WO2012171308A1 - Procédé destiné à la production par coulée de silicium quasi-monocristallin - Google Patents

Procédé destiné à la production par coulée de silicium quasi-monocristallin Download PDF

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Publication number
WO2012171308A1
WO2012171308A1 PCT/CN2011/083714 CN2011083714W WO2012171308A1 WO 2012171308 A1 WO2012171308 A1 WO 2012171308A1 CN 2011083714 W CN2011083714 W CN 2011083714W WO 2012171308 A1 WO2012171308 A1 WO 2012171308A1
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WIPO (PCT)
Prior art keywords
furnace
single crystal
degrees celsius
heat insulating
ingot
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2011/083714
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English (en)
Chinese (zh)
Inventor
石坚
熊涛涛
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ANYANG PHOENIX PHOTOVOLTAIC TECHNOLOGY Co Ltd
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ANYANG PHOENIX PHOTOVOLTAIC TECHNOLOGY Co Ltd
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Priority claimed from CN2011101608010A external-priority patent/CN102242394A/zh
Priority claimed from CN201110160797.8A external-priority patent/CN102242392B/zh
Priority claimed from CN 201110160794 external-priority patent/CN102242390B/zh
Priority claimed from CN2011101608082A external-priority patent/CN102644104A/zh
Application filed by ANYANG PHOENIX PHOTOVOLTAIC TECHNOLOGY Co Ltd filed Critical ANYANG PHOENIX PHOTOVOLTAIC TECHNOLOGY Co Ltd
Publication of WO2012171308A1 publication Critical patent/WO2012171308A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • 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

Definitions

  • the present invention relates to the field of crystal growth technology, and further relates to a method of producing a single crystal similar to silicon by a casting method. Background technique
  • the methods for producing silicon ingots include: CZ method for producing single crystal silicon ingot, ingot casting method for producing polycrystalline silicon ingot, FZ method for producing single crystal silicon ingot, and EFG for producing silicon ribbon. Due to cost issues, current solar cell wafers mainly use CZ single crystal silicon wafers and cast polycrystalline silicon wafers.
  • the CZ method of single crystal silicon is 4 to 5 times higher than the ingot polycrystalline silicon, and the energy consumption is 5 to 7 times higher, resulting in less and less market share of CZ single crystal silicon.
  • the growth of a single crystal can only start from the bottom, which requires that the seed crystal at the bottom cannot be melted or floated when the silicon material is melted. Since the ingot furnace and the growth temperature curve of the GT ingot furnace or the four-sided top heater are not flat, if there is no good chemical and growth isotherm curve, the seed crystal will melt during the melting process and the center will not be welded normally. In the case, it is necessary to require a seed crystal of a height of 30 mm (mm, the same below) to maintain the material, and there is still seed crystal on the bottom of the furnace. This will inevitably increase the cost of seed crystals, resulting in high cost of similar single crystals and incapable of mass production. Or it can not produce similar single crystals.
  • the ingot furnace of GT or four-sided and top surface heaters is generally prior art, that is, the structure before improvement is shown in Fig. 1.
  • the heat conducting block 1 is placed in the lower part of the graphite crucible bottom plate 2, and the graphite crucible bottom plate 2 is placed with ceramics. ⁇ 5; the side of the ceramic crucible 5 is provided with a graphite crucible side guard 3; a side heater 4 is disposed above the periphery of the ceramic crucible 5 (the height of the ceramic crucible 5 (the height is generally 400 mm to 600 mm, if necessary)
  • a top heater 6 is disposed above the ceramic crucible 5; a heat insulating cage 7 is disposed around the side heater 4 and the top heater 6.
  • the simulated isothermal curve 8 is shown in Fig. 1.
  • the chemical and growth isothermal curves are not flat enough. It is shown that if the thermal field temperature gradient is not improved, it will not be possible to produce a similar single crystal (quasi-single crystal) with an ingot furnace of GT or four-sided and top-side heaters. This is why, until now, manufacturers of ingot furnaces that do not use GT or four-sided and top-side heaters have announced the possibility of producing a single crystal.
  • the method of stabilizing the bottom of the seed crystal can significantly improve the isothermal curve of the chemical material and the growth; thereby solving the problem of melting similar to the single crystal seed crystal, solving the problem of high equipment modification cost and high production cost similar to single crystal production.
