CN113818074A - Device and method for preparing monocrystalline silicon by directly using granular silicon in CCZ Czochralski method - Google Patents
Device and method for preparing monocrystalline silicon by directly using granular silicon in CCZ Czochralski method Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses a device for preparing monocrystalline silicon by directly using granular silicon in a CCZ Czochralski method, which comprises a monocrystalline furnace and a granular silicon feeding device, wherein the monocrystalline furnace comprises a furnace body, a quartz crucible is arranged in the furnace body, a first heater is arranged outside the quartz crucible, a guide cylinder is arranged above the quartz crucible, a heat-preserving cylinder is arranged in the furnace body, the heat-preserving cylinder comprises an upper heat-preserving cylinder and a lower heat-preserving cylinder, a graphite large cover is arranged on the upper heat-preserving cylinder, the guide cylinder is assembled in a through hole of the graphite large cover, a water screen is arranged in the guide cylinder, a bottom protecting pressing plate is arranged below the lower heat-preserving cylinder, a heating electrode is arranged at the bottom end of the furnace body, a melt crucible, a material pipeline, a second heater and a gas-solid cyclone separator are also arranged in the furnace body, the granular silicon feeding device comprises a granular silicon charging barrel, a quartz material pipe, an air inlet and an air outlet, and the quartz material pipe is connected with the gas-solid cyclone separator through a feeding pipeline and a valve; the direct addition and use of the granular silicon in the monocrystalline silicon industry are realized by simply modifying a normal monocrystalline furnace, the drawing cost of the monocrystalline silicon is reduced, and the preparation method is simple and easy to implement.
Description
Technical Field
The invention relates to a device and a method for producing monocrystalline silicon, in particular to a device and a method for producing monocrystalline silicon by using granular silicon for CCZ Czochralski method.
Background
According to different crystal growth modes, the current technology for preparing the monocrystalline silicon mainly comprises a suspension zone melting method (FZ method) and a Czochralski method (CZ method), wherein the Czochralski method is relatively low in cost and high in growth rate, and is more suitable for pulling large-size monocrystalline silicon rods, more than 90% of solar-grade monocrystalline silicon in China is produced by the Czochralski method at present, and a large proportion of the solar-grade monocrystalline silicon is expected to be still used in the future.
The Czochralski method is characterized in that a high-purity polycrystalline silicon raw material is placed in a quartz crucible to be heated and melted, then a monocrystalline silicon seed crystal is inserted into the surface of a melt, after the seed crystal is melted with the melt, the seed crystal is slowly pulled upwards, the crystal grows at the lower end of the seed crystal, and the crystal gradually grows along with the pulling of the seed crystal to form a crystal bar.
The original Czochralski method was a batch Czochralski method (BatchCzochralski), in which only one ingot was pulled from one crucible, and the crucible was broken due to cooling after the pulling and was not reused.
At present, RCZ multi-time crystal pulling technology (Rechargeable Czochralski) is mostly adopted in the industrial production of monocrystalline silicon, and the RCZ multi-time crystal pulling technology is improved by adding a feeding device to equipment on the basis of a batch Czochralski method. However, in both the batch pulling method and the RCZ method, the amount of silicon melt in the crucible decreases as the single crystal silicon rod is pulled, which causes a drop in the liquid level, causes instability of the thermodynamic environment in the pulling environment, and tends to cause nonuniformity of the properties of the single crystal silicon rod being pulled.
In addition, the efficiency improvement space of the RCZ method is limited. When one pulled crystal is cooled in the shutter, the next pulled silicon raw material is added to the remaining silicon melt in the crucible through the feed tube. The addition of the silicon charge is thus completed when the crystal cools. However, it is necessary to wait for the single-silicon ingot to be completely cooled and removed in the gate chamber before the next drawing is performed, which causes low efficiency in industrial production.
The pulling and charging melting of the CCZ (continuous outer Czochralski) continuous Czochralski method crystal bar are carried out at the same time with high efficiency, the CCZ czochralski method concept has been existed for a long time, but the industrialized production can not be realized, the main reason is that the raw materials meeting the conditions are less, and meanwhile, the quartz crucible is also special and has more problems in normal use; the granular silicon used in the prior Czochralski method contains a certain amount of hydrogen due to the production process, so that the problems of hydrogen jump, silicon splashing and the like easily occur when melting materials at high temperature, and the granular silicon can not be directly used for the production of monocrystalline silicon.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a method for producing monocrystalline silicon by directly using granular silicon in a CCZ Czochralski method.
