Figure 11 is a diagram showing the steps of filling a conventional refill tube. Figure 12 is a flowchart showing the refilling method in this embodiment.

The recharging method of this embodiment is shown in Fig. 12, which can have a recharging amount setting step S01, a connection length setting step S02, a washing step S03, a lowermost divided pipe setting step S04, a tilting step S05, and raw materials. Filling step S06, refilling amount judging step S07, dividing pipe setting step S08, connecting step S09, erecting step S10, refilling step S11, dividing step S12, refilling frequency counting step S13, refilling frequency judging Step S14, visually confirming step S15 through the tube, replacement step S16, washing step S17, regeneration processing step S20, deformation amount determining step S21, and discarding step S22.

In the recharging method of this embodiment, as the recharging amount setting step S01 shown in Fig. 12, the amount of solid raw material S1 to be additionally charged or recharged to the crucible is set. As the connection length setting step S02 shown in Fig. 12, the number of connections of the divided pipes of the refilling pipe 10 will be set so that it can fill the volume of the solid raw material S1 set in the refilling amount setting step S01. .

At this time, in consideration of the falling distance of the solid raw material S1 described later and damage to the inner surface of the recharging pipe 10, the length of the split pipe (the number of connections) is set. In addition, in the present embodiment, the refill tube 10 is a two-divided pipe of the lower divided pipe 10A and the upper divided pipe 10B, so it is set whether or not to connect the upper divided pipe 10B.

Next, as the washing step shown in Fig. 12, after washing the inner surface of the divided pipe to be used, as the lowermost divided pipe installation step S04 shown in Fig. 12, prepare not to connect to the upper divided pipe 10B The lower divided pipe 10A in the separated state. Next, the bottom cover 14 is inserted into the lower open end of the lower divided tube 10A to form a closed state, and the lower end of the metal shaft 15 penetrating the protection tube 16 is attached to the bottom cover 14 to form a filling preparation state.

Next, as the tilting step S05 shown in Fig. 12, the lower divided tube 10A is supported in a state of being inclined at a predetermined angle, as the raw material filling step S06 shown in Fig. 12, as shown in Fig. 9, The solid raw material S1 is filled in the lower divided pipe 10A. At this time, although the solid raw material S1 collides with the inner wall surface of the lower divided tube 10A, compared to the conventional recharge tube 100 shown in FIG. 11, which is not divided in the prior art, the solid raw material S1 has a shorter falling distance, so it will There is less damage to the inner wall surface of the lower divided pipe 10A.

Next, as the refill amount determination step S07 shown in Figure 12, it is determined whether the amount of solid raw material S1 set in the refill amount setting step S01 is filled. If it is insufficient, it is used as shown in Figure 12. In step S08, the upper divided pipe 10B is set to the upper side of the lower divided pipe 10A, as the connection step S09 shown in Figure 12, the lower divided pipe 10A is connected to the upper divided pipe by the connecting portion 11 10B connection. At this time, even in the upper divided pipe 10B, the metal shaft 15 penetrates the protective pipe 16.

Next, as the raw material filling step S06 shown in FIG. 12, as shown in FIG. 10, following the lower divided pipe 10A, the solid raw material S1 is filled into the upper divided pipe 10B. At this time, the lower divided pipe 10A is in a filled state with the solid material S1. Therefore, the injected solid material S1 falls and collides with the inner wall surface of the upper divided pipe 10B, but does not cause a drop impact on the inner wall surface of the lower divided pipe 10A. Therefore, compared with the conventional non-divided refill tube 100 shown in FIG. 11, since the solid raw material S1 falls away from the tube, the upper divided tube 10B is less damaged.

Next, as the refill amount determination step S07 shown in Figure 12, it is determined whether the amount of solid material S1 set in the refill amount setting step S01 is filled. When the set amount is reached, it is used as Figure 12. As shown in the erecting step S10, the refill tube 10 is erected so that its axis is parallel to the vertical direction.

Fig. 13 is a cross-sectional view showing the overall structure of the single crystal pulling device equipped with the raw material supply device of this embodiment. Fig. 14 shows the state of the molten raw material in which the solid raw material is poured into the crucible.

The single crystal pulling device in this embodiment is made into a furnace that uses CZ farad to pull single crystals. As shown in Figures 13 and 14, the furnace body is composed of a main chamber 1 and a pulling chamber 2. , In addition, it has a gate valve 13. The pull-up chamber 2 is composed of a cylindrical shape with a smaller diameter than the main chamber 1, and is arranged on the upper part through the gate valve 13 on the same central axis as the main chamber 1.

The gate valve 13 is configured to operate to communicate or block the inside of the main chamber 1 and the pull-up chamber 2, and the communication diameter of the gate valve 13 is smaller than that of the pull-up chamber 2.

A crucible 3 is provided in the center of the main chamber 1. This crucible 3 has a double structure combining the quartz crucible 3a on the inner side and the graphite crucible 3b on the outer side, and is supported on a support shaft 4 called a "stand" through a holder 4A. The support shaft 4 can lift the crucible 3 in the axial direction, and can drive the crucible 3 to rotate in the circumferential direction.

The heater 5 is arranged to surround the crucible 3. A heat insulating material 6 extending along the inner surface of the main chamber 1 is arranged on the outer side of the heater 5. The upper side of the crucible 3 is provided with a heat shield 12 along the circumference to isolate the single crystal to be pulled up from the heater 5 and the heat of the molten raw material melt S2 in the crucible 3. The heat shield 12 has a cylindrical shape or an inverted conical trapezoid shape, etc., and its lower end is located near the upper side of the raw material melt S2.

The solid raw material put 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 the initially charged solid raw material is melted, in order to make up for the shortage of the raw material melt S2 in the crucible 3 and ensure a desired amount of melt, additional charging is performed.

Therefore, the lifting shaft 7 hangs down into the lifting chamber 2 and suspends the refilling pipe 10 used in the raw material supply device of this embodiment. At this time, the refill tube 10 filled with the solid raw material S1 passes through the suspension jig 8 connected to the lower end of the lift shaft 7 and is located above the crucible 3 where the raw material melt S2 is formed. The pull-up shaft 7 is provided in the uppermost driving mechanism 2a of the pull-up chamber 2 for rotation drive and lift drive. The elevating shaft 7, the suspension jig 8, the driving mechanism 2a, the metal flange 9a, and the like constitute the elevating means.

In the single crystal pulling device of this embodiment, as the recharging step S11 shown in FIG. 12, a raw material supply device equipped with a recharging pipe 10 is used to recharge the solid raw material S1.

