WO2005092791A1 - シリコン鋳造装置および多結晶シリコンインゴットの製造方法 - Google Patents
シリコン鋳造装置および多結晶シリコンインゴットの製造方法 Download PDFInfo
- Publication number
- WO2005092791A1 WO2005092791A1 PCT/JP2005/006549 JP2005006549W WO2005092791A1 WO 2005092791 A1 WO2005092791 A1 WO 2005092791A1 JP 2005006549 W JP2005006549 W JP 2005006549W WO 2005092791 A1 WO2005092791 A1 WO 2005092791A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silicon
- heat
- cooling
- pedestal
- area
- Prior art date
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 256
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 248
- 239000010703 silicon Substances 0.000 title claims abstract description 248
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000005266 casting Methods 0.000 title abstract 2
- 238000001816 cooling Methods 0.000 claims abstract description 198
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 103
- 238000007711 solidification Methods 0.000 claims abstract description 82
- 230000008023 solidification Effects 0.000 claims abstract description 82
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 90
- 239000011261 inert gas Substances 0.000 claims description 41
- 230000008859 change Effects 0.000 claims description 19
- 239000000835 fiber Substances 0.000 claims description 18
- 230000001965 increasing effect Effects 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 15
- 230000000630 rising effect Effects 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 10
- 238000005345 coagulation Methods 0.000 claims description 9
- 230000015271 coagulation Effects 0.000 claims description 9
- 230000017525 heat dissipation Effects 0.000 claims description 5
- 241000283074 Equus asinus Species 0.000 claims 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims 1
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 241000282472 Canis lupus familiaris Species 0.000 description 23
- 239000002994 raw material Substances 0.000 description 19
- 239000013078 crystal Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 11
- 239000002210 silicon-based material Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000000498 cooling water Substances 0.000 description 9
- 230000007547 defect Effects 0.000 description 9
- 229920001864 tannin Polymers 0.000 description 9
- 239000001648 tannin Substances 0.000 description 9
- 235000018553 tannin Nutrition 0.000 description 9
- 230000003028 elevating effect Effects 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 210000002414 leg Anatomy 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 241000238631 Hexapoda Species 0.000 description 5
- 239000011810 insulating material Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 230000002093 peripheral effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 230000001174 ascending effect Effects 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 210000000689 upper leg Anatomy 0.000 description 4
- 241000219995 Wisteria Species 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012809 cooling fluid Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000110 cooling liquid Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 241000269350 Anura Species 0.000 description 1
- 235000007575 Calluna vulgaris Nutrition 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- MMOXZBCLCQITDF-UHFFFAOYSA-N N,N-diethyl-m-toluamide Chemical compound CCN(CC)C(=O)C1=CC=CC(C)=C1 MMOXZBCLCQITDF-UHFFFAOYSA-N 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- -1 for example Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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
- 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
-
- 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
- C30B11/002—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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
- H01L31/182—Special manufacturing methods for polycrystalline Si, e.g. Si ribbon, poly Si ingots, thin films of polycrystalline Si
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/546—Polycrystalline silicon PV cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1056—Seed pulling including details of precursor replenishment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1064—Seed pulling including a fully-sealed or vacuum-maintained crystallization chamber [e.g., ampoule]
Definitions
- the present invention is used for silicon S for solar cells, etc. ⁇ !
- the present invention relates to a silicon manufacturing apparatus for setting Yoshiaki silicon ingots and a method for manufacturing polycrystalline silicon ingots. Background leakage
- the quality of the polycrystalline silicon ingot which reduces the carrier mobility in the solar cell and reduces the energy sensitivity of the solar cell, is a factor in the end result. It depends greatly on the number (area), the properties of the grain boundaries, the orientation in the formation, the defect density, and the like. Therefore, in order to improve the energy J rate of a solar cell using polycrystalline silicon, it is necessary to establish a wide range of research and research on these items.
- Polycrystalline silicon ingot is made by pouring a silicon melt that has been heated and melted into a mirror mold, or by putting silicon raw material into ⁇ and melting it by calo-heating to reduce silicon rain. After that, while keeping or heating the upper part of the inversion, the child in the face of the face is rubbed, and the silicon in the face is removed by giving a positive gradient upward from the comfort side.
- the melt is produced by unidirectional solidification.
- the polycrystalline silicon ingot obtained in this way has the side and bottom surfaces of the ingot with many defects and impurities.
- FIGS. 12A and 12B show polycrystalline silicon ingots obtained by the above-described unidirectional solidification technique described in Japanese Patent Publication No. JP-A-04-068276B (1992).
- FIG. 4 is a longitudinal sectional view showing an example of a silicon device for manufacturing a got.
- the silicon-t apparatus of this example includes a furnace 21 whose bottom is opened by an opening 21a.
- a water-coolable chill plate 26 that can be moved up and down is arranged at the opening 2 la of the furnace 21, and a gap between the outer peripheral edge of the water-cooled chinole plate 26 and the inner peripheral surface of the opening 21 a is provided.
- a cylindrical apology book 27 is provided which can be moved up and down in the opening 21 a separately from the cold chill plate 26.
- Fujitan 24a and a side plate 24b rising upward from the periphery of this play: Anti24a and holds the silicon melt 22 inside.
- Key 24 is provided in such a manner that it can be moved up and down together with the book 27.
- ⁇ 24 holding silicon ⁇ 22 inside is replaced with a predetermined ⁇ . It is placed at the ascending position inside the furnace 21 where the ass heats. At this time, the water-cooled chill plate 26 is lowered and separated from the bottom surface of 24.
- the water-cooled chill plate 26 is raised while being cooled through the cooling water 25, and is brought into contact with the bottom surface of the radiator 24. ⁇ Cool 24 a side. Then, the ⁇ -type 24, the water-cooled chill plate 26, and the shouting book 27 are gradually lowered, and are gradually drawn out of the furnace 21 through the opening 2la. Since the inside of 1 is heated to a predetermined temperature as in Chapter 3, a gradient is generated in the silicon 22 in the surface 24, and the silicon ⁇ 22 is solidified in the negative direction, so that the polycrystal is formed. Silicon ingot
- the solid-liquid interface of silicon night 22 exists near the water-cooled chill plate 26 and near the sickle 24 a of type 24,
- the solidification avoidance is large, as the solidification progresses and the solid-liquid interface rises, the amount of heat generated due to the thickness of the solid layer increases, and the heat removal capacity by the water-cooled chill plate 26 decreases. It tends to be smaller. Therefore, in the above-mentioned document, the type 24, the water-cooled chill plate 26, and the apology book 27 are lowered to prevent them from being pulled out of the furnace 21 and the addition of the furnace 21. According to the combination, it is stated that the coagulation is $ Sir.
- the cooling capacity of the water-cooled chill plate 26 is constant Therefore, even if the key 24 is pulled out of the furnace 21 or the calorie of the furnace 21 is adjusted as described above, the gradient is maintained until the initial solidification or complete solidification. It is difficult to grow silicon crystallographically while keeping silicon within a certain range and solidifying silicon ⁇ with almost constant evacuation. Therefore, a polycrystalline silicon ingot having substantially uniform crystal grain size, the number of crystal grain boundaries, properties of grain boundaries, orientation within crystal grains, defect density, and the like in the thickness direction (that is, sliced in the thickness direction) Therefore, there is a problem that S3 ⁇ 4g cannot be carefully re-produced (a polycrystalline silicon base I: a polycrystalline silicon ingot that can produce as many as possible).
- FIG. 13 shows a method for producing a polycrystalline silicon ingot by the
- FIG. 5 is a longitudinal sectional view showing another example of the silicon ⁇ i device of FIG.
- the silicon device in this example has an upper chamber (furnace) 31 having a force n 34 as a groove and a cooling water cooled by cooling water 42.
- the lower chamber 3 2 having the plate 4 1 is measured with a barrier 3 3 made of a heat insulating material, and connected with a perforation 35 provided on the barrier 3.3, and a sickle 38 a and a periphery of the sickle 38 a
- the side plate 3 8b raised from the side, the customer 3 8 for holding the silicon 3 9 inside is raised and lowered by the ascending and closing 37 in the upper chamber 3 1, so that the communication port 3 5 is set to be possible for $ 1.
- the mold 38 closes the shaft 35 and heat insulating material 40 for insulating the space between the table 36 and the cooling plate 41.
- a mirror 36 is thermally connected to the cooling plate 41, and a table 36 for cooling is arranged on the ascending and closing 37 in this order. It is arranged.
- the quality of the polycrystalline silicon ingot is influenced by the quality.
- the ⁇ -type 38 is lowered as described above, so there is a distance between 1 ⁇ 38 and the heel, 34 Due to the variation of the temperature of the type 38 with respect to the upper chamber 31, the flow of heat into and out of the type 38 is likely to fluctuate.
- the atmosphere in the upper chamber 31 was made of an atmosphere of an inert gas such as Ar; t, and most of the heat from the sun 34 was transferred to ⁇ 38 by the thigh, so that both g The change in concealment causes a significant change in the amount of heat input from hir — 34 to ⁇ 38.
- a nozzle is provided in the furnace as described in Japanese Patent Disclosure II: Open Publication JP 2011-1081 OA.
- an inert gas such as Ar
- the silicon can be agitated by the heat flow and the concentration of impurities at the solid-liquid interface is suppressed.
- the unidirectional solidification S3 ⁇ 4 method is performed in which the impurities having a small distribution coefficient are refined in the upper part of the ingot to reduce the amount of impurity elements in the ingot.
- the pedestal on which is mounted is fixed to the caro furnace, and cooled by water. It describes a silicon-it device that is designed to work with a bottom plate through a pedestal. Also, in the above literature, the amount of heat from ⁇ is suppressed by suppressing the amount of ⁇ 3 ⁇ 4 ⁇ water supplied to the pedestal in the early stage of silicon solidification at night, and the amount of cooling water is gradually increased with the progress of solidification. It is stated that increasing the amount of heat from awakening stably stabilizes the gradient from the initial solidification to complete solidification.
- the effect of adjusting the amount of heat provided by changes in the amount of cooling water is not sufficient.
- the amount of thigh from the hot mirror is proportional to the difference between ⁇ and ⁇ 3 ⁇ 4] awakening and the size of the area where heat exchange takes place (heat area).
- heat area the area where heat exchange is performed.
- the area where heat exchange is performed is constant only by changing the difference between the mirror type and the P leak by increasing or decreasing the amount of cooling water.
- the change in the amount of cooling water is also caused by the change in the amount of cooling water.
- the change is only a small change compared to the separation of silicon at night, which is a high temperature of more than 144 ° C.
- An object of the present invention is to combine a silicon arrangement capable of producing a higher quality polycrystalline silicon ingot with good reproducibility and as low cost as possible, and a method of manufacturing a polycrystalline silicon ingot. is there.
