EP3126549A1 - Creuset, procédé de fabrication du creuset, et procédé de fabrication d'un matériau cristallin au moyen d'un tel creuset - Google Patents
Creuset, procédé de fabrication du creuset, et procédé de fabrication d'un matériau cristallin au moyen d'un tel creusetInfo
- Publication number
- EP3126549A1 EP3126549A1 EP15717572.0A EP15717572A EP3126549A1 EP 3126549 A1 EP3126549 A1 EP 3126549A1 EP 15717572 A EP15717572 A EP 15717572A EP 3126549 A1 EP3126549 A1 EP 3126549A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- crucible
- marks
- side wall
- seed
- cutting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000002178 crystalline material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims description 19
- 238000004519 manufacturing process Methods 0.000 title description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 49
- 238000007711 solidification Methods 0.000 claims abstract description 14
- 230000008023 solidification Effects 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 239000011449 brick Substances 0.000 claims description 25
- 238000002425 crystallisation Methods 0.000 claims description 23
- 230000008025 crystallization Effects 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000003754 machining Methods 0.000 description 3
- 239000003550 marker Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000001459 lithography Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000012768 molten material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 230000000181 anti-adherent effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007713 directional crystallization Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/22—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
-
- 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
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/06—Joining of crystals
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/002—Crucibles or containers
-
- 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
-
- 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
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1864—Annealing
-
- 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
- Y02E10/547—Monocrystalline silicon PV cells
Definitions
- the invention relates to a crucible for the manufacture of a crystalline material by solidification and in particular by directed crystallization.
- the invention also relates to the method of manufacturing such a crucible, and the method of manufacturing a crystalline material from such a crucible.
- the invention relates primarily to the growth of silicon ingots for photovoltaic applications, but it can also potentially be applicable to any type of material to be cut according to precise ribs after a solidification process.
- the ingot In the case of a directed growth from a tiling of monocrystalline seeds deposited at the bottom of the crucible, the crystalline material is melted above the seeds which will impose the crystalline orientation during the solidification.
- the ingot In order to guarantee the good electrical and mechanical quality of the crystalline bricks, the ingot should advantageously be cut off at the level of the monocrystalline seed joints, so as to relegate the defects induced at these seals of seeds at the periphery of the bricks. This cutting phase of the brick ingot is delicate because the molten material has flowed throughout the crucible and monocrystalline seed seals are no longer visible.
- An object of the invention is to provide a crucible for the manufacture of a crystalline material by solidification by germ recovery having good electrical and mechanical properties.
- the crucible comprises a bottom and at least one orthogonal lateral wall at the bottom of the crucible, and means for materializing the position of at least one seed intended to be positioned at the bottom of the crucible, said seed comprising at least first and second orthogonal faces at the bottom of the crucible.
- the materialization means advantageously comprise at least two marks extending on the internal face of the at least one side wall along an orthogonal axis at the bottom of the crucible.
- the respective positions of at least two of the marks on at least one of the lateral walls define, in the crystalline material, a first cutting plane tangential to the first face of said seed and a second cutting plane tangential to the second face of said seed.
- a crucible comprising at least one bottom and at least one orthogonal lateral wall at the bottom of the crucible,
- the invention finally relates to the method of producing a crystalline material brick by solidification using such a crucible, the method comprising the following steps:
- Performing a directed crystallization operation comprising placing at least one monocrystalline seed at the bottom of the crucible using at least two markers, to form an ingot of crystalline material in the crucible,
- FIG. 1 is a perspective view of a crucible according to a particular embodiment of the invention
- FIGS. 2 and 3 represent two different embodiments of the crucible of FIG. 1,
- FIG. 4 is a top view of the way in which monocrystalline seeds are positioned in the crucible
- FIG. 5 shows the cutting of the ingot after removal of the crucible.
- a crucible 1 is conventionally used to form an ingot of crystalline material by solidification by resumption on seed, and in particular by directed crystallization.
- the crystalline material may for example be a semiconductor material such as silicon or germanium. It can also be an oxide, for example aluminum oxide (sapphire).
- the crucible 1 advantageously comprises a bottom 2 and at least one side wall 3 orthogonal to the bottom 2. According to a particular embodiment illustrated in the figures, the crucible 1 may for example comprise four side walls 3, so as to form a crystalline ingot parallelepiped, and preferably having a rectangular parallelepiped shape or cube.
- the shape of the crucible 1 facilitates the cutting of the ingot brick as will be seen later. But it is for example quite possible to use a crucible of any shape, for example a cylindrical crucible.
- the crucible 1 is advantageously provided with means for materializing the position of at least one seed intended to be positioned at the bottom of the crucible before the formation of the crystalline material by solidification by resumption on seed.
- the means of materialization may comprise at least two marks 4 on the internal face of the side wall 3 of the crucible 1, advantageously positioned along an orthogonal axis at the bottom 2 of the crucible 1.
- the positions of at least two of these pins 4 are chosen so as to define first and second cutting planes of the crystalline ingot obtained by solidification by resumption on seed. Indeed, once solidified, the ingot has the imprint of the marks 4 on its side walls, so that the determination of the cutting planes is facilitated.
- Each cutting plane is advantageously tangential to one of the faces of a seed positioned at the bottom of the crucible before the directed crystallization, and passes through one of the marks 4.
- the first mark 4 may be positioned so that the first cutting plane is orthogonal to a plane tangential to the internal face of the side wall 3.
- the second cutting plane is itself orthogonal to the first plane of cutting and passes through a second marker 4.
- the crucible 1 has two adjacent perpendicular side walls, at least two of the marks 4 can be positioned respectively on two adjacent side walls 3.
- the first cutting plane can then be advantageously parallel to a first side wall 3, and the second cutting plane parallel to a second side wall 3 adjacent to the first side wall.
- This configuration of the crucible 1 is particularly advantageous for forming ingots of parallelepipedal shape, rectangular parallelepiped shape or cubic shape.
- the crucible 1 may comprise at least one additional mark, advantageously positioned opposite one of the markers 4, for example on a side wall 3 opposite to the side wall having the mark 4 when the crucible 1 is parallelepipedic.
- the fact of positioning two pins 4 facing each other makes it possible to determine the position of the cutting plane of the ingot after crystallization with increased precision.
- the crucible 1 may include positioning means (not shown) at the bottom of the crucible 1. Their role is to allow the placement of the seeds in predefined positions relative to the pins 4. These positioning means are for example those described in the international application WO 2013/034819, that is to say, holes for positioning the seeds. . They can also take the form of markers such as grooves, ribs, or studs facilitating the placement of germs.
- the marks 4 advantageously extend over the entire height of the internal faces of the side walls 3 along an axis orthogonal to the bottom 2 of the crucible 1.
- each reference 4 may extend only over part of the height of the internal faces of the side walls 3, for example from the bottom 2 of the crucible, or from the upper edge of the side walls 3.
- the length of each marker 4 is greater than 10% of the height of the side walls 3, preferably greater than 30% of the height of the side walls 3, and preferably greater than 50% of the height of the side walls 3.
- the marks 4 may also be continuous or discontinuous, and present different heights.
- Each reference 4 of the crucible 1 may therefore have characteristics of its own, for example when the crucible 1 is intended for the crystallization of several types of crystalline materials whose properties differ, thus leading to different possible cuts of the ingot.
- the position of each marker 4 can be judiciously chosen depending on the type of crystallization performed, and depending on the type of material to be crystallized. 4 marks can be placed a few centimeters from the ends of the side walls 3 to keep only the central portion of the ingot during cutting. Indeed, the edges of the ingots are generally contaminated by elements from the crucible 1 and are therefore of lower quality of use. This phenomenon is particularly well known in the case of silicon for photovoltaic applications where the edges of the ingot are qualified under the name red zone in English.
- the marks 4 make it possible to ensure the centering of the crystalline bricks which are cut in the ingot in order to ensure the quality thereof, and to ensure the reproducibility of the positioning of the ingot during the cutting of the latter.
- the ingot should be advantageously cut at the monocrystalline seed seals, so as to relegate the defects induced at these seals seeds at the periphery of the bricks.