In the case of additional charging, as shown in Figure 13, after the solid raw material initially charged in the crucible 3 is melted, the recharging tube 10 filled with the solid raw material S1 is connected to the lower end of the lifting shaft 7. The suspension jig 8 is located above the crucible 3 where the raw material melt S2 is formed. Since the volume of the solid raw material charged in the crucible 3 in the initial stage is limited compared to the volume of the crucible, the raw material melt S2 in the crucible 3 may be insufficient relative to the volume of the crucible.

When the solid raw material initially charged in the crucible 3 has almost completely melted, and the remaining part of the solid raw material melted to form a floating island state, the recharging tube 10 is lowered. At this time, as shown in FIG. 13, the metal flange 9a is in contact with a predetermined height position, for example, provided in the small diameter part of the gate valve 13, and only the lowering of the refill tube 10 stops.

Here, as shown in Figures 13 and 14, the length of the lower divided pipe 10A is set so that the connecting portion 11 is located above the lower end position of the heat shield 12, and the connecting portion 11 will be isolated from the raw material melt. The liquid S2 or the heat of the heater 5 does not rise to the same temperature as the raw material melt S2.

On the other hand, the conical bottom cover connected to the metal shaft 15 will not hinder the lowering. If the lifting shaft 7 is lowered from this position, the bottom cover 14 will be opened as shown in Figure 14, and the filling tube will be refilled. The granular solid raw material S1 in 10 falls by its own weight and is supplied to the raw material melt S2.

At this time, as shown in Figure 14, the metal shaft 15 penetrating the refill tube 10 is fixedly provided on the sliding protection tube 16a on the inner surface of the refill tube 10, and the metal shaft is directly covered and inserted into this The sliding protection tube 16a is protected by the covered protection tube 16b, so it can prevent contamination of the solid raw material S1, eliminate the deviation from the center axis of the metal shaft 15, and evenly supply the solid raw material S1 to the crucible 3 in the circumferential direction Inside.

Once the input of the solid raw material S1 is completed, the recharging tube 10 is pulled upward and taken out from the pulling chamber 2. Here, when the amount of raw material melt in the crucible 3 does not reach the target value, the recharge tube 10 can be used again to repeatedly input the solid raw material S1. However, in this embodiment, the recharge amount setting step In S01, the refilling amount is set, so a sufficient amount of solid raw material S1 can be injected without the need to repeatedly input the solid raw material.

When the additional recharging is completed and the raw material melt 12 in the crucible 3 reaches the target amount, the suspension jig 8 connected to the lower end of the lifting shaft 7 is loaded with seed crystals and moved to the single crystal growing process.

Above, the operation steps of additional charging are explained, but the recharging is also through the same operation steps. After the initial single crystal growth, the solid raw material S1 corresponding to the reduced amount of the raw material melt is added to the raw material remaining in the crucible 3. In the melt S2. In addition, recharging means the additional charging performed after the initial raw material is put into the crucible 3 and melted as described above, and the recharging when the single crystal is pulled up and processed continuously. In both the additional charging and the recharging, the solid raw material S1 is additionally charged in the state where the raw material melt S2 is in the crucible 3.

When the recharging step S11 ends, as the dividing step S12 shown in FIG. 12, the recharging pipe 10 is divided into a lower divided pipe 10A and an upper divided pipe 10B. Next, as step S13 of counting the number of refills shown in Fig. 12, the number of refills used so far is counted for each divided tube.

Next, as the refilling frequency determination step S14 shown in Fig. 12, if it is determined that the refilling frequency counted in the refilling frequency counting step S13 does not exceed the predetermined number of times, it is divided for each for reuse. Pipe, the upper divided pipe 10B is sent to the washing step S17 shown in Fig. 12, and the lower divided pipe 10A is sent to the washing step S03 shown in Fig. 12.

Here, the number of refills that can be reused is set to about 40-50 times, and the predetermined number of times of the lower divided pipe 10A and the predetermined number of upper divided pipes are set in advance for each divided pipe. This is because when the lengths of the lower divided pipe 10A and the upper divided pipe 10B are different, the falling distance of the solid material S1 will be different, and the damage caused by the impact of the drop of the solid material S1 will also be different.

Next, as the transparent tube visual confirmation step S15 shown in FIG. 12, the damage caused by the falling impact of the solid raw material S1 is visually determined for each divided tube. At this time, only the divided pipes whose inner surface is damaged to a predetermined state due to the filling of the solid raw material S1 are replaced. Therefore, it is possible to selectively exchange only the divided pipes whose inner surface condition is greatly deteriorated due to the falling of the solid raw material S1.

As a reference for the replacement in step S15 to be visually confirmed through the tube, the lower split tube 10A and/or the upper split tube 10B, when there is no damage compared to the unused state, damage to the inner surface caused by the filling of the solid material S1 , The transmittance is lower than 70%, and the part that can be confirmed visually can be replaced in the case of white turbidity.

In particular, although this part with a transmittance of less than 70% is the part with the largest area, it can be an area of about 10 cm square. Alternatively, it is preferable to set the portion with a transmittance of less than 70% to be in a state where 3 to 4 areas are formed in a quadrilateral with a side length of 5 cm.

In step S15 of visually confirming through the tube, if it is judged that the white turbidity area has not reached the standard, for reuse, the upper divided tube 10B is sent to the washing step S17 shown in Fig. 12 for each divided tube, and the lower divided tube 10A is sent to the washing step S03 shown in Fig. 12.

In addition, only one of the recharging frequency determination step S14 and the through-tube visual confirmation step S15 can be implemented. Alternatively, after step S15 is visually confirmed through the tube, the refilling frequency determination step S14 may be implemented.

When it is judged that the white turbidity area has reached the standard in the through-tube visual confirmation step S15, as the replacement step S16 shown in FIG. 12, the divided tube is replaced, and the regeneration processing step S20 shown in FIG. 12 is performed. In the regeneration treatment step S20, the inner surface of the damaged and replaced divided pipe is heated and melted to remove the scar and regenerate it transparently, so that the replaced divided pipe can be reused. Here, in step S20 of the regeneration process, the axial lengths of the lower divided pipe 10A and the upper divided pipe 10B can be set to be shorter than the conventional undivided refill pipe 100 shown in FIG. 11, and therefore less The total heating capacity can be completed, and less deformation due to regeneration treatment can be completed.

After the regeneration processing step S20 is completed, it is used as the deformation amount determination step S21 shown in Fig. 12, and when it is determined that the deformation generated during the regeneration processing exceeds a predetermined amount, the division is discarded as the discarding step S22 shown in Fig. 12 tube. In addition, as the deformation amount determination step S21, when it is determined that the amount of deformation generated in the regeneration process does not exceed a predetermined amount, for reuse, for each divided tube, the upper divided tube 10B is sent to the cleaning shown in Fig. 12 In step S17, the lower divided pipe 10A is sent to the washing step S03 shown in Fig. 12.

This concludes the recharging method in this embodiment.

According to the raw material supply device with the refill tube 10 of this embodiment and the refill method using a single crystal pull-up device, even if the filling amount of the solid raw material S1 is the same, it can be compared with the refill tube 100 without division. The falling distance of the filled solid material S1 is reduced, the impact on the inner surface of the recharging tube 10 during filling is reduced, and the occurrence of damage to the inner surface of the recharging tube 10 is reduced.

Thereby, even if the filling amount of the solid raw material S1 for recharging is greatly increased, the usable life of the recharging tube 10 can be extended. In addition, in accordance with the degree of progress of the inner surface deterioration state, the replacement time of each of the split pipes 10A and 10B can be changed from each other, in an attempt to improve safety and prevent the occurrence of misalignment.

In addition, by providing the buffer member 11e and determining that the split pipes 10A and 10B are to be regenerated, it is possible to prevent the sealing state of the refill pipe 10 from deteriorating. In addition, the efficiency of the raw material supply operation can be achieved.

Hereinafter, based on the drawings, the second embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. Fig. 15 is a schematic diagram showing the inclined support table in step S04 of installing the lowermost divided pipe in this embodiment. FIG. 16 is a schematic diagram showing the tilting support table in the tilting step S05 and the material filling step S06 of this embodiment. Fig. 17 is a schematic diagram showing the inclined pipe support table in the divided pipe setting step S08 and the raw material filling step S06 of this embodiment. Fig. 18 is a schematic diagram showing the inclined support table in the erecting step S10 and the refilling step S11 of this embodiment.

The difference between this embodiment and the above-mentioned first embodiment is related to the tilt support 30, and the corresponding components will be denoted by the same reference numerals, and descriptions thereof will be omitted.

In this embodiment, the lowermost divided pipe setting step S04, tilting step S05, raw material filling step S06, divided pipe setting step S08, connecting step S09, erecting step S10 and other steps can be used to support refilling pipes. 10 of the inclined support table 30.

As shown in Figures 15 to 18, the tilt support table 30 includes: a support trolley portion 32 having a support portion 31 for supporting the refill tube 10; a tilt table 34 having a tilt support portion 35 that tilts the support trolley portion 32; and tilt The drive unit 39 inclines the tilt table 34.

As shown in Figures 15 to 18, the support part 31 is erected on a single side of the substantially flat support trolley part 32, and can support the split pipes 10A and 10B when tilted, and wheels 33, 33 are provided on the underside of the support trolley 32 , And able to move.

The substantially flat inclined table 34 is connected to a base 36 arranged on the ground or the like so as to be rotatable about a horizontal axis 35a. The tilt support part 35 is connected to the tilt table 34, and the tilt support part 35 is erected on the upper side of the tilted horizontal shaft 35a.

The back side of the tilt support part 35 is provided with a tilt drive part 39, and the base part 36 located further outside than the tilt table 34 is connected by the axes 37 and 38 parallel to the horizontal shaft 35a so that both ends can be rotatably connected. .

The tilt driving part 39 is composed of, for example, an air cylinder, an oil cylinder, a ball screw, etc., and forms a driving part whose extension length can be changed. By changing the extension length of the tilt driving part 39, the tilt table 34 can be driven from a horizontal position around a horizontal position. The shaft 35a is rotated to the inclined position, or the inclined support stand 35 is rotated from the vertical position around the horizontal shaft 35a to the inclined position.

By the driving of this tilt driving part 39, it is possible to drive the support trolley part 32 placed on the tilt table 34 to follow from the horizontal position and rotate around the horizontal axis 35a to the tilt position, or the support part 31 to follow from the vertical position Turn around the horizontal axis 35a to the inclined position.

At the same time, the tilt drive part 39 can support the refill tube 10 which is placed and supported by the support trolley part 32 and the support part 31, as well as the filling tube 10 when it reaches the tilt position and in the state of the tilt position. The weight of the solid raw material S1 in the pipe 10 is recharged.

The base 36 is provided with an inclined portion 31a at an end on the opposite side to the horizontal axis 35a of the inclined table 34, and is arranged to support the carriage portion 32 to be able to travel from the upper surface of the inclined table 34 to the ground without height difference.

The inclined support table 30 in this embodiment is shown in FIG. 15. In the extended state of the inclined drive unit 39, the inclined table 34 and the support trolley portion 32 are placed in a horizontal position, and the inclined support portion 35 and the support portion 31 are placed in a horizontal position. The state of being in a vertical position.

Then, as the lowermost divided pipe installation step S04, the lower open end of the lower divided pipe 10A is inserted into the bottom cover 14 to form a closed state, and then the lower end of the metal shaft 15 penetrating through the protective tube 16 is mounted to the bottom cover 14 to prepare for filling The lower divided pipe 10A in the state is placed on the support carriage portion 32 so that its axis is parallel to the vertical direction.

Next, as a tilting step S05, drive to reduce the tilt drive unit 39, as shown in Fig. 16, drive to rotate the tilt table 34 from the horizontal position around the horizontal axis 35a to the tilt position, and also move the tilt support unit 35 from the vertical The position is rotated from about the horizontal axis 35a to the inclined position.

Thereby, the supporting trolley portion 32 is driven to follow from the horizontal position around the horizontal axis 35a to the inclined position, and the supporting portion 31 is driven to follow the vertical position around the horizontal axis 35a to the inclined position, thereby forming a The lower divided tube 10A is in a supported state while being inclined at a predetermined angle.

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

In addition, as step S08 for installing the divided pipes, as shown in Figure 17, the upper divided pipe 10B is installed at the upper position of the lower divided pipe 10A, and as the connecting step S09, the lower divided pipe 10A is connected by the connecting portion 11 And the upper side divided pipe 10B. At this time, the stretching and tilting drive unit 39 is driven to respectively drive the supporting trolley unit 32 to rotate from the inclined position around the horizontal axis 35a to the horizontal position, and to rotate the supporting unit 31 from the inclined position around the horizontal axis 35a to the vertical position. Thereby, as shown in FIG. 15, the lower divided pipe 10A is supported so that its axis is parallel to the vertical direction, and the nut and screw 11d as the locking portion are locked in the connecting portion 11. In addition, even if the pipe 10B is divided on the upper side, the metal shaft 15 penetrates the protective pipe 16.

Next, as a raw material filling step S06, the solid raw material S1 is filled in the upper divided pipe 10B connected to the lower divided pipe 10A. At this time, the reduction and tilt drive unit 39 is driven to respectively drive the support carriage unit 32 to rotate from the horizontal position around the horizontal axis 35a to the inclined position, and also to rotate the support unit 31 from the vertical position around the horizontal axis 35a to the inclined position, by As shown in Fig. 17, the refill tube 10 is supported so that its axis is in an inclined direction, and then the solid raw material S1 is filled into the upper divided tube 10B.

When the raw material filling step S06 is completed, the stretching and tilting drive unit 39 is driven to rotate the tilting table 34 from the tilted position around the horizontal axis 35a to the horizontal position, and the support unit 35 is rotated from the tilted position around the horizontal axis 35a to the vertical position. position.

Thereby, the supporting trolley part 32 is driven to rotate from the inclined position around the horizontal axis 35a to the horizontal position, and the supporting part 31 is rotated from the inclined position around the horizontal axis 35a to the vertical position, thereby supporting the refill tube 10 It becomes a filling state with its axis in the vertical direction.

In this state, as shown in Fig. 18, the support cart portion 32 is smoothly transported from the inclined platform 34 through the inclined portion 31a, and the refill tube 10 filled with the solid material S1 placed on the support cart portion 32 is transported To the vicinity of the single crystal pulling furnace, the metal shaft 15 is connected to the lower end of the pulling shaft 7 by the suspension jig 8, and it is pulled up by the driving mechanism 2a.

Next, the recharging pipe 10 is positioned above the crucible 3 where the raw material melt S2 is formed, and as the recharging step S11, a raw material supply device equipped with the recharging pipe 10 is used to recharge the solid raw material S1.

After the reloading tube 10 is completed, the reloading tube 10 is placed on the supporting trolley part 32, and the supporting trolley part 32 is transported to the tilting table 34, and the small tilt driving part 39 is driven to drive the supporting trolley part 32 respectively. Rotate from the horizontal position around the horizontal axis 35a to the inclined position, and turn the support part 31 from the vertical position around the horizontal axis 35a to the inclined position, thereby supporting the connected refill tube 10 so that its axis is in the inclined direction, The connection portion 11 is separated to separate the lower divided pipe 10A and the upper divided pipe 10B.

According to this embodiment, by using the inclined support table 30, it is possible to efficiently and safely perform the filling step of the divided and connected refill tubes of the divided tubes 10A and 10B. In addition, by tilting the support table 30, the angle can be adjusted to reduce the impact of the filled solid raw material S1 on the refill tube 10 and the like.

Hereinafter, based on the drawings, a third embodiment of the recharging tube, raw material supply device, single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. The difference between this embodiment and the above-mentioned first or second embodiment is the addition of a split tube 10C, and the corresponding constituent elements other than that are denoted by the same reference numerals and the description is omitted.

Fig. 19 is a schematic front cross-sectional view showing the recharging pipe in the raw material supply device of this embodiment. Fig. 20 is an enlarged cross-sectional view showing the connecting portion of this embodiment. Figure 21 is an exploded perspective view showing the refill tube of this embodiment. Figure 22 is a front cross-sectional view showing the seed crystal pulling device of this embodiment.

As shown in Figs. 19-21, the refill tube 10 of this embodiment has an additional split tube (split tube) 10C added or extended on the upper side of the upper split tube 10B to increase the amount of solid raw material S1 filled. .

The additional split tube 10C, as shown in Figures 19-21, is slightly cylindrical, unlike the lower split tube 10A and the upper split tube 10B, which has flanges 11a, 11b as the connecting portion 11, and its end It 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, it is set so that these inner surfaces form the same plane in the vertical direction. In addition, in the figure, the present embodiment shows a state where the buffer member 11e is not used.

Add the lower end of the split pipe 10C, as shown in Figures 19-21, as the connecting portion 11, with a circle of fitting grooves 11h provided at the outer peripheral position, and at the inner peripheral position of the upper end of the upper split pipe 10B as The connecting portion 11 is also provided with a round of fitting grooves 11g. Thereby, when the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the fitting groove 11h is fitted into the upper end of the upper divided pipe 10B, and the fitting groove 11g supports the lower end of the upper additional divided pipe 10C. At this time, the inner peripheral surface located on the radially outer side of the fitting groove 11g is in a state of being slightly in contact with the outer peripheral surface located on the radially inner side of the fitting groove 11h. The height direction dimensions of the fitting groove 11h and the fitting groove 11g can be set such that the fitting groove 11h is greater than the thickness of the side wall of the upper divided tube 10B and the fitting groove 11g is longer than the fitting groove 11h.

In addition, the protective tube 16 in the upper divided pipe 10C is similar to the lower divided pipe 10A and the upper divided pipe 10B, and the axial center of the upper additional divided pipe 10C extends in the vertical direction (axial direction). However, in the additional split tube 10C, instead of the plate-shaped fixed plate portion 16c extending in the radial direction from the inner surface of the refill tube 10 to the axial center, the lower end of the additional split tube 10C is installed across the diameter direction. The fixed inclined plate 16f enables the lower end of the protection tube 16 to be supported.

In addition, the upper end of the protection pipe 16 in the upper divided pipe 10B is connected to the lower end of the protection pipe 16 added with the divided pipe 10C without a gap. In addition, the lower end of the protection tube 16 of the upper divided pipe 10B and the upper end of the protection pipe 16 of the lower divided pipe 10A are connected without a gap. Thereby, it is possible to prevent the injected solid raw material S1 from being caught in the connection part of the protection tube 16 and hindering the input of raw material. In addition, the state in which the protection tubes 16 are connected means that they are in contact with each other, or even if they are separated, the solid raw material S1 will not be caught in this connection part.

Regarding the fixed inclined plate 16f, two pieces are provided symmetrically to the center of the C axis of the upper additional divided pipe 10 so that the width direction end is located at the center of the C axis of the upper additional divided pipe 10. Each of the fixed inclined plates 16f is arranged to be inclined in the width direction, and the angle in the width direction is an angle at which the axial center of the divided pipe 10C is added from the top toward the outer side in the radial direction. In addition, the fixed inclined plate 16f has a through hole penetrating in the vertical direction at the center position of the axis of the additional divided tube 10C, and the periphery of this through hole is connected to the lower end of the protective tube 16.

