EP2132366A2 - Device and method for producing self-sustained plates of silicon or other crystalline materials - Google Patents

Device and method for producing self-sustained plates of silicon or other crystalline materials

Info

Publication number
EP2132366A2
EP2132366A2 EP08775638A EP08775638A EP2132366A2 EP 2132366 A2 EP2132366 A2 EP 2132366A2 EP 08775638 A EP08775638 A EP 08775638A EP 08775638 A EP08775638 A EP 08775638A EP 2132366 A2 EP2132366 A2 EP 2132366A2
Authority
EP
European Patent Office
Prior art keywords
crucible
slot
liquid
plate
phase material
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Withdrawn
Application number
EP08775638A
Other languages
German (de)
French (fr)
Inventor
Roland Einhaus
François Lissalde
Yves Delannoy
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Centre National de la Recherche Scientifique CNRS
Institut Polytechnique de Grenoble
Apollon Solar SAS
Cyberstar
Original Assignee
Centre National de la Recherche Scientifique CNRS
Institut Polytechnique de Grenoble
Apollon Solar SAS
Cyberstar
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Centre National de la Recherche Scientifique CNRS, Institut Polytechnique de Grenoble, Apollon Solar SAS, Cyberstar filed Critical Centre National de la Recherche Scientifique CNRS
Publication of EP2132366A2 publication Critical patent/EP2132366A2/en
Withdrawn legal-status Critical Current

Links

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
    • C30B11/001—Continuous growth
    • 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
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • 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
    • C30B15/06—Non-vertical pulling
    • 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
    • C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
    • 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
    • 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
    • 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

Definitions

  • the invention relates to a device for producing a plate of crystalline material by directed crystallization of a liquid phase material in a crucible provided with a bottom, side walls and at least one plate outlet slot, said slot being horizontal and formed in a lower part of a side wall.
  • the purpose of the invention is to overcome these drawbacks and in particular to provide a device and a method for manufacturing crystalline material plates by directed crystallization, which is easier to implement and whose rejection of impurities in the liquid phase is more important.
  • the crucible has, on its outer surface, in the immediate vicinity of the plate exit slot, electromagnetic means of creation, at least at the level of the slot of plate outlet, magnetic repulsion forces on the liquid phase material, said electromagnetic means being traversed by an alternating current whose frequency is between 1OkHz and 30OkHz.
  • FIG. 1 shows a schematic sectional view of a particular embodiment of the device according to the invention.
  • FIG. 1 shows a front view of the slot of the device according to Figure 1.
  • FIG. 3 shows a schematic sectional view of another particular embodiment of the device according to the invention.
  • Figure 4 shows an enlargement of Figure 3, centered on the slot and the magnetic means for creating magnetic forces.
  • the device represented in FIGS. 1 and 2 comprises a crucible 1 having a bottom 2 and side walls 3.
  • the crucible 1 has a lateral outlet slot 4 arranged horizontally in the lower part of the the right side wall 3 in FIG. 1.
  • the crucible 1 is partially filled with a material in the liquid phase 5.
  • the exit slot 4 is in communication with the surrounding atmosphere 7 the crucible 1, generally consisting of a neutral gas, such as argon.
  • a plate 8 of crystalline material, obtained by directed crystallization of the material in the crucible 1, is drawn through the slot 4.
  • the crystalline material is, for example silicon, germanium, gallium arsenide ...
  • the thermal gradient inside the crucible 1 is vertical, the temperature decreasing from the top of the crucible 1 to the bottom 2.
  • the solidification of the material inside the crucible 1 causes the formation of grain boundaries perpendicular to the plate 8 of solid phase material. This configuration is advantageous for use in photovoltaic devices.
  • the directed crystallization of the material preferably takes place at the bottom 2 of the crucible 1 and the solid phase material forming the plate 8 is withdrawn from the bath through the outlet slot 4, as and when it is solidified by any means of appropriate grip not shown in Figure 1.
  • the thermal regulation within the crucible 1 is carried out by any means known to maintain, stable and vertical, the thermal gradient in the crucible 1.
  • the crucible 1 may advantageously be coupled to a heating system 9, preferably situated above the crucible 1, and to a calorie extraction system 10, preferably located under the crucible 1, in order to maintain the temperature gradient substantially vertical.
  • the thermal gradient is, in the crucible 1, substantially perpendicular to the solidification interface.
  • the calorie extraction system 10 regulates the heat flux extracted under the material being solidified and the distribution of the heat flow according to the distance to the slot 4.
  • the calorie extraction system 10 is, for example, a radiative heat transfer through a transparent bottom 2 of the crucible 1.
  • the side walls 3 of the crucible 1 are advantageously coupled to a thermal insulator 11.
  • This thermal insulator 11 is preferably placed outside the crucible 1 over the entire surface delimited by the side walls 3. way, there is no heat loss on the side walls 3 and the thermal gradient is maintained substantially vertical.
  • the solidification interface of the material is located in the lower part of the crucible 1, preferably near the bottom 2 of the crucible 1. This position is adjusted by means of the thermal gradient in the crucible 1.
  • the thickness of the plate 8 thus obtained is essentially defined by the thermal distribution in the crucible 1 and the drawing speed of the plate 8 out of the crucible 1.
  • the drawing speed of the plate 8 is preferably located in the range 0.5 - 10 meters / minute.
  • the height of the slot 4 is chosen to be greater than the thickness of the plate 8, so as to avoid any mechanical catching and any parasitic solidification during the exit of the plate 8 through the slot 4.
  • the device further comprises at least one inductor 6 outside the crucible 1, against the side wall 3, in the immediate vicinity of the exit slot 4.
  • the inductor 6 constitutes a preferred embodiment of the electromagnetic means of 6.
  • the inductor 6 is traversed by an alternating current having a frequency of between 10kHz and 30OkHz and an intensity, preferably between 100A and 3000A. the inductor 6 thus creates magnetic repulsion forces on the material in the liquid phase 5.
  • the inductor 6 may be arranged above or below the slot 4. In the particular embodiment of FIG. 1, two inductors 6 are arranged on either side of the slot 4.
  • the interface between the liquid phase material 5 and the atmosphere 7 is in the form of a meniscus 12.
  • the latter is preferably situated inside the slot 4, so as to prohibit any exit of the material in the liquid phase. through the slot 4 without disturbing the crystallization of the material in the liquid phase 5 inside the crucible 1.
  • the magnetic repulsion forces created by the inductor 6 are adjusted so that the repulsion of the liquid phase material 5 takes place at the exit slot 4, above the plate 8. Repulsion forces also act between the edges of the plate 8 and each lateral end.
  • the material in the liquid phase 5 is thus kept inside the crucible 1.
  • the amplitude of the current in the inductor 6 is determined as a function of the hydrostatic pressure of the liquid-phase material 5 in the crucible 1 and the distance between the inductor 6 and the meniscus 12.
  • