WO2011157382A1 - Verfahren und vorrichtung zum herstellen von polykristallinen siliziumblöcken - Google Patents
Verfahren und vorrichtung zum herstellen von polykristallinen siliziumblöcken Download PDFInfo
- Publication number
- WO2011157382A1 WO2011157382A1 PCT/EP2011/002858 EP2011002858W WO2011157382A1 WO 2011157382 A1 WO2011157382 A1 WO 2011157382A1 EP 2011002858 W EP2011002858 W EP 2011002858W WO 2011157382 A1 WO2011157382 A1 WO 2011157382A1
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- WIPO (PCT)
- Prior art keywords
- silicon
- crucible
- melt
- silicon material
- process chamber
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 67
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 119
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 116
- 239000010703 silicon Substances 0.000 claims abstract description 116
- 230000008569 process Effects 0.000 claims abstract description 55
- 239000002210 silicon-based material Substances 0.000 claims abstract description 37
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 238000007711 solidification Methods 0.000 claims abstract description 15
- 230000008023 solidification Effects 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 230000002123 temporal effect Effects 0.000 claims 1
- 235000012431 wafers Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000000717 retained effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 50
- 239000002994 raw material Substances 0.000 description 21
- 238000009413 insulation Methods 0.000 description 13
- 238000011049 filling Methods 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000155 melt Substances 0.000 description 8
- 239000008187 granular material Substances 0.000 description 6
- 239000003570 air Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
-
- 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
-
- 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
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Definitions
- the present invention relates to a method and an apparatus for producing polycrystalline silicon ingots.
- the desired level of silicon melt in the crucible When the desired level of silicon melt in the crucible is reached, it is then cooled in a controlled manner for directional solidification.
- the type of cooling and the atmosphere has a significant influence on the size and orientation of the crystallites, which arise in the directional solidification.
- the above-mentioned device offers few possibilities to influence the cooling and the atmosphere.
- the replenisher unit is also direction consuming.
- the preparation of the dried, free-flowing silicon material is complex and associated with high costs.
- silicon rods such as those produced by the Siemens process, are mechanically comminuted. It is known, for example, to work the silicon rods with hammers, chisels or a grinder in order to obtain silicon fragments.
- these are usually etched in an HF / HNO 3 mixture, whereby a partial area of the surface (typically 20 ⁇ m) of the silicon fragments is removed.
- the reason for the etching is the cleaning of the fragments, and in particular the removal of contamination from the surface, which can be caused by the tools used, as well as the necessity of removing the silicon oxide layer on the silicon surface.
- metallic contaminants generated by the tools such as iron, chromium, nickel, copper, are to be removed from the silicon fragments.
- further contaminants that are caused by the ambient atmosphere air, oxygen, dust and particles in the air) can be removed.
- Such contaminants may include, but are not limited to, native oxides.
- the surface removal of each fragment is usually minimally about 7.5 ⁇ . Subsequently, the fragments are usually rinsed with deionized water and then dried in a purified stream of air (N 2 stream).
- N 2 stream a purified stream of air
- a crucible is disposed within a process chamber, wherein the crucible is filled with solid silicon material or filled in the process chamber with silicon material. Subsequently, the silicon material in the crucible is heated above its melting temperature when the process chamber is closed in order to form a silicon melt in the crucible, and then the silicon melt in the crucible is cooled below its solidification temperature.
- a plate member disposed in the process chamber having at least one gas supply passage is lowered over the crucible, and during at least a portion of time within the period of solidification of the silicon melt, gas flow is directed to the surface of the silicon melt, the gas flow at least partially over the at least one through opening in the plate element is directed onto the surface of the silicon melt.
- the gas flow may additionally be directed to the surface of the silicon in the crucible during the heating process and / or during the cooling process. Passing gas onto the surface of the silicon melt in the space formed between the surface and the plate member allows a good adjustment of cooling parameters as well as the atmosphere at the surface of the melt.
- the term period of solidification of the silicon melt should be understood as the period in which the change of silicon from the liquid state of aggregation to the solid state of aggregation takes place.
- additional silicon material Prior to closing the process chamber, additional silicon material is attached to the plate member such that at least a portion of the additional silicon material is immersed and melted in the crucible as the plate member is lowered into the silicon melt, thereby increasing the fill level of the silicon melt in the crucible.
- the plate element serves both as a gas-conducting element and as a recharging unit.
- the additional silicon material is preferably formed by silicon rod material and / or silicon wafer material, which facilitates appropriate processing. In addition, such material is easy to attach to the plate member because of its size.
- the amount of solid silicon material in the crucible and the amount of additional silicon material are matched. This can be done, for example, simply by the weight of the material.
- the device has the following: a process chamber, with a crucible receptacle for receiving a crucible, a plate element arranged inside the process chamber above the crucible receptacle and having at least one passage opening for a gas feed, optionally a lifting mechanism for the plate element, at least one gas feed tube, extending into or through the at least one through hole in the plate member, and at least one gas supply unit outside the process chamber for directing gas flow into and through the gas supply pipe into an area below the plate member.
- the plate element means for fixing silicon material in order to serve as a charging unit.
- the additional silicon material can be introduced into the silicon melt solely by the one stroke movement of the plate element, so that no additional guide elements are required.
- the device can also have a retaining ring arranged in the process chamber, which can have internal dimensions corresponding to the inner dimensions of side walls of a crucible, and optionally a lifting mechanism for the retaining ring.
- the retaining ring is also able to hold silicon material above the crucible prior to reflow, thus improving the fill level of the silicon melt in the crucible during the process.
- the optional lifting unit allows the Lift the retaining ring from the crucible after melting the silicon material during the process so that it does not adversely affect the process.
- the retaining ring is made of silicon nitride or has at least one silicon nitride coating on the inner circumference.
- At least one side heater spaced apart from the side of the crucible, at least one gas outlet and at least one film curtain are provided, wherein the at least one film curtain is arranged between the at least one side heater and the crucible such that the one passed through the at least one gas supply pipe Gas flow are directed in the direction of at least one gas outlet, without flowing on the at least one side heater along.
- a gas flow conducted over the surface of the silicon melt, after sweeping over the silicon surface can be guided substantially along the side of the film curtain facing the crucible directly in the direction of the gas outlet, without reaching the region of the at least one side heater.
- Such a curtain protects the side heaters from the fact that gases from the process space (such as gaseous silicon taken from the melt) reach the heater directly and coat or destroy it over time.
- the film curtain is preferably temperature-resistant and gas-tight and easily replaceable received in the process chamber. As soon as the film curtain loses its functionality due to the stress during the process after a number of process cycles, it can be easily exchanged.
- the plate member may also be formed as a heater or wear such.
- the invention will be explained in more detail with reference to the drawings; in the drawings shows: 1 shows a schematic sectional view through an apparatus for producing a polycrystalline silicon block with a crucible filled with silicon raw material;
- Figure 2 is a schematic view similar to Figure 1, wherein the silicon raw material is melted in the crucible.
- Fig. 3 is a schematic view similar to Fig. 2, but with additional silicon raw material immersed in the crucible;
- Fig. 4 is a schematic view similar to Fig. 3 during a cooling phase
- FIG. 5 shows a schematic sectional view through an alternative apparatus for producing a polycrystalline silicon block with a crucible filled with silicon raw material
- Fig. 6 is a schematic view similar to Figure 5, in which the silicon raw material is melted in the crucible.
- FIG. 1 shows a schematic sectional view through an apparatus 1 for producing a polycrystalline silicon block.
- the device 1 consists essentially of an insulation box 3, which defines a process space 4. Within the process space 4, a receiving unit not shown in detail for receiving a crucible 6, a Bodenmoretician 8 and 9.habdoien 9 are provided. At least one gas outlet 10 is provided at the lower end of the side wall of the insulation box 3. A plate member 1 1 is provided above the receptacle for the crucible 6, and further, a gas supply line 13 is provided, which extends from above through the insulation box 3 and through the plate member 11 into the process space 4. Between the side heaters 9 and the crucible 6 optional film curtains 14 are also provided, which are mounted above the uppermost side heater unit. The insulation box 3 is constructed of a suitable insulating material as known in the art and will therefore not be described further. The process chamber 4 communicates via means not shown in more detail with gas supply and discharge lines in order to set a specific process atmosphere therein. These are not shown in detail except for the gas supply line 13 and the outlets 10.
- the crucible 6 is made of a suitable known material, such as silicon carbide, fused silica, silicon nitride, or coated with silicon nitride fused silica, which does not affect the manufacturing process and withstands the high temperatures during melting of silicon material.