In each of the fixed inclined plates 16f, the lower end of the upper additional divided pipe 10C, which is more radially outward than the lowered width direction end, is made into a lower opening. When the upper additional divided pipe 10C is placed on the upper divided pipe 10B, the upper additional divided pipe 10B 10C can communicate with the inner side of the upper divided pipe 10B.

The ridgeline formed by the rising width direction end of each fixed inclined plate 16f has a length equal to the diameter of the upper additional divided pipe 10C. In addition, the longitudinal end portion of the fixed inclined plate 16f, that is, the part connected to the lower end of the upper additional divided pipe 10C, is formed in a state where the lower side of the fixed inclined plate 16f forming a mountain shape is notched.

The part formed on the lower side of the two-piece fixed inclined plate 16f that forms a mountain shape. When the upper additional split tube 10C is placed on the upper split tube 10B, it will be located at the upper end of the protection tube 16 of the upper split tube 10B and can communicate with the supporting metal.制轴15。 System shaft 15.

As a result, as the axial length dimension of the recharging tube 10 becomes larger, and at the same time, in the axial center position of the recharging tube 10, the divided pipe 10C, the upper divided pipe 10B, and the lower divided pipe 10A are added. , The metal shaft 15 penetrates through each protection tube 16 in a state of being connected in the axial direction.

In this embodiment, as the raw material filling step S06, the solid raw material S1 is filled into the lower divided pipe 10A. As the divided pipe installation step S08, the upper divided pipe 10B is installed at the upper position of the lower divided pipe 10A. As the connecting step S09, the lower divided pipe 10A and the upper divided pipe 10B are connected by the connecting portion 11. As the raw material filling step S06, the solid raw material S1 is filled into the upper divided pipe 10B. As the refill amount determination step S07, it is determined whether or not the solid raw material S1 of the amount set in the refill amount setting step S01 is filled.

After that, as the divided pipe installation step S08, the upper additional divided pipe 10C is placed on the upper divided pipe 10B. In this embodiment, as the connection step S09, the metal shaft 15 only needs to penetrate the protective tube 16, and it is not necessary to lock the screw or nut 11d of the locking part.

In addition, as the raw material filling step S06, the solid raw material S1 is filled on the additional divided pipe 10C. As the erecting step S10, erect the refill tube 10 so that its axis is parallel to the vertical direction. Next, as shown in Figure 22, the suspension jig 8 is placed above the crucible where the raw material melt S2 is formed, and the granular solid raw material S1 in the charging tube 10 falls due to its own weight and is supplied to Raw material melt S2.

In this embodiment, the split pipe 10C is added from the top, which can increase the amount of refilling. In addition, by reducing the number of refilling, the time required for the refilling step can be shortened, and the production efficiency can be improved.

Hereinafter, based on the drawings, the fourth embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. The difference between this embodiment and the above-mentioned third embodiment is related to the connection portion, and the corresponding components other than that will be denoted by the same reference numerals, and the description will be omitted. Fig. 23 is an enlarged cross-sectional view showing the connecting portion in the refill tube of this embodiment.

As shown in FIG. 23, the refill tube 10 of this embodiment does not have a circle of fitting grooves 11h at the outer peripheral position of the lower end of the additional divided tube 10C. At the same time, at the inner peripheral position of the upper end of the upper divided pipe 10B, a circle of fitting grooves 11g is provided as a step difference, which has a radial dimension that is approximately the same as the thickness dimension of the lower end of the upper additional divided pipe 10C.

Therefore, on the outer periphery of the upper end of the upper divided pipe 10B, an enlarged diameter portion 11j is provided, which expands toward the outside in the radial direction by the length of the portion corresponding to the fitting groove 11g. In addition, the axial dimension of this enlarged diameter portion 11j, that is, the length of the lower end of the upper split pipe 10C fitted into the fitting groove 11g, can be larger than that of the third embodiment in which the fitting groove 11h is provided.

Specifically, the height-direction dimensions of the enlarged diameter portion 11j and the fitting groove 11g can be respectively made larger than 1/6 of the outer diameter of the upper divided pipe 10B, and the fitting groove 11g can be made larger than the enlarged diameter portion 11j. Longer.

Thereby, in the refill tube 10 of this embodiment, the upper additional divided tube 10C can be placed on the upper divided tube 10B in a state with increased stability. In addition, instead of adding the divided pipe 10C, for example, a divided pipe having no flange formed at the lower end such as the lower divided pipe 10A can be placed on the upper divided pipe 10B.

In order to prevent the upper end surface of the upper divided pipe 10B from directly contacting the lower end surface of the upper additional divided pipe 10C, a thin ring-shaped buffer member 11e is used, or a cylindrical shape is used at the inner surface of the enlarged diameter portion 11j. Buffer member 11e.

Hereinafter, based on the drawings, the fifth embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. The difference between this embodiment and the above-mentioned first to fourth embodiments is related to the inner diameter of the split tube, and the corresponding components other than that will be marked with the same symbols and descriptions will be omitted. Figure 24 is a front cross-sectional view showing the refill tube of this embodiment.

As shown in FIG. 24, the refill tube 10 of this embodiment is set so that the inner diameter of the lower end 10Ab of the lower divided pipe 10A is relatively smaller than the upper end 10Aa of the lower divided pipe 10A. Similarly, it is set so that the inner diameter of the lower end 10Bb in the upper divided pipe 10B is relatively smaller than the upper end 10Ba in the upper divided pipe 10B.

Therefore, both the upper side divided pipe 10B and the lower side divided pipe 10A have an inner conical trapezoid on the inner surface, and the diameter is reduced from the upper end side toward the lower end side. Moreover, the thickness of any one of the upper side divided pipe 10B and the lower side divided pipe 10A increases from the upper end side to the lower end side.

In addition, the inner diameter of the upper end 10Aa of the lower divided pipe 10A is smaller than that of the lower end 10Bb of the upper divided pipe 10B. When viewed from the upper side, it is set so that the upper end of the lower divided pipe 10A is not more divided than the upper end. The lower end of the tube 10B protrudes to the inside of the refilling tube 10.

In the refill tube 10 of this embodiment, when viewed from above, the buffer member 11e is hidden at the lower end 10Bb of the upper divided tube 10B, so that the filled solid raw material S1 does not directly collide with the buffer member 11e. In this way, it is possible to prevent the generation of impurities due to the buffer member 11e. For example, it is possible to prevent the mixing of the buffer member 11e of graphite properties and the deterioration of the crystal characteristics such as the fluctuation of the carbon concentration.

