TW201435157A - Charging method, feedstock, and single-crystal manufacturing device - Google Patents

Abstract

The present invention provides a method for charging a crucible with a feedstock when using the Czochralski technique to manufacture a single-crystal sapphire. To manufacture said single-crystal sapphire, said method uses a single-crystal manufacturing device provided with the following: a heater that heats a feedstock inside a crucible a main chamber in which said crucible is placed and a pull chamber that is connected above the main chamber such that a gate valve can be used for partitioning. In this method, a charging tool holding the aforementioned feedstock is suspended from the pull chamber to charge the crucible with the feedstock. A method is thus provided in which the crucible can be charged with the feedstock efficiently without needing to turn off the power supply to the heater.

Description

Feeding method, raw material and single crystal manufacturing device

The present invention relates to a method of feeding a raw material into a crucible when manufacturing a sapphire single crystal.

In the manufacture of sapphire (oxide) single crystals, in addition to the mainstream Kyropoulos method, Bridgman method, edge defined film fed growth method (edge defined film fed growth method) In addition to the guide mold method (EFG method), various methods such as the Czochralski method (CZ method) are also used (see Patent Documents 1 and 2). Among these methods, although ruthenium can be reused, in the manufacture of the second single crystal, a step of temporarily turning off the heater power supply, cooling, feeding the raw material to the crucible again, and then heating it again is employed.

However, if the raw material is fed by this method, there is a problem that the productivity of the sapphire single crystal is lowered and the cost is increased due to the time required for cooling or reheating due to the shutdown of the heater power source.

[Advanced technical literature] (Patent Literature)

Patent Document 1: Japanese Laid-Open Patent Publication No. 2009-242150

Patent Document 2: Japanese Laid-Open Patent Publication No. 2011-195423

Patent Document 3: Japanese Patent Laid-Open Publication No. 9-25192

In the claims 8 and 9 of Patent Document 3, when the raw material for crystal growth is a powder, the raw material powder is formed into a rod shape by press working, and heated and melted to be filled in a crucible.

As described in the embodiment of the invention, a raw material for press processing is proposed as a measure for easily decomposing a powder material due to high temperature. The high-purity alumina of the sapphire single crystal raw material is not thermally decomposed by high temperature, but if the powdery raw material or the granular raw material is directly placed on the molten surface or the solidified surface of the melt surface layer, it is adsorbed in the raw material powder. Traces of moisture and gases will rapidly expand and produce the same thermal decomposition. Even if the degassing step is carried out by vacuum replacement in advance, it is not easy to completely remove moisture and gas.

Further, in Patent Document 3, when a rod-shaped press material is formed of a high-hardness alumina material and is melted from the lower side, a member corresponding to a crystal diameter control frame made of a high-melting-point metal is provided, and wear is caused by abrasion. This metal or dust enters the melt and prevents crystal growth.

Further, as shown in FIG. 3 of Patent Document 3, in order to immerse the tip end of the crystal diameter control frame in the melt, the powder having a bulk density smaller than the melt must be fed to a higher level than the melt level. The gas accumulated in the closed portion of the outer diameter of the control frame may not be removed.

As described above, in the past, in the production of a sapphire single crystal, a method of feeding a raw material to a crucible has not been efficiently performed.

The present invention has been made in view of the above problems, and an object thereof is to provide a method for efficiently feeding a raw material when a raw material is fed to a crucible, and it is not necessary to turn off the heater power supply in the production of the sapphire single crystal.

In order to achieve the above object, the present invention provides a feeding method for feeding a raw material into a crucible when a sapphire single crystal is produced by a CZ method, which is characterized in that a single crystal manufacturing apparatus is used as a manufacturing method. In the apparatus for sapphire single crystal, the single crystal manufacturing apparatus includes a heater that heats the raw material in the crucible, a main chamber in which the crucible is disposed, and a sub chamber that is separably connected to the main chamber by a gate valve (lifting A pull chamber is used, and at the time of feeding the aforementioned raw materials, the feeder for holding the aforementioned raw materials is suspended from the sub-chamber, and the raw material is fed into the crucible.