- the directed crystallization is carried out by resumption on seeds, it may be useful to place the markers 4 at the edges of the monocrystalline seeds, so as to relegate the defects induced in the crystal at these seals of seeds at the periphery of the bricks and improve their mechanical and electrical quality.
- the defects are eliminated without the user needing to look for signs of solidification on the upper and lower faces of the ingot.
- the bricks used advantageously have a rectangular parallelepiped shape or cube, whose sides have dimensions generally between 50 and 200 mm.
- Photovoltaic panels comprise for example cells whose standard size is equal to 156 mm side.
- the crucible 1 may advantageously comprise pins 4 placed on its inner side wall 3 so that two consecutive marks of the same side wall 3 are spaced 50 to 200 mm, and preferably distant of 156 mm.
- pins 4 placed on its inner side wall 3 so that two consecutive marks of the same side wall 3 are spaced 50 to 200 mm, and preferably distant of 156 mm.
- the marks 4 may be ribs, that is to say reliefs formed in over-thickness, or grooves, that is to say, reliefs formed in under-thickness on the side walls 3 of the crucible 1.
- ribs are preferred especially when the crucible is silicon oxide, and the crystalline material is silicon.
- the pins 4 are ribs
- the indentations left on the crystalline ingot are then grooves, that is to say reliefs in sub-thickness.
- the marks 4 are grooves
- the impressions left on the ingot are ribs, that is to say reliefs in over-thickness.
- the grooves may for example be formed by machining the internal faces of the side walls 3, or by etching through a mask according to any conventional lithography technique.
- machining is meant a mechanical removal of the material forming the crucible.
- etching is meant a chemical elimination, for example an HF solution for a silica crucible.
- the grooves preferably have a depth of less than 2 mm.
- the pins 4 are ribs, they can be made by means of a template (not shown) to give a homogeneous shape over the entire length of the marks 4. An input material is then made on one side internal side wall 3 of the crucible 1. The ribs protrude over a thickness preferably less than 2 mm.
- the marks 4 may advantageously have a triangular shape, and in particular an isosceles triangular shape. This triangular shape is visible in a plane parallel to the bottom 2 of the crucible 1.
- a template of suitable size and shape may, for example, enable the production of ribs advantageously having a section whose base, ie the width of the rib, measures between 100 ⁇ m and 6 mm, preferably between 500 ⁇ m and 2 mm, and whose apex angle is between 30 ° and 120 °, preferably between 45 ° and 90 °. These dimensions form a good compromise between the constraints of realization of the ribs, and the accuracy of the positioning of the cutting axis of the ingot.
- the ribs may for example be made by a localized deposit of a solution containing a powder compatible with the material to be crystallized, and a heat treatment allowing the sintering of the powder.
- a solution containing a powder compatible with the material to be crystallized for example if the material to be crystallized is Si If the powder can be Si 3 N 4 .
- the crucible 1 may advantageously be used in a crystallization furnace (not shown) in which a thermal gradient of crystallization is applied during the directional crystallization operation, in order to achieve the growth of the crystalline material.
- This thermal gradient is advantageously applied along an orthogonal axis to the bottom 2 of the crucible, the temperature being all the colder as one approaches the bottom 2 of the crucible 1.
- the invention also relates to the method of producing a crucible 1.
- This can be implemented from a crucible of any shape and size. It may for example be silica or graphite (crystallization of semiconductors) or precious metals (crystallization of oxides). Whether the crucible is reusable or not, it deforms during the melting and solidification phases of the material.
- the resultant forces exerted by the molten material on the side faces 3 deforms the corners of the crucible 1 which become more pointed, and push the lateral faces 3 towards the outside of the crucible 1. Then, as the temperature decreases, the volume of the crystalline ingot decreases by crystallizing.
- the silica crucibles undergo a glass transition and crystallization during the crystalline growth of the material. These phase changes generate variations of about 2% between the initial and final dimensions of the crucible, these variations being dependent on the exact composition of the crucible. It is therefore impossible to make an abacus deformation of the crucible during the crystalline growth of the material.
- the presence of the marks 4 makes it possible to precisely define the position of the cutout independently of the deformation of the ingot.