- the silicon device of the present invention comprises a wisteria, a side plate rising upward from the periphery of the game, and a key for holding silicon acid night inside, ⁇ which is located above the mold and
- the mirror type and the kanji are arranged in a state where the distance is fixed.
- the bottom surface which is the lower surface of the ⁇ type is provided.
- the ⁇ -type is placed opposite to the heat-dissipating surface, which is the surface other than the mounting surface, of the pedestal on which the bottom surface is placed on the mounting surface in a state of being insulted. It has a ⁇ surface that constitutes a heat zone together with the incendiary surface, and is moved relative to the ⁇ or the pedestal to change the heat exchange area between the opposing thigh surface and the heat receiving surface. It is.
- ⁇ and I » are arranged in a state where the distance is constant, the key is changed from the force-playing fiber structure to the key due to the fluctuation of the above character. Fluctuations in the amount of heat can be suppressed.
- the bottom cooling member which is cooled, is moved relative to the mold, etc., so that it is formed between the heat receiving surface provided on the JS surface cooling and the heat radiation surface provided on the bottom surface of the key. Since the area of the heat exchanger in the heat exchange area is changed, the amount of heat removed from the heat due to cooling can be sufficiently improved. Therefore, according to the present invention, during the period from the initial solidification to ⁇ : solidification, the separation gradient is stably maintained within a certain range, and the silicon penetrates at a substantially constant speed while the silicon penetrates. Since the crystal growth of the crystal can be achieved, the number of cubic diameters, the number of cubic boundaries, the properties of the grain boundaries, the orientation within the lattice, the defect density, etc. are almost uniform in the thickness direction, resulting in higher quality polycrystals. It is possible to produce silicon ingots with good reproducibility and as low cost as possible.
- the sigma between ⁇ and k should be kept constant at least during the sst step of the polycrystalline silicon ingot by unidirectional solidification.
- the sigma between ⁇ and k should be kept constant at least during the sst step of the polycrystalline silicon ingot by unidirectional solidification.
- the surface is moved in the direction of the key or the pedestal in the direction of the surface while the surface is recited to the hot surface and the concubine in order to change the surface area.
- the as-surface member has a high thermal coefficient because the heat receiving surface is directly assigned to the thigh surface of the torsion, etc. When changed, the calorific value can be changed quickly with good response.
- the bottom ⁇ ⁇ ! In order to change the area of the heat sink, the heat receiving surface is spaced apart from the heat radiating surface at a fixed interval, while being moved in the surface direction with respect to the triangle or pedestal. 3 ⁇ 4 of 3 ⁇ 4.
- the surface should be kept at a fixed interval without directly contacting the heat-dissipating surface of the mold, etc. In this state, the antarctica is heated while working together, so that it is possible to prevent target wear on both sides.
- the heat tan is the radiation of heat between the heat radiating surface and the heat receiving surface or the heat radiation. It is done by flow. Therefore, in order to perform thermal tannin more efficiently, it is preferable that the distance between the heat receiving surface and the heat receiving surface is 10 mm or less.
- the pedestal When the heat radiating surface is other than the surface on which the key is placed on the pedestal, in order to more efficiently leak the key from the key to the bottom cooling member via the pedestal, the pedestal must pay 4 OW. It is preferably at least / (m ⁇ K).
- the pedestal is used in order to reduce the distribution of frogs on the wisteria side of the key and to improve the unidirectional solidification of the silicon substrate 8. It is preferable to be thick. That is, the pedestal has one side, the mounting surface, and the mounting surface, and the opposite surface is TO. The pedestal is formed to have a constant thickness, and the thickness is set to the mounting surface, and It is preferable that the length is 1/61 ⁇ ⁇ of the length of the ⁇ 4 region between the bottom surface of the device and the bottom surface of the device.
- the silicon device according to the present invention is capable of stabilizing the gradient from the initial solidification to the complete solidification more stably and producing a high-quality polycrystalline silicon ingot with high reproducibility.
- the silicon device of the present invention has It has inert injection gas discharge means for blowing inert gas at night, and it is preferable that the inert gas discharge means be ejected in a state where the distance from ⁇ and the heating mechanism is fixed. Better.
- the inert gas discharge means is kept vertically shielded from ⁇ and ⁇ at least during the process of making the polycrystalline silicon ingot difficult at least by unidirectional solidification. Should be fine.
- an inert gas discharging means is used in order to improve the efficiency. It is also possible to allow the bow to be drawn out from the space between the character and the bonfire.
- Another silicon ⁇ i device of the present invention comprises a mirror, a side plate rising from the periphery of the sickle, and a mirror type for holding the silicon ring inside,
- a gradient is created in the silicon ribbon in the inversion by heating by the force playing structure and cooling by ⁇ , so that the silicon can be moved upward in one direction from the return side of the ⁇ type A silicon fermentation device for solidifying,
- the shape and shape are arranged in a state where the distance is constant.
- the ablated IW has a bottom surface cooling member for cooling the bottom surface, which is the lower surface of the Tantan, and a side cooling member for cooling the side surface, which is the outer surface of the side plate.
- the side cooling » has a surface that forms a heat exchange area together with the side face of the ⁇ type, and the heat tannin area is sequentially arranged from the bottom to the top in the height direction of the ⁇ type. It is said that the dog is moved relative to the dog in order to raise the dog.
- ⁇ and 3 ⁇ 4 are arranged in such a manner that the distance between them is constant, the distance from the power leakage to the ⁇ ⁇ due to the fluctuation of the upper S3S separation is changed. Fluctuations in the amount of heat can be suppressed.
- the side cooling surface is moved relative to the key, so that the surface provided on the side cooling surface and the heat dissipation surface The tan region between the side of the view and the tan is changed so as to increase from the bottom in the height direction to the top as the solidification of the silicon in the bath progresses and the solid-liquid interface rises. Can be done.
- the amount of ⁇ from the ⁇ by the shin can be controlled sufficiently and satisfactorily, and the ⁇ S gradient can be stably maintained from the initial coagulation to the ⁇ : coagulation. Therefore, according to the present invention, a higher-quality polycrystalline silicon ingot, in which the crystal grain size, the number of indentation boundaries, the properties of the grain boundaries, the orientation in crystal grains, the defect density, and the like are almost uniform in the thickness direction, With good reproducibility and as low cost as possible. It should be noted that the distance between the ⁇ type and the crushing stage is kept constant during at least the step of manufacturing a polycrystalline silicon ingot by unidirectional solidification as in the third volume.
- the heat receiving surface was made to be the side surface of the ⁇ and the Hi concubine in order to enlarge the ⁇ -shaped side suntan area composed of the ⁇ -shaped side picture in order from the bottom in the key height direction. While maintaining the condition, it can be seen that the surface is moved from below to above in the plane direction.
- the heat receiving surface facing the side surface of the key is provided with a plurality of cooling portions having divided heat receiving surfaces obtained by dividing the heat receiving surface into a plurality of portions in the height direction, and each cooling portion has a ⁇ -shaped side surface.
- the divided heat receiving surfaces were individually separated from the state in which the divided heat receiving surfaces abutted or contacted the side surfaces. There are also things that move between ⁇ and ⁇ .
- the divided heat receiving surface of each cooling portion is individually moved without contact with the side surface of the right side without sliding, between the tongue state and the separated state. Since the heat is exchanged by the mutual movement, the sliding surfaces can be eliminated, and the target surfaces can be prevented from abrasion.
- ⁇ ⁇ which makes the divided heat receiving surface directly contact the side of, can improve the heat exchange rate and change the area of the heat sink by moving it in phase with the ⁇ type. In this case, the leakage can be changed quickly with good response.
- the ⁇ type is placed opposite to the heat-dissipating surface, which is the surface other than the mounting surface, of the pedestal on which the bottom surface is laid on the mounting surface in a state of fiber.
- the surface cooling member is combined with the side cooling, the arrangement from the initial solidification to the complete solidification can be further stabilized more stably, and a higher quality polycrystalline silicon ingot can be obtained. , With good reproducibility and as low cost as possible.
- each cooling part will cause the hot male area, which is formed on the bottom of the torso, to erode from the center to the periphery of the bottom in order.
- the divided heat receiving surfaces are operated between a pillow state in which the bottom surface is in contact with or in contact with the bottom surface and a separated state.
- the brittle surface ⁇ 3 ⁇ 4 If the P member is combined with the side cooling, the ⁇ g gradient can be more finely controlled according to the solidification of the silicon inside the mold, and a higher quality polycrystalline silicon ingot can be obtained. It can be manufactured with good reproducibility and as low cost as possible.
- the silicon device of the present invention has a gradient from the initial solidification to the complete solidification.
- temperature detecting means for measuring the temperature of the mirror mold, and this temperature detecting means Based on the 3 ⁇ 4g of ⁇ measured by the method described above, a control means for controlling the degree of coagulation by caro and the area of the heat tannin in the heat tansan region of the day structure to control the appropriate coagulation degree of silicon tanning.
- a control means for controlling the degree of coagulation by caro and the area of the heat tannin in the heat tansan region of the day structure to control the appropriate coagulation degree of silicon tanning.
- it is provided.
- the silicon unidirectional solidification purification method described above is held inside the, in order to ensure smooth and uniform processing. It has an inert gas discharge means that blows inert gas at night, and the inert ffi gas discharge means is in a state where the distance between the ⁇ type and the Kasin Akira is kept constant. Is preferred.
- the reason why the distance between the inert gas discharge means and the body and the heating element is kept constant is that at least during the process of manufacturing a polycrystalline silicon ingot by one-way solidification as in the third edition. I just need.
- the method of polycrystalline silicon ingot of the present invention is a method of forming a polycrystalline silicon ingot using the above-mentioned silicon position, wherein ⁇ , and a side plate rising upward from the periphery of ⁇ .
- the process of inverting the Siligon melt inside the ⁇ , and the condition in which the distance between the ti and the key arranged above ⁇ is kept constant, and below the ⁇ , or below and ⁇ In response to the rise of the solid-liquid interface inside the silicon inside and outside due to the cooling by the cooler that is forced to the side, at least one of the return side and the working side of the key While increasing the heat exchange area of the heat sink area formed between the upper heat surface and the opposite heat receiving surface in the cooling process, the silicon is unidirectionally solidified upward from the serving side of the chain. It is assumed that
- the gradient is stably maintained from the initial stage of solidification to complete; It is possible to stably and inexpensively reduce the cost of a polycrystalline silicon ingot having a substantially uniform number, grain boundary properties, crystal grain orientation, defect density, etc. in the thickness direction.
- the control means controls the heat state of the heat-insulating region of the heat-swing region of the heat-shrinking region by the control means. If the silicon rain removal is controlled to be unidirectionally solidified from the opposite side of the ⁇ type, the gradient from the initial solidification to the complete solidification can be further stabilized. To make high-quality polycrystalline silicon ingots with good reproducibility and low cost. it can.