As such, by using a sub-chamber that is separably connected by a gate valve, by feeding the raw material by feeding the feeder, it is possible to turn off the heater power supply without the feeder or the raw material being contacted. The way of the parts in the furnace, the raw materials are efficiently fed. That is to say, if there is a gate valve, after the raw material is fed, the heater is not turned off, but the gate valve is closed, the feeder is removed (removed), then the gate valve is opened and the single crystal is pulled.

In this case, it is preferable to use a resistance heating heater as the heater, and to use tungsten or molybdenum as a main component or a metal crucible containing both tungsten and molybdenum as a main component.

By using a device having such a heater and crucible, the cost of crucible can be reduced.

At this time, it is preferable to have a stopper at the lower end. A shaft or a wire is used as the aforementioned feeder, and a pellet material provided with a hole is used as the aforementioned raw material, and the aforementioned shaft or cable is passed through the aforementioned hole and the stopper at the lower end is used. Locking is performed whereby a plurality of the aforementioned sheet materials are laminated and held.

In this manner, by using a sheet material having a large bulk density, a hole is further provided, and a layer is stacked and held for feeding, the raw material can be fed more efficiently. Further, in the case of a sheet material, the weight of the feed can be easily adjusted.

In this case, it is preferable that the sheet material or the sapphire substrate provided with the holes pass through the shaft or the cable and be locked by the stopper, and the setting is made on the locked sheet material or the sapphire substrate. The sheet material having the holes is laminated and held, wherein the aperture of the locked sheet material or the sapphire substrate has a smaller aperture than the stopper of the lower end of the shaft or the cable, and the plurality of layers are held and held The aperture of the sheet-like material has a larger aperture than the aforementioned stopper.

By holding in this manner, a plurality of sheet materials can be held in a simple structure, and the raw material can be fed more efficiently.

In this case, it is preferable that the plurality of sheet materials held by the shaft or the cable are placed above the crucible, and the sheet material or the sapphire substrate located at the lower end of the stopper is locked. The laminated sheet material is fed into the aforementioned crucible.

By feeding in this manner, the sheet material and the sapphire substrate at the lower end can be further immersed in the melt directly above the melt, and the raw material can be fed safely and efficiently.

In this case, it is preferable to set the stopper of the aforementioned shaft or the cable as a collar. The shape or the cone that expands below.

According to such a stopper, the sheet material and the sapphire substrate at the lower end can be surely locked, and a plurality of sheet materials can be safely laminated and held.

In this case, it is preferable that the shaft or the steel wire is made of tungsten, molybdenum, niobium, or two or more of these metals.

In the case of such a material, the shaft or the steel wire is not melted by the high temperature, and further, since it can be made of the same material as the crucible, there is no fear that the molten metal will be contaminated even when the shaft or the steel cord contacts the molten metal.

In this case, it is preferable that the sub chamber is provided with a device capable of performing vacuum replacement and gas replacement.

In the case of such a sub-chamber, after the raw material is placed in the feeder, the sub-chamber can be set to the same furnace condition as the main chamber, and the heater power supply can be turned off, and the feed can be more efficiently.

In this case, it is preferable to suspend the shaft or the cable which holds the sheet material by a single wire pulling shaft of a wire type or a shaft type.

Thereby, the feeder can be used with almost no need to modify the single crystal manufacturing apparatus of the CZ method, and the cost can be further reduced.

Further, the present invention provides a raw material which is fed into a crucible when a sapphire single crystal is produced, and is characterized in that it is a sheet-like material provided with a hole.

In the case of such a sheet-like material, the bulk density is higher than that of the powdery or granular raw material, and the feed efficiency is good because the amount of the raw material that can be fed per feed can be increased. In addition, there is no such thing as scattering of raw material powder during feeding, and it can be easily adjusted by adjusting the thickness and outer diameter of the sheet material. The amount of raw material.