  • the invention improves the furnace silicon material and the seed crystal placing method, the chemical material heating method, and the method for stabilizing the furnace bottom after melting in the furnace by changing the heat field device and material of the GT furnace or the four-sided heater plus the top heater, Thereby changing the internal temperature curve of the thermal field, improving the reliability of production, and achieving this goal.
  • the invention also provides a thermal field device and material improvement method for a GT furnace or a four-sided heater plus a top heater. By changing the thermal field gradient, stable production similar to single crystal is realized, and the success rate of similar single crystal production is improved.
  • the casting method produces a thermal field gradient improvement device similar to a single crystal silicon ingot, which is characterized in that: in a GT ingot furnace or an ingot furnace of four-sided and top heaters, four layers of insulation layers are provided outside the slab or slab . Used to insulate panels or rafts.
  • the insulation layer is disposed at one or two or three or four of the following positions: fixed on the sill plate, or fixed between the raft and the slab, or fixed on the heat insulation cage, or fixed on the heating On the device, or on the heat block.
  • the insulation layer can be divided into a vertical insulation layer and a horizontal insulation layer, wherein the height of the vertical insulation layer ensures that the upward edge of the slab and the sill is not upward; the lower edge of the heat conduction block does not exceed the thermal conduction block.
  • the lower edge is 100mm.
  • the insulating layer is set to one of the following cases a, b, c, d or a combination:
  • a heat insulation layer is disposed on the outer side surface of the sill guard plate, and the heat insulation layer is set from the position of the ⁇ 650mm upward from the bottom of the rafter; further, starting from the bottom of the rafter, the position of 5 ⁇ 600mm is the starting position.
  • the insulation layer is further provided; further, the insulation layer is set from the position of 10 to 550 mm from the bottom of the crucible; the specific starting position of the insulation layer is set from the bottom of the crucible to the following: lmm, 5mm, 10mm, 50mm, 90mm, 130mm, 170mm, 210mm, 250mm, 290mm, 330mm, 370mm, 410mm, 450mm, 490mm, 530mm, 550mm, 570mm, 600mm, 650mm.
  • the insulation layer is set vertically.
  • the heat insulating layer is disposed on the outer side surface of the sill guard plate and the outer side surface of the heat conducting block, and the heat insulating layer is set from a position 1 to 200 mm downward from the bottom of the rafter; further, 5 to 170 mm downward from the bottom of the rafter.
  • the position is the initial position to set the insulation layer; further, the insulation layer is set from the position of 10 ⁇ 150mm downward from the bottom of the crucible; the specific starting position of the insulation layer can be selected from the bottom of the crucible.
  • the insulation layer is set vertically.
  • the heat insulation layer is disposed on the inner side of the sill guard plate and on the outer side of the rafter, and the heat insulation layer is set from the position of the ⁇ 650mm upward from the bottom of the rafter; further, the position is 5 ⁇ 600mm upward from the bottom of the rafter.
  • Start to set the insulation layer further, set the insulation layer from the position of 10 ⁇ 550mm from the bottom of the crucible to the starting position; from the bottom of the crucible to the specific starting position of the insulation layer, you can choose one of the following: lmm, 5mm, 10, 50, 90, 130, 170, 210, 250, 290, 330, 370, 410, 450, 490,
  • the insulation layer is set vertically.
  • the insulating layer is disposed on the heat insulating cage or the heater or the heat conducting block, and the heat insulating layer is disposed from a position of ⁇ 1 to 400 mm from the bottom of the crucible; further, an insulating layer is disposed from a position of ⁇ 10 to 350 mm from the bottom of the crucible; further
  • the insulation layer is set from the bottom of the crucible ⁇ 20 ⁇ 300mm; one of the following positions can be selected: lmm, 5mm, 10mm, 20mm, 50mm, 100mm, 150mm, 200mm, 250mm, 300mm, 350mm, 400mm.
  • the insulating layer is horizontally disposed, and the width of the insulating layer is 50 to 500 mm; further 100 to 450 mm; further 150 to 400 mm.