- the crucible 6 is usually partially destroyed during the process by thermal expansion processes and can be easily removed to remove the finished silicon block.
- the crucible 6 forms an upwardly open trough, which, as shown in Figure 1, can be filled with silicon raw material 20 to its upper edge. Silicon rods are used for the filling, for example, and the gaps are at least partially filled with silicon fracture, as indicated on the left side in FIG. As a result, a relatively good degree of filling can be achieved, however, air pockets still remain within the filled crucible. As a result, the silicon raw material 20, when melted, does not completely fill the crucible 6, as indicated in FIG. 2, the cross-hatched region being a silicon melt 22.
- the bottom heater 8 and the side heaters 9 are suitable heating units capable of sufficiently heating the process chamber 4, and in particular, the crucible 6 and the silicon raw material 20 therein, so that the raw material 20 melts and forms a melt 22, as in FIG Figure 2 is shown.
- the plate element 11 arranged above the crucible 6 is made of a suitable material which does not melt at the temperatures used for melting the silicon raw material and which does not introduce impurities into the process.
- the plate element 11 can be moved up and down within the process chamber via a mechanism (not shown), as will be explained in more detail below with reference to FIGS. 3 and 4.
- Holding units 24 capable of holding additional silicon raw material, such as silicon rods 26, below the plate member 11 are provided on the underside of the plate member 11. In the illustration according to FIG. 1, four silicon rods 26 are shown, which are arranged in a row below the plate element 11. Of course, more such retaining elements are provided over the depth (ie, perpendicular to the plane of view) to hold additional silicon rods 26.
- the holding elements 24 can be made e.g. Wear silicon raw material in the form of disks or rod sections of different length.
- the retaining elements are shown only as simple rods, which are screwed, for example, in the silicon rods. But they can also be grippers or other elements that are suitable to carry the silicon rods 26. Again, they should be made of temperature-resistant material that does not contaminate the silicon melt.
- the plate element 11 has a peripheral shape that approximately corresponds to the inner circumference of the crucible 6.
- the plate member further has a central passage opening 30 through which the gas supply pipe 13 extends.
- the gas feed tube 13 is made of a suitable material, such as graphite. It extends out of the process chamber 4 through the insulation box 3 to the outside and is there connected to a suitable gas supply for example argon. Gas can be introduced into the process chamber 4 via the gas supply pipe 13, as explained in more detail below becomes.
- the gas supply pipe 13 may provide a guide for the plate member 11 during an up or down movement thereof.
- the film curtains 14 attached thereto can extend in a region between side heaters 9 and crucible 6, as indicated in FIGS. 1 to 4, and optionally also at least partially cover the ceiling region of the process space 4 (FIG. 6).
- the film curtains 14 are made of a temperature-resistant, gas-tight material.
- Fig. 1 shows the device 1, before the start of the actual manufacturing process.
- the crucible 6 is filled with silicon raw material 20 up to its upper edge.
- silicon rods and silicon granules have been used to fill the crucible 6.
- Silicon rods 26 are attached to the plate element 11 via the holding elements 24.
- the silicon raw material 20 is now melted in the crucible 6 while supplying heat through the bottom heater 8 and the side heaters 9.
- the side heaters 9 and the bottom heater are regulated in such a way that heat is supplied primarily from below, so that the silicon rods 26, which are held above the crucible 6 by the plate element 11, are indeed heated, but do not melt.
- a silicon melt 22 is formed in the crucible 6, as shown in FIG.
- the silicon rods 26 on the plate member 11 are not yet melted at this time.
- the plate member 1 1 is lowered via the lifting mechanism, not shown, to the silicon rods 26th into the silicon melt 22, as shown in FIG.
- the degree of filling of the silicon melt 22 within the crucible increases substantially, as can be seen in Fig. 3.
- the immersed silicon rods 26 are completely melted by the contact with the silicon melt 22 and optionally additional heat through the bottom heater 8 and the side heaters 9 and enter the melt 22 a.
- the plate element can be left either in the position according to FIG. 3, provided that the holding elements 24 do not contact the silicon melt 22. If this is the case, the plate member 11 is slightly raised to lift the holding members 24 out of the melt 22, as shown in Figure 4.
- the bottom heater 8 and the side heaters 9 can be significantly reduced in their heat supply at this time, or turned off to achieve a cooling of the silicon melt 22 within the crucible 6.