- the dimensions of the marks 4 are small enough not to have any influence on the variations in size of the crucible during its phase changes.
- Another role played by the marks 4 is to keep the memory of the position of the seeds after the crystallization cycle.
- the marks 4 on the lateral faces 3 may be judicious to form the marks 4 in zones of the lateral faces 3 which deform little, for example in the vicinity of the center of the latter if the crucible 1 has a parallelepipedic shape.
- a crucible 1 As described above, use is made of a crucible comprising at least one bottom 2 and at least one side wall 3 orthogonal to the bottom 2, and at least two orthogonal markers 4 are formed at the bottom 2 on the internal faces. at least one of the side walls 3.
- the marks 4 may be made continuously from the bottom 2 or the upper edge of the side walls 3, or discontinuously on the side walls 3. Their lengths may be greater than at least 10% of the total height of the side walls. 3, preferentially over lengths greater than 30%, even more preferably over lengths greater than 50%, and advantageously the entire height of the side walls 3.
- the marks 4 may advantageously have a triangular section, so as to be able to pinpoint the cutting axis of the ingot.
- the base of the triangular section may for example be between 100 ⁇ and 6 mm, and the apex angle may be between 45 ° and 90 °.
- At least one of the marks 4 may be a groove formed for example by machining at least one of the internal faces of the side walls 3, or by engraving according to conventional lithography techniques.
- the marks 4 may advantageously be ribs manufactured using a template.
- the crucible 1 is made of silicon oxide and the material to be crystallized is silicon
- the marks 4 may advantageously be made using a material comprising a powder of Si 3 N 4 .
- 35% to 55% of powder of Si 3 N 4 , 1% to 4% of polyvinyl alcohol, and deionized water are advantageously mixed. This mixture is applied locally on the inner faces of the side walls 3 of the crucible 1 using the template to form the marks 4.
- This mixture must be sufficiently viscous not to sink or spread during application to the walls.
- the assembly is then annealed in a heated oven at a temperature between 900 ° and 1200 ° C, preferably between 1000 ° C and 1100 ° C.
- the annealing time is between 30 min and 4 h, preferably between 1 h and 3 h.
- the marks 4 are ribs comprising 43% of powder of Si 3 N 4 , 2.3% of polyvinyl alcohol, and deionized water.
- the crucible 1 is annealed in an oven at 1050 ° C for 2 hours. Si 3 N 4 having anti-adhesive properties, this makes it easier to demold the ingot after crystallization.
- the material is introduced into the crucible 1, for example silicon, and then the assembly is placed in a crystallization furnace such as the one mentioned above.
- a thermal gradient is applied in the crystallization furnace, and this gradient is advantageously directed along an orthogonal axis to the bottom 2 of the crucible 1.
- the material goes through a melting phase, then solidification.
- the ingot is then demolded when the material is completely crystallized. Traces due to the marks 4 appear on the side walls of the ingot.
- the traces are used to correctly position cutting wires or blades 6 along the first and second cutting axes, so as to obtain crystalline bricks, for example bricks of crystalline silicon. This step of manufacturing the bricks 5 is illustrated in FIG.
- germ-directed growth can be used.
- at least one monocrystalline seed is deposited on the bottom 2 of the crucible 1, advantageously using the means for positioning the seeds on the bottom 2 of the crucible 1.
- the positioning means may for example be pins 4 whose positions on the side walls 3 of the crucible 1 are chosen to be adapted to the dimensions of the seeds.
- the traces left by the marks 4 advantageously make it possible to make the cutting planes coincide with the planes of the joints of the monocrystalline seeds.
- additional cutting planes may be chosen in order to perform one or more additional cutting steps.
- Two additional cutting planes may for example be used, these two additional planes being advantageously parallel to the first and second cutting planes.
- the Additional cutting planes can be positioned for example by means of additional marks 4 placed on the side walls 3 of the crucible 1. They can also be determined from the position of the first and second cutting planes.
- five square shaped seeds and four rectangular shaped seeds are used to form the crystalline material by directed crystallization.
- the seeds are arranged to occupy the entire bottom 2 of the crucible 1, and eight pins 4 have advantageously been placed on the side walls 3 of the crucible 1 at the junctions between the seeds.