When viewed from above, the upper end 10Aa of the lower divided pipe 10A is hidden from the lower end 10Bb of the upper divided pipe 10B so that the filled solid material S1 does not directly collide with the upper end 10Aa of the lower divided pipe 10A. Thereby, it is possible to prevent the upper end portion 10Aa of the lower divided pipe 10A from being cracked or chipped. In addition, since the lower end portions 10Ab and lower end portions 10Bb of the divided pipes 10A and 10B are thick, it is possible to try to increase the strength of the lower end portions 10Ab and the lower end portions 10Bb to reduce the generation of deformation during the regeneration process.

Hereinafter, based on the drawings, the sixth embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. The difference between this embodiment and the above-mentioned first to fifth embodiments is the ratio of the lengths in the axial direction of the divided pipes. The corresponding components other than that are denoted by the same reference numerals, and the description is omitted. Figure 25 is a front cross-sectional view showing the refill tube of this embodiment.

As shown in FIG. 25, the refill tube 10 of this embodiment is set so that the axial length of 10 A of lower side divided pipes may be larger than the length of the upper side divided pipe 10B. Thereby, the amount of refilling can be increased, and 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. The influence of high temperature on the connecting portion 11 in the recharging step S11 is reduced.

Also, the axial length of the lower divided pipe 10A can be set to the same level as the conventional refill pipe 100 shown in Fig. 11. However, in this case, it can be used by connecting the upper divided pipe 10B. , The amount of refilling once is increased, and as a result, the usable number of times of the refilling tube 10 can be increased.

Hereinafter, based on the drawings, the seventh embodiment of the recharging tube, the raw material supply device, the single crystal pulling device, the method of using the recharging tube, the recharging method, and the single crystal pulling method of the present invention will be described. The difference between this embodiment and the above-mentioned first to fifth embodiments is the number of divisions in the filling tube, that is, the number of connections of the division tube, and other corresponding components will be The same symbols are assigned, and the description is omitted. Figure 26 is a front cross-sectional view showing the refill tube of this embodiment.

The refill tube 10 of this embodiment is divided into three in the vertical direction. As shown in FIG. 26, a middle side divided tube (divided tube) 10D is provided between the lower side divided tube 10A and the upper side divided tube 10B.

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

As the connecting portion 11, it is the same as the lower divided pipe 10A and the upper divided pipe 10B, having a flange portion 11n at the upper end of the middle divided pipe 10D, a flange portion 11m at the lower end of the middle divided pipe (divided pipe) 10D, and circumferential direction The plural connecting holes 11c and 11c provided in the flange portion 11n and the flange portion 11m, the screws and nuts 11d and 11d that are used as locking portions to lock them together. In addition, in this embodiment, although the buffer member 11e is not used, it may be provided.

In this embodiment, as the dividing tube setting step S08, the middle dividing tube 10D is set at the upper side of the lower dividing tube 10A. As the connection step S09, the flange portion 11a of the lower divided pipe 10A and the flange portion 11m of the middle divided pipe 10D are connected through the locking portion. In addition, as the divided pipe installation step S08, the upper divided pipe 10B is installed at the upper position of the middle divided pipe 10D. As the connection 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 through the locking portion.

In this embodiment, the recharging tube 10 is divided into three in the vertical direction, which can further shorten the falling distance of the solid raw material S1 in the raw material filling step S06. In the raw material filling step S06, the divided pipes 10A, 10B, and 10D are The damage of the inner wall surface is reduced. In addition, it is possible to connect a plurality of middle side divided pipes 10D between the lower side divided pipe 10A and the upper side divided pipe 10B, it is easy to increase the refilling amount to a desired amount, and it is possible to reduce refilling relative to the refilling amount. frequency.

In addition, in the present invention, it is also possible to appropriately combine the features in each of the above-mentioned embodiments, or it is also possible to make a state in which no specific feature is adopted. [Example]

Hereinafter, examples of the present invention will be described.

In the ψ300mm single crystal pull-up device, as a recharge tube for reloading, a quartz tube of about ψ300mm and a length of 1.8m in the axial direction is used for reloading. Take this as Experimental Example 1.

Similarly, as the recharging tube, a two-divided quartz tube with an axial length of 1.5 m on the lower side and 0.3 m on the upper side was used for recharging. Take this as Experimental Example 2.

Similarly, as the recharging tube, a two-divided quartz tube with an axial length of 0.9 m on the lower side and 0.9 m on the upper side was used for recharging. Take this as Experimental Example 3.

Similarly, as the recharging tube, a two-segmented quartz tube with an axial length of 0.6 m on the lower side, 0.6 m on the middle side, and 0.6 m on the upper side was used for recharging. Take this as Experimental Example 4.

The inner surface of the recharging tube of Experimental Example 1 became turbid due to damage caused by the falling of the solid raw material, and the number of recharging times when it was judged visually that the regeneration treatment was necessary was regarded as the reference frequency.

In Experimental Example 2, in this refilling tube, the number of times when regeneration treatment is similarly required for the lower divided tube is 1.21 times the reference number. In addition, the number of times when regeneration processing is similarly required for the upper divided pipe is 2.29 times the reference number.

In Experimental Example 3, in this refilling tube, the number of times when regeneration treatment was similarly required for the lower divided tube was 1.45 times the reference number. In addition, the number of times when regeneration processing is similarly required for the upper divided pipe is 1.49 times the reference number.

In Experimental Example 4, in this refilling tube, the number of times when regeneration treatment was similarly required for the lower divided tube was 1.90 times the reference number. In addition, the number of times when the split pipe on the center side is similarly required to undergo regeneration processing is 2.05 times the reference number. In addition, the number of times when regeneration is similarly required for the upper divided pipe is 2.15 times the reference number.

In each example, after the regeneration process, each split tube was reused, and the regeneration process was performed multiple times.

In the refilling tube of Example 1, in the multiple times of regeneration treatment, if it is judged that the deformation caused by heating exceeds the reference value and cannot be used (to be discarded), the number of refills so far is determined The sum is used as the reference life.

In Example 2, in this refill tube, the total number of times when it is judged to be discarded in the same manner for the lower divided tube is 1.10 times the reference life. In addition, the total number of times when it is judged to be discarded in the same manner for the upper split tube is 1.51 times the reference life.

In Example 3, in this refill tube, the total number of times when it is judged that the lower split tube is to be discarded in the same manner is 1.15 times the reference life. In addition, the total number of times when it is judged to be discarded in the same manner for the upper split tube is 1.37 times the reference life.

In Example 4, in this refill tube, the total number of times when it is judged to be discarded in the same manner for the lower divided tube is 1.25 times the reference life. In addition, the total number of times when the split tube on the center side is judged to be discarded in the same manner is 1.40 times the reference life. In addition, the total number of times when it is judged to be discarded in the same manner for the upper split tube is 1.49 times the reference life. In addition, for any of the above-mentioned times, about 3 refill tubes were used for each, and the average value at the end of the service life was calculated.