- the silicon melt is blown upward from the other side of J while blowing the inert gas onto the silicon melt held inside the mirror from the inert gas discharge means.
- the directional solidification allows the unidirectional solidification method to be performed smoothly and uniformly, so that the amount of impurity elements is significantly reduced, and a higher quality polycrystalline silicon ingot can be obtained. High reproducibility and low cost.
- FIG. 1A is a vertical cross-sectional view showing " ⁇ " in a difficult form of the silicon device according to the present invention
- FIG. 1B is a diagram showing a state where the bottom surface of the silicon device according to the above example is activated.
- Fig. 2 is a vertical cross-sectional view showing another example of the state of implementation of the combination of the silicon detection device of Fig. 1A and Fig. 1B with the 3 ⁇ 4g detection means and the control means. It is.
- FIG. 3 is a longitudinal sectional view showing another example of the embodiment of the silicon mirror making apparatus of the present invention in which an inert gas discharging means is combined.
- FIG. 4A is a fiber surface view showing another example of the silicon device according to the present invention
- FIG. 4B is a diagram showing the operation of cooling the bottom surface of the silicon device of the above example.
- O is a longitudinal sectional view showing
- FIG. 5A is a orchid view showing another example of the shape of the silicon fiber according to the present invention
- FIG. 5B is a state in which cooling of the bottom of the silicon fiber device of the above example is activated.
- FIG. 6A is a front view showing another example of a silicon form of the present invention
- FIG. 6B is a view showing a state where a bottom cooling member of the silicon manufacturing apparatus of the above example is relatively moved.
- FIG. 7A is a schematic view showing another example of the shape of the silicon device of the present invention
- FIG. 7 is a bottom view and side cooling of the silicon fiber device of the above example.
- FIG. 4 is a longitudinal sectional view showing a state in which members are moved together.
- FIG. 8 is a plan view showing another example of the Wei form of the silicon device of the present invention
- FIG. 8B is a diagram illustrating the bottom cooling device and the side cooling member of the silicon chain device of the above example.
- FIG. 4 is a vertical cross-sectional view showing the state in which it has been made.
- FIG. 9A shows another example of the difficult configuration of the silicon device according to the present invention.
- FIG. 4 is a vertical cross-sectional view showing a state in which the bottom surface cooling and the side surface cooling of the silicon key device of the above example are sculpted.
- FIG. 10 is a longitudinal sectional view showing another example of the embodiment in which the detection means and the control means are combined with the silicon device shown in FIGS. 9A and 9B.
- FIG. 11A is a front view showing the separated silicon device in the example of the present invention
- FIG. 11B is a clear view showing a modified portion of the silicon device manufactured in the example.
- FIG. 12A is a vertical cross-sectional view showing an example of a silicon device
- FIG. 12B is a vertical cross-sectional view showing a state where the silicon mirror of the above example is lowered.
- FIG. 13 is a vertical cross-sectional view showing another example of the arrangement of the silicon on the surface. Best mode for making invention
- FIG. 1A is a schematic view showing a difficult configuration of the silicon device 1 of the present invention
- FIG. 1B is a bottom surface cooling 6 of the silicon device 1 of the above example. It is a longitudinal cross-sectional view showing a state.
- the silicon device 1 of this example includes an old 4a and a side plate 4b rising upward from the periphery of the 4a, and holds a silicon melt 8 inside. 4 type 4 to perform, 51
- a heat insulating member 2 arranged to surround the periphery of these members;
- the heater 3 and the mirror mold 4 form a polycrystalline silicon ingot by at least one-way solidification! During the process, the distance is kept constant.
- J ⁇ k for example, when storing silicon raw material inside or removing the manufactured polycrystalline silicon ingot from the mold, in order to improve its performance, It is preferable to move one of them to increase the distance between them, to put on the, or to remove the force c-fiber structure.
- ⁇ 4 is not particularly, for example, silicon dioxide (S i 0 2) or black, carbon ⁇ It is preferable that the polycrystalline silicon ingot is made of a difficult-to-make material or the like and can be divided when the polycrystalline silicon ingot is taken out, and that the ingot can be assembled again after being taken out. Also, although not shown, a layer is formed on the inner surface of 4 to prevent fusion of the polycrystalline silicon ingot to facilitate removal, and to allow, 4 to be repeatedly removed. It is preferred to provide.
- nitride is a nitride of silicon (S i 3 N 4), a carbide der Ru carbide crane (S i C) ⁇ oxide Kamatoi of (S i 0 2) or the like, Tsuruka ⁇ ) Layer.
- the powder of the above formula)) is mixed with ⁇ 0 with an appropriate binder to form a slurry, and this slurry is applied or sprayed. Then, it is only necessary to coat the inside of the bed 4.
- Heater 3 heats and melts the silicon raw material contained in, 4, causing the silicon ⁇ 8 to pirate, or heating the pierced silicon x8 from above the mirror mold 4, heating it from above In combination with cooling from the bottom surface 4 c side of the 4, 4, it is possible to generate various gradients in the silicon bed 8 to solidify it in one direction, and so on.
- the heater 3 having these functions, for example, a doughnut-heated knitted-hole heater, an induction heating coil, and the like are given.
- the heater 3 may be provided not only on the ceiling portion in the furnace shown in the figure but also on both the side surface portion and the ceiling portion in the furnace so as to surround the mold 4 (not shown).
- the pedestal 5 Since the pedestal 5 is used to heat the bottom 4 c of the, 4 and heat it to the bottom 3 ⁇ 4 3 3 ⁇ 4 i 6 i 6, the pedestal 5 is highly acknowledged.
- the pedestal 5 is made of silicon in an inert gas atmosphere such as Ar. 1 ° C) or more, especially 160 ° C. It is preferable to use a material capable of withstanding the high temperature of C, particularly, a material having a heat resistance of 40 W / (m'K) and high heat resistance.
- Materials that meet these conditions and are suitable for forming the pedestal 5 include, for example, graphite (X 49 W / (mK)), sapphire (X 45 W / (mK)), Aluminum nitride [ ⁇ 1 ⁇ , # ⁇ 8 4W / (m-K) Carbide [SiC, Xiyun 200 W / (m-K), etc. For this reason, graphite is preferred.
- the heat insulating member 2 is arranged so as to surround the mold 4, the heater 3, and the pedestal 5 as described above. Insulation member 2 separates the carbon in consideration of the It is preferably formed of a material including, for example, graphite felt.
- the heat insulating member 2 it is possible to transmit the heat radiation from the sun 3 to the silicon rich 8 inside the dragon 4 with little loss.
- the silicon can be efficiently treated with only the bottom cooling member 6 of the cooling C to effectively reduce silicon It can be unidirectionally solidified.
- the thermal insulation 2 on the lower surface 5 c side of the pedestal 5 is provided with an opening 2 a for inserting the side plate 6 c having the keyed heat receiving surface 6 a of the bottom cooling g
- the mechanism C has a heat-receiving surface 6a that is directly connected to the heat-radiating surface 5b as a heat-dissipating surface and extends downward from the periphery of the mounting surface 5a of the pedestal 5, as shown by the solid arrow in the figure.
- the heat receiving surface 6a is referred to as the side surface 5b
- the surface cooling device 6 is moved in the direction of the side surface 5b relative to the pedestal 5, while the bottom surface cooling member is provided. 6 is provided with a lifting / lowering motor (12 in FIG. 2) for moving the same in the above-mentioned plane direction.
- ⁇ ⁇ 6 is raised below the pedestal 5 from the edge of this pedestal 6 b, with a flat plate-shaped play 6 b drawn on the lower surface 5 c of the base 5 and the ⁇ A side plate 6 whose inner surface is a ⁇ 3 ⁇ surface 6a.
- a connecting portion 6d extending downward from the center of the lower surface of the drama 6b and connected to the lowering motor 12 is formed into, for example, stainless steel or other material into ⁇ f pieces. It is configured.
- the side plate 6c is preferably formed around the side surface 5b of the pedestal 5.
- the pedestal 5 is a rectangular ⁇ dog: ⁇ means that the side plate 6 c is formed as a four-sided plate that is fitted to the four sides 5 b of the rectangular parallelepiped, sold together, or individually independent do it.
- the pedestal 5 has a columnar shape: ⁇ can be formed by forming the side plate 6c into a cylindrical shape that matches the side surface 5b of the cylinder, or by dividing the cylinder into multiple parts in the circumferential direction. good.
- the pedestal 5 is formed such that the distribution of the mounting surface 5a is made as uniform as possible and the bottom surface 4c of the ⁇ type 4 is uniformly cooled. It is desirable that the thickness be as large as possible within the range that does not hinder the heat exchange between them.
- a movable heat insulating piece 7 for closing the opening 2 a is mounted so as to be able to move up and down together with the bottom surface cooling member 6.
- the movable insulation piece 7 is insulated It is provided by the same heat insulating material as member 2.
- 3 liquid, such as water, is provided inside the bottom ⁇ 3 ⁇ 4 member 6 so that the bottom liquid can be cooled by the circulation of this cooling liquid. You may. What is necessary is just to make the cooling liquid circulated in the piping inside the bottom cooling member 6 after returning to the outside by the heat ⁇ outside the silicon ⁇ t device 1, and then return to the heat ⁇ again.
- the bottom cooling member 6 is moved up and down by the elevating motor 12 so as to be moved relative to the pedestal 5 in the surface direction of the side surface 5b as a side combustion surface. Then, the heat male area of the heat sink region HE (shown in FIG. IB) formed between the side surface 5b and the heat receiving surface 6a is changed.
- FIG. 1A shows a state in which the bottom member 6 is lowered to the lowest position.
- the opening 2 a of the heat insulating member 2 is closed by the movable heat insulating piece 7, particularly when the silicon raw material is melted to form the silicon layer 8.
- the cooling C is not limited, heat can be effectively prevented from leaking to the equipment from the highly accommodating pedestal 5 etc., and the time and cost of the polycrystalline silicon ingot can be saved. You can save.
- FIG. 1B shows a state in which the bottom surface Pg
- the side surface 5 b of the pedestal 5 and the surface 6 a of the bottom surface cooling member 6 are connected.
- the fiber is woven over the widest area set by the apparatus in the example in the figure, and the heat exchange area of the heat-shrink region HE is 3 ⁇ 4 ⁇ .
- the heat exchange area of the heather area HE becomes zero and maximum. It can be set to any area between steps without any steps.
- the bottom cooling member 6 is gradually raised in accordance with the rise of the solid-liquid interface due to the progress of solidification of the silicon melt 8, and the thermal male area of the tantalum region HE is gradually increased.
- heat from the bottom surface 4c which is the lower surface of ⁇ 4a, of the type 4 via the pedestal 5 and the bottom cooling S ⁇ i6 through the thermal tannin region HE (see the white arrow in FIG. IB) ), The amount of heat, can be gradually increased.