In order to solve the technical problems, the invention provides a device for preparing monocrystalline silicon by directly using granular silicon in a CCZ Czochralski method, which comprises a monocrystalline furnace and a granular silicon feeding device arranged on one side of the monocrystalline furnace, wherein:
the single crystal furnace comprises a furnace body, a quartz crucible used for placing raw materials is arranged in the furnace body, a graphite crucible is arranged outside the quartz crucible, a first heater is arranged on the periphery of the graphite crucible, a guide cylinder is arranged above the quartz crucible, a heat preservation cylinder is arranged in the furnace body, a first heat preservation material layer is arranged between the heat preservation cylinder and the wall of the furnace body, the heat preservation cylinder comprises an upper heat preservation cylinder and a lower heat preservation cylinder, the upper heat preservation cylinder is arranged on the periphery of the guide cylinder, the lower heat preservation cylinder is arranged on the periphery of the graphite crucible, a large graphite cover is further arranged on the upper heat preservation cylinder, a through hole is formed in the middle of the large graphite cover, the guide cylinder is assembled in the through hole, a water-cooling screen is arranged in the guide cylinder, a bottom protection pressing plate is further arranged below the lower heat preservation cylinder, a second heat preservation material layer is arranged between the bottom protection pressing plate and the bottom end of the furnace body, a heating electrode is arranged at the bottom end of the furnace body, the heating electrode penetrates through the bottom protection pressing plate and the second heat preservation material layer, a crucible and a material pipeline are further arranged in the furnace body, The second heater (19) and the gas-solid cyclone separator, the melt crucible is arranged between the guide cylinder and the upper heat-insulating cylinder and is positioned above the quartz crucible, the bottom end of the melt crucible is provided with a hole, one end of the material pipeline is provided with the gas-solid cyclone separator of which the upper end is provided with an exhaust port, the other end penetrates through the graphite large cover and is connected with the melt crucible, and the second heaters are arranged on two sides of the bottom end of the melt crucible;
granule silicon feeding device includes granule silicon feed cylinder, quartz capsule, air inlet and gas outlet, and granule silicon feed cylinder is used for placing granule silicon, and quartz capsule is vertical to be set up in granule silicon feed cylinder, and one side of granule silicon feed cylinder upper end is equipped with the air inlet, and the opposite side is equipped with the gas outlet, and the one end of keeping away from granule silicon on the quartz capsule is passed through conveying pipeline and valve and is connected with gas-solid cyclone's feed inlet.
The technical scheme of the invention is further defined as follows:
further, the granular silicon is directly used in the device for preparing the monocrystalline silicon by the CCZ Czochralski method, and the quartz crucible adopts a single-layer quartz crucible with the height of 400 mm. Compared with a double-layer quartz crucible used in a CCZ method in the prior art, the single-layer quartz crucible adopted by the invention has the advantages of low cost and good stability; the RCZ repeated charging Czochralski method is expected to be large as much as possible, the more charging intervals of materials in the crucible are long, the effect is high, but the CCZ continuous charging Czochralski method is different.
Among the device that aforementioned granule silicon directly was used for CCZ czochralski method preparation monocrystalline silicon, graphite crucible includes that crucible bang and crucible hold in the palm, and crucible holds in the palm and sets up in the bottom of crucible bang, and the bottom that crucible held in the palm still is equipped with the die-pin, and the lower extreme that the die-pin passed the furnace body sets up graphite crucible in the furnace body.
The granular silicon is directly used in the device for preparing the monocrystalline silicon by the CCZ Czochralski method, the first heater comprises a side heater and a bottom heater, the side heater is arranged at two sides of the graphite crucible, the side heater is positioned between the graphite crucible and the lower heat-preserving cylinder, the bottom heater is fixed at the bottom of the furnace body through a heating electrode, and the bottom heater is positioned below the graphite crucible.
The granular silicon is directly used in the device for preparing the monocrystalline silicon by the CCZ Czochralski method, the guide cylinder comprises an outer guide cylinder and an inner guide cylinder arranged in the outer guide cylinder, the inner guide cylinder is in a cone frustum shape, the outer guide cylinder is in a cylindrical shape, a third heat insulation material layer is filled between the inner guide cylinder and the outer guide cylinder, the upper ends of the inner guide cylinder and the outer guide cylinder extend outwards to form an annular convex edge, and the guide cylinder is embedded on the graphite large cover through the annular convex edge.