  • the width of the specific insulation layer can be selected from one of the following: 50mm, 100mm, 150mm, 200mm, 250mm, 300mm, 350mm, 400mm, 450mm, 500mm.
  • the height of the insulating layer is from 1 to 650 mm; further from 20 to 600 mm; further from 50 to 550 mm.
  • the height of the specific insulation layer can be selected from one of the following: lmm, 10mm, 20mm, 50mm, 90mm, 130mm, 170mm, 210mm, 250mm, 290mm, 330mm, 370mm, 410mm, 450mm, 490mm, 530mm, 550mm, 570mm, 600mm, 650mm .
  • the thickness of the insulating layer is 0.01 to 100 mm; further 0.1 to 60 mm; further 1 to 40 mm.
  • the thickness of the specific insulation layer can be selected as follows: 0.01mm, 0.1mm, 3.0mm, 6.0mm, 9.0mm, 12mm, 15mm, 18mm, 21mm, 24mm, 27mm, 30mm, 33mm, 36mm, 39mm, 42mm, 45mm, 48mm, 51mm, 55mm, 60mm, 65mm, 70mm, 75mm, 80mm, 85mm, 90mm, 95mm, 100mm.
  • the heat insulating layer is arranged by a step from 2 to 5 on the inside to the outside, from the top to the bottom or from the top to the bottom or from the top to the bottom, or on the upper and lower thin middle portions or the upper, lower, middle and lower portions, and the insulation layer of the adjacent step is adopted.
  • the materials are the same or different.
  • the material of the insulation layer is made of a non-metal insulation material or a metal insulation material.
  • the material of the heat insulating layer is a non-metal heat insulating material
  • the non-metal heat insulating material comprises one or a combination of the following materials: graphite felt, ceramic, quartz, various curing felts, fiber mats, carbon felt, carbon fiber or ceramic fiber.
  • Insulation felt or insulation block made of raw materials, alumina fiber felt, thermal insulation felt or thermal insulation block using various structural alumina fibers as main raw materials, thermal insulation felt or thermal insulation block using various structural zirconia fibers as main raw materials.
  • the material of the heat insulating layer is made of a metal heat insulating material, and the metal heat insulating material comprises one or a combination of the following materials: tungsten, molybdenum and a high temperature alloy having a melting point of 1600 degrees Celsius or more.
  • the thermal conductivity of the non-metallic thermal insulation material is between 0.001 and 5 W/mK (Watt/m*Kelvin); the thermal conductivity of the non-metallic thermal insulation material is between 0.05 and 3 W/mK; further thermal conductivity of the non-metallic thermal insulation material The coefficient is between 0.1 and 1 W/mK.
  • the beneficial effects of the method are as follows: the device is used in the GT furnace or the ingot furnace of the four-sided and top heaters, and the isothermal curve of the chemical material and the growth can be significantly improved; and the seed crystal can be solidified at the bottom of the furnace without melting or floating.
  • the seed height can be further reduced, and the seed crystal can be controlled to be 20 mm or less by this method.
  • the drop in seed height can effectively reduce production costs.
  • the invention simultaneously provides the improvement of the photoelectric conversion efficiency of the product in the process of growing a similar single crystal (quasi-single crystal) in the ingot furnace of the GT or the four-sided and top surface heaters, thereby improving the photoelectric conversion efficiency of the product, improving the similar single crystal A method of producing problems in the middle seed crystal that is easy to melt.
  • the casting method produces a silicon-like material and a seed crystal placement method similar to a single crystal silicon ingot, which is characterized in that: A single piece of silicon material weighing 200 g (g, the same below) is spread over the seed crystal by a thickness of 0.5 to 60 cm (cm, the same below); b is a distance between the seed crystals of 0.1 mm.
  • the silicon material has a thickness of 0.5 to 50 cm.
  • the silicon material has a thickness of 1 to 20 cm.
  • the silicon material has a thickness of 2 to 10 cm.
  • the thickness of the silicon material can also be selected as follows: 0.5 to 5 cm, or 5 to 10 cm, or 10 to 20 cm, or 20 to 30 cm, or 30 to 40 cm, or 40 to 50 cm, or 50 to 60 cm.