- the gradient imparted to the silicon night 8 in the mirror mold 4 by the heater 3 and the cooling chamber C from the initial solidification phase to the complete solidification phase related to the increase in f »t accompanying the rise of the solid-liquid interface Until the grain size, the number of grain boundaries, the number of grain boundaries, the properties of grain boundaries, the orientation in crystal grains, the defect density, etc. are almost uniform in the thickness direction. It is possible to reduce the cost of polycrystalline silicon ingots with good reproducibility and low cost.
- the pedestal 5 has a thickness D as large as possible.
- the knee area is not kneeled, but the mounting surface 5a and the bottom surface 4c of the ⁇ 4 placed on it ⁇ the length L of the fiber region (see FIG.
- the thickness D should be However, even within the above range, it is particularly preferable that the length is not more than 2/3 of the passing length L.
- the passing length L is defined as a line between the mounting surface 5a and the bottom surface 4c of the key 4 placed on the mounting surface 5a, which intersects the center of gravity of the flat frequent dog in the fiber region. It refers to the line segment that shows the minimum length among the line segments cut out by the contour line of the plane ⁇ ⁇ .
- the plane ⁇ of the contact area is rectangular ⁇ !
- the passing length L is equal to the length of ⁇ 2 of the: R3 ⁇ 4 shape.
- the flat dog in the invertebrate area is circular
- the passing length L matches the diameter of the circle.
- the mounting surface 5a of the pedestal 5 is smaller than the bottom surface 4c of the wake 4, as shown in the examples of FIGS. 1A and IB
- the plane ⁇ of the fiber region is the flat surface of the mounting surface 5a.
- FIG. 2 is a vertical cross-sectional view showing another example of a configuration in which a heat sink 10 as a 3 ⁇ 4 ⁇ detecting means and a control means 11 are combined with the silicon ⁇ device 1 of Figs. 1A and 1B. is there. Since the configuration other than these members is as described above, only the phases will be described below.
- thermocouples 10 are provided at three locations on the side plate 4 b of the rectangular mold 4, near the upper and lower sides, near the lower side, and between the two. Thereby, the temperature gradient applied to the silicon
- the output of each heat ItM 10 is supplied to the control means 11 via the control cable 13.
- the control means 11 calculates the gradient applied to the silicon 8 from the output of the three thermal plays 10 and, based on the result, passes through the control cable 13 via the control cable 13 for heating and lifting.
- the detection means is not limited to i0.
- an infrared ⁇ g It can also be used.
- a well-known programmable controller or the like can be used as the main means 11, for example.
- Programmable controllers are very well-known in the field of Lord Sir, and are used as a unit by combining modules having a single function, or using a single module with a reduced function. Can be configured. Since the output from the heat 3 ⁇ 43 ⁇ 410 is taken in, for example, as an analog ⁇ value, the leg means 11 1 can be combined with a module that converts this into digital data. Just fine.
- the control means 11 moves the bottom cooling member 6 of the P mechanism C to the lowest as shown in FIG. 1A.
- the opening 2 a of the heat insulating member 2 is closed by the movable heat insulating piece 7, so that the roof 3, 4, and the pedestal 5 are surrounded by the separating member 2 and the movable heat insulating piece 7.
- the silicon raw material is melted by energizing the heater 3 and heating the mold 4 to a temperature of about 144 ° C. to 150 ° C.
- loss of radiant heat from the heater 3 can be prevented, and the silicon raw material can be melted efficiently and in a shorter time.
- the can 11 means drives the elevating motor 12 while monitoring the temperature gradient of the silicon melt 8 from the output of the three heats ⁇ o.
- the bottom cooling member 6 is gradually raised, and a heat exchange area HE is generated between the bottom cooling member 6 and the pedestal 5 to start the heat.
- the gradient of the solid-liquid interface Regardless of the increase in dignity associated with the rise, the rise and fall of the bottom cooling member 6 and the accompanying increase / decrease in the area of the heat tannin of the HE between the base 5 and the pedestal 5 are controlled so that the fiber is stably woven.
- the power to be supplied to Heath 3 is controlled.
- the leg means 11 includes, for example, a silicon sickle with a separation gradient smaller than a predetermined value: ⁇ , (a) increasing the power supplied to the heater 3, (b) raising the bottom cooling member 6 Then, increase the heat exchange area of the heat exchange area HE and / or increase the heat exchange area to increase the 3 ⁇ 4S gradient.
- the gradient is larger than a predetermined value.
- the temperature at the time of unidirectional solidification of silicon The temperature gradient can be improved more stably from the initial stage of solidification to complete solidification, and it is possible to produce high-quality polycrystalline silicon ingots with good reproducibility and at low cost. Become.
- the heater 3, the pedestal 5, the atmosphere inside the apparatus 1 ⁇ 4P member 6, the cooling fluid, etc., or the cooling fluid ⁇ *, etc. are measured and controlled. Higher reproducibility can be obtained.
- an elevating motor 12 for raising and lowering the bottom cooling device 6 an inverter-controlled motor, a stepping motor, and a regenerator that can move up and down variably are used.
- the slope can be controlled more finely.
- FIG. 3 is a front view showing another example of the difficulty of the silicon observation device 1 of the present invention. 0
- the majority of the structure of the silicon ⁇ g device 1 is shown in FIGS. 1A and 1B described above. Therefore, only the differences will be described below.
- the heat receiving surface 6 a of the bottom surface 6 is spaced a certain distance from the side surface 5 b of the pedestal 5, which is the iL hot surface.
- the rooster HI is separated by G and the bottom cooling g
- the sliding surface can be eliminated, and the wear on both surfaces can be prevented, and the heat tan is performed by radiating or flowing heat between the side surface 5b and the heat receiving surface 6a.
- the gap G between the two surfaces 5b and 6a is 10 mm or less.
- the pedestal 5 has a thickness D as large as possible.
- the specific range of the thickness D is not particularly limited, but is not less than 1/6 of the length L of the insect removal area between the placement surface 5a and the bottom surface 4c of the ridge 4 placed thereon. It is preferred that In order to prevent the pedestal 5 from being too thick and hindering the heat sink between the mold 4 and the bottom cooling 6, the thickness D should be within the above range, especially, It is preferably at most 2/3 of L.
- the passing length L is defined as a straight line extending from the center of gravity of the plane ⁇ of the insect removal area between the mounting surface 5a and the bottom surface 4c of the sample 4 mounted thereon. It refers to a line segment having the minimum length among the line segments cut out by the outline of the dog.
- the passing length L is equal to the length of the square of the shape.
- the plane ⁇ of the inverting region is circular, the passing length L matches the diameter of the circle.
- the plane brain dog in the machine area matches the flat surface of the mounting surface 5a.
- the opposite matches the flat dog on the bottom face 4c of Luo 4.
- the base 5 is to uniformly cool the bottom surface 4c of the mold 4, the mounting surface 5a and the lower surface 5c are both flat and the Ffi 1 Therefore, it is preferable that the thickness is uniform, and the thickness D at that time can be lengthened depending on the distance between both surfaces.
- the pedestal 5 has the minimum thickness. Work with a thickness of D.
- ⁇ ⁇ was inserted through the heat insulating member 2 so that ⁇ ⁇ protruded into the area between As described above, at least during the process of weaving the polycrystalline silicon ingot by one-way solidification, the distance between the mirror mold 4 and the heater 3 is kept constant.
- Nozzle 9 is provided. Therefore, when the polycrystalline silicon ingot is fiberized by unidirectional solidification, the nozzle 9 is used to inject the inert f raw gas such as Ar into silicon The spray can be always sprayed in a constant state without changing the g level between the liquid level of 8 and the tip of the nozzle 9 or changing the desorption state of the inert gas.
- the nozzle 9 is used to improve the workability other than the one-way solidification process, for example, when storing a silicon raw material in a rope or removing an iterated polycrystalline silicon ingot from ⁇ .
- the bow is formed so as to be able to be ejected from between the mold 4 and the heater 3.
- the tip of the nozzle 9 is disposed so as to eject the inert gas at substantially the center of the liquid surface of the silicon layer 8.
- the inert gas include rare gases such as He, Ne, and Ar; from the viewpoint of availability, Ar is preferable as described above.
- the one-way coagulation refining method when an inert gas is blown from the nozzle 9 to the liquid surface of the silicon substrate 8, a cavity is formed at the center of the sprayed liquid surface, and the liquid is swept around the surface. A covering flow is formed. Then, along with this flow, the surface of the silicon melt 8 is swung by the blowing of the inert gas, so that new silicon melts 8 are successively added to the liquid surface. Since it is supplied, the SiO 2 gas inside the silicon layer 8 is discharged into the surrounding atmosphere, and is effectively removed as an impurity. Further, since the surface of the silicon melt 8 is covered by the flow of the inert gas, the CO gas is prevented from entering the silicon melt 8 from the surrounding atmosphere.
- An inert gas is supplied to the nozzle 9 from a gas supply means provided outside the apparatus through a pipe (both not shown).
- the simplest configuration of the gas supply means consists of connecting a gas regulator and a gas regulator to a cylinder filled with inert gas. Can be supplied to the equipment. Further, the gas flow rate may be adjusted more finely by using a single-mass mouth controller.
- FIG. 4A is a longitudinal sectional view showing another example of the separated form of the silicon device 1 of the present invention
- FIG. 4B is a diagram showing the bottom material 6 of the silicon device 1 of the above example.
- FIG. 4 is a longitudinal sectional view showing the state.
- the silicon unit 1 moves the movable heat-insulating piece 7, which moves up and down in conjunction with the bottom cooling member 6, in the vertical direction to the side surface 4d, which is the outer surface of the mirror 4b.
- the side surface 4 d of the mirror type 4 and the pedestal 501 ′ surface 5 b are formed on the same plane, and the movable insulating piece 7 and the side plate 6 of the bottom cooling 6 are provided between both side surfaces and the cut m 2.
- a gap 2c having a width approximately equal to that of c and capable of receiving these is provided.
- the movable heat insulating piece 7 which has been raised together with the bottom surface ⁇ 6 covers the entire side surface 4d of the ⁇ 4, Insulated from the heat of heater 3. Also, although not shown, when the bottom surface ⁇ SP fine 6 is raised to an arbitrary position between the above FIGS. 4A and 4B, only the lower part of the side 4 d of the customer 4 is covered by the movable heat insulating piece 7. The upper part becomes the exposed chin state.
- the bottom cooling member 6 and the movable insulating piece 7 are gradually raised in accordance with the rise of the solid-liquid interface of silicon ⁇ night 8, and the silicon ⁇ night 8 in ⁇ 4 is moved to the upper part of the chain 4. Then, the heat is efficiently heated by the heat of the sun 3 and the lower part is insulated from the heat of the heat 3 by the movable insulating piece 7, and the bottom 4 c of the mirror 4 is connected to the side 5 b of the pedestal 5.