- the cooling is controlled by suitable mechanisms, not shown in detail, that a solidification of the melt 22 from bottom to top takes place in a directed manner.
- Fig. 4 can be seen at 32, as the lower part of the silicon material is solidified in the crucible, while on top of silicon melt 22 is still present.
- gas such as argon, is directed onto the surface of the silicon melt 22 via the gas feed tube 13.
- the gas flows over the surface of the silicon melt 22 to the outside and then between the crucible 6 and the film curtain 14 to the gas outlet 10, as can be seen in Figure 4.
- the film curtain 14 serves as protection of the side heaters 9 against contact with the guided over the surface of the silicon melt, and therefore gas-containing silicon gas.
- the side heaters 9 may be chemically reacted by an additional gas introduced, for example, separately between the film curtain 14 and the insulation box 3, which does not react chemically with the material of the side heaters or with the gas flow derived from the surface of the silicon melt (For example, with argon or with another noble gas) are surrounded. This prevents that the gas, which was passed over the silicon melt 22 and has gaseous silicon, reaches the heater. Both the additional gas conducted via the side heaters 9 and the gas conducted via the silicon melt 22 can be discharged via the gas outlets 10.
- a block of silicon is formed within the crucible 6, which is the final product.
- the block can be further cooled within the process chamber 4 to a handling temperature before it is removed therefrom.
- FIGS. 5 and 6 show an alternative embodiment of a device 1 for producing a polycrystalline silicon block according to the present invention.
- the same reference numerals are used in FIGS. 5 and 6, if identical or similar elements are designated.
- the device 1 in turn essentially consists of an insulation box 3, which forms a process space 4 in the interior.
- a receptacle for a crucible 6 is provided within the process space 4.
- a bottom heater 8 and side heater 9 are again provided in the process space.
- film curtains 14 may be provided in the process space 4, which may additionally extend at least partially along the ceiling area of the insulation box 3, so that the film curtain 14 at least partially extends the side walls of the crucible similar to a canopy covers all page heaters outside of the covered area.
- a plate element 11 is again arranged above the crucible 6.
- the plate element 1 1 is again made of a suitable material, which is the manufacturing process of the polycrystalline silicon blocks are not affected. However, in these embodiments (FIGS. 5 and 6), the plate element 11 does not have holding elements for receiving additional silicon material.
- the plate member 11 has a plurality of passage openings 30 for passing a corresponding plurality of gas supply pipes 13, each extending out of the process space 4 through the insulation box 3 to the outside.
- the gas supply pipes 13 may be constructed in the same manner as the gas supply pipes 13 shown in Fig. 1. However, a larger number are provided. In the illustration according to FIG. 5, gas supply tubes 13 are shown across the width of the device 3.
- three gas supply tubes 13 would also be arranged in series across the depth of the device, so that a total of nine gas supply tubes 13 would be provided.
- the plate member 11 could also have a further plurality of passage openings for passing a corresponding further plurality of Gasab USArohren (not shown) and be equipped with the appropriate number of Gasab Technologyrohren, through which the silicon melt supplied gas could be discharged again. This would have the advantage that the gas overflowing the surface of the silicon melt would immediately be discharged upwards again, without being conducted past the side heaters.
- a retaining ring 40 is disposed within the process space 4.
- the retaining ring 40 has an inner peripheral shape corresponding substantially to the inner periphery of the side walls of the crucible 6, as shown in FIG.
- the retaining ring 40 is made of a suitable reusable material, such as silicon nitride, which does not melt during the fusing process for the silicon raw material 20 itself.
- silicon nitride is relatively robust and non-wetting for molten silicon. That is, molten silicon contacting the retaining ring 40 would flow away therefrom.
- the retaining ring 40 can be moved up and down via a mechanism, not shown, as will be explained in more detail below. The operation of the device 1 will be explained in more detail below with reference to Figures 5 and 6.
- the crucible 6 is charged into the process chamber 4, and loaded with silicon raw material 20, which may for example again consist of silicon rods and silicon granules, as shown in FIG.
- silicon raw material 20 which may for example again consist of silicon rods and silicon granules, as shown in FIG.
- the crucible 6 can in turn be loaded up to its upper edge.
- the retaining ring 40 is placed in its position on the edge of the crucible 6, or held closely spaced thereto.