Moreover, the present invention provides a single crystal manufacturing apparatus which produces a sapphire single crystal from a melt obtained by heating a molten raw material in a crucible by a CZ method, and the single crystal manufacturing apparatus includes a heater that heats the crucible a raw material; a main chamber configured with the foregoing enthalpy; a sub-chamber that is separably connected to the main chamber by a gate valve; and a feeder that feeds the raw material into the crucible, The aforementioned raw materials are maintained and suspended from the aforementioned sub-chamber.

In the case of such a single crystal manufacturing apparatus, by feeding the raw material by feeding the feeder, it is possible to efficiently feed the raw material without turning off the power of the heater and the feeder or the raw material does not contact the parts in the furnace. Feeding.

At this time, it is preferable that the aforementioned feeder is a shaft or a cable having a stopper at the lower end.

In the case of such a stopper, the raw material can be surely held in a suspended state, and it becomes a device capable of carrying out a safe raw material feed.

At this time, it is preferable that the stopper of the aforementioned shaft or the cable is a taper shape or a taper which is developed downward.

In the case of such a stopper, the raw material can be surely locked, and it becomes a device which can hold the raw material safely.

In this case, it is preferable that the shaft or the wire is made of tungsten, molybdenum, niobium or two or more of these metals.

In the case of such a material, the shaft or the steel wire is not melted by the high temperature, and further, since it can be made of the same material as the crucible, there is no fear that the molten metal will be contaminated even when the shaft or the steel cord contacts the molten metal.

As described above, according to the present invention, in the manufacture of a sapphire single crystal, The heater power needs to be turned off, and the raw material can be efficiently fed.

10‧‧‧Single crystal manufacturing equipment

11‧‧‧ main chamber

12‧‧‧ gate valve

13‧‧‧Sub-chamber

14‧‧‧坩埚

15‧‧‧ melt

16‧‧‧Insulation materials

17‧‧‧ single crystal

18‧‧‧Graphite holder

19‧‧‧坩埚 Support shaft

20‧‧‧Tip shaft

21‧‧‧ seed chuck

22‧‧‧heater

23‧‧‧ feeder

24, 24', 24", 24'''‧‧‧ raw materials (sheet material)

25‧‧‧ shaft or cable

26, 26' ‧ ‧ stop

27‧‧‧ Raw materials

28‧‧‧Expanding section

29, 29’ ‧ ‧ holes

30‧‧‧Sapphire substrate

31‧‧‧ gas introduction tube

32‧‧‧ gas discharge pipe

33‧‧‧Valve components

34‧‧‧Refeed tube

35‧‧‧vacuum pump

36‧‧‧Gas discharge pipe for subchamber

Fig. 1 is a schematic view showing an example of a single crystal production apparatus of the present invention.

Fig. 2 is a schematic view showing an example of a state in which a raw material is fed in the single crystal production apparatus of the present invention.

Fig. 3(a) is a schematic view showing an example of a sheet material which can be used in the present invention, and Fig. 3(b) is a schematic view showing an example of a sheet material provided with a hole.

Fig. 4 is a schematic view showing a state in which a sheet material is held in the present invention.

Fig. 5(a) is a schematic view showing another example of the shaft in the present invention, and Fig. 5(b) is a schematic view showing another example of the sheet material in which the holes are provided.

Figure 6 is a flow chart showing the feeding of raw materials in accordance with the present invention.

Fig. 7 is a schematic view showing another example of a state in which a raw material is fed in the single crystal production apparatus of the present invention.

Hereinafter, the present invention will be described in detail with reference to the drawings as an example of the embodiments, but the present invention is not limited to the embodiments.

Fig. 1 is a schematic view showing an example of a state in single crystal growth in the single crystal production apparatus of the present invention. Fig. 2 is a schematic view showing an example of a state in which a raw material is fed in the single crystal production apparatus of the present invention.

The single crystal manufacturing apparatus 10 of the present invention in Fig. 1 is a device for producing a sapphire single crystal 17 by pulling a molten metal 15 obtained by heating a molten raw material in a crucible 14 by a CZ method.