- the heat male area of the heat sink region HE formed between the heat receiving surface 6a of the bottom cooling sound 6 and the heat male area is gradually increased, and the heat transferred to the bottom cooling surface 6 through the heat exchange region HE (Fig.
- FIG. 5A is a longitudinal sectional view showing another example of a fiber form of the silicon device 1 of the present invention
- FIG. 5B is a diagram showing the bottom cooling of the silicon device 1 in the above example.
- FIG. 5 is a drawing of a curtain showing the state in which it is performed.
- the dog of the pedestal 5 and the bottom cooling member 6 are different.
- the bottom cooling device 6 is composed of a single thick plate portion 6 e having a heat receiving surface 6 a on its outer peripheral side, and a lower portion 6 f extending downward from the lower surface 6 f of the plate portion 6 e.
- the connection part 6d of the connection ffl with the heat sink 12 and the connection part 6d are formed in a number of- ⁇ from a material S such as stainless steel, for example.
- the pedestal 5 has, on the lower surface 5c, a counterbore portion 5d into which the plate portion 6e of the bottom cooling member 6 is inserted, and the surface 6a of the counterbore portion 5d is viewed as a male. It is formed on Jl3 ⁇ 4 dogs with the inner side 5e as the heat dissipation surface.
- the plate portion 6e is inserted into the counterbore portion 5d, and the heat receiving surface 6a is made to face the inner surface 5e.
- the bottom surface cooling member 6 is moved relative to the pedestal 5 in the surface direction of the inner side surface 5 e, so that the thermal male area of the heat anvil region HE formed between the both sides is reduced. It is configured so as to make it look funny.
- the entire surface of the upper surface 6 g of the plate portion 6 e of the bottom surface: extinguishing 6 is covered with the movable heat insulating piece 7 in order to prevent unnecessary heat tannins between the pedestal 5.
- the opening 2a of the heat insulating member 2 is closed by the movable heat insulating piece 7 which has been lowered together with the opening s of the heat insulating member 2 and the bottom member 6, so that, for example, the silicon raw material is melted to produce the silicon melt 8
- the silicon raw material is melted to produce the silicon melt 8
- the inner surface 5 e of the pedestal 5 and the heat receiving surface 6 a of the bottom 3 ⁇ 4 ⁇ member 6 are set by the device in the example of the figure. It has the widest area, and the heat exchange area of the heat is 3 mm. Further, although not shown, if the bottom cooling member 6 is moved to an arbitrary position between FIGS. 5A and 5B, the heat exchange area: Any area between them can be steplessly reduced by 1 mm.
- the bottom cooling member 6 is gradually raised in accordance with the rise of the solid-liquid interface, and the heat exchange region HE
- the heat from the bottom 4c of the ⁇ 4 through the pedestal 5 to the bottom cooling 6 through the tannin HE can be gradually increased.
- the gradient imparted to the silicon melt 8 in the mold 4 by the heater 3 and the P mechanism C can be stably reduced from the solidified skin to the solidified state ⁇ : high quality This makes it possible to produce polycrystalline silicon ingots with good reproducibility and at low cost.
- the entire silicon device 1 can be made compact by placing the bottom surface cooling member 6 inside the pedestal 5.
- FIG. 6A is a longitudinal sectional view showing another example of a haze form of the silicon device 1 of the present invention
- FIG. 6B is a bottom view of the silicon device 1 of the above example
- FIG. 7 is a screen diagram showing a state in which the user is caused to perform the operation.
- the silicon i unit 1 has a different bottom cooling direction 6 and a different direction of movement.
- the bottom surface cooling plate 6 is formed by a plurality of plate members 6 h whose upper surface is the heat receiving surface 6 a. Then, as shown in Fig. 6B, the Wei surface 6a is directly simulated on the lower surface 5c of the pedestal 5, which is the heat dissipating surface. As shown by, the plate material 6 h is moved relative to the pedestal 5 in the surface direction of the lower surface 5 c so as to change the heat tandem area of the heat tannin region HE formed between the both surfaces. Is configured.
- the plate material 6h ⁇ 5 is pulled out from the opening 2a provided on the side surface of the insulation sound attachment 2 to close the opening 2a.
- the movable heat insulating piece 7 is movably mounted together with the plate 6 h.
- the space between the T® 5 c of the pedestal 5 and the heat insulating member 2 therebelow has a width substantially equal to that of the plate material 6 h and is capable of receiving the plate material 6 h. Between 2 d is provided.
- the sheet material 6 h is gradually inserted into the gap 2 d as the solid-liquid interface rises.
- the heat is extracted to the bottom cooling member 6 through the heat exchange area HE through the base 4 and the pedestal 5 of the key 4 (Fig. (The white arrow in 6B) can gradually increase the heat removal.
- the gradient imparted to the silicon melt 8 in 4 by Hi-Ichiyu 3 and Kyosho Satoshi C is stable from the solidification to the complete solidification. This makes it possible to produce polycrystalline silicon ingots with good reproducibility and at low cost.
- the bottom surface 5c which is wider than the side surface 5b and the inner surface 5e of the pedestal 5, is used as the heat dissipation surface.
- the rate can be improved.
- the side surface 5 b and the inner surface 5 e of the pedestal 5 are set to be hot surfaces; in comparison with ⁇ , the entire assemblage distribution of the pedestal 5 is made more uniform, and the bottom surface 4 c of the key 4 is made more uniform.
- the unidirectional solidification of the silicon melt 8 can be improved.
- FIG. 7A is a longitudinal sectional view showing another example of the construction of the silicon device 1 of the present invention
- FIG. 7B is a bottom cooling gP # C 1 and side surface of the silicon device 1 of the above example.
- FIG. 6 is a longitudinal sectional view showing a state in which the attachment C2 is operated.
- the silicon marrow device 1 of this example includes a ⁇ 4 a and a side plate 4 b rising upward from the periphery of the sickle 4 a, and holds a silicon melt 8 therein.
- a heat insulating member 2 for dispersing the radiation from the heater 3 to the silicon in the mold 4 while minimizing the loss of members is arranged. It is set up.
- the heat insulating member 2 those having the same configuration as that of FIG. 3 can be used.
- the heaters 3 and 4 as in the case of ⁇ "above, are maintained in a condition in which the bandits are constantly knitted, at least during the process of producing the polycrystalline silicon ingot by unidirectional solidification.
- one of the two methods may be used. It is preferable to construct the robot so that it can be moved to increase the distance between the two, to equip, or to remove the force ni3 ⁇ 4W.
- the ⁇ -type 4 has only the periphery of the bottom surface 4c in order to make the bottom surface cooling ⁇ iC 1 contact, and is supported at a predetermined position in the shell la by the support ⁇ 1 exposing the others.
- the support member 51 can be made of various materials that can withstand high temperatures of about 160 ° C. in an inert gas atmosphere, but the calorie is simple and the cost is low.
- the ingot is formed of graphite.
- the surface la is formed by, for example, stainless steel.
- the bottom cooling member C 1 has a plurality of cooling portions 6 having divided heat receiving surfaces 6 la and 6 2 a obtained by dividing a heat receiving surface contacting the bottom surface 4 c of the mold 4 into a central portion and a peripheral portion thereof. 1, 6 2 are provided. At the lower side of each cooling part 6 1, 6 2, connecting parts 6 lb, 62 b extending downward and reaching the outside of the shell la are connected, and each connecting part 6 1 b, An elevator (not shown) for raising and lowering the cooling sections 61 and 62 individually is connected to 62b.
- Each cooling part 6 1, 6 2 has a heat sink area formed on the bottom 4 c
- the lifting and lowering motors are individually hidden, and the divided heat receiving surfaces 6 la and 62 a are individually brought into contact with the bottom surface 4 c of the ⁇ type 4 and ⁇ were, between was separated state, perpendicular to the bottom surface 4 C, is phase ⁇ (lift) in the vertical direction indicated by the solid line arrow in FIG.
- the cooling portion 61 can form the divided heat receiving surface 6 la into an arbitrary plane dog such as a circle, an ellipse, and a polygon.
- the cooling portion 62 can be formed in an annular shape with a divided dog surface 62 a surrounding the divided heat receiving surface 61 a having the flat dog.
- a plurality of cooling sections 62 can be placed in prison around the cooling section 61.
- the member C 2 is a heat receiving surface that is in contact with the side 4 d of the mirror mold 4 and is divided into three in the height direction of
- Each of the cooling sections 63, 64, and 65 has a horizontal movement motor that is individually concealed in order to make the heat tandem area formed on the side 4d of the ⁇ type 4 from bottom to top in order!
- a horizontal movement motor that is individually concealed in order to make the heat tandem area formed on the side 4d of the ⁇ type 4 from bottom to top in order!
- a plurality of the 13 portions 63 to 65 be provided so as to surround the periphery of the subsection 4.
- a key 4 s four flat side plates 4 b are provided;
- ⁇ means that each cooling part 63-65 is arranged around, 4 by four corresponding to each surface. it can.
- the mold 4 has a cylindrical side plate 4b; in the ⁇ , each cooling part 63 to 65 can be disposed around the cylinder 4 one by one so as to surround this cylinder. .
- Each of the above [3 ⁇ 4] portions 61 to 65 can be formed of stainless steel or the like. Further, a liquid such as water may be circulated in the inside to cool the liquid.
- the first step is to fill silicon material into the difficulties 4 and seal the shell 1a. To a reduced pressure inert gas atmosphere.
- the divided wei surfaces 61a to 65a of all the cooling parts 61 to 65 of the bottom cooling member Cl and the side cooling member C2 are
- the heater 3 is energized in a state where it is separated from the bottom surface 4 c and the regular surface 4 d to melt the silicon raw material charged in the key 4, thereby forming a silicon towel 8. This prevents loss of radiant heat from the light source 3 and allows the silicon material to be melted efficiently and in a shorter time.
- the ⁇ portion 62 of the bottom cooling 3 ⁇ 43 ⁇ 4 ⁇ C1 is raised, and the divided heat receiving surface 62a is brought into contact with the periphery of the BJ3 ⁇ 4 surface 4c.
- the mouth portions 63 to 65 of the side cooling member C2 are horizontally moved in order from the bottom as described above, and each of the divided heat receiving surfaces 63a to 65a is moved to the side 4 of the ridge 4.
- Contact d in order from the bottom the heat tan region between the side surface cooling member C2 and the side surface 4d of the body 4 can be changed so as to increase in order from the lower side to the upper side in the height direction.
- the amount of heat from the metal 4 caused by the cooling and rising C is controlled more precisely, and the ⁇ gradient is stabilized vertically from the initial solidification to complete solidification. This makes it possible to produce higher quality polycrystalline silicon ingots with good reproducibility and at the lowest possible cost. Further, in the above arrangement 1, the sliding surface can be eliminated to prevent the visual abrasion of each surface.