  • the beneficial effects of the method are as follows: 1. By the control of the method, the defects caused by the seed crystal can be reduced. The problem that the photoelectric conversion efficiency of the product is low due to a large number of dislocations in the single crystal can be improved, and the photoelectric conversion efficiency of the single crystal growth of the ingot furnace is improved, and the relevant test shows that the absolute value of the efficiency can be increased by about 0.1%. 2. At the same time, improve the high cost of similar single crystal production. When the seed crystal thickness is controlled below 20mm, the success rate of growing a single crystal is increased by 20%, and the production cost of a single furnace (about 450kg or kilogram) can be reduced by more than 1,000 yuan.
  • the invention also provides a casting method for producing a similar single crystal silicon ingot heating method.
  • the method is adopted, and the temperature gradient is controlled by the ceramic material.
  • ⁇ does not crack due to excessive thermal stress, and the crystal does not melt or float.
  • the growth of a single crystal can only start from the bottom, which requires that the seed crystal at the bottom cannot be melted or floated when the silicon material is melted.
  • the seed crystal of the bottom of the furnace in order to make the seed crystals not melt, the seed crystal of the bottom of the furnace must be kept at a lower temperature, and the heater must be kept at a temperature of 1420 ° C or higher at a lower temperature of the bottom of the furnace, which causes the ceramic crucible to withstand very much during the heating process. Large temperature gradients, if this temperature gradient cannot be controlled within the temperature gradient that the ceramic material can withstand, will cause the ceramic crucible to crack, causing silicon leakage, resulting in a safety accident. It is impossible to grow a single crystal, which causes the entire process to fail.
  • the chemical heating process is performed to fix the seed crystal to the bottom of the furnace without undulating or melting, and ⁇ does not appear. Cracking situation.
  • the casting method produces a heating method similar to a single crystal silicon ingot, which is characterized in that the ingot furnace is heated from a room temperature to a predetermined maximum temperature, and the following is employed. Control measures:
  • TC1 the temperature value of the thermocouple near the top heater
  • AT TC1 (temperature value of the thermocouple near the top heater) - TC2 (temperature sensor temperature value under the thermal block at the bottom)
  • ⁇ ⁇ is the difference between the temperature value of the temperature sensor near the top heater and the temperature of the temperature sensor under the heat block at the bottom);
  • the predetermined maximum temperature refers to 1420 to 1600 degrees Celsius, and further the predetermined maximum temperature refers to 1440 to 1580 degrees Celsius, and further the predetermined maximum temperature refers to 1460 to 1560 degrees Celsius.
  • the maximum temperature can also be set to 1420 to 1440 degrees Celsius, or 1440 to 1460 degrees Celsius, or 1460 to 1480 degrees Celsius, or 1480 to 1500 degrees Celsius, or 1500 to 1520 degrees Celsius, or 1520 to 1550 degrees Celsius, or 1550 to 1580 degrees Celsius, Or 1580 ⁇ 1600 degrees Celsius.
  • the control refers to controlling the heating power and heating time, or controlling the heating temperature and heating time, or controlling the heating power and heating time as well as the position of the cage, or controlling the heating temperature and heating time and the position of the cage.
  • the beneficial effects of the method are as follows: Through the application of the method, during the heating process, the temperature gradient is controlled within the range that the material of the tantalum ceramic can withstand, and the crucible is not cracked due to excessive thermal stress. And the seed crystals are solidified at the bottom of the furnace without melting or floating. It not only ensures production safety, but also improves production efficiency.
  • the invention also provides a method for producing a seed crystal-stabilized furnace bottom after melting in a single crystal silicon ingot furnace, and a similar single crystal (quasi-single crystal) process in an ingot furnace of a GT or four-sided and top surface heater. Medium, the seed crystal is fixed at the bottom of the furnace without undulation.
  • the method performs the grasping seed crystal process by controlling the temperature of the temperature measuring coupler under the heat conducting block at the bottom of the furnace (TC2), so that the seed crystal is fixed at the bottom of the furnace without undulation.
