KR101309521B1 - Apparatus for manufacturing polysilicon with high purity using electron-beam melting and method of manufacturing polysilicon using the same - Google Patents
Apparatus for manufacturing polysilicon with high purity using electron-beam melting and method of manufacturing polysilicon using the same Download PDFInfo
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- KR101309521B1 KR101309521B1 KR20100120058A KR20100120058A KR101309521B1 KR 101309521 B1 KR101309521 B1 KR 101309521B1 KR 20100120058 A KR20100120058 A KR 20100120058A KR 20100120058 A KR20100120058 A KR 20100120058A KR 101309521 B1 KR101309521 B1 KR 101309521B1
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Abstract
Disclosed is a polysilicon production apparatus and method capable of producing high purity polysilicon using electron beam melting.
Polysilicon manufacturing apparatus according to the present invention comprises a vacuum chamber for maintaining a vacuum atmosphere; First and second electron guns disposed on top of the vacuum chamber such that an electron beam is irradiated into the vacuum chamber; A silicon melting part disposed in the first electron beam irradiation region by the first electron gun and charged with the silicon raw material in the form of particles to be melted by the first electron beam; And a start block disposed in a second electron beam irradiation area by the second electron gun, connected to the silicon melter through a conduit, a cooling channel formed at a lower side thereof, and being driven in a lower direction therein. start block), and the molten silicon supplied from the silicon melting part is transferred downward by the start block while being molten by the second electron beam and then solidified upward through the cooling channel. It is characterized in that it comprises a; one-way solidification unit.
Description
TECHNICAL FIELD The present invention relates to polysilicon manufacturing technology, and more particularly, to 99.9999% (6N) from a metal-grade silicon raw material having a purity range of 99 to 99.9% (2 to 3N) by using electron-beam melting. The present invention relates to a technology capable of producing high purity polysilicon having a purity range of about 6).
The purity of silicon is usually expressed as 2N, 3N, 6N, 11N, and the like. Here, the number before 'N' means the number of 9 in terms of weight%, 99% purity for 2N, 99.9999% purity for 6N and 99.999999999% for 11N.
Purity of semiconductor grade silicon requiring ultra high purity reaches 11N. However, it is known that the silicon used as the raw material of the solar cell is similar in light conversion efficiency to that of 11N purity silicon even when the purity of 5N-7N is relatively low compared with the purity of semiconductor-grade silicon of 11N.
Semiconductor grade silicon is being manufactured through a chemical gasification process. However, it is known that such a silicon production process causes a large amount of pollutants, low production efficiency, and high production cost.
Accordingly, metallurgical refining processes capable of mass-producing high-purity silicon at a low manufacturing cost are difficult to apply to silicon used as a raw material for a photovoltaic cell.
Typical processes such as vacuum refining, wet refining, oxidation treatment and unidirectional solidification refining have been developed for the metallurgical refining of high purity silicon for solar power generation, and some of them have been commercialized.
Among these metallurgical refining methods, silicon manufacturing technology by a metal melting method such as a vacuum refining method and a unidirectional solidifying refining method is easy to control characteristics, and there is little contamination due to impurities during operation, and active research is proceeding.
Here, vacuum refining generally refers to a refining process of melting a metal raw material and removing impurities having a lower boiling point and vapor pressure from the molten metal than silicon. It is a refining process that moves (segregates) impurities to a liquid along the liquid interface.
Vacuum and separation refining have been developed in various ways according to the volatilized energy source, and most of them use a magnetic induction heating method.
An object of the present invention is to provide a polysilicon production apparatus capable of producing high purity polysilicon using electron beam melting.
Another object of the present invention is to manufacture a high-purity polysilicon manufacturing method that can maximize the silicon refining effect by controlling the electron beam melting process using the polysilicon manufacturing apparatus.
Polysilicon manufacturing apparatus according to an embodiment of the present invention for achieving the above object is a vacuum chamber for maintaining a vacuum atmosphere; First and second electron guns disposed on top of the vacuum chamber such that an electron beam is irradiated into the vacuum chamber; A silicon melting part disposed in the first electron beam irradiation region by the first electron gun and charged with the silicon raw material in the form of particles to be melted by the first electron beam; And a start block disposed in a second electron beam irradiation area by the second electron gun, connected to the silicon melter through a conduit, a cooling channel formed at a lower side thereof, and being driven in a lower direction therein. start block), and the molten silicon supplied from the silicon melting part is transferred downward by the start block while being molten by the second electron beam and then solidified upward through the cooling channel. It is characterized in that it comprises a; one-way solidification unit.