The invention has the technical effects that the guide shell is arranged on the graphite big cover by adopting the annular convex edge, so that the heat insulation effect of the contact part of the guide shell and the graphite big cover is improved, and the heat loss is reduced.
The granular silicon is directly used in a device for preparing the monocrystalline silicon by the CCZ Czochralski method, and the first heat-insulating material layer, the second heat-insulating material layer and the third heat-insulating material layer are all heat-insulating carbon felts or solid felts.
The granular silicon is directly used in the device for preparing the monocrystalline silicon by the CCZ Czochralski method, two positioning blocks are symmetrically arranged at the bottom in a granular silicon charging barrel, a groove with a triangular section is formed between the two positioning blocks, and a quartz material pipe is arranged at the bottommost end of the groove.
The technical effect is that a groove with a triangular cross section is formed in the particle silicon charging barrel, because the particle silicon is spherical or sphere-like, after materials in the groove are sucked away, the particle silicon on the upper part can automatically flow to the groove under the action of gravity for supplement, and the particle silicon is convenient and fast to feed into a melting crucible.
The invention also discloses a method for preparing monocrystalline silicon by adopting the device, which comprises the following steps: thermal field clearance, feed, manage to find time leak, pressure gasification, melt, secondary feeding, crystal pulling, wherein:
step one, cleaning a thermal field: cleaning a thermal field in a single crystal furnace, installing a thermal field piece, and installing a melting crucible, a second heater, a material pipeline, a gas-solid cyclone separator and a feeding pipeline;
step two, secondary feeding: when the silicon material in the quartz crucible in the single crystal furnace is changed into molten silicon, a certain space is left in the quartz crucible, and the silicon material is continuously filled, which specifically comprises the following steps:
pressure inside the single crystal furnace-pressure in the granular silicon barrel =0-0.5 torr;
opening an external protective gas valve to add protective gas into the charging barrel through a gas inlet on the granular silicon charging barrel, then opening a valve on the feeding pipe, wherein the granular silicon in the granular silicon charging barrel is taken into the single crystal furnace by the protective gas and enters a gas-solid cyclone separator from a feed inlet due to the pressure difference between the single crystal furnace body and the granular silicon charging barrel;
step three, CCZ crystal pulling: the method is operated according to a normal crystal pulling flow, when monocrystalline silicon is pulled out of silicon liquid, a protective gas inlet valve of granular silicon and a valve on a feeding pipeline are opened, the granular silicon continuously enters a melting crucible, and the silicon liquid can supplement the silicon liquid in the quartz crucible in time, so that the whole crystal pulling process is stably operated;
when the single crystal rod reaches the target length, ending operation is carried out, the silicon material inlet flow is gradually reduced, and finally feeding operation is stopped;
and when the crystal bar is cooled and pulled out, continuing to perform bar pulling operation.
The granular silicon is directly used in the method for preparing the monocrystalline silicon by the CCZ Czochralski method, and the gas-solid cyclone separator is a cyclone separator made of quartz or silicon carbide.
The invention has the beneficial effects that:
the invention realizes the direct adding and using problem of the granular silicon in the monocrystalline silicon industry by simply modifying the normal monocrystalline furnace in the prior art; the CCZ direct method can be industrially operated, the CCZ is moved from a laboratory to a factory, the drawing cost of the monocrystalline silicon is reduced, and the problems encountered in the past are well solved.
The height of the single-layer quartz crucible in the single crystal furnace is reduced a little, and is controlled to be 400mm from the original 600 mm; the gas-solid separator, the melting crucible and the second heater matched with the melting crucible are additionally arranged in the single crystal furnace, and the structures enable hydrogen in the granular silicon to volatilize under the action of the second heater, so that the problems of hydrogen jump, silicon splashing and the like easily caused by melting at high temperature are effectively solved, and the solid granular silicon can be directly used for producing monocrystalline silicon; the granular silicon feeding device is designed outside the single crystal furnace, so that the granular silicon feeding is directly used for preparing the single crystal silicon.