  • the casting method produces a method for stabilizing the bottom of the furnace after melting in a single crystal silicon ingot furnace, which is characterized by: GT polycrystalline ingot furnace or four-sided heater plus top heater ingot furnace:
  • TC1 the temperature of the thermocouple near the top heater
  • TC2 the temperature of the thermocouple under the thermal block at the bottom
  • the control time of TC2 is 20 ⁇ 500 minutes
  • the beneficial effects of the method are as follows: In the process of growing a similar single crystal (quasi-single crystal) in an ingot furnace of a GT or four-sided and top-side heater by the control of the method, the molten silicon liquid is always undercooled at the bottom of the furnace. The viscous state, so that the seed crystal is solidified at the bottom of the furnace, does not melt or float, and at the same time, the seed crystal height can be further reduced, thereby reducing the cost.
  • the overall beneficial effects of the present invention are: Providing a casting method for producing similar single crystal silicon, including improvement of thermal field gradient of ingot furnace, furnace silicon material and seed crystal placement method, chemical heating method, furnace interior
  • the method of stabilizing the bottom of the seed after melting can significantly improve the isothermal curve of the chemical material and the growth; thereby solving the problem of melting similar to the single crystal seed crystal, and solving the problem of high equipment modification cost and high production cost similar to single crystal production.
  • the seed crystal can be controlled to be 20 mm or less. The decrease in seed height can effectively reduce production costs and increase production safety.
  • FIGS. 2 to 5 are schematic views of the present invention.
  • Example 1 An embodiment of a casting method for producing a thermal field gradient improving device similar to a single crystal silicon ingot: Example 1:
  • the heat conducting block 1 is placed on the lower part of the bottom guard 2 (the bottom guard is generally made of graphite material), and the bottom cover 2 is placed with ⁇ 5 (---------------
  • the side side is provided with a side guard 3 (the side guard is generally made of graphite material); a side heater 4 is arranged above the circumference of the ⁇ 5 ( ⁇ 5-like height 400mm to 600mm, if necessary, can be raised)
  • a top heater 6 is disposed above the crucible 5; a heat insulating cage 7 is disposed around the side heater 4 and the top heater 6, wherein the lower heat insulating cage 7 is fixed, and the upper and surrounding heat insulating cages 7 are One, can be improved.
  • Surrounding insulation layer 9 (only one side insulation layer 9 is shown for clarity of illustration) is disposed on the side of the crucible side panel 3 of the crucible 5 and the heat conducting block 1, and is in close contact with the side panel 3 and the heat conducting block 1
  • the simulated isotherm curve 8 formed after the improvement is shown in Fig. 2.
  • the isothermal curve is obviously flat, indicating that the improved thermal field already has the basic conditions for producing a single crystal.
  • the insulation layer is divided into two vertical and horizontal directions.
  • the vertical insulation layer is divided into three layers.
  • the innermost layer is graphite felt.
  • the thickness of the graphite felt is 10mm.
  • the upper end of the graphite felt and the side cover 3 are along.
  • the lower end is flush with the lower end of the thermal block 1; the overall height is 1000mm (or about 1000mm) (this height can be called the height of the insulation layer, that is, the height of the largest single layer of the multi-layer insulation layer, which can be called the multi-layer insulation layer the height of).
  • the middle layer material is quartz, the thickness of the quartz is 5mm, the upper end of the quartz is 150mm (or 150mm) from the side of the side guard 3, and the lower end is flush with the lower end of the heat conducting block 1; the overall height is 850mm (or about 850mm).
  • the outermost layer material is alumina fiber felt, the thickness of the alumina fiber felt is 20mm, the upper end of the alumina fiber felt is 450mm (or 450mm) from the side of the side guard 3, and the lower end is flush with the lower end of the heat conducting block 1; the overall height It is 550mm (or 550mm or so).
  • the three-layer vertical insulation layer 9 is formed by a stepped upper and lower thickness from the inside to the outside.
  • a horizontal insulation layer is arranged on the lower edge portion of the heat conducting block.
  • the material is selected from alumina fiber felt with a width of 300 mm (or about 300 mm), and the outer end is flush with the outer edge of the vertical insulation layer, and the thickness of the insulation layer is 20 mm.