Polysilicon manufacturing method according to an embodiment of the present invention for achieving the above another object is (a) a polysilicon manufacturing apparatus comprising the vacuum chamber, the first, the second electron gun, the silicon melting portion and the unidirectional solidification portion of claim 1 Providing a; (b) mounting a dummy bar in the one-way solidification unit; (c) mounting a start block inside the one-way solidification part through melting of the silicon button on the dummy bar; (d) feeding the silicon raw material in the form of particles into the silicon melting part, and melting the fed silicon raw material by irradiating a first electron beam with the first electron gun; (e) the molten silicon overflowing while the feeding of the silicon raw material and the melting of the fed silicon raw material are continuously performed; (f) receiving molten silicon overflowed from the one-way solidification part, and irradiating a second electron beam with the second electron gun to drive the start block downward while maintaining a molten state to transfer molten silicon downward; Thereafter, cooling the lower portion of the molten silicon and refining it through solidification in an upward direction; And (g) cutting the upper part of the refined silicon to remove metal impurities on the upper part of the refined silicon.
Apparatus and method for producing polysilicon using electron beam melting according to the present invention is capable of vacuum refining and unidirectional solidification refining of silicon by applying electron beam melting, thereby producing polysilicon of high purity.
In addition, the polysilicon manufacturing apparatus and method according to the present invention can improve the removal efficiency of volatile impurities and metal impurities by applying an electron beam of high vacuum and high energy density.
Polysilicon prepared by the manufacturing method according to the present invention can be utilized as silicon for solar power by having a purity of 5N ~ 7N grade.
Figure 1 schematically shows a high purity polysilicon manufacturing apparatus using electron beam melting according to an embodiment of the present invention.
Figure 2 schematically shows an example of a start block applied to the present invention.
3 is a flow chart schematically showing a polysilicon manufacturing method according to an embodiment of the present invention.
Fig. 4 shows an example of a solid-liquid interface formed by an electron beam pattern applied to the present invention.
5 shows an example of an electron beam irradiation pattern of the first electron gun.
6 shows an example of the electron beam irradiation pattern of the second electron gun.
Figure 7 shows a photo of the polysilicon prepared by the process according to the embodiment.
8 is a photograph showing a cross section of an impurity concentration boundary part in the polysilicon prepared by the process according to the embodiment.
Brief Description of the Drawings The advantages and features of the present invention, and how to accomplish them, will become apparent with reference to the following detailed description, taken in conjunction with the accompanying drawings. However, it should be understood that the present invention is not limited to the embodiments described below, but may be embodied in various forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete and will fully convey the concept of the invention to those skilled in the art. To fully disclose the scope of the invention, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.
Hereinafter, an apparatus and method for manufacturing high purity polysilicon using electron beam melting according to the present invention will be described in detail with reference to the accompanying drawings.
Figure 1 schematically shows a high purity polysilicon manufacturing apparatus using electron beam melting according to an embodiment of the present invention.
Referring to FIG. 1, the illustrated polysilicon manufacturing apparatus includes a
The
The
The
At this time, it is preferable that the
It is preferable that the
The one-
The unidirectional solidifying
A
The
In the one-
A second electron gun (120b) is a second electron beam to have an output energy of 1000 ~ 2000kW / m 2, it can be accelerated, and integrating the second electron beam. When the output energy of the second electron beam is less than 1000 kW / m 2 , it is difficult to maintain the molten state of silicon. When the output energy of the second electron beam exceeds 2000 kW / m 2 , There is a possibility that the behavior of the molten metal becomes unstable. This unstable melt behavior also affects the overflow process control from the melt.
The one-
2 schematically shows an example of a
Referring to FIG. 2, the start block 145 may be formed by bonding a high-
The
The dummy bars 146 may be made of a graphite material.
The
In this case, the material of the
In the polysilicon manufacturing apparatus according to the present invention, the electron beam pattern by the first electron gun (120a), the second electron gun (120b), the output energy of the first and second electron beams, the cooling water supplied to the one-
3 is a flow chart schematically showing a polysilicon manufacturing method according to an embodiment of the present invention.
Referring to FIG. 3, the method for manufacturing polysilicon according to the present invention includes a step of preparing a polysilicon manufacturing apparatus (S310), a step of mounting a dummy bar (S320), a step of manufacturing a start block by melting a silicon button (S330) And a melting step S340, a molten metal overflow step S350, a refining step S360 through silicon solidification, and an upper silicon cutting step S370.