The single crystal manufacturing apparatus 10 of the present invention includes a heater 22 that heats the raw material in the crucible 14, a main chamber 11 in which the crucible 14 is disposed, and a sub chamber 13 that is partitionably connected to the main chamber 11 by the gate valve 12.

Further, as shown in Fig. 2, the single crystal manufacturing apparatus 10 of the present invention is provided with a feeder 23 which holds the raw material 24 when the raw material 24 is fed into the crucible 14, and can be supplied from the sub chamber. 13 hang down.

With such a device 10, in the present invention, as shown in Fig. 2, in the feed of the raw material 24, the feeder 23 holding the raw material 24 is suspended from the sub-chamber 13, and the raw material 24 is turned toward the crucible 14. Internal feed.

After the raw material which has been initially filled in the crucible is melted, in order to maintain the molten metal at a predetermined amount, the raw material is additionally fed by the addition, or the molten metal which is reduced after the pulling of the single crystal is added. When the raw material is fed to the crucible feed, in the past, the heater power is turned off, cooled, the raw material is fed, heated, and melted. However, such a feeding method takes too much time and cost, and has a significant influence on the manufacturing cost and productivity of the sapphire single crystal.

The apparatus 10 of the present invention has the sub-chamber 13 which is separably connected by the gate valve 12, and the raw material 24 is fed by suspending the feeder 23, so that it is possible to turn off the heater power supply without The feeder 23 and the raw material 24 are fed into the raw material 24 efficiently without contacting the parts in the furnace. That is, if the gate valve 12 is provided, after the raw material is fed, the heater power supply is not turned off, the gate valve 12 is closed, the feeder 23 is removed (removed), and then the gate valve 12 is opened and the single crystal 17 is pulled. . Further, in order to hang the raw material, the diameter of the opening portion of the upper portion of the heat insulating material 16 for feeding can be minimized, since it can be discharged from the hot region. The heat release is reduced, so that the raw material feed can be efficiently performed.

Further, the apparatus 10 includes a heat insulating material 16 made of carbon surrounding the crucible 14 and the heater 22, a pulling shaft 20 for pulling up the single crystal 17, a seed chuck 21 for holding the seed crystal, and a support crucible 14. The graphite holder 18 and the support shaft 19 supporting the crucible 14 via the graphite holder 18 are interposed. Further, in the upper portion of the heat insulating material 16, there may be an enlarged diameter portion 28, wherein the enlarged diameter portion 28 is, for example, detachable or movable to enlarge the diameter of the opening portion at the time of feeding, so that the feeder 23 can Pass through the opening.

Further, it is preferable to use a resistance heating heater as such a heater 22, and it is preferable to use a metal crucible containing tungsten or molybdenum as a main component or mainly composed of tungsten and molybdenum as the crucible 14.

Although a high frequency heat generating heater can be used as the heater 22 of the apparatus 10 of the present invention, and 铱坩埚 can also be used as the crucible 14, in the present invention, it is preferable to use the inexpensive one as described above. A metal crucible containing tungsten and/or molybdenum as a main component. In this case, since the oxidation resistance is lower than that of ruthenium, a carbon heat insulating material 16 is used. Since carbon is a good conductor, the use of the high frequency heating method is inferior in thermal efficiency, and thus it is inevitable that it will go. Use a resistance heating heater.

Further, as shown in Fig. 1, the single crystal manufacturing apparatus 10 preferably includes a device capable of performing vacuum replacement and gas replacement (the gas introduction pipe 31, the gas discharge pipe 32, and the vacuum pump 35). For example, when a single crystal is grown or the like, an inert gas or the like may be introduced into the furnace through the gas introduction pipe 31 from above the sub chamber 13, or the introduced gas may be taken from the main chamber by a vacuum pump 35 or the like. The gas discharge pipe 32 at the bottom of the 11 is discharged to the outside of the furnace. On the other hand, let the feeder When the raw material 24 is held or the raw material 24 is fed to the crucible 14, and the feeder 23 is taken out, the operation can be performed by closing the gate valve 12 and in the sub-chamber 13, and then using the sub-chamber. The gas discharge pipe 36 for the chamber and the gas introduction pipe 31 exchange gas in the sub-chamber 13, and the sub-chamber 13 is made into the same furnace condition as the main chamber 11, and then the gate valve 12 is opened, thereby not closing. With the power supply, the single crystal growth step can be continued.