  • the heat conducting block 1 is placed on the lower part of the bottom guard 2 (the bottom guard is generally made of graphite material), and the bottom cover 2 is placed with ⁇ 5 (-----------
  • the side side is provided with a side guard 3 (the side guard is generally made of graphite material); a side heater 4 is arranged above the circumference of the ⁇ 5 ( ⁇ 5-like height 400mm to 600mm, if necessary, can be raised)
  • a top heater 6 is disposed above the crucible 5; a heat insulating cage 7 is disposed around the side heater 4 and the top heater 6, wherein the lower heat insulating cage 7 is fixed, and the upper and surrounding heat insulating cages 7 are One, can be improved.
  • the insulating layer 9 is horizontally oriented, the material is an insulating block made of carbon fiber as the main raw material, and the outer edge is fixed on the heat insulating cage 7 at a position of 250 mm (or about 250 mm) at the bottom of the ⁇ 5, the thermal insulation block.
  • the width is 300mm (or about 300mm) and the thickness is 100mm (or about 100mm).
  • the heat conducting block 1 is placed on the lower part of the bottom guard 2 (the bottom guard is generally made of graphite material), and the bottom cover 2 is placed with ⁇ 5 (---------------
  • the side side is provided with a side guard 3 (the side guard is generally made of graphite material); a side heater 4 is arranged above the circumference of the ⁇ 5 ( ⁇ 5-like height 400mm to 600mm, if necessary, can be raised)
  • a top heater 6 is disposed above the crucible 5; a heat insulating cage 7 is disposed around the side heater 4 and the top heater 6, wherein the lower heat insulating cage 7 is fixed, and the upper and surrounding heat insulating cages 7 are One, can be improved.
  • Surrounding insulation layer 9 (only one side insulation layer 9 is shown for clarity of illustration) is placed outside the ⁇ 5 side sill 3, close to the sill side sill 3; simulated isothermal formation Curve 8 is shown in Figure 4. As can be seen from the figure, the curve is clearly flat, indicating that the improved thermal field already has the basic conditions for producing a single crystal.
  • the insulating layer 9 is vertically divided into three layers, the innermost layer material is carbon felt, the thickness of the carbon felt is 5 mm, the end is aligned with the top side guard plate 3, and the lower end is flush with the lower end of the heat conducting block 1; the overall height About 1000mm (or about 1000mm) (this height can be called the height of the insulation layer, that is, the height of the largest single layer of the multi-layer insulation layer, which can be called the height of the multi-layer insulation layer).
  • the middle layer material is carbon felt, the thickness of the carbon felt is 10mm, the upper end of the carbon felt is 150mm from the upper side of the side guard 3, and the lower end is placed at the lower end of the heat conducting block 1 of the bottom guard 2; the overall height is about 500mm (or 500mm) about).
  • the outermost material is a tungsten superalloy, the thickness of the tungsten superalloy is 0.1 mm, and the lower end of the tungsten superalloy is flush with the bottom of the bottom shield 2; the overall height is about 250 mm (or about 250 mm).
  • the three-layer vertical insulation layer 9 is formed by a stepped upper and lower thickness from the inside to the outside.
  • the heat conducting block 1 is placed on the lower part of the bottom guard 2 (the bottom guard is generally made of graphite material), and the bottom cover 2 is placed with ⁇ 5 (---------------
  • the side side is provided with a side guard 3 (the side guard is generally made of graphite material); a side heater 4 is arranged above the circumference of the ⁇ 5 ( ⁇ 5-like height 400mm to 600mm, if necessary, can be raised) , a top heater is placed above the ⁇ 5 6;
  • the side heater 4 and the top heater 6 are provided with a heat insulating cage 7 around the bottom, wherein the lower heat insulating cage 7 is fixed, and the upper and the surrounding heat insulating cages 7 are integrated and can be lifted.
  • the material selected carbon fiber as the main raw material of the thermal insulation felt is the height is the same as ⁇ 5, the thickness of the insulation layer is 20mm.
  • the casting method produces a silicon-like ingot-like silicon furnace and a seed crystal placement method as follows:
  • the casting method produces a single crystal silicon ingot furnace silicon material and a seed crystal placement method, and produces a similar single crystal in a cast polycrystalline furnace (GT furnace, and a structural polycrystalline casting furnace using a four-sided heater and a top heater). Quasi-single crystal), using a silicon material with a weight of less than or equal to 10g, and a thickness of 5cm above the seed crystal; the distance between the seeds is less than 0.03mm.