In the polysilicon manufacturing apparatus preparing step (S310), a polysilicon manufacturing apparatus including a vacuum chamber, first and second electron guns, a silicon melting part, and a unidirectional solidification part is prepared as in the example shown in FIG. 1.
In the dummy bar attaching step (S320), the dummy bar is mounted inside the unidirectional solidifying portion. Then, in the start block manufacturing step (S330), a start block is formed by melting the silicon button.
Dummy bar mounting and manufacturing of the start block can be made in more detail as follows.
First, a dummy bar formed of graphite material or the like is mounted inside the one-way solidification part. The silicon chunks are then placed on the dummy bar. Next, the silicon chunks are fusion bonded to the dummy bars by the second electron beam in a vacuum atmosphere of about 10 -5 torr. Through this process, a start block is formed by bonding the upper silicon button and the lower dummy bar.
Next, in the low-purity silicon feeding and melting step (S340), the silicon raw material in the form of particles is fed to the silicon melting portion, and the first electron beam is irradiated using the first electron gun to melt the fed silicon raw material. The silicon raw material in the form of particles may be one having a purity of 2N and an average particle diameter of 1 to 2 mm.
As the silicon raw material is melted by the first electron beam, volatile impurities such as aluminum (Al), calcium (Ca), phosphorus (P), magnesium (Mg), manganese (Mn), and the like contained in the silicon raw material are volatilized under vacuum. Removed.
Volatile impurities having a higher boiling point and vapor pressure than silicon are volatilized by high vacuum and high heating temperature by the first electron beam. In this case, when the first electron beam output energy is increased and the first electron beam irradiation time is increased, refining efficiency may be improved.
In this step S340, the first electron beam may have an output energy of about 4000 kW / m < 2 > to accelerate and accumulate the first electron beam in the first electron gun so as to facilitate silicon melting and removal of volatile impurities.
In this case, the first electron gun is irradiated with the first electron beam in a comb-shaped pattern in which the head is in the furnace side as in the example shown in FIG. Design to control the flow of surface melt. In addition, as shown in FIGS. 5B and 5C, the flow path is irradiated with a first electron beam in a linear reciprocating pattern to maintain a uniform temperature of the silicon melt in the flow path while allowing the molten metal to move to the one-way solidification part. Serves to control. The energy density of the first electron beam to be irradiated can be adjusted to maintain the temperature of such molten metal in the process.
Next, in the molten metal overflow step (S350), the feeding of the silicon raw material to the silicon melting portion is continuously performed and the amount of the molten silicon formed in the silicon melting portion is increased, and the molten silicon is overflowed, And is supplied to the solidifying portion.
Next, in the refining step (S360) through silicon solidification, molten silicon is supplied from the one-way solidification unit, and is melted by driving the internal start block downward while maintaining a molten state by irradiating a second electron beam with a second electron gun. After transferring the silicon to the lower side, the lower part of the molten silicon is cooled so that the molten silicon is refined simultaneously with solidification from the lower side to the upper side.
In this step S360, the second electron beam can be accelerated and accumulated in the second electron gun so that the second electron beam has an output energy of 1000 to 2000 kW / m < 2 > have.
In this case, as shown in the example of FIG. 6, the second electron gun may irradiate the second electron beam in a circular or spiral complex pattern to the one-way solidification part.
The pattern of the second electron beam is an important process variable that influences the refining efficiency by determining not only the surface state of the silicon melt and the contact area of the inner wall of the water-freezing crucible, but also the temperature profile inside the melt. The circular or spiral composite pattern proposed in the present invention keeps the molten surface shape convex during the process and minimizes contact with the inner wall of the water-freezing crucible.
4 shows an example of the interface between the
On the other hand, the start block in the step S360 may be driven to descend at a rate of 0.005 ~ 0.05 mm / s. When the start block is lowered at a speed less than 0.005 mm / s, the level of the silicon melt is continuously increased and the process control is impossible. When the start block is lowered beyond 0.05 mm / s, There is a problem that the molten metal leaks into the lower portion of the unidirectional solidification portion.
During this process, metal impurities such as iron (Fe), nickel (Ni), titanium (Ti), chromium (Cr), and copper (Cu) contained in the molten silicon are moved upward along the solid-liquid interface. The segregation effect of such impurities can be sufficiently exhibited when the temperature difference between the solid and liquid is high while the interface between the solid and liquid phases is perpendicular to the growth direction during the silicon solidification process.
In the present invention, while maintaining the molten state of the molten silicon by the second electron beam in the one-way solidification unit, while maintaining the solid-liquid interface perpendicular to the growth direction by the optimally designed electron beam pattern, the solid phase and the liquid phase through cooling from the bottom of the molten silicon The temperature difference can be maximized to improve the effect of impurity segregation.
Next, in the upper silicon cutting step (S370), the upper portion of the cast silicon is cut. As the metal impurity contained in the molten silicon moves upward along the solid-liquid interface, segregation of the metal impurity is concentrated at the top of the cast silicon (see FIG. 8). The polysilicon of can be manufactured.
In the embodiment of the present invention, the final polysilicon is approximately 100 mm in diameter, the height of the operation time, the growth rate can be 1 ~ 1000 mm by adjusting the growth rate. At this time, the process was controlled so that the height of the upper portion where the impurities were concentrated was less than 20% of the total specimen height.
Polysilicon produced through the above process may have a purity of 5N ~ 7N, it can be usefully used as a silicon for solar power generation.
Example
Hereinafter, the configuration and operation of the present invention through the preferred embodiment of the present invention will be described in more detail. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense.
Details that are not described herein will be omitted since those skilled in the art can sufficiently infer technically.
First, polysilicon was produced by the following procedure.
The dummy bar was mounted in a one-way solidification part, charged with a mass of silicon having a purity of 9N and a mass of 180g, and then irradiated with a vacuum atmosphere at 10-5 torr and an electron beam at 2000 kW / m 2 for 10 minutes to melt the silicon, The dummy bar of was bonded together.
The pattern shown in FIG. 5 is supplied to the silicon melt with 1 to 10 mm size silicon particles supplied to the water-cooling crucible through the raw material supply device and at the same time the output energy of 1000 to 1500 kW / m 2 using the first electron gun. Was applied to irradiate the first electron beam.
Then, the molten silicon is supplied to the one-way solidification unit along the flow path, and a second electron beam having an output energy of 1000 to 2000 kW / m 2 is irradiated using the second electron gun using the circular composite pattern shown in FIG. 6. In a state in which the molten state of silicon was maintained, the start block was lowered to 0.005 to 0.05 mm per second, and then the start block was cooled.
7 is a photograph showing a polysilicon produced by the process according to the embodiment, Figure 8 is a photograph showing a cross section of the impurity concentration portion boundary portion in the polysilicon prepared by the process according to the embodiment.
Referring to FIGS. 7 and 8, it can be seen that metal impurities and the like move to the top of the ingot while polysilicon is being produced.
Table 1 shows the results of purity analysis of the impurity layer and the refined layer by ICP-AES analysis of the polysilicon prepared according to the embodiment.
[Table 1] (Unit: ppm)
Referring to Table 1, as a result of manufacturing polysilicon using the polysilicon manufacturing apparatus according to the present invention, it can be seen that the silicon raw material of 2N purity is refined to 6N purity, and the impurities are concentrated on the top impurity layer. You can see that.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. I will understand.
Accordingly, the true scope of protection of the present invention should be defined by the following claims.
110:
120b: second electron gun 130: silicon melt part
135: Tang Ro 140: Unidirectional solidification part
142: Cooling channel 145: Start block
146: Dummy bar 147: Silicone button
S310: Polysilicon manufacturing equipment preparation step
S320: Dummy bar mounting step
S330: Start block manufacturing step
S340: Purity Silicon Feeding and Melting Step
S350: overflow step of the molten metal
S360: refining step with silicon solidification
S370: Silicon upper cutting step
Claims (17)
First and second electron guns disposed on top of the vacuum chamber such that an electron beam is irradiated into the vacuum chamber;
A silicon melting part disposed in the first electron beam irradiation region by the first electron gun and charged with the silicon raw material in the form of particles to be melted by the first electron beam; And
A start block disposed in the second electron beam irradiation area by the second electron gun and connected to the silicon melt part through a trench, a cooling channel formed on the lower side, and a start block the molten silicon supplied from the silicon melt portion is transported downward by the start block in a state where the molten silicon is maintained in a molten state by the second electron beam and then solidified in an upward direction through the cooling channel A one-way solidifying portion,
The start block is driven downward in the one-way solidification part, and the start block includes a dummy bar made of graphite material, a silicon button bonded on the dummy bar, and having a purity of 8N to 10N.