- the divided heat-receiving surfaces 63-65 of the cooling portions 63-65 located above it contact the side surface 4d of the life 4,
- the nighttime state must be maintained until the final stage of directional solidification. ⁇
- the vicinity of the liquid surface of the silicon melt 8 has solidified, and the nighttime state is left inside the solidified structure.
- the divided heat receiving surfaces 63a to 65a should be brought into contact with the side surface 4d when the solid-liquid interface at that time is sufficiently high, specifically, 50 mmWJ: when it rises Is preferred.
- the heat-receiving surfaces 61a to 65a are separated from the bottom surface 4c and the side surface 4d of the ⁇ 4, they contact the bottom surface 4c and the side surface 4d. If a separate movable heat shield 3 ⁇ 43 ⁇ 4 ⁇ is provided, for example, the heat leak when melting the silicon raw material to make the silicon night 8 can be effectively suppressed, further reducing the time and cost of the polycrystalline silicon ingot. You can save.
- FIG. 8A is a longitudinal sectional view showing another example of the silicon device 1 according to the present invention
- FIG. 8B is a bottom cooling device C 1 and a side cooling device of the silicon chain device 1 of the above example.
- FIG. 4 is a cross-sectional view showing a state where C 2 is sculpted.
- the silicon device 1 of this example is different in the configuration of both cooling devices Cl and C2.
- the bottom cooling ⁇ iCl has a flat dog corresponding to almost the entire flat dog exposed between ⁇ Appendix 51 on the bottom 4 c of the type 4 and directly contacting the upper face 4 c.
- Only one cooling section 66 with a heat receiving surface 66 a is provided.
- ⁇ ⁇ Below the P part 66, a connecting part 66b extending downward and reaching the outside of the main part 1a is connected, and the cooling part 66 is connected to the connecting part 66b,
- An elevating motor ( ⁇ "1 2 in Fig. 10) is connected to move the elevating motor 12 vertically upward and downward as indicated by the solid arrow in the figure.
- the heat receiving surface 66a is separated from the bottom surface 4c of, 4 as shown in Fig. 8A.
- the side surface C2 has a heat receiving surface 67a that works directly on the ⁇ type 4 ⁇ f law surface 4d, and the labor surface 67a as shown by the solid arrow in the figure.
- a cooling part 67 which is moved in the direction of the side surface 4d, is provided with respect to the side surface 4 while removing the insects in 4d.
- the lower part of the cooling part ⁇ 7 ” is connected with a connecting part 67b extending downward and reaching the outside of the shell 1a, and the connecting part ⁇ 7b has a ⁇ [3 ⁇ 4]
- a motor for raising and lowering the part 67 in the vertical direction as described above (reference numeral 12 in FIG. 10) is connected to the motor.
- a movable heat insulating piece 7 is attached to the upper part of the P part 67 so as to be able to move up and down together with the cooling part 67.
- the side surface 4d of the ⁇ 4 and the side surface of the attachment 51 are formed on the same plane, and the cooling portion 67 and the movable heat insulating piece 7 are almost between the both side surfaces and the heat insulation »2.
- a gap 2e having an equal width and capable of receiving these is provided.
- the third part 67 has the heat receiving surface 67 a force and the j surface, as shown in FIG. 8A, which are bowed downward by concealing the elevating motor 12. 4d, the lowest position where it does not starve, and as shown in FIG. 8B, the highest position where the heat receiving surface 67a is in contact with the side surface 4d over the largest area through the gap 2e, Although not shown, it is raised and lowered between the two positions ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ It is configured to be able to.
- the cooling part 67 is preferably formed in a dog surrounding the side 4 d of the square 4.
- the ⁇ 3 ⁇ 43 portion 67 is aligned with the side surface 4 d of the side plate 4 b, and is continuous or individually independent. It may be formed in the shape of a plate.
- the cooling part 67 is formed into a cylindrical shape adapted to the side surface 4d or a shape obtained by dividing the cylinder into a plurality of parts in the circumferential direction, etc. I'll do it.
- silicon material was filled in the parent 4, the shell 1a was sealed, and Inert gas atmosphere.
- the cooling portion 66 of the bottom cooling member C1 is lowered to the lowest position, the heat receiving surface 66a is separated from the bottom surface 4c of the mold 4, and the side cooling is performed.
- the part 67 of the extinction C 2 is completely pulled out from the gap 2 e and lowered to the lowest position, and the heater 3 is energized as the heat receiving surface 67 a and the simple surface 4 d and the insects are not removed.
- the cooling part 6 The movable insulating piece 7 that has been lowered together with the cover 7 closes the opening of the gap 2 e on the support member 5 1 side, and the side 4 d of the key 4 is exposed inside the furnace.
- the heat of the heat source 3 can be more efficiently iSl, the silicon material can be melted quickly, and silicon can be generated efficiently and in a shorter time.
- the cooling part ⁇ 6 of the bottom cooling device C 1 is raised to the highest position shown in FIG. 8B, and its heat receiving surface 66 a is brought into contact with the bottom surface 4 c of the mirror 4.
- a gradient is generated between the silicon melt 8 in the inside and that heated by the heater 3, and a unidirectional solidification is started, and the solidified layer (solidified structure) 8 a of the silicon and the silicon : ⁇
- Solid-liquid interface: ⁇ begins to rise too much.
- the side 4 d of the key 4 and the cooling portion 67 are insulated by the movable heat insulating piece 7 interposed therebetween and closing the opening of the gap 2 e, so that at the very early stage of solidification, The vicinity of the lower side of the side surface 4d of the side 4d is cooled by the cooling member 67, so that the start of the smooth one-way solidification by the cooling portion 66 can be prevented.
- the amount of fiber increases and the temperature gradient tends to decrease.
- the cooling part 67 of the side P ⁇ iC 2 is gradually raised, and the heat receiving surface 67 a is gradually removed from the bottom to the side 4 of the mold 4 from below.
- the heat sink area between the side cooling member C 2 and the side 4 d of the key 4 is arranged in order from the lower side to the upper side in the height direction, and furthermore, this experiment is performed steplessly as described above. It can be changed to spoil. Therefore, according to the above silicon device 1, the amount of heat removed from the mold 4 by m-structure C is more precisely controlled, and the gradient is stabilized from solidification to complete solidification. This makes it possible to produce high-quality polycrystalline silicon ingots with high reproducibility and low cost as much as possible.
- the compensation amount 67 is gradually increased according to the rise of the solid-liquid interface while the state that the upper part is always a predetermined dimension (preferably 50 mm) or more below the solid-liquid interface is gradually reduced. It is preferable to raise the pressure.
- FIG. 9A is a longitudinal sectional view showing another example of the difficult embodiment of the silicon device 1 of the present invention.
- B is a longitudinal sectional view showing a state in which bottom cooling 1 and side cooling of the silicon device 1 of the above example are activated.
- the silicon device 1 of this example is different in that it has a nozzle 9 as an inert gas discharging means.
- the nozzle 9 penetrates the shell la on the upper side of the heater 3 and the heat insulating member 2 so that, for example, the tip ⁇ protrudes into the center of the heater 3 of the ring dog. Both are arranged in such a manner that the distance between the silicon 4 and the silicon 3 is fixed during the process of forming the polycrystalline silicon ingot by directional solidification.
- the inert gas such as Ar is supplied from the nozzle 9 to the silicon melt 8 held in the nozzle 4 and the silicon melt 8 is cooled.
- the spray can be sprayed with a constant pillow without changing the level of the liquid surface and the tip of the nozzle 9 or changing the inert gas condition.
- the method is smooth and uniform, so that you can re-view well.
- the nozzle 9 is also used in other than the one-way solidification process, for example, when storing silicon raw material in the inside or when removing the i-g polycrystalline silicon ingot from the inside.
- the bow can be ejected from between the mold 4 and the heater 3.
- the tip of the nozzle 9 is disposed so as to eject the inert gas at a substantially central portion of the liquid surface of the silicon melt 8.
- the height of the portion 67 in the vertical direction is made larger than the dimension of the cooling portion 67 in the same direction, and as shown in FIG. When it is lowered to the lowering position, it cools off! ] It functions to cover so that the heat receiving surface 67 a of the portion 67 is not exposed below the portion 4.
- the movable heat insulating piece 7 on the cooling portion 67 has the same height as the height of the side surface 4 d of the mold 4 in the vertical direction, as shown in FIG. 9A. In the state where 6 7 is lowered to the lowest position, it covers the side 4 d of the radiator 4 and functions to prevent heat from escaping. Therefore, the heat of heat sink 3 can be more efficiently fSl-typed to the 4-type 4 and the silicon material can be melted quickly, and silicon S 8 can be pirated efficiently and in a shorter time. it can.
- FIG. 10 is a vertical cross-sectional view showing another example of the wei form in which the assembling detecting means and the controlling means are combined with the silicon devices shown in FIGS. 9A and 9B. Since the configuration other than these members is as described above, only the differences will be described below.
- heat TT 10 is provided at three places on the side of the side plate 4 b, near the bottom, and between the two. As a result, the key gradient applied to the silicon layer 8 in the area 4 can be obtained.
- the output of each hot rice cake 10 is supplied to the control means 11 via the eternal cable 13.
- the control means 11 calculates the gradient to be applied to the silicon 8 from the outputs of the three thermal plays 10, and based on the result, via the cable 13, setstle down and rises and falls. 1/2 Further, although not shown, the $ lord means 11 also controls the gas supply means connected to the nozzle 9 and the exhaust pump system for filling the inside of the shell la. As each of the above parts, those having the same configuration as that of the knitting can be used.
- silicon material is filled into the inside of the shell 4 and the shell la is sealed and the main means 11 is started.
- the $ 11 means activates the exhaust pump system, and the inside of the shell la is activated.
- the inert gas is supplied to the inside of the shell 1a through the nozzle 9 by operating the gas supply means, so that the inside of the shell la is made an inert gas atmosphere.
- the leg means 11 lowers the cooling portion 66 of the bottom cooling to the lowest position, and separates the heat receiving surface 66a from the bottom surface 4c of the key 4.
- the cooling part 67 of the iC 2 is lowered to the lowest position, so that the heat sink 3 and the face 4 are surrounded by the heat insulating member 2 and the movable heat insulating piece 7.
- the silicon raw material is melted by heating the mold 4 to a temperature of 144 ° C. or more;
- loss of the radiation from the heater 3 can be prevented, and the silicon material can be melted efficiently and in a shorter time.
- the leg means 11 sprays an inert gas from the nozzle 9 onto the liquid surface of the silicon wisteria 8 and outputs the three thermocouples 10. From above, while monitoring the slope of the silicon bed 8, hide the elevating motor 12, and raise the cooling part 66 of the bottom (! Member 01 to the top position shown in 09 B. Then, the heat receiving surface 6 6a is brought into contact with the bottom surface 4c of the continuous 4 to start ⁇ Then, the solid-liquid interface force between the silicon solid layer (solidification structure) 8a and the silicon substrate 8 is formed. Start climbing each time.