- additional silicon raw material for example in the form of silicon rods, can be loaded into the retaining ring 40.
- a loading of the crucible 6 is possible beyond its upper edge, as shown in Figure 5.
- such a loading can also take place outside the process chamber 4 and the crucible 6 with retaining ring 40 can be loaded into the process chamber 4.
- the silicon raw material 20 within the crucible 6 and the additional silicon raw material in the region of the retaining ring 40 are then completely melted to form a silicon melt 22 within the crucible 6.
- the total material is dimensioned such that the silicon melt 22 can be completely absorbed by the crucible 6. This can be achieved, for example, by weighing the silicon raw material used before loading.
- the holder ring 40 can then be lifted off the crucible 6.
- the plate member 11 can be lowered in a position adjacent to the top of the melt 22 in the crucible 6, as shown in Figure 6.
- the film curtains 14 can in turn be brought into a position between side heaters 9 and crucible 6, as also shown in FIG.
- FIG. 6 again shows in a lower region at 32 the already partially solidified silicon block with silicon melt 22 located above it.
- a gas flow such as an argon flow
- a controlled flow space is formed between the plate member 11 and the top of the silicon melt. The fact that the retaining ring 40 is raised, it does not affect the corresponding gas flow.
- the plate element can also be used with other Nachchargererüen and it can be designed as a heating unit or wear such. The plate element could then be used as an adjustable ceiling heater.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP11725343.5A EP2582639A1 (de) | 2010-06-16 | 2011-06-10 | Verfahren und vorrichtung zum herstellen von polykristallinen siliziumblöcken |
JP2013514576A JP2013532111A (ja) | 2010-06-16 | 2011-06-10 | 多結晶シリコンインゴットの製造方法及び装置 |
KR1020137001086A KR20130113422A (ko) | 2010-06-16 | 2011-06-10 | 다결정성 규소 블록을 생산하기 위한 방법 및 장치 |
US13/703,922 US20130219967A1 (en) | 2010-06-16 | 2011-06-10 | Method and device for producing polycrystalline silicon blocks |
CN2011800378039A CN103038180A (zh) | 2010-06-16 | 2011-06-10 | 用于生产多晶硅锭的方法和装置 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE102010024010A DE102010024010B4 (de) | 2010-06-16 | 2010-06-16 | Verfahren und Vorrichtung zum Herstellen von polykristallinen Siliziumblöcken |
DE102010024010.9 | 2010-06-16 |
Publications (1)
Publication Number | Publication Date |
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WO2011157382A1 true WO2011157382A1 (de) | 2011-12-22 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2011/002858 WO2011157382A1 (de) | 2010-06-16 | 2011-06-10 | Verfahren und vorrichtung zum herstellen von polykristallinen siliziumblöcken |
Country Status (7)
Country | Link |
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US (1) | US20130219967A1 (de) |
EP (1) | EP2582639A1 (de) |
JP (1) | JP2013532111A (de) |
KR (1) | KR20130113422A (de) |
CN (1) | CN103038180A (de) |
DE (1) | DE102010024010B4 (de) |
WO (1) | WO2011157382A1 (de) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20130255318A1 (en) * | 2010-06-16 | 2013-10-03 | Centrotherm Sitec Gmbh | Process and apparatus for manufacturing polycrystalline silicon ingots |
DE102010031819B4 (de) | 2010-07-21 | 2012-11-15 | Centrotherm Sitec Gmbh | Verfahren und Vorrichtung zum Herstellen von polykristallinen Siliziumblöcken |
DE102011002156B4 (de) * | 2011-04-19 | 2013-02-14 | Q-Cells Se | Kristallherstellungsverfahren |
DE102014201096A1 (de) | 2014-01-22 | 2015-07-23 | Wacker Chemie Ag | Verfahren zur Herstellung von polykristallinem Silicium |
JP6414408B2 (ja) * | 2014-07-25 | 2018-10-31 | 株式会社Sumco | シリコン単結晶の製造方法 |