The invention can realize the relevant characteristics of the monocrystalline silicon produced by the CCZ direct method, the resistance distribution is uniform, the resistance distribution surface of the monocrystalline silicon produced by the normal CZ method and RCZ method has the phenomena of head, bottom and tail height, the monocrystalline silicon produced by the CCZ method has very uniform resistance distribution because the raw materials and the dopant can be continuously added in the crystal pulling process, and the application performance stability such as minority carrier lifetime of the finally pulled monocrystalline silicon is also very good.
The invention adopts the practical principle that the protective gas drives the granular silicon to enter the single crystal furnace; a design scheme and a principle of separating granular silicon from protective gas by a gas-solid cyclone separator; the melt is melted under the action of a small heater in the furnace by the small melt crucible, so that the design principle of continuously adding silicon liquid in a large quartz crucible experiment is realized, the granular silicon is directly used for preparing the monocrystalline silicon by the CCZ czochralski method, the CCZ is moved to a factory from a laboratory, and the drawing cost of the monocrystalline silicon is reduced.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for producing single crystal silicon by direct use of granular silicon in CCZ Czochralski method in accordance with an embodiment of the present invention;
in the figure: 1-a positioning block, 2-a water-cooling screen, 3-an inner guide cylinder, 4-an outer guide cylinder, 5-an upper heat preservation cylinder, 6-a side heater, 7-a crucible, 8-a quartz crucible, 9-a crucible holder, 10-a support rod, 11-a bottom heater, 12-a heating electrode, 13-a first heat preservation material layer, 14-a lower heat preservation cylinder, 15-a graphite large cover, 16-a bottom protection pressing plate, 17-a second heat preservation material layer, 18-a melt crucible, 19-a second heater, 20-a material pipeline, 21-a gas-solid cyclone separator, 22-an exhaust port, 23-a feed port, 24-a third heat preservation material layer, 25-a valve, 26-a feed pipeline, 27-a quartz material pipe, 28-an air inlet and 29-a granular silicon material cylinder, 30-granular silicon, 31-gas outlet and 32-annular convex edge.
Detailed Description
Example 1
The apparatus for preparing single crystal silicon by using granular silicon directly in CCZ czochralski method provided by this embodiment has a structure as shown in fig. 1, and comprises a single crystal furnace and a granular silicon feeding device arranged at one side of the single crystal furnace, wherein:
the single crystal furnace comprises a furnace body, the furnace body comprises a furnace body and a furnace cover arranged on the furnace body, a quartz crucible 8 for placing raw materials is arranged in the furnace body, a graphite crucible is arranged outside the quartz crucible 8, a first heater is arranged on the periphery of the graphite crucible, a guide cylinder is arranged above the quartz crucible 8, a heat preservation cylinder is arranged in the furnace body, a first heat preservation material layer 13 is arranged between the heat preservation cylinder and the wall of the furnace body, the heat preservation cylinder comprises an upper heat preservation cylinder 5 and a lower heat preservation cylinder 14, the upper heat preservation cylinder 5 is arranged on the periphery of the guide cylinder, the lower heat preservation cylinder 14 is arranged on the periphery of the graphite crucible, a graphite big cover 15 is further arranged on the upper heat preservation cylinder 5, a through hole is arranged in the middle of the graphite big cover 15, the guide cylinder is assembled in the through hole, a water screen 2 is arranged in the guide cylinder, a bottom protection pressing plate 16 is further arranged below the lower heat preservation cylinder 14, a second heat preservation material layer 17 is arranged between the bottom protection pressing plate 16 and the bottom end of the furnace body, a heating electrode 12 is arranged at the bottom end of the furnace body, the heating electrode 12 penetrates through a bottom protecting pressing plate 16 and a second heat insulating material layer 17, a melt crucible 18, a material pipeline 20, a second heater 19 and a gas-solid cyclone separator 21 are further arranged in the furnace body, the melt crucible 18 is arranged between the guide cylinder and the upper heat insulating cylinder 5 and located above the quartz crucible 8, a hole is formed in the bottom end of the melt crucible 18, the gas-solid cyclone separator 21 with an exhaust port 22 formed in the upper end is arranged at one end of the material pipeline 20, the other end of the material pipeline penetrates through a graphite large cover 15 to be connected with the melt crucible 18, the second heater 19 is arranged on two sides of the bottom end of the melt crucible 18, a supporting material of the second heater is designed on one side of the outer guide cylinder, the second heater is supported on two sides of the bottom end of the melt crucible or a fixing device of the second heater is directly designed on the furnace cover, and a suspender is used for hoisting the melt of the second heater on two sides of the bottom end of the crucible;
the particle silicon feeding device comprises a particle silicon charging barrel 29, a quartz tube 27, an air inlet 28 and an air outlet 31, the particle silicon charging barrel 29 is used for placing particle silicon 30, the quartz tube 27 is vertically arranged in the particle silicon charging barrel 29, the air inlet 28 is arranged on one side of the upper end of the particle silicon charging barrel 29, the air outlet 31 is arranged on the other side of the upper end of the particle silicon charging barrel 29, and one end, far away from the particle silicon 30, of the quartz tube 27 is connected with the feeding hole 23 of the gas-solid cyclone separator 21 through a feeding pipeline 26 and a valve 25.