- the latter is demolded and cut into bricks according to four parallel cutting planes in pairs, the cutting planes coinciding with the planes of the seed joints.
- Crystalline bricks without grain boundaries or having grain boundaries relegated to the periphery of the crystalline bricks are thus obtained.
- the latter thus have a high electrical and mechanical quality, and meet the requirements in the field of photovoltaics.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1400784A FR3019189B1 (fr) | 2014-03-31 | 2014-03-31 | Creuset, procede de fabrication du creuset, et procede de fabrication d'un materiau cristallin au moyen d'un tel creuset |
PCT/FR2015/050818 WO2015150681A1 (fr) | 2014-03-31 | 2015-03-30 | Creuset, procédé de fabrication du creuset, et procédé de fabrication d'un matériau cristallin au moyen d'un tel creuset |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3126549A1 true EP3126549A1 (fr) | 2017-02-08 |
Family
ID=50976738
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP15717572.0A Withdrawn EP3126549A1 (fr) | 2014-03-31 | 2015-03-30 | Creuset, procédé de fabrication du creuset, et procédé de fabrication d'un matériau cristallin au moyen d'un tel creuset |
Country Status (4)
Country | Link |
---|---|
US (1) | US20170016140A1 (fr) |
EP (1) | EP3126549A1 (fr) |
FR (1) | FR3019189B1 (fr) |
WO (1) | WO2015150681A1 (fr) |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1577413A (en) * | 1976-03-17 | 1980-10-22 | Metals Research Ltd | Growth of crystalline material |
USH520H (en) * | 1985-12-06 | 1988-09-06 | Technique for increasing oxygen incorporation during silicon czochralski crystal growth | |
US6277351B1 (en) * | 2000-03-20 | 2001-08-21 | Carl Francis Swinehart | Crucible for growing macrocrystals |
JP4545505B2 (ja) * | 2004-07-22 | 2010-09-15 | 株式会社トクヤマ | シリコンの製造方法 |
EP1974077A2 (fr) * | 2006-01-20 | 2008-10-01 | BP Corporation North America Inc. | Procédés et appareils destinés à fabriquer du silicium coulé monocristallin et des corps de silicium coulé monocristallin pour des applications photovoltaïques |
TW200846509A (en) * | 2007-01-19 | 2008-12-01 | Vesuvius Crucible Co | Crucible and filling method for melting a non-ferrous product |
JP2011251891A (ja) * | 2010-05-06 | 2011-12-15 | Sumitomo Electric Ind Ltd | 単結晶の製造方法および単結晶製造用るつぼ |
DE102010048602A1 (de) * | 2010-10-15 | 2012-04-19 | Centrotherm Sitec Gmbh | Schmelztiegel für Silizium, Schmelztiegelanordnung und Trenneinheit für einen Schmelztiegel |
US20120167817A1 (en) * | 2010-12-30 | 2012-07-05 | Bernhard Freudenberg | Method and device for producing silicon blocks |
KR20140060549A (ko) * | 2011-08-31 | 2014-05-20 | 이에스케이 세라믹스 게엠베하 운트 코. 카게 | 경도가 큰 질화규소-함유 중간층 |
FR2979638A1 (fr) | 2011-09-05 | 2013-03-08 | Commissariat Energie Atomique | Dispositif de fabrication de materiau cristallin a partir d'un creuset a resistance thermique non uniforme |
-
2014
- 2014-03-31 FR FR1400784A patent/FR3019189B1/fr not_active Expired - Fee Related
-
2015
- 2015-03-30 WO PCT/FR2015/050818 patent/WO2015150681A1/fr active Application Filing
- 2015-03-30 US US15/124,319 patent/US20170016140A1/en not_active Abandoned
- 2015-03-30 EP EP15717572.0A patent/EP3126549A1/fr not_active Withdrawn
Also Published As
Publication number | Publication date |
---|---|
FR3019189A1 (fr) | 2015-10-02 |
US20170016140A1 (en) | 2017-01-19 |
FR3019189B1 (fr) | 2018-07-27 |
WO2015150681A1 (fr) | 2015-10-08 |
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