JP2007284320A - Solid melting apparatus and method for feeding raw material - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus and a method for shortening the melting time of a solid raw material fed additionally. <P>SOLUTION: The apparatus and the method for shortening the melting time of a silicon raw material fed additionally comprise changing the silicon mass in a crucible 1 into a perfectly molten state, thereafter filling a granular silicon raw material in a raw material holding part 6a in a raw material feeding section 6, then feeding it onto a silicon molten liquid 2 in the crucible 1; and blowing an inert gas by means of an inert gas blowing part 7 onto the silicon raw material floating in a mass state on the central part of the surface of the silicon molten liquid 2 to thereby scatter the above massive silicon raw material toward the side wall of the crucible 1; and moreover continuing to blow the inert gas onto the surface of the silicon molten liquid 2 with shaking the surface of the silicon molten liquid 2 and with leveling down the silicon raw material of a chevron shape; consequently shortening the melting time of the additionally fed silicon raw material with increasing a contact surface between the additionally fed silicon raw material and the silicon molten liquid 2. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a solid melting apparatus that additionally supplies a solid raw material to a raw material that has been melted in a crucible, and a method for supplying the raw material to the solid melting apparatus.

  Conventionally, there are CZ method (Czochralski method), FZ method (Floating Zone method), casting method and the like as a method for melting and further recrystallizing a silicon raw material as a solid raw material. Further, as a method for directly producing a plate-like silicon, there are an EFG method (Edge-defined Film-fed. Growth method), a dendritic web method, and the like.

  In order to increase the production efficiency at the time of recrystallization, it is desirable to continuously perform recrystallization, and for this purpose, it is necessary to additionally supply a silicon raw material or a silicon melt while holding the silicon melt. However, when a certain amount of the silicon raw material at room temperature is supplied to the silicon melt, the silicon raw material floats on the silicon melt. For this reason, the temperature of the silicon melt partially decreases, or the floating silicon raw material comes into physical contact with the recrystallized silicon crystal, which adversely affects the shape and quality of the recrystallized silicon crystal. I will.

  In addition, when the silicon melt is added, recrystallization is affected by a temperature difference or a concentration difference.

  By the way, as a method of additionally supplying raw materials at the time of recrystallization, there are a method of simultaneously performing recrystallization and addition of raw materials and a method of additionally supplying a reduced amount of silicon raw material after a certain amount of recrystallization. .

  As a method for simultaneously performing the former recrystallization and raw material addition, there is a continuous CZ method using a double crucible structure. However, in order to prevent the influence of adding the raw material to the recrystallized silicon crystal, a complicated apparatus structure and a high degree of control associated therewith are required such as double crucibles.

  On the other hand, in the latter method in which recrystallization and addition of raw materials are performed separately, a reduction in time required for addition of raw materials is required in order to improve productivity. As a method for shortening the raw material addition time, it is also applied to the continuous CZ method. For example, as in “Single crystal pulling apparatus and pulling method” disclosed in JP-A-6-183876 (Patent Document 1), As in the method of melting or heating the raw material in advance or the “silicon single crystal growth method” disclosed in JP-A-10-279391 (Patent Document 2), a magnetic field is applied to the silicon raw material to There is a method of promoting stirring.

  However, the method of separately performing recrystallization and addition of raw materials when additional raw materials are supplied during the conventional recrystallization has the following problems.

  That is, the “single crystal pulling apparatus and pulling method” disclosed in Patent Document 1 has a problem that another heating apparatus is required in addition to the heating apparatus that heats the crucible. In addition, in the “silicon single crystal growth method” disclosed in Patent Document 2, a device for applying a magnetic field to the crucible and the melt in the crucible is required in addition to the device for heating the crucible. Therefore, there is a problem that the structure of the recrystallization apparatus for silicon material becomes complicated and the cost of the recrystallization apparatus increases.

  If recrystallization and addition of raw materials are not performed at the same time, the dropping position when adding the silicon raw material into the silicon melt is the crucible considering the scattering of the silicon melt and the silicon raw material itself. The central part is chosen.