- the control means 11 is provided to the silicon wafer 8 by the heater 3 and the cooling mechanism C.
- the slope is continuously monitored by the output of the heat m ⁇ i 0, and based on the result, the elevation motor 12 is driven at the time of the departure to cool the side member C 2
- the portion 67 is gradually raised, and the heat receiving surface 67a is made to fiber on the side surface 4d of the ⁇ type 4, and the heat exchange region, which is the recitation region on both sides, is moved from the bottom in the height direction to ⁇ ⁇ .
- the leg means 11 controls electric power supplied to the heater 3.
- the gradient when unidirectionally solidifying silicon 3 ⁇ 4t night 8 can be made more stable from the initial solidification to complete solidification, and a high-quality polycrystalline silicon ingot can be obtained.
- the reproducibility and cost can be reduced.
- the temperature of 4 not only the temperature of 4, but also the temperature of the cooling part 66, 67, ⁇ 413 fluid, etc., and the cooling fluid ⁇ *, etc. If controlled, higher reproducibility can be obtained.
- a motor for invertor control, a stepping motor, or a linear motor for which the degree of ascending is variable is used as the motor 12 for raising and lowering the cooling part 67 for the side cooling. If the speed of the ascent / descent is set to $ L in accordance with, the 3 ⁇ 4g slope can be controlled more finely.
- control means 11 For example, in the examples of FIG. 2 and FIG. 10, a programable controller is illustrated as the control means 11, but instead,? An ordinary personal computer combined with an interface for can I legs can be used as the control means 11. So-called columns
- the silicon device 1 shown in FIG. 11A having the configuration described above was configured by combining the following items.
- heat insulating member 2 a member having a thickness of 30 mm, which was obtained by coating graphite felt with a carbon powder, was used. (heater)
- a doughnut-shaped black heater with an outer diameter of 360 mni and an inner diameter of 220 mm was used.
- Mirror type 4 is a combination of 2 mm thick plates made of Takaito Shukuro J &, and four flat side plates 4 b are set up from the periphery of the square sickle 4 a.
- the inner dimensions were 33 Omm x 33 Omm x 32 Omm in depth, and 334 mm in width and 334 mm in width on the bottom surface 4 c.
- the inner surface of the mold was formed of a nitride powder and a dioxide powder.
- the pedestal 5 has a size of 40 Ommx 40 Omm in width of the mounting surface 5a and a thickness D between the mounting surface 5a of the pedestal 5 and the bottom surface 4c of the display 4 mounted thereon.
- the pedestal 5 was formed of graphite (49W / ( ⁇ ⁇ K)), but in order to see the effect of the pedestal 5, the same ceramic formed by the following ceramic was used. A pedestal 5 having a former and a different one and different from each other was also used.
- the bottom cooling member 6 of the cooling Note C a member formed of stainless steel and having a water pipe formed therein was used.
- a heat receiving surface 6a is referred to as the side surface 5b of the pedestal 5, and a member that can move in the surface direction of the side surface 5b is used.
- the surface was separated from the Wei surface 6a: 3 ⁇ 4 and the side surface 5b of the pedestal 5 by the surface method G shown in Table 1 to see the effect when the In this embodiment, the one that can be moved in the direction of the side surface 5b was also used.
- thermocouples 10 A programmable controller was used as the control means 11, and the temperature gradient of the silicon melt 8 in 4 was monitored by the outputs of thermocouples 10 provided at three places in the height direction of ⁇ 4.
- a stepping motor / night that can freely set the amount of lifting / lowering of the bottom cooling 6 according to the time was used.
- the following hand jet was used to make a polycrystalline silicon ingot.
- the desired silicon raw material was filled into the chamber 4, and the inside of the apparatus was set to an Ar gas atmosphere at 10.7 kPa, and then the heater 3 was energized to 150 ° C. Heating melted the silicon raw material to make ⁇ g of silicon ⁇ ⁇ 8. Then, using the bottom cooling g
- the bottom cooling member 6 is raised by hiding the elevating motor, so that the side 5b of the base 5 and the bottom 6a of the bottom cooling Heat tan region
- the time required for this change in area to appear as a change in ⁇ of, 4, which was measured by heat transfer 10 was determined. Therefore, the follow-up note was pared based on the following criteria.
- ⁇ More than 5 minutes and within 10 minutes. Within the acceptable range.
- the above-mentioned polycrystalline silicon ingots are repeated five times under the same conditions to produce five polycrystalline silicon ingots, and each of the polycrystalline silicon ingots is subjected to light using microwaves.
- Conduction decay method ( ⁇ PCD method) Carrier ⁇ was measured. When all the minority carriers in the five polycrystalline silicon ingots were equal to or greater than 20 sec, the following was passed, and the following remarkable fresh and crystalline quality relanguability was described.
- the minority carrier ⁇ of all five polycrystalline silicon ingots is 25 sec or more and less than 3 O S ⁇ c. Good.
- At least one polycrystalline silicon ingot has a low intensity carrier of at least 20 2sec and less than 25 ⁇ sec (other than 25 ⁇ sec). Within the acceptable range.
- At least one polycrystalline silicon ingot with less carrier ⁇ is less than 20 2sec. No.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/599,544 US7867334B2 (en) | 2004-03-29 | 2005-03-29 | Silicon casting apparatus and method of producing silicon ingot |
JP2006511615A JP4777880B2 (ja) | 2004-03-29 | 2005-03-29 | シリコン鋳造装置およびシリコンインゴットの製造方法 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004093936 | 2004-03-29 | ||
JP2004-093936 | 2004-03-29 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2005092791A1 true WO2005092791A1 (ja) | 2005-10-06 |
Family
ID=35056106
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2005/006549 WO2005092791A1 (ja) | 2004-03-29 | 2005-03-29 | シリコン鋳造装置および多結晶シリコンインゴットの製造方法 |
Country Status (3)
Country | Link |
---|---|
US (1) | US7867334B2 (ja) |
JP (1) | JP4777880B2 (ja) |
WO (1) | WO2005092791A1 (ja) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008534414A (ja) * | 2005-03-23 | 2008-08-28 | ドイチェ ソーラー アクチェンゲゼルシャフト | 非鉄金属材料の結晶化の為の装置及び方法 |
WO2009014961A1 (en) * | 2007-07-20 | 2009-01-29 | Bp Corporation North America Inc. | Methods and apparatuses for manufacturing cast silicon from seed crystals |
KR20110106304A (ko) * | 2008-12-19 | 2011-09-28 | 꼼미사리아 아 레네르지 아토미끄 에뜨 옥스 에너지스 앨터네이티브즈 | 측벽을 통하여 가변 열교환하는 용융/응고 노 |
US8048221B2 (en) | 2006-01-20 | 2011-11-01 | Stoddard Nathan G | Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics |
WO2013128758A1 (ja) * | 2012-02-28 | 2013-09-06 | シャープ株式会社 | シリコン鋳造用鋳型、シリコン鋳造方法、シリコン材料および太陽電池の製造方法 |
JP2014500216A (ja) * | 2010-11-17 | 2014-01-09 | シリコー マテリアルズ インコーポレイテッド | シリコンの方向性凝固のための機器および方法 |
JP2014527013A (ja) * | 2011-08-01 | 2014-10-09 | ジーティーエイティー・コーポレーション | 液冷式熱交換機 |
Families Citing this family (30)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2928665B1 (fr) * | 2008-03-14 | 2010-04-09 | Thermique Ind Vide | Four industriel pour la fabrication d'un lingot de materiau cristallin |
US20110259262A1 (en) * | 2008-06-16 | 2011-10-27 | Gt Solar, Inc. | Systems and methods for growing monocrystalline silicon ingots by directional solidification |
US9567691B2 (en) * | 2008-06-20 | 2017-02-14 | Varian Semiconductor Equipment Associates, Inc. | Melt purification and delivery system |
TW201012988A (en) * | 2008-08-27 | 2010-04-01 | Bp Corp North America Inc | Gas recirculation heat exchanger for casting silicon |
DE102009022412A1 (de) * | 2009-05-22 | 2010-11-25 | Ald Vacuum Technologies Gmbh | Vorrichtung zum gerichteten Erstarren geschmolzener Metalle |
WO2011001689A1 (ja) * | 2009-07-02 | 2011-01-06 | パナソニック株式会社 | 薄膜製造方法およびその方法に使用できるシリコン材料 |
KR100947836B1 (ko) * | 2009-09-28 | 2010-03-18 | (주)세미머티리얼즈 | 실리콘 잉곳 제조장치 |
DE102009044893B4 (de) * | 2009-12-14 | 2014-10-30 | Hanwha Q.CELLS GmbH | Herstellungsverfahren zur Herstellung eines Kristallkörpers aus einem Halbleitermaterial |
CN101906657B (zh) * | 2010-07-08 | 2013-04-03 | 王敬 | 制造单晶锭的*** |
JP2012106886A (ja) * | 2010-11-17 | 2012-06-07 | Nippon Steel Materials Co Ltd | 金属シリコンの凝固精製方法及び装置 |
CN102010120B (zh) * | 2010-12-14 | 2012-09-05 | 维苏威太阳能坩埚(苏州)有限公司 | 恒温恒湿浇铸装置 |
US20120248286A1 (en) | 2011-03-31 | 2012-10-04 | Memc Singapore Pte. Ltd. (Uen200614794D) | Systems For Insulating Directional Solidification Furnaces |
US20130252011A1 (en) * | 2011-09-14 | 2013-09-26 | MEMC Singapore, Pte. Ltd. (UEN200614797D) | Multi-Crystalline Silicon Ingot And Directional Solidification Furnace |