Fig. 3(a) shows a plan view and a side view of the sheet material, and Fig. 3(b) shows a plan view and a side view of the sheet material provided with the holes.

As shown in Fig. 2, in the present invention, it is preferable that the shaft or the cable 25 having the stopper 26 at the lower end is used as the feeder 23, and the sheet material 24 provided with the holes 29 is used as a raw material, and A plurality of sheet materials 24 are laminated and held by the stopper 26 which passes the shaft or the cable 25 through the hole 29 and at the lower end. In this case, it is preferable to set the material of the stopper 26 to be the same as that of the shaft or the cable 25, and to set the stopper 26 to be tungsten, molybdenum, niobium, or two or more of these metals. Formed.

As described above, in the present invention, the holes 29 can be provided as shown in Fig. 3(b) on the sheet material 24' of alumina which is commercially available as shown in Fig. 3(a).

If the sheet material 24 provided with such a hole 29 is high in bulk density, if it is laminated, the apparent bulk density (also called apparent density) is almost the same as the density of sapphire crystal, and is efficient. Ground feed. In particular, although the additional weight varies depending on the crystal weight of the pulling at the time of refeeding, the predetermined weight can be easily adjusted by adjusting the thickness and the outer diameter of the sheet material. On the other hand, even if it is used as in Patent Document 3 It is also possible to add a feed structure in advance to the rod-shaped raw material prepared in advance, and it is also difficult to adjust the weight or the like arbitrarily.

Here, when the single crystal manufacturing apparatus 10 is fed, if the outer diameter of the opening above the heat insulating material 16 through which the sheet material 24 passes is increased, heat dissipation becomes large, and thus the sheet material 24 is formed. The outer diameter of the single crystal 17 is preferably not much larger than the crystal diameter of the single crystal 17 to be pulled. In that case, if the single crystal having a diameter of 110 mm is to be pulled, since the outer diameter of the opening portion of the heat insulating material 16 needs to be 130 to 140 mm, the outer diameter of the sheet material 24 may be about 110 to 130 mm, and When the thickness is about 10 to 30 mm, the handling is easy. Further, in the case where the diameter-enlarged portion 28 is provided, the diameter of the expanded diameter can be considered together and the outer diameter of the sheet-like material 24 can be set.

Further, although the hole diameter of the hole 29 is as small as possible, in order to be able to fall smoothly, a diameter of about 20 mm is most suitable.

Further, as shown in Fig. 3(a), for example, in the center of the sheet material 24' of alumina having a diameter of 100 mm × a thickness of 10 mm and a bulk density of 3.2 g/cm ³ , as shown in the third (b) In the case of a hole 29 of 20 mm in diameter, the weight will be reduced from 303.9 g to 293.9 g. In this case, the apparent bulk density becomes 3.1 g/cm ³ , which is almost the same as the sheet material 24' before opening the void, and is 1.2 to 2.3 g/cm ³ compared with the powdery raw material or the granular raw material. , a considerable bulk density can be obtained, and the raw material can be efficiently added.

Fig. 4 is a schematic view showing two examples of the state in which the sheet material 24' is held.

In the present invention, it is preferred that the sheet material 24" (Fig. 4(a)) or the sapphire substrate 30 (Fig. 4(b)) provided with the holes 29 pass through the shaft or steel. The cable 25 is locked by the stopper 26, and on the locked sheet material 24" or the sapphire substrate 30, the sheet material 24' provided with the holes 29 is laminated and held; wherein the card is held The aperture of the sheet material 24" or the aperture 29 of the sapphire substrate 30 is smaller than the width (width) of the stopper 26 at the lower end of the shaft or cable 25, and the plurality of apertures 29 of the sheet material 24' are held and held. The aperture is larger than the amplitude (width) of the stopper 26.