  By the way, when heating the crucible holding the silicon melt, a method of heating the side wall side of the crucible including the above-mentioned Patent Document 1 and Patent Document 2 is often employed. This is because it is difficult to dispose a heating device on the upper surface side of the crucible in order to take out silicon crystals, and it is necessary to provide a mechanism for supporting, raising and lowering and rotating the crucible on the lower surface side of the crucible. This is because it is difficult. When the crucible is heated from the side wall, the temperature of the silicon melt in the crucible is higher on the side wall and lower in the center.

As mentioned above, when the crucible central part is selected as the silicon raw material dropping position, the silicon raw material will be added to the low temperature central part, and it takes time to melt the silicon raw material, In continuous production, there is also a problem that production efficiency decreases.
Japanese Patent Laid-Open No. 6-183876 JP-A-10-279391

  Therefore, the object of the present invention is to provide a low-cost solid melting apparatus capable of improving the production efficiency in recrystallization by shortening the melting time of the additionally supplied solid raw material, and the raw material supply to the solid melting apparatus It is to provide a method.

In order to solve the above problems, the solid melting apparatus of the present invention is:
A crucible for melting the charged solid raw material and holding the molten melt,
A raw material supply unit for additionally supplying the solid raw material into the crucible;
An inert gas spraying unit for spraying an inert gas to the additionally supplied solid raw material floating on the surface of the melt in the crucible is provided.

  According to the above configuration, the side wall of the crucible is supplied by the inert gas sprayed from the inert gas spraying section by the additional feedstock additionally supplied by the raw material supply section and floating on the surface of the melt in the crucible. It will be distributed around. In that case, since the side wall of the crucible is heated by a heating device, the melt in the crucible has a higher temperature around the side wall than at the center.

  Therefore, the additional feed material dispersed around the side wall of the crucible is quickly melted by the melt having a higher temperature than the central portion. As a result, the melting time of the additionally supplied solid raw material can be shortened, and the production efficiency in recrystallization can be improved.

  Furthermore, according to the present invention, it is only necessary to provide the inert gas spraying section, a heating device other than the heating device for heating the crucible, a device for applying a magnetic field to the crucible and the melt in the crucible, and the like. Do not need. Therefore, the solid melting apparatus can be provided at low cost.

  The “inert gas” referred to here is a gas that does not cause a chemical reaction with the solid raw material and its melt.

In the solid melting apparatus of one embodiment,
The raw material supply unit
A raw material holding unit for holding additional feed materials;
A transport unit that transports the raw material holding unit to a position directly above the melt in the crucible;
A tilting section for tilting the raw material holding section and dropping the additional feedstock into the crucible.

  According to this embodiment, when the solid raw material is additionally supplied into the crucible, the raw material holding unit holding the additional supply raw material is transported by the transporting unit to just above the melt in the crucible. Further, by tilting by the tilting part, the additional feed material in the raw material holding part can be reliably and quickly dropped into the crucible.

In the solid melting apparatus of one embodiment,
The inert gas blowing part has an inert gas outlet for blowing out the inert gas,
The inert gas outlet is provided at a position that tilts in conjunction with the raw material holding part or the raw material holding part.

  According to this embodiment, since the inert gas outlet of the inert gas spraying part is provided at a position that tilts in conjunction with the raw material holding part or the raw material holding part, the raw material holding part is tilted. When the additional feedstock is dropped into the crucible, the inert gas blowout port faces the additional feedstock floating on the melt in the crucible. The direction of the outlet can be set.

  In such a case, after dropping the additional feed material into the crucible, the inert gas spraying section is connected to the additional feed material in which the inert gas outlet is floating above the melt in the crucible. It is possible to save the time and effort to operate the camera.

In the solid melting apparatus of one embodiment,
The transport unit includes a pipe-like inert gas supply unit that constitutes a part of the inert gas blowing unit and has one end attached and fixed to the raw material holding unit and communicating with the inert gas outlet. Yes.

  According to this embodiment, the said conveyance part which conveys the said raw material holding part to just above the melt in the said crucible, and the said inert gas spraying part can be comprised integrally. Therefore, the configuration of the solid melting apparatus can be simplified.