In addition, from the increase in the number of times when the regeneration process was required and the increase in the deformation resistance life, the ratio of the cost of change to the initial manufacturing cost of each split tube in each experimental example was calculated. The sum of the cost of each split tube was calculated as the total cost in the refill tube of the experimental example.

In the refill tube of Experimental Example 1, the initial manufacturing cost is assumed to be 10, the regeneration treatment cost is assumed to be 1, the deformation resistance cost is assumed to be 1, and the total cost when it is used to the final life is assumed to be 10.

In contrast, in Experimental Example 2, in the regeneration pipe, the initial manufacturing cost was calculated to be 9 and the cost was 6.76 in the same manner for the lower divided pipe. In addition, the initial manufacturing cost of the split pipe on the upper side is calculated to be 3 and the cost is 0.87 in the same way. In the refill tube of Experimental Example 2, the total cost at the end of its life is 7.63.

In contrast, in Experimental Example 3, in the regeneration pipe, the initial manufacturing cost was calculated to be 6, and the cost was 3.60 in the same manner for the lower divided pipe. In addition, the initial manufacturing cost of the split pipe on the upper side is similarly calculated to be 6, and the cost is 2.94. In the refill tube of Experimental Example 3, the total cost at the end of its life is 6.54.

In contrast, in Experimental Example 4, in the regeneration pipe, the initial manufacturing cost was calculated to be 5 and the cost was 2.11 in the same manner for the lower divided pipe. In addition, for the split tube on the center side, the initial manufacturing cost is similarly calculated to be 5, and the cost is 1.74. In addition, the initial manufacturing cost of the split pipe on the upper side is calculated to be 5 and the cost is 1.56 in the same way. In the refill tube of Experimental Example 3, the total cost at the end of its life is 5.41.

From these results, it can be seen that the number of times that can be used increases by using the refill tube divided in the axial direction, and as a result, the cost of refilling can be reduced.

In addition, when the number of times of using the refill tube of Experimental Example 1 increases, the displacement caused by the quartz powder from the inner surface of the refill tube can be significantly reduced in Experimental Examples 2 to 4 .

In addition, in Experimental Examples 2 to 4, the abnormality of the carbon concentration never occurred, and it was also confirmed that the mixing of fragments of the buffer member did not occur.

S1‧‧‧Solid raw material S2‧‧‧Raw material melt 1‧‧‧Main chamber 2‧‧‧Lifting chamber 2a‧‧‧Drive mechanism (lifting means) 3‧‧‧Crucible 4‧‧‧Support axis 4a‧‧‧Supporting device 5‧‧‧Heater 6‧‧‧Insulation material 7‧‧‧Pull shaft (lifting means) 8‧‧‧Suspended fixture (lifting means) 9‧‧‧Upper flange 9a‧‧‧Metal flange 10‧‧‧Refill tube 10A‧‧‧Lower side split tube (split tube) 10Aa‧‧‧upper end 10Ab‧‧‧Lower end 10B‧‧‧Upper side split tube (split tube) 10Ba‧‧‧upper end 10Bb‧‧‧Lower end 10C‧‧‧Added a split tube (split tube) 10D‧‧‧Middle side split tube (split tube) 11‧‧‧Connecting part 11a, 11b, 11m, 11n‧‧‧Flange 11c‧‧‧Connecting hole 11d‧‧‧Screw, nut (locking part) 11e‧‧‧Cushioning member 11g‧‧‧Mosaic groove 11h‧‧‧Mosaic groove 12‧‧‧Heat shielding body 13‧‧‧Gate valve 14‧‧‧Bottom cover 15‧‧‧Metal shaft (lifting means) 16‧‧‧Protection tube (lifting means) 16a‧‧‧Sliding protection tube 16b‧‧‧Coated protection tube 16c‧‧‧Fixed plate 16f‧‧‧Fixed inclined plate 18‧‧‧Hanger 19‧‧‧Metal washer 20‧‧‧Metal upper part 21‧‧‧Long screw 30‧‧‧Tilt support table 31‧‧‧Support Desk 32‧‧‧Support Trolley Department 33‧‧‧Wheels 34‧‧‧Tilt table 35‧‧‧Tilt Support 35a‧‧‧Horizontal axis 36‧‧‧Base 36a‧‧‧inclined part 37、38‧‧‧Axis 39‧‧‧Tilt Drive

Fig. 1 is a front cross-sectional view showing the first embodiment of the refill tube used in the raw material supply device of the present invention. Fig. 2 is an exploded perspective view showing the first embodiment of the refill tube of the present invention. Fig. 3 is an enlarged cross-sectional view showing the connecting portion of the divided pipe in the first embodiment of the refill pipe of the present invention. Fig. 4 is an enlarged front cross-sectional view showing the lower end side in the first embodiment of the refill tube used in the raw material supply device of the present invention. Fig. 5 is a plan sectional view showing the first embodiment of the refill tube used in the raw material supply device of the present invention. Fig. 6 is an enlarged front cross-sectional view showing the upper end side of the recharging pipe in the first embodiment of the recharging pipe used in the raw material supply device of the present invention in a state where the ascent of the recharging pipe is stopped. Fig. 7 is an enlarged front view showing the upper end side of the first embodiment of the refill tube used in the raw material supply device of the present invention, and is a state where the metal shaft is lowered and the bottom cover is opened. Fig. 8 is a plan view showing the metal upper member used on the upper end side in the first embodiment of the refill tube used in the raw material supply device of the present invention. Fig. 9 is a schematic diagram showing the filling step of the divided tube in the first embodiment of the refilling method of the present invention. Fig. 10 is a schematic diagram showing the filling step of the divided tube in the first embodiment of the refilling method of the present invention. Figure 11 is a schematic diagram showing the filling steps of the conventional refill tube. Figure 12 is a flowchart showing the first embodiment of the refilling method of the present invention. Fig. 13 is a schematic diagram showing the first embodiment of the single crystal pulling device equipped with the raw material supply device of the present invention. Fig. 14 is a schematic diagram showing the first embodiment of the single crystal pulling device equipped with the raw material supply device of the present invention. Fig. 15 is a schematic diagram showing the inclined support table in the second embodiment of the single crystal lifting device of the present invention. Fig. 16 is a schematic diagram showing the inclined support table in the second embodiment of the single crystal lifting device of the present invention. Fig. 17 is a schematic diagram showing the inclined support table in the second embodiment of the single crystal lifting device of the present invention. Fig. 18 is a schematic diagram showing the inclined support table in the second embodiment of the single crystal lifting device of the present invention. Figure 19 is a schematic cross-sectional view showing the third embodiment of the refill tube of the present invention. Fig. 20 is an enlarged cross-sectional view showing the split pipe connecting portion in the third embodiment of the refill pipe of the present invention. Fig. 21 is an exploded perspective view showing the third embodiment of the refill tube of the present invention. Fig. 22 is a schematic diagram showing the raw material supply device in the third embodiment of the single crystal pull-up device of the present invention. Fig. 23 is a schematic diagram showing the split pipe connecting portion in the fourth embodiment of the refill pipe of the present invention. Figure 24 is a schematic diagram showing the fifth embodiment of the refill tube of the present invention. Figure 25 is a schematic diagram showing the sixth embodiment of the refill tube of the present invention. Figure 26 is a schematic diagram showing the seventh embodiment of the refill tube of the present invention.