In the present embodiment, the quartz crucible 8 is a single-layer quartz crucible having a height of 400 mm. In this embodiment, graphite crucible includes that crucible nation 7 and crucible hold in the palm 9, and crucible holds in the palm 9 and sets up in crucible nation 7's bottom, and crucible holds in the palm 9's bottom still is equipped with die-pin 10, and die-pin 10 passes the lower extreme of furnace body and sets up graphite crucible in the furnace body.
In this embodiment, the first heater includes a side heater 6 and a bottom heater 11, the side heater 6 is disposed on both sides of the graphite crucible, the side heater 6 is located between the graphite crucible and the lower heat-insulating cylinder 14, the bottom heater 11 is fixed on the bottom of the furnace body by a heating electrode 12, and the bottom heater 11 is located below the graphite crucible.
In this embodiment, the draft tube includes outer draft tube 4 and sets up interior draft tube 3 in outer draft tube 4, and interior draft tube 3 is the circular truncated cone shape, and outer draft tube 4 is cylindrical, and it has third insulation material layer 24 to fill between interior draft tube 3 and the outer draft tube 4, and the upper end of interior draft tube 3 and outer draft tube 4 outwards extends and forms annular chimb 32, and the draft tube inlays through annular chimb 32 and adorns on graphite big lid 15.
In this embodiment, the first thermal insulation material layer 13, the second thermal insulation material layer 17 and the third thermal insulation material layer 24 are all thermal insulation carbon felt or solid felt.
In this embodiment, two positioning blocks 1 are symmetrically arranged at the bottom of the granular silicon charging barrel 29, a groove with a triangular cross section is formed between the two positioning blocks 1, and the quartz tube 27 is arranged at the bottom of the groove.
Example 2
The method for preparing the monocrystalline silicon by adopting the device in the embodiment 1 specifically comprises the following steps: thermal field clearance, feed, manage to find time leak, pressure gasification, melt, secondary feeding, crystal pulling, wherein:
step one, cleaning a thermal field: cleaning a thermal field in a single crystal furnace, installing a thermal field piece, and installing a melting crucible, a second heater, a material pipeline, a gas-solid cyclone separator and a feeding pipeline;
step two, secondary feeding: when the silicon material in the quartz crucible in the single crystal furnace is changed into molten silicon, a certain space is left in the quartz crucible, and the silicon material is continuously filled, which specifically comprises the following steps:
opening an external argon valve to add argon into the charging barrel through an air inlet on the granular silicon charging barrel, then opening a valve on the feeding pipe, wherein the granular silicon in the granular silicon charging barrel is brought into the single crystal furnace by the argon to enter a gas-solid cyclone separator from an inlet due to pressure difference between a single crystal furnace body and the granular silicon charging barrel;
step three, CCZ crystal pulling: the method is operated according to the normal crystal pulling process of the prior art, when monocrystalline silicon is pulled out of silicon liquid, an argon valve of granular silicon and a valve on a feeding pipeline are opened, the granular silicon continuously enters a melting crucible, and the silicon liquid can supplement the silicon liquid in the quartz crucible in time, so that the whole crystal pulling process is stably operated;
when the single crystal rod reaches the target length, ending operation is carried out, the silicon material inlet flow is gradually reduced, and finally feeding operation is stopped;
and when the crystal bar is cooled and pulled out, continuing to perform bar pulling operation.
In this embodiment, the gas-solid cyclone is a cyclone made of quartz or silicon carbide.