  • the casting method produces a single crystal silicon ingot furnace silicon material and a seed crystal placement method, and produces a similar single crystal in a cast polycrystalline furnace (GT furnace, and a structural polycrystalline casting furnace using a four-sided heater and a top heater). Quasi-single crystal), using a silicon material with a weight of less than or equal to 5g, and a thickness of 40cm above the seed crystal; the distance between the seeds is less than 0.03mm.
  • the casting method produces a single crystal silicon ingot furnace silicon material and a seed crystal placement method, and produces a similar single crystal in a cast polycrystalline furnace (GT furnace, and a structural polycrystalline casting furnace using a four-sided heater and a top heater). Quasi-single crystal), using a single piece of silicon material having a weight less than or equal to 50 g, and a thickness of 30 cm above the seed crystal; the distance between the seed crystals is less than or equal to 0.1 mm.
  • the casting method produces a similar heating method for a single crystal silicon ingot chemical material as follows:
  • the casting method produces a heating method similar to that of a single crystal silicon ingot.
  • the ingot furnace is heated from room temperature, and the following control is performed as required:
  • the casting method produces a heating method similar to that of a single crystal silicon ingot.
  • the ingot furnace is heated from room temperature, and the following control is performed as required:
  • the casting method produces a heating method similar to that of a single crystal silicon ingot.
  • the ingot furnace is heated from room temperature, and the following control is performed as required:
  • the casting method produces a method similar to the case where the seed crystal is stabilized at the bottom of the furnace after melting in a single crystal silicon ingot furnace, and is characterized by: GT polycrystalline ingot furnace or four-sided heater plus top heater ingot furnace:
  • the TC2 is raised to 1370 ⁇ 1375 degrees Celsius by controlling the insulation cage, and the second step is stabilized for 30 minutes;

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

On divulgue dans la présente invention un procédé pour la production par coulée de silicium quasi-monocristallin, des procédés associés, comprenant une amélioration de l'équipement d'un four à lingot pour un four à GT (gradient de température) ou pour un chauffage des quatre côtés et du sommet, et la régulation de la croissance de cristaux quasi-monocristallins. L'amélioration de l'équipement d'un four à lingot comprend un dispositif destiné à l'amélioration du gradient de température des lingots de silicium quasi-monocristallin. La régulation de la croissance des cristaux quasi-monocristallins peut comprendre un procédé ou une combinaison de procédés : un procédé d'agencement du matériau de silicium et du germe cristallin dans un four, un procédé de chauffage des matériaux chimiques et un procédé de stabilisation au fond d'un germe cristallin après fusion du contenu du four. L'avantage de la présente invention réside en ce que, au moyen d'une modification du dispositif de champ thermique et des matériaux du four à GT ou du chauffage des quatre côtés et du sommet, du procédé pour la coulée de matériau de silicium et l'agencement d'un germe cristallin, du procédé de chauffage des matériaux chimiques et du procédé de stabilisation au fond d'un germe cristallin après fusion du contenu du four, la courbe de température interne du champ thermique est modifiée et les courbes isothermes des matériaux chimiques et de la croissance sont toutes deux améliorées. La présente invention résout les problèmes de fusion des germes cristallins quasi-monocristallins et les problèmes associés au coût élevé, à la faible fiabilité et au faible taux de succès de leur production
PCT/CN2011/083714 2011-06-15 2011-12-08 Procédé destiné à la production par coulée de silicium quasi-monocristallin Ceased WO2012171308A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
CN2011101608010A CN102242394A (zh) 2011-06-15 2011-06-15 铸造法生产类似单晶硅锭投炉硅料和晶种摆放方法
CN201110160801.0 2011-06-15
CN201110160797.8A CN102242392B (zh) 2011-06-15 2011-06-15 铸造法生产类似单晶硅锭炉内融化后晶种稳定于炉底的方法
CN201110160797.8 2011-06-15
CN 201110160794 CN102242390B (zh) 2011-06-15 2011-06-15 铸造法生产类似单晶硅锭化料加热方法
CN201110160808.2 2011-06-15
CN2011101608082A CN102644104A (zh) 2011-06-15 2011-06-15 铸造法生产类似单晶硅锭热场梯度改进装置
CN201110160794.4 2011-06-15

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