In the solid melting apparatus of one embodiment,
The transport unit includes a moving device that moves the inert gas supply unit until the raw material holding unit attached to one end of the inert gas supply unit reaches directly above the melt in the crucible,
The tilting unit includes a rotating device that rotates the pipe-like inert gas supply unit around a central axis to tilt the raw material holding unit attached to one end of the inert gas supply unit. .

  According to this embodiment, by moving and rotating the inert gas supply unit by the moving device and the rotating device, the additional supply material held in the raw material holding unit can be easily put in the crucible. Can be dropped. Thereafter, the direction of the inert gas outlet is accurately corrected to be the direction of the additional feed by further moving and rotating the inert gas supply unit by the moving device and the rotating device. It becomes possible to do.

The raw material supply method of the present invention is
In the crucible holding a melt obtained by melting the charged solid raw material, the solid raw material is additionally supplied by the raw material supply unit,
An inert gas spraying unit sprays an inert gas on the additionally supplied solid raw material floating on the surface of the melt in the crucible, and the floating additional raw material is Dispersed around the side wall of the crucible.

  According to the above configuration, the solid additional feed material floating on the surface of the melt in the crucible is dispersed around the side wall of the crucible by the inert gas sprayed from the inert gas spraying section. In that case, since the side wall of the crucible is heated by a heating device, the melt in the crucible has a higher temperature around the side wall than at the center.

  Therefore, the additional feed material dispersed around the side wall of the crucible is quickly melted by the melt having a higher temperature than the central portion. As a result, the melting time of the additionally supplied solid raw material can be shortened, and the production efficiency in recrystallization can be improved.

In the raw material supply method of one embodiment,
After the floating additional feedstock is dispersed around the side wall of the crucible, an inert gas is subsequently sprayed onto the surface of the melt in the crucible by the inert gas spraying section, so that the melt Shake the surface to increase the contact area between the floating additional feed and the melt.

  According to this embodiment, the surface of the melt in the crucible is shaken to collapse the additional feedstock, and the contact area between the additional feedstock and the melt is increased. Therefore, the melting of the additional feedstock is further promoted, and the melting time of the additional feedstock is further shortened.

  As is apparent from the above, the solid melting apparatus of the present invention is not supplied to the solid raw material additionally supplied by the raw material supply unit and floating on the surface of the melt in the crucible by the inert gas blowing unit. Since the active gas is blown, the side wall of the crucible is heated by the heating device, so that the additional feed material is dispersed by the inert gas around the side wall of the crucible, which is at a higher temperature than the center of the crucible. Can do. Therefore, the additional feedstock can be quickly melted by the high-temperature melt around the side wall.

  That is, according to the present invention, the melting time of the additionally supplied solid raw material can be shortened, and the production efficiency in recrystallization can be improved. Further, it is only necessary to provide the inert gas spraying portion, and a heating device other than the heating device for heating the crucible, a device for applying a magnetic field to the crucible and the melt in the crucible, and the like are not required. Therefore, according to this invention, a solid melting apparatus can be provided at low cost.

  Furthermore, a conveying part for conveying the raw material holding part for holding the additional supply raw material to a position directly above the melt in the crucible constitutes a part of the inert gas blowing part, and one end is attached to the raw material holding part. If the pipe-shaped inert gas supply unit that is fixed and communicates with the inert gas outlet is included, the transfer unit and the inert gas blowing unit can be configured integrally. Therefore, the configuration of the solid melting apparatus can be simplified.

  Further, the raw material supply method of the present invention is an inert gas in which a solid additional supply material that is additionally supplied by the raw material supply unit and is floating on the surface of the melt in the crucible is sprayed from the inert gas spraying unit. Is distributed around the side wall of the crucible by the heating device, so that the side wall of the crucible is heated by a heating device, so that the dispersed additional liquid is melted by the melt around the side wall of the crucible. The feedstock can be quickly melted. Therefore, the melting time of the additionally supplied solid raw material can be shortened, and the production efficiency in recrystallization can be improved.