The performance ratio of the single crystal silicon prepared by the apparatus and the method of the present embodiment to the single crystal silicon prepared by the RCZ method in the prior art is shown in table 1;
TABLE 1 comparison of properties of single crystal silicon prepared according to the present invention and single crystal silicon prepared by the RCZ method
| Drawing method | Head resistance (omega. cm 3) | Tail resistor (omega. cm 3) | Head minority (us) | Tail minority carrier (us) |
| RCZ | 0.9 | 0.4 | 700 | 70 |
| CCZ (invention) | 0.85 | 0.85 | 700 | 650 |
As shown in Table 1, the method can realize that the granular silicon is directly used for producing the monocrystalline silicon by the CCZ method, the produced monocrystalline silicon has good relevant characteristics and uniform resistance distribution, and the resistance distribution surface of the monocrystalline silicon produced by normal RCZ drawing has the phenomenon of top and bottom height.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (9)
1. An apparatus for preparing monocrystalline silicon by directly using granular silicon in CCZ Czochralski method is characterized in that: including single crystal growing furnace and set up the granule silicon feeding device in single crystal growing furnace one side, wherein:
the single crystal furnace comprises a furnace body, a quartz crucible (8) used for placing raw materials is arranged in the furnace body, a graphite crucible is arranged outside the quartz crucible (8), a first heater is arranged on the periphery of the graphite crucible, a guide cylinder is arranged above the quartz crucible (8), a heat preservation cylinder is arranged in the furnace body, a first heat preservation material layer (13) is arranged between the heat preservation cylinder and the wall of the furnace body, the heat preservation cylinder comprises an upper heat preservation cylinder (5) and a lower heat preservation cylinder (14), the upper heat preservation cylinder (5) is arranged on the periphery of the guide cylinder, the lower heat preservation cylinder (14) is arranged on the periphery of the graphite crucible, a graphite large cover (15) is further arranged on the upper heat preservation cylinder (5), a through hole is formed in the middle of the graphite large cover (15), the guide cylinder is assembled in the through hole, a water screen (2) is arranged in the guide cylinder, a bottom protection pressing plate (16) is further arranged below the lower heat preservation cylinder (14), a second heat-insulating material layer (17) is arranged between the bottom protection pressing plate (16) and the bottom end of the furnace body, the bottom end of the furnace body is provided with a heating electrode (12), the heating electrode (12) penetrates through the bottom protection pressing plate (16) and the second heat insulation material layer (17), a melting material crucible (18), a material pipeline (20), a second heater (19) and a gas-solid cyclone separator (21) are also arranged in the furnace body, the melting crucible (18) is arranged between the guide cylinder and the upper heat-preserving cylinder (5) and is positioned above the quartz crucible (8), the bottom end of the melting material crucible (18) is provided with a hole, one end of the material pipeline (20) is provided with the gas-solid cyclone separator (21) the upper end of which is provided with an exhaust port (22), the other end penetrates through the graphite big cover (15) to be connected with the melting material crucible (18), the second heaters (19) are arranged on two sides of the bottom end of the melting crucible (18);
granule silicon feeding device includes granule silicon feed cylinder (29), quartz tube (27), air inlet (28) and gas outlet (31), granule silicon feed cylinder (29) are used for placing granule silicon (30), quartz tube (27) vertical set up in granule silicon feed cylinder (29), one side of granule silicon feed cylinder (29) upper end is equipped with air inlet (28), and the opposite side is equipped with gas outlet (31), the one end of keeping away from granule silicon (30) on quartz tube (27) pass through conveying pipeline (26) and valve (25) with feed inlet (23) of gas-solid cyclone (21) are connected.
2. The apparatus for the preparation of single crystal silicon by the CCZ czochralski method using granular silicon as claimed in claim 1, wherein: the quartz crucible (8) is a single-layer quartz crucible with the height of 400 mm.
3. The apparatus for the preparation of single crystal silicon by the CCZ czochralski method using granular silicon as claimed in claim 1, wherein: graphite crucible includes that crucible bang (7) and crucible hold in the palm (9), crucible hold in the palm (9) set up in the bottom of crucible bang (7), the crucible holds in the palm the bottom of (9) and still is equipped with die-pin (10), die-pin (10) pass the lower extreme of furnace body with graphite crucible set up in the furnace body.