Thereby, the sheet material can be surely held with a simple configuration.

Fig. 5(a) is a schematic view showing an example of a shaft, and Fig. 5(b) is a plan view and a side view showing a sheet material stuck to the lower end of the shaft.

The shaft or cable 25 is preferably a collar 26 having a collar shape (Fig. 4) or a tapered stopper 26' (Fig. 5(a)).

In the case of such a stopper, the raw material can be surely locked, and the raw material can be safely held.

If it is a stopper 26' having a taper which is unfolded downward as shown in Fig. 5(a), it is preferable to provide a conical hole 29' which is expanded downward as shown in Fig. 5(b). The sheet material 24"" is locked to the lower end of the shaft or cable 25.

Thereby, the holding can be performed more stably.

The shaft or cable 25 is preferably made of tungsten, molybdenum, niobium or two or more of these metals.

If it is such a material, the shaft or the cable 25 is not melted by the heater heating to a high temperature, and further, since it is made of the same material as the crucible 14, the melt can be prevented even when the shaft or the cable 25 contacts the melt 15. 15 is contaminated.

Further, it is preferable to suspend the shaft or the cable 25 holding the sheet material 24 by the single-wire pulling shaft 20 (Fig. 1) of the steel cable method or the shaft type.

With the seed chuck 21 that holds the shaft or cable 25 of the sheet material 24 to the front end of the pulling shaft 20, for example, it can be kept stable and suspended; in addition, since no special modification is required to the single crystal manufacturing apparatus The feed of the present invention can be carried out, and is therefore also preferable from the viewpoint of cost.

As shown in Fig. 2, it is preferable to use a device 10 in which a plurality of sheet materials 24 held by a shaft or a cable 25 are placed above the crucible 14, and the sheet at the lower end which is locked by the stopper 26 is melted. The material 24" or the sapphire substrate 30 (see Fig. 4) is used to feed the laminated sheet material 24' into the crucible 14.

In the above method of laminating the sheet material and further melting the sheet material 24" or the sapphire substrate 30 to be fed, since the sheet material is high, the filling rate is high, and further, there is no fear that the raw material powder is scattered or Blowing up. At this time, the sheet material 24" or the sapphire substrate 30 stuck at the lower end can be lowered to a position where it can be melted to melt it, for example, to a position lower than the upper end of the crucible 14 (melt 15) Just above it). Alternatively, the lower sheet material 24" or the sapphire substrate 30 may be immersed in the melt 15. The sheet material 24" or the sapphire substrate 30 which is the lower end of the hole 29 is melted thereon. The sheet material 24' provided with the holes 29 having a larger diameter than the diameter of the stopper 26 is sequentially dropped into the crucible 14 to complete the feeding.

As described above, after the raw material is fed, for example, in the flow chart shown in Fig. 6, the raw material can be heated to be melted into a molten metal, and the sapphire single crystal can be pulled from the molten metal.

In addition to the above, although the method of feeding the sheet material in the state of laminating is described above, in the apparatus having the gate valve of the present invention, for example, as shown in FIG. 7, it is possible to use granular or Powdered raw material 27 is filled in re-feed The tube 34 is suspended and opened, and a conical valve member 33 is opened to feed the raw material 27.

In this case, the raw material can also be fed without turning off the heater power.

According to the present invention as described above, it is possible to efficiently feed, and further, since there is no need to turn off the power of the heater for feeding, the productivity of the production of the sapphire single crystal can be improved or the cost can be reduced.

Hereinafter, the invention will be more specifically described by way of examples, but the invention is not limited thereto.

(Example)

After the sapphire single crystal was grown using the single crystal production apparatus shown in Fig. 1, the raw material was additionally fed by the method shown in Fig. 2 .