CN103797164A (zh) * | 2011-09-14 | 2014-05-14 | Memc新加坡私人有限公司 | 具有可移动式热交换器的定向固化炉 |
US20130239621A1 (en) * | 2011-09-14 | 2013-09-19 | MEMC Singapore, Pte. Ltd. (UEN200614797D) | Directional Solidification Furnace With Laterally Movable Insulation System |
US9352389B2 (en) * | 2011-09-16 | 2016-05-31 | Silicor Materials, Inc. | Directional solidification system and method |
TWM457160U (zh) * | 2011-11-02 | 2013-07-11 | Morgan Advanced Materials And Technology Inc | 熔爐、一罩與隔熱箱之總成及隔熱箱 |
EP2589687A1 (en) | 2011-11-04 | 2013-05-08 | Vesuvius France (S.A.) | Crucible and method for the production of a (near ) monocrystalline semiconductor ingot |
EP2604728A1 (en) | 2011-12-12 | 2013-06-19 | Vesuvius France S.A. | Crucible for the production of crystalline semiconductor ingots and process for manufacturing the same |
TWI539039B (zh) * | 2012-01-26 | 2016-06-21 | 希利柯爾材料股份有限公司 | 矽的純化方法 |
BR112014032592A2 (pt) * | 2012-06-25 | 2017-06-27 | Silicor Mat Inc | forro para superfícies de um cadinho refratário para purificação de silício e método de purificação da corrida de silício usando o(s) cadinho(s) para fundir e solidificação adicional |
TWI643983B (zh) | 2013-03-14 | 2018-12-11 | 美商希利柯爾材料股份有限公司 | 定向凝固系統及方法 |
ITTO20130258A1 (it) * | 2013-03-28 | 2014-09-29 | Saet Spa | Dispositivo e metodo per produrre un blocco di materiale multicristallino, in particolare silicio, mediante solidificazione direzionale |
US10065239B2 (en) | 2013-09-17 | 2018-09-04 | United Technologies Corporation | Casting molds, manufacture and use methods |
US20150090181A1 (en) * | 2013-09-30 | 2015-04-02 | Gt Crystal Systems, Llc | Automated heat exchanger alignment |
GB201319671D0 (en) * | 2013-11-07 | 2013-12-25 | Ebner Ind Ofenbau | Controlling a temperature of a crucible inside an oven |
CN103741211B (zh) * | 2013-12-19 | 2016-08-31 | 镇江环太硅科技有限公司 | 长晶炉及长晶炉均匀散热的控制方法 |
US10724796B2 (en) * | 2018-05-24 | 2020-07-28 | Silfex, Inc | Furnace for casting near-net shape (NNS) silicon |
JP7186534B2 (ja) * | 2018-07-25 | 2022-12-09 | 昭和電工株式会社 | 結晶成長装置 |
TWI771007B (zh) * | 2020-05-19 | 2022-07-11 | 環球晶圓股份有限公司 | 矽單晶錠的製造方法、矽單晶錠及其製造裝置 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0971497A (ja) * | 1995-09-05 | 1997-03-18 | Sharp Corp | 多結晶半導体の製造方法 |
JPH1111924A (ja) * | 1997-06-23 | 1999-01-19 | Sharp Corp | 多結晶半導体インゴットの製造方法および装置 |
JP2002293526A (ja) * | 2001-03-29 | 2002-10-09 | Kawasaki Steel Corp | 多結晶シリコンの製造装置 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1519897B2 (de) * | 1966-08-06 | 1974-07-18 | Siemens Ag, 1000 Berlin Und 8000 Muenchen | Verfahren und Vorrichtung zum tiegelfreien Zonenschmelzen eines kristallinen Stabes, insbesondere Halbleiterstabes |
JPS60137891A (ja) * | 1983-12-24 | 1985-07-22 | Sumitomo Electric Ind Ltd | 化合物半導体単結晶引き上げ方法と装置 |
JPS63166711A (ja) | 1986-12-26 | 1988-07-09 | Osaka Titanium Seizo Kk | 多結晶シリコン鋳塊の製造法 |
JPH07122535B2 (ja) | 1990-07-09 | 1995-12-25 | ダイエー食品工業株式会社 | 飲食用氷の製造方法 |
DE19607098C2 (de) * | 1996-02-24 | 1999-06-17 | Ald Vacuum Techn Gmbh | Verfahren und Vorrichtung zum gerichteten Erstarren einer Schmelze aus Silizium zu einem Block in einem bodenlosen metallischen Kaltwandtiegel |
JP3885452B2 (ja) | 1999-04-30 | 2007-02-21 | 三菱マテリアル株式会社 | 結晶シリコンの製造方法 |
JP2002292458A (ja) | 2001-03-29 | 2002-10-08 | Kyocera Corp | シリコン鋳造装置およびシリコン鋳造方法 |
-
2005
- 2005-03-29 JP JP2006511615A patent/JP4777880B2/ja not_active Expired - Fee Related
- 2005-03-29 US US10/599,544 patent/US7867334B2/en not_active Expired - Fee Related
- 2005-03-29 WO PCT/JP2005/006549 patent/WO2005092791A1/ja active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0971497A (ja) * | 1995-09-05 | 1997-03-18 | Sharp Corp | 多結晶半導体の製造方法 |
JPH1111924A (ja) * | 1997-06-23 | 1999-01-19 | Sharp Corp | 多結晶半導体インゴットの製造方法および装置 |
JP2002293526A (ja) * | 2001-03-29 | 2002-10-09 | Kawasaki Steel Corp | 多結晶シリコンの製造装置 |
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008534414A (ja) * | 2005-03-23 | 2008-08-28 | ドイチェ ソーラー アクチェンゲゼルシャフト | 非鉄金属材料の結晶化の為の装置及び方法 |
US8951344B2 (en) | 2006-01-20 | 2015-02-10 | Amg Idealcast Solar Corporation | Methods and apparatuses for manufacturing geometric multicrystalline cast silicon and geometric multicrystalline cast silicon bodies for photovoltaics |
US8048221B2 (en) | 2006-01-20 | 2011-11-01 | Stoddard Nathan G | Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics |
US8628614B2 (en) | 2006-01-20 | 2014-01-14 | Amg Idealcast Solar Corporation | Methods and apparatus for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics |
WO2009014961A1 (en) * | 2007-07-20 | 2009-01-29 | Bp Corporation North America Inc. | Methods and apparatuses for manufacturing cast silicon from seed crystals |
JP2011528308A (ja) * | 2007-07-20 | 2011-11-17 | ビーピー・コーポレーション・ノース・アメリカ・インコーポレーテッド | シード結晶からキャストシリコンを製造するための方法及び装置 |
US20100197070A1 (en) * | 2007-07-20 | 2010-08-05 | BP Corproation North America Inc. | Methods and Apparatuses for Manufacturing Cast Silicon From Seed Crystals |
KR20110106304A (ko) * | 2008-12-19 | 2011-09-28 | 꼼미사리아 아 레네르지 아토미끄 에뜨 옥스 에너지스 앨터네이티브즈 | 측벽을 통하여 가변 열교환하는 용융/응고 노 |
JP2012512797A (ja) * | 2008-12-19 | 2012-06-07 | コミサリア ア レネルジー アトミック エ オ ゼネルジー アルテルナティブ | 側壁を介した可変熱交換を備える溶融凝固炉 |
KR101699987B1 (ko) * | 2008-12-19 | 2017-01-26 | 꼼미사리아 아 레네르지 아토미끄 에뜨 옥스 에너지스 앨터네이티브즈 | 측벽을 통하여 가변 열교환하는 용융/응고 노 |
US9127373B2 (en) | 2008-12-19 | 2015-09-08 | Commissariat A L'Energie Atomique Et Aux Energies Alternative | Melting-solidification furnace with variable heat exchange via the side walls |
JP2014500216A (ja) * | 2010-11-17 | 2014-01-09 | シリコー マテリアルズ インコーポレイテッド | シリコンの方向性凝固のための機器および方法 |
JP2014527013A (ja) * | 2011-08-01 | 2014-10-09 | ジーティーエイティー・コーポレーション | 液冷式熱交換機 |
JP2017149641A (ja) * | 2011-08-01 | 2017-08-31 | ジーティーエイティー・コーポレーション | 液冷式熱交換機 |
WO2013128758A1 (ja) * | 2012-02-28 | 2013-09-06 | シャープ株式会社 | シリコン鋳造用鋳型、シリコン鋳造方法、シリコン材料および太陽電池の製造方法 |
JP2013177274A (ja) * | 2012-02-28 | 2013-09-09 | Sharp Corp | シリコン鋳造用鋳型、シリコン鋳造方法、シリコン材料および用途 |
Also Published As
Publication number | Publication date |
---|---|
US20070227189A1 (en) | 2007-10-04 |
JPWO2005092791A1 (ja) | 2008-02-14 |
JP4777880B2 (ja) | 2011-09-21 |
US7867334B2 (en) | 2011-01-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2005092791A1 (ja) | シリコン鋳造装置および多結晶シリコンインゴットの製造方法 | |
KR100861412B1 (ko) | 다결정 실리콘 잉곳 제조장치 | |
US6299682B1 (en) | Method for producing silicon ingot having directional solidification structure and apparatus for producing the same | |
EP1867759B1 (en) | Manufacturing equipment for polysilicon ingot | |
ES2494416T3 (es) | Homogeneización y tratamiento térmico de metales colados | |
EP2640874B1 (en) | Apparatus and method for directional solidification of silicon | |
JP4357810B2 (ja) | 鋳造装置及び鋳造方法 | |
CN103813983B (zh) | 定向凝固***和方法 | |
CN105229206B (zh) | 定向凝固***和方法 | |
CN103890242B (zh) | 液体冷却热交换器 | |
KR20130033410A (ko) | 다결정성 규소 잉곳을 제조하기 위한 방법 및 장치 | |
TW201335445A (zh) | 製造單晶矽的方法 | |
WO1999064369A1 (en) | Method and apparatus for preparing a crystal of cremated remains | |
JP2010162573A (ja) | ポーラス金属の製造方法及びヒートシンクの製造方法 | |
JPH10139580A (ja) | 一方向凝固材の製造方法および一方向凝固装置 | |
TW201213251A (en) | Float bath for manufacturing float glass and cooling method of the same | |
US9410266B2 (en) | Process for producing multicrystalline silicon ingots by the induction method, and apparatus for carrying out the same | |
WO2012011523A1 (ja) | 多結晶シリコンインゴット製造装置、多結晶シリコンインゴットの製造方法及び多結晶シリコンインゴット | |
JP2002308616A (ja) | 多結晶シリコンの製造方法 | |
JP2000016893A (ja) | 単結晶引上方法および単結晶引上装置 | |
JP2001278613A (ja) | シリコンの一方向凝固装置 | |
JP4480357B2 (ja) | 板状シリコン製造装置 | |
JP2006199511A (ja) | 結晶製造装置 | |
JP2004203687A (ja) | 化合物半導体製造装置 | |
JP2002293527A (ja) | 多結晶シリコンの製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
AK | Designated states |
Kind code of ref document: A1 Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BW BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE EG ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NA NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SM SY TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW |
|
AL | Designated countries for regional patents |
Kind code of ref document: A1 Designated state(s): BW GH GM KE LS MW MZ NA SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LT LU MC NL PL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application | ||
DPEN | Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed from 20040101) | ||
WWE | Wipo information: entry into national phase |
Ref document number: 2006511615 Country of ref document: JP |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
WWW | Wipo information: withdrawn in national office |
Country of ref document: DE |
|
WWE | Wipo information: entry into national phase |
Ref document number: 10599544 Country of ref document: US Ref document number: 2007227189 Country of ref document: US |
|
122 | Ep: pct application non-entry in european phase | ||
WWP | Wipo information: published in national office |
Ref document number: 10599544 Country of ref document: US |