9‧‧‧Upper flange

10‧‧‧Refill tube

10A‧‧‧Lower side split tube (split tube)

10B‧‧‧Upper side split tube (split tube)

11‧‧‧Connecting part

11a, 11b‧‧‧Flange

11e‧‧‧Cushioning member

Claims (19)

A recharging tube used for the cultivation of single crystals in the Tchaikovsky method. It is used for the additional charging of granular solid raw materials or recharged into the raw material supply device in the raw material melt in the crucible. A cylindrical recharging tube comprising: a plurality of divided tubes which are divided in the axial direction when the solid raw material is filled; and a connecting part which connects the divided tubes up and down when the solid raw material is put into the crucible, wherein The connecting portion is provided with a flange portion extending to the outside in the radial direction, and a locking portion that locks this flange portion. In the connecting portion, the upper end of the divided pipe that is located at the lower side when connecting is connected to the upper end Fit the lower end of the divided pipe at the position. As for the refilling pipe described in item 1 of the scope of patent application, in the split pipe, the inner diameter of the upper end of the split pipe located at the lower side when connected is set to be equal to the inner diameter of the lower end of the split pipe located at the upper side. , Or larger than the inner diameter of the lower end of the divided pipe located at the upper side. For the refilling pipe described in item 1 of the scope of patent application, the inner diameter of the upper end of the split pipe will be set equal to the inner diameter of the lower end, or larger than the inner diameter of the lower end. As for the refilling pipe described in item 1 of the scope of patent application, the connecting portion is connected by abutting the upper end surface and the lower end surface of the divided pipe. As for the refilling pipe described in the first item of the scope of patent application, a buffer member is provided on the connecting portion where the upper side of the divided pipe and the lower side of the divided pipe are in contact with each other. For the refilling pipe described in item 5 of the scope of the patent application, the inner diameter of the buffer member is set to be equal to the inner diameter of the lower end of the divided pipe located at the upper side, or to be larger than the lower end of the divided pipe located at the upper side. Large inner diameter. The refill tube described in item 5 of the scope of patent application, wherein the split tube is composed of quartz, and the buffer member is composed of a flexible carbon-containing material. A raw material supply device, which is used for the cultivation of single crystals of the Tchaikrasky method, is a raw material supply device for additionally charging granular solid raw materials or recharging them into the raw material melt in the crucible, which includes : The reloading tube as described in any one of items 1 to 7 in the scope of the patent application; a conical bottom cover that can be detachably installed on the lower open end of the reloading tube; and a lifting means that can be suspended The recharge tube and the bottom cover are raised and lowered, and the lower open end of the recharge tube can be opened, and the solid raw material can be poured into the raw material melt in the crucible. A single crystal pulling device, which is bred from the raw material melt by the Tchaikrasky method, includes: the raw material supply device as described in item 8 of the scope of patent application; a furnace body with the crucible inside; heat The shielding body is arranged in the furnace body at the upper position of the crucible and is a cylindrical shape with a reduced inner circumference of the lower end, which is used to shield the radiant heat from the single crystal grown from the raw material melt. When recharging, insert the recharging tube into the inner side of the heat shield from above, and place the lower end of the recharging tube below the lower end of the heat shield, and put the solid raw material in this state The raw material melt in the crucible. The single crystal pulling device described in claim 9, wherein when the solid raw material is dropped into the raw material melt in the crucible, the connecting portion is set at a higher position than the lower end of the heat shield . The single crystal pulling device described in item 9 of the scope of patent application, wherein the outer side of the furnace body, when filling the solid raw material in the recharging tube, has an inclined support platform, wherein the inclined support platform is installed at the lower end The divided tube of the bottom cover is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is supported by the connecting portion to be able to connect the upper side. A method of using a refill tube, as described in any one of items 1 to 7 in the scope of the patent application, includes: only replacing the inner surface of the refill tube due to the filling of the solid raw material to a predetermined state Of the split tube. As described in Article 12 of the Patent Application Act, the method of using the refill tube is only in a state where there is no damage, because the filling of the solid raw material damages the inner surface and causes the transmission rate to be less than 70%. In this case, replace the split tube. As described in item 12 of the scope of patent application, the method of using the refill tube includes heating the inner surface of the split tube that was replaced due to damage to regenerate it. As described in item 14 of the scope of patent application, when the deformation of the split tube regenerated by heating exceeds a predetermined amount, it will no longer be used. A recharging method is a method of adding or recharging the raw material melt in the crucible in the single crystal pulling device described in item 9 of the scope of patent application, including: installing the lower end The divided tube of the bottom cover is inclined and supported, and the divided tube inclined with the filling of the solid raw material is erected on the vertical side, and the divided tube is connected to the upper side by the connecting portion, and then the solid raw material is filled . A recharging method is a method of additionally charging or recharging the raw material melt in the crucible in the single crystal pulling device described in item 11 of the scope of patent application, including: supporting by the tilt Stand, let the divided pipe with the bottom cover installed at the lower end be inclined and supported, and erect the divided pipe inclined with the filling of the solid raw material on the vertical side, and connect the divided pipe to the vertical side by the connecting part. The upper side is filled with the solid raw material. A recharging method is a method of adding or recharging the raw material melt in the crucible in the single crystal pulling device described in item 11 of the scope of patent application, including: additional charging or After the raw material melt is charged in the crucible, the inclined support platform supports the connected plural divided pipes so that they are inclined and connected by the Partly separate the dividing tube. A single crystal pulling method, by the recharging method as described in item 16 of the scope of patent application, after additional charging or recharging of the raw material melt in the crucible, incubate from the raw material melt Single crystal.

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