First, an alumina raw material powder having an initial feed amount of 15 kg is filled in a molybdenum crucible having an inner diameter of 230 mm and a height of 200 mm so that the alumina raw material powder and the upper end surface of the crucible are almost equal, and heated by a resistance heating heater. Melt. Next, a sapphire single crystal having an outer diameter of 110 mm was pulled up to 250 mm to obtain about 9.5 kg of crystals.

After the crystal grows, the upper portion (expanded diameter portion) of the heat insulating material is pulled together, the gate valve is closed, and the gate valve is taken out from the sub chamber, and then the donut-shaped sheet material holding the alumina is additionally fed. The molybdenum shaft is disposed on the pulling shaft, and replaces the gas in the auxiliary chamber, opens the gate valve, and lowers the molybdenum shaft for additional feeding from the auxiliary chamber, and additionally feeds into the remaining melt. In this case, if a plurality of sheet-like materials having an outer diameter of 110 mm having an inner diameter of 20 mm are passed through the shaft and held, the total laminated height of the sheet material becomes 323 mm, due to the single crystal which becomes thinner than the pulling It is also 73 mm high, so that the same amount of raw material as the crystal of the pulling can be added at a time. And this height is from the structure of the single crystal manufacturing device. Create a size that will not cause problems.

In the above embodiment, after the single crystal is pulled, the additional feed of the raw material is carried out, and the heating of the raw material is not performed, and the heater power supply is not turned off. Further, since the sheet material having a high bulk density is used as described above, the raw material having a reduced amount of the melt can be placed in one feed.

Further, in order to efficiently grow the crystal, it is necessary to increase the amount of the raw material melt to be fed, and to increase the cultivation weight of each of the cultivated crystals. However, since the bulk density of the raw material powder is small, etc. After the entire amount of the material is melted, the height of the melt is still reduced by 30 to 40%, and the volume of the crucible cannot be utilized efficiently enough. However, according to the present invention, the upper limit of the initial feed amount is 16 kg, and it is possible to further add 3 to 4 kg of feed without turning off the heater power supply, and the total feed amount can be increased to about 20 kg, so that it can be effectively utilized. The volume inside the raft.

Furthermore, the present invention is not limited to the above embodiment. The above-described embodiments are exemplified, and all the inventions having substantially the same configuration as the technical idea described in the claims of the present invention and exhibiting the same effects are included in the technical scope of the present invention.

10‧‧‧Single crystal manufacturing equipment

11‧‧‧ main chamber

12‧‧‧ gate valve

13‧‧‧Sub-chamber

14‧‧‧坩埚

15‧‧‧ melt

16‧‧‧Insulation materials

17‧‧‧ single crystal

18‧‧‧Graphite holder

19‧‧‧坩埚 Support shaft

20‧‧‧Tip shaft

21‧‧‧ seed chuck

22‧‧‧heater

28‧‧‧Expanding section

31‧‧‧ gas introduction tube

32‧‧‧ gas discharge pipe

35‧‧‧vacuum pump

36‧‧‧Gas discharge pipe for subchamber

Claims (20)