JP6472732B2 (ja) | 2015-09-15 | 2019-02-20 | 信越化学工業株式会社 | 樹脂材料、ビニール製袋、多結晶シリコン棒、多結晶シリコン塊 |
CN108884563A (zh) * | 2015-11-16 | 2018-11-23 | Gtat公司 | 化学气相沉积方法和装置 |
DE102016001730A1 (de) * | 2016-02-16 | 2017-08-17 | Krasimir Kosev | Polykristallherstellungsvorrichtung |
CN114751416A (zh) * | 2022-04-28 | 2022-07-15 | 成都惠锋智造科技有限公司 | 一种球状氧化物制造方法 |
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DE3644746A1 (de) * | 1986-12-30 | 1988-07-14 | Hagen Hans Dr Ing | Verfahren und vorrichtung zum zuechten von kristallen |
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FR2817560A1 (fr) * | 2000-12-01 | 2002-06-07 | Sharp Kk | Creuset et procede pour realiser la croissance de silicium polycristallin a l'aide dudit creuset |
US20020108557A1 (en) * | 2000-10-31 | 2002-08-15 | Wood Henry D. | Rod replenishment system for use in single crystal silicon production |
EP1384538A1 (de) * | 2002-07-25 | 2004-01-28 | Mitsubishi Materials Corporation | Giessvorrichtung zum Herstellen polykristalliner Siliziumbarren und Giessverfahren |
DE10234250A1 (de) * | 2002-07-27 | 2004-02-05 | Deutsche Solar Ag | Vorrichtung sowie Verfahren zur Überwachung der Kristallisation eines Mediums, insbesondere von Silizium |
DE102006017622A1 (de) * | 2006-04-12 | 2007-10-18 | Schott Ag | Verfahren und Vorrichtung zur Herstellung von multikristallinem Silizium |
WO2009100694A1 (de) * | 2008-02-14 | 2009-08-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Vorrichtung und verfahren zur herstellung von kristallinen körpern durch gerichtete erstarrung |
-
2010
- 2010-06-16 DE DE102010024010A patent/DE102010024010B4/de not_active Expired - Fee Related
-
2011
- 2011-06-10 JP JP2013514576A patent/JP2013532111A/ja not_active Withdrawn
- 2011-06-10 EP EP11725343.5A patent/EP2582639A1/de not_active Withdrawn
- 2011-06-10 KR KR1020137001086A patent/KR20130113422A/ko not_active Application Discontinuation
- 2011-06-10 CN CN2011800378039A patent/CN103038180A/zh active Pending
- 2011-06-10 US US13/703,922 patent/US20130219967A1/en not_active Abandoned
- 2011-06-10 WO PCT/EP2011/002858 patent/WO2011157382A1/de active Application Filing
Patent Citations (8)
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DE3644746A1 (de) * | 1986-12-30 | 1988-07-14 | Hagen Hans Dr Ing | Verfahren und vorrichtung zum zuechten von kristallen |
DE19934940C2 (de) | 1999-07-26 | 2001-12-13 | Ald Vacuum Techn Ag | Vorrichtung zum Herstellen von gerichtet erstarrten Blöcken und Betriebsverfahren hierfür |
US20020108557A1 (en) * | 2000-10-31 | 2002-08-15 | Wood Henry D. | Rod replenishment system for use in single crystal silicon production |
FR2817560A1 (fr) * | 2000-12-01 | 2002-06-07 | Sharp Kk | Creuset et procede pour realiser la croissance de silicium polycristallin a l'aide dudit creuset |
EP1384538A1 (de) * | 2002-07-25 | 2004-01-28 | Mitsubishi Materials Corporation | Giessvorrichtung zum Herstellen polykristalliner Siliziumbarren und Giessverfahren |
DE10234250A1 (de) * | 2002-07-27 | 2004-02-05 | Deutsche Solar Ag | Vorrichtung sowie Verfahren zur Überwachung der Kristallisation eines Mediums, insbesondere von Silizium |
DE102006017622A1 (de) * | 2006-04-12 | 2007-10-18 | Schott Ag | Verfahren und Vorrichtung zur Herstellung von multikristallinem Silizium |
WO2009100694A1 (de) * | 2008-02-14 | 2009-08-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Vorrichtung und verfahren zur herstellung von kristallinen körpern durch gerichtete erstarrung |
Also Published As
Publication number | Publication date |
---|---|
CN103038180A (zh) | 2013-04-10 |
KR20130113422A (ko) | 2013-10-15 |
DE102010024010A1 (de) | 2011-12-22 |
DE102010024010B4 (de) | 2012-03-22 |
EP2582639A1 (de) | 2013-04-24 |
US20130219967A1 (en) | 2013-08-29 |
JP2013532111A (ja) | 2013-08-15 |
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