  Furthermore, after the floating additional feedstock is dispersed around the side wall of the crucible, an inert gas is subsequently sprayed onto the surface of the melt in the crucible by the inert gas spraying unit, so that the melt is melted. If the surface area of the liquid is shaken to increase the contact area between the floating additional feedstock and the melt, the melting of the additional feedstock is further promoted and the melting time of the additional feedstock is increased. Can be further shortened.

  Hereinafter, the present invention will be described in detail with reference to the illustrated embodiments. FIG. 1 is a schematic diagram showing the overall configuration of the solid melting apparatus of the present embodiment. Hereinafter, a case where the solid melting apparatus is applied to melting silicon will be described. However, the solid melting apparatus is not limited to silicon, and can be applied to melting a solid raw material having a higher liquid density than a solid.

  First, according to FIG. 1, the whole structure of this solid melting apparatus is demonstrated.

  In FIG. 1, 1 is a crucible, 2 is a silicon melt, 3 is a heater, 4 is a crucible base, 5 is a heat insulating material, 6 is a raw material supply section, and 7 is an inert gas blowing section. Needless to say, the crucible 1 must be formed of a material having sufficient heat resistance or coated with a material having sufficient heat resistance for other apparatuses.

  Since the raw material supply unit 6 and the inert gas spraying unit 7 require complicated processing for their functions, it is desirable to use a graphite material having both heat resistance and workability. Further, the crucible 1 to the inert gas spraying portion 7 are installed in a chamber (not shown) with good sealing properties, and can be replaced with an inert gas after evacuation. It is preferable to do. In this case, argon, helium, or the like can be used as the inert gas, but argon is more preferable in consideration of cost. In addition, when a gas containing an oxygen component is used, it is necessary to remove the oxygen component as much as possible because silicon oxide is generated and adheres to the substrate surface and the chamber wall.

  The raw material supply unit 6 can be separated from the inside of the chamber preferably in an airtight state, and a raw material holding unit 6a is housed in a sub chamber 8 in which the inside can be replaced with an inert gas. And the raw material supply part 6 conveys the raw material holding part 6a to the top of the silicon melt 2 in the crucible 1 and a tilting part (not shown) for dropping the raw material into the crucible 1. The additional supply of the raw material to the crucible 1 is made possible continuously.

  FIG. 2 shows a configuration of a main part in the embodiment in which the raw material supply unit 6 and the inert gas spraying unit 7 in FIG. 1 are integrally configured. In FIG. 2, a pipe-like inert gas supply unit 9 is attached to the raw material holding unit 6 a of the raw material supply unit 6. The inert gas supply unit 9 is moved by a moving device (not shown) so that the raw material holding unit 6a can be transported to the top of the silicon melt 2 in the crucible 1. Further, by rotating the inert gas supply unit 9 around the central axis by a rotating device (not shown), the raw material holding unit 6a can be tilted and the raw material can be dropped into the crucible 1. Yes.

  Examples of the moving device include an air cylinder, and examples of the rotating device include a motor and a gear train.

  That is, the inert gas supply unit 9 includes a part of the transporting part that transports the raw material holding part 6a to the position immediately above the silicon melt 2 in the crucible 1, and a part of the tilting part that tilts the raw material holding part 6a. It also doubles.

  In the vicinity of the raw material supply unit 6 in the inert gas supply unit 9, an angle at which the inert gas supply unit 9 rotates around the axis so that the raw material supply unit 6 can drop the raw material into the crucible 1. An inert gas outlet 11 is provided for blowing the inert gas introduced from the inert gas inlet 10 toward the center of the crucible 1 when tilted to the center.

  By configuring the raw material supply unit 6 and the inert gas supply unit 9 in this way, the structure of the solid melting apparatus is simplified, and the inert gas supply unit 9 constituting the tilting unit of the raw material supply unit 6 is configured. Can be easily adjusted with respect to the crucible 1 by rotating the inert gas.

  Hereinafter, the silicon raw material supply method will be described with reference to FIG.

  In FIG. 1, a silicon lump whose boron concentration is adjusted so that the specific resistance of the plate-like silicon becomes a desired concentration is filled in the crucible 1 made of high-purity graphite until it is full. Next, the inside of the chamber is evacuated, and the inside of the chamber is reduced to a predetermined pressure. Thereafter, Ar (argon) gas is introduced into the chamber, and Ar gas is always allowed to flow from the upper part of the chamber at a flow rate of 10 L / min. As described above, the reason why the gas is constantly flowed is to obtain a clean silicon hot water surface.

  Next, the temperature of the heater 3 is set to 1500 ° C., and the silicon lump in the crucible 1 is completely melted. Furthermore, the raw material holding unit 6 a of the raw material supply unit 6 is filled with granular silicon raw material, and the raw material supply unit 6 supplies the silicon raw material to the silicon melt 2 in the crucible 1. In that case, the supplied silicon raw material floats in the shape of a mountain-shaped lump in the center of the surface of the silicon melt 2 (see FIG. 2). An inert gas is sprayed onto the bulk silicon raw material by the inert gas spraying unit 7. Then, as shown in FIG. 3, the lump silicon raw material is dispersed toward the side wall of the crucible 1. In this state, if an inert gas is further blown onto the surface of the silicon melt 2, the surface of the silicon melt 2 is shaken as shown in FIG. By doing so, the contact area between the additionally supplied silicon material and the silicon melt 2 is increased, and the melting time of the silicon material is shortened.

It is a figure which shows the whole structure in the solid melting apparatus of this invention. It is a figure which shows the structure of the principal part in the solid melting apparatus which comprised integrally the raw material supply part and inert gas spraying part in FIG. It is a schematic diagram which shows the blowing state of the inert gas in the solid melting apparatus shown in FIG. It is a schematic diagram which shows the blowing state of the inert gas different from FIG.

Explanation of symbols

1 ... crucible,
2 ... silicon melt,
3. Heating heater,
4 ... crucible stand,
5. Insulation material
6 ... Raw material supply section,
6a ... Raw material holding part,
7 ... inert gas spraying part,
8 ... Sub-room,
9: Inert gas supply unit,
10 ... inert gas inlet,
11 ... Inert gas outlet,
12 ... Inert gas blowing port,
13 ... Additional raw material.

Claims (7)

A crucible for melting the charged solid raw material and holding the molten melt,
A raw material supply unit for additionally supplying the solid raw material into the crucible;
A solid-melting apparatus comprising an inert gas spraying section for spraying an inert gas to the additionally supplied solid raw material floating on the surface of the melt in the crucible. The solid melting apparatus according to claim 1,
The raw material supply unit
A raw material holding unit for holding additional feed materials;
A transport unit that transports the raw material holding unit to a position directly above the melt in the crucible;
And a tilting part for tilting the raw material holding part to drop the additional feedstock into the crucible. The solid melting apparatus according to claim 2, wherein
The inert gas blowing part has an inert gas outlet for blowing out the inert gas,
The solid gas melting apparatus, wherein the inert gas outlet is provided at a position tilted in conjunction with the raw material holding part or the raw material holding part. The solid melting apparatus according to claim 3, wherein
The transport unit includes a pipe-like inert gas supply unit that constitutes a part of the inert gas blowing unit and has one end attached and fixed to the raw material holding unit and communicating with the inert gas outlet. A solid melting apparatus characterized by comprising: The solid melting apparatus according to claim 4, wherein
The transport unit includes a moving device that moves the inert gas supply unit until the raw material holding unit attached to one end of the inert gas supply unit reaches directly above the melt in the crucible,
The tilting unit includes a rotating device that rotates the pipe-like inert gas supply unit around a central axis to tilt the raw material holding unit attached to one end of the inert gas supply unit. A solid melting apparatus characterized by that. In the crucible holding a melt obtained by melting the charged solid raw material, the solid raw material is additionally supplied by the raw material supply unit,
An inert gas spraying unit sprays an inert gas on the additionally supplied solid raw material floating on the surface of the melt in the crucible, and the floating additional raw material is A raw material supply method, characterized by being dispersed around the side wall of a crucible. The raw material supply method according to claim 6,
After the floating additional feedstock is dispersed around the side wall of the crucible, an inert gas is subsequently sprayed onto the surface of the melt in the crucible by the inert gas spraying section, so that the melt A raw material supply method characterized by increasing the contact area between the additional feed material floating and the melt by shaking the surface.

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