A feeding method for feeding a raw material into a crucible when a sapphire single crystal is produced by a CZ method, characterized in that a single crystal manufacturing apparatus is used as a device for manufacturing the aforementioned sapphire single crystal, The single crystal manufacturing apparatus includes a heater that heats the raw material in the crucible, a main chamber in which the crucible is disposed, and a sub chamber that is separably connected to the main chamber by a gate valve, and when the raw material is fed The feeder for holding the aforementioned raw materials is suspended from the aforementioned sub-chamber, and the raw material is fed into the aforementioned crucible. The feeding method according to claim 1, wherein a resistance heating heater is used as the heater, and a metal crucible containing tungsten or molybdenum as a main component or mainly composed of tungsten and molybdenum is used as the crucible. . The feeding method according to claim 1, wherein a shaft or a cable having a stopper at a lower end is used as the feeder, and a sheet material provided with a hole is used as the raw material, and the shaft or the shaft is The wire passes through the aforementioned hole and is locked by the stopper at the lower end, whereby a plurality of the aforementioned sheet materials are laminated and held. The feeding method according to claim 2, wherein a shaft or a steel wire having a stopper at a lower end is used as the aforementioned feeder, and a sheet material provided with a hole is used as the aforementioned raw material, and the aforementioned shaft or The wire passes through the aforementioned hole and is locked by the stopper at the lower end, thereby laminating a plurality of the aforementioned sheet materials and Keep it. The feeding method according to claim 3, wherein the sheet material or the sapphire substrate provided with the holes is passed through the aforementioned shaft or cable and locked by the stopper, and the sheet material or the stuck material is On the sapphire substrate, the plurality of sheet materials provided with the holes are laminated and held, wherein the aperture of the locked sheet material or the sapphire substrate has a smaller aperture than the stopper of the lower end of the shaft or the cable, The aperture of the plurality of laminated and held sheet-like materials has a larger aperture than the aforementioned stopper. The feeding method according to claim 4, wherein the sheet material or the sapphire substrate provided with the holes is passed through the aforementioned shaft or cable and locked by the stopper, and the sheet material or On the sapphire substrate, the plurality of sheet materials provided with the holes are laminated and held, wherein the aperture of the locked sheet material or the sapphire substrate has a smaller aperture than the stopper of the lower end of the shaft or the cable, The aperture of the plurality of laminated and held sheet-like materials has a larger aperture than the aforementioned stopper. The feeding method according to claim 3, wherein the plurality of sheet materials held by the shaft or the cable are placed above the crucible, and the sheet material located at the lower end of the stopper with the stopper is melted. Or a sapphire substrate, wherein the laminated sheet material is fed into the aforementioned crucible. The feeding method according to claim 6, wherein the plurality of sheet materials held by the shaft or the cable are placed above the crucible, and the melting is located at the front The sheet material or the sapphire substrate at the lower end of the stopper is locked, and the laminated sheet material is fed into the crucible. The feeding method according to claim 3, wherein the stopper of the shaft or the cable is set to a collar shape or a taper which is developed downward. The feeding method according to claim 8, wherein the stopper of the shaft or the cable is set to a collar shape or a taper which is developed downward. The feeding method according to claim 3, wherein the shaft or the steel wire is made of tungsten, molybdenum, niobium or two or more of these metals. The feeding method according to claim 10, wherein the shaft or the steel wire is made of tungsten, molybdenum, niobium or two or more of these metals. The feeding method according to any one of claims 1 to 12, wherein the sub chamber is provided with a device capable of performing vacuum replacement and gas replacement. The feeding method according to any one of claims 3 to 12, wherein the shaft or the wire rope holding the sheet material is suspended by a single wire pulling shaft of a wire rope method or a shaft type. The feeding method according to claim 13, wherein the aforementioned shaft or steel for holding the sheet material is retained by a single wire pulling shaft of a wire rope method or a shaft type Suspension down. A raw material, which is fed into a crucible when the sapphire single crystal is produced, is characterized in that it is a sheet-like material provided with pores. A single crystal manufacturing apparatus for producing a sapphire single crystal from a melt obtained by heating a molten raw material in a crucible by a CZ method, the single crystal manufacturing apparatus comprising: a heater for heating a raw material in the crucible; a chamber configured with the foregoing enthalpy; a sub-chamber that is separably coupled to the main chamber by a gate valve; and a feeder that holds the aforementioned raw material while feeding the raw material into the crucible Suspended from the aforementioned sub-chamber. The single crystal manufacturing apparatus according to claim 17, wherein the feeder is a shaft or a cable having a stopper at a lower end. The single crystal manufacturing apparatus according to claim 18, wherein the stopper of the shaft or the cable is a collar shape or a taper which is developed downward. The single crystal manufacturing apparatus according to claim 18 or 19, wherein the shaft or the steel wire is formed of tungsten, molybdenum, niobium or two or more of these metals.