And the second electron gun irradiates the second electron beam in a circular or spiral complex pattern on the unidirectional solidification part.
The first electron gun
And accelerating and integrating the first electron beam such that the first electron beam has an energy of 4000 kW / m 2 or less.
The second electron gun
And accelerating and integrating the second electron beam such that the second electron beam has an energy of 1000 to 2000 kW / m 2 .
The silicon melt portion
An apparatus for producing polysilicon, comprising a water-cooled crucible.
The one-way solidification unit
Polysilicon manufacturing apparatus characterized in that it comprises a casting vessel made of copper formed with a cooling channel on the lower side.
Inside the vacuum chamber
An apparatus for producing polysilicon, which is maintained in a vacuum atmosphere of 10 −4 torr or less.
(b) mounting a dummy bar in the one-way solidification unit;
(c) manufacturing a start block inside the one-way solidification part through melting of the silicon button on the dummy bar;
(d) feeding the silicon raw material in the form of particles into the silicon melting part, and melting the fed silicon raw material by irradiating a first electron beam with the first electron gun;
(e) the molten silicon overflowing while the feeding of the silicon raw material and the melting of the fed silicon raw material are continuously performed;
(f) receiving molten silicon overflowed from the one-way solidification part, and driving the start block downward while maintaining a molten state by irradiating a second electron beam in a circular or spiral complex pattern using the second electron gun to melt After transferring the silicon to the lower side, cooling the lower portion of the molten silicon to refine the solidification through the upward direction; And
(g) cutting the top of the refined silicon to remove metal impurities on the top of the refined silicon;
In the step (c), the dummy bar is made of a graphite material, the silicon button is a polysilicon manufacturing method, characterized in that having a purity of 8N ~ 10N.
In the step (d)
A method for producing polysilicon, comprising charging a silicon raw material having a purity of 2N and an average particle diameter of 1 to 2 mm.
In step (d)
And vacuum volatilizing the volatile impurities contained in the silicon raw material with the first electron beam.
In the step (d)
And accelerating and integrating the first electron beam in the first electron gun such that the first electron beam has an energy of 4000 kW / m 2 or less.
In the steps (d) and (e), the first electron gun
The silicon melting portion is irradiated with the first electron beam in a comb-shaped pattern in which the head is a waterway,
And the first electron beam is irradiated to the hot water path in a linear reciprocating pattern.
In the step (f), the start block is
Method for producing polysilicon, characterized in that descending at a rate of 0.005 ~ 0.05 mm / s.
In the step (f)
The method for producing polysilicon, characterized in that the metal impurities contained in the molten silicon is moved upward along the solid-liquid interface.
In the step (f)
And accelerating and integrating the second electron beam in the second electron gun such that the second electron beam has an energy of 1000 to 2000 kW / m 2 .
In steps (d) to (f), the inside of the vacuum chamber is
A method for producing polysilicon, which is maintained in a vacuum atmosphere of 10 −4 torr or less.
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| KR20100120058A KR101309521B1 (en) | 2010-11-29 | 2010-11-29 | Apparatus for manufacturing polysilicon with high purity using electron-beam melting and method of manufacturing polysilicon using the same |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07309614A (en) * | 1994-03-24 | 1995-11-28 | Kawasaki Steel Corp | Method for purifying silicon |
| JPH10273313A (en) * | 1997-03-28 | 1998-10-13 | Kawasaki Steel Corp | Production of polycrystal silicon ingot |
| JPH11209195A (en) * | 1998-01-21 | 1999-08-03 | Kawasaki Steel Corp | Purification method of silicon |
| KR20100042506A (en) * | 2008-10-16 | 2010-04-26 | 주식회사 엔씨비네트웍스 | Manufacturing device for silicon ingot having refining function |
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2010
- 2010-11-29 KR KR20100120058A patent/KR101309521B1/en active IP Right Grant
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07309614A (en) * | 1994-03-24 | 1995-11-28 | Kawasaki Steel Corp | Method for purifying silicon |
| JPH10273313A (en) * | 1997-03-28 | 1998-10-13 | Kawasaki Steel Corp | Production of polycrystal silicon ingot |
| JPH11209195A (en) * | 1998-01-21 | 1999-08-03 | Kawasaki Steel Corp | Purification method of silicon |
| KR20100042506A (en) * | 2008-10-16 | 2010-04-26 | 주식회사 엔씨비네트웍스 | Manufacturing device for silicon ingot having refining function |
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