4. The apparatus for the preparation of single crystal silicon by the CCZ czochralski method using granular silicon as claimed in claim 2, wherein: the first heater comprises a side heater (6) and a bottom heater (11), the side heater (6) is arranged on two sides of the graphite crucible, the side heater (6) is located between the graphite crucible and a lower heat preservation cylinder (14), the bottom heater (11) is fixed at the bottom of the furnace body through the heating electrode (12), and the bottom heater (11) is located below the graphite crucible.
5. The apparatus for the preparation of single crystal silicon by the CCZ czochralski method using granular silicon as claimed in claim 1, wherein: the draft tube comprises an outer draft tube (4) and an inner draft tube (3) arranged in the outer draft tube (4), the inner draft tube (3) is in a cone frustum shape, the outer draft tube (4) is cylindrical, a third heat insulation material layer (24) is filled between the inner draft tube (3) and the outer draft tube (4), the upper ends of the inner draft tube (3) and the outer draft tube (4) extend outwards to form an annular convex edge (32), and the draft tube is embedded in the graphite big cover (15) through the annular convex edge (32).
6. The apparatus for preparing single crystal silicon by the CCZ Czochralski method using the granular silicon as defined in claim 5, wherein: the first heat-insulating material layer (13), the second heat-insulating material layer (17) and the third heat-insulating material layer (24) are all heat-insulating carbon felts or solid felts.
7. The apparatus for the preparation of single crystal silicon by the CCZ czochralski method using granular silicon as claimed in claim 1, wherein: two positioning blocks (1) are symmetrically arranged at the bottom in the particle silicon charging barrel (29), a groove with a triangular section is formed between the two positioning blocks (1), and the quartz tube (27) is arranged at the bottommost end of the groove.
8. A method for preparing single crystal silicon by using the device of any one of claims 1 to 7, comprising the following steps: thermal field clearance, feed, manage to find time leak, pressure gasification, melt, secondary feeding, crystal pulling, wherein:
step one, cleaning a thermal field: cleaning a thermal field in a single crystal furnace, installing a thermal field piece, and installing a melting crucible, a second heater, a material pipeline, a gas-solid cyclone separator and a feeding pipeline;
step two, secondary feeding: when the silicon material in the quartz crucible in the single crystal furnace is changed into molten silicon, a certain space is left in the quartz crucible, and the silicon material is continuously filled, which specifically comprises the following steps:
pressure inside the single crystal furnace-pressure in the granular silicon barrel =0-0.5 torr;
opening an external protective gas valve to add protective gas into the charging barrel through a gas inlet on the granular silicon charging barrel, then opening a valve on a feeding pipe, wherein granular silicon in the granular silicon charging barrel is taken into the single crystal furnace by the protective gas and enters a gas-solid cyclone separator from a feed inlet, when the protective gas and the granular silicon pass through the gas-solid cyclone separator, the protective gas is separated from the granular silicon, the protective gas is discharged through a gas outlet, the granular silicon falls into a material pipeline through a discharge outlet at the bottom end of the gas-solid cyclone separator and is finally conveyed into a melting crucible, the granular silicon is melted in the melting crucible by a second heater, and the melted silicon flows into a quartz crucible through a small hole at the bottom of the melting crucible;
step three, CCZ crystal pulling: the method is operated according to a normal crystal pulling flow, when monocrystalline silicon is pulled out of silicon liquid, a protective gas valve of granular silicon and a valve on a feeding pipeline are opened, the granular silicon continuously enters a melting crucible, and the silicon liquid can supplement the silicon liquid in the quartz crucible in time, so that the whole crystal pulling process is stably operated;
when the single crystal rod reaches the target length, ending operation is carried out, the silicon material inlet flow is gradually reduced, and finally feeding operation is stopped;
and when the crystal bar is cooled and pulled out, continuing to perform bar pulling operation.
9. The method of using granular silicon directly in the CCZ czochralski process for the production of single crystal silicon according to claim 8, wherein: the gas-solid cyclone separator is made of quartz or silicon carbide.
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| CN114959874A (en) * | 2022-04-24 | 2022-08-30 | 杭州中欣晶圆半导体股份有限公司 | System and method for improving RRG value of radial crystal bar by using pull rate |
| CN114959874B (en) * | 2022-04-24 | 2024-04-23 | 杭州中欣晶圆半导体股份有限公司 | System and method for improving RRG value of radial crystal bar by using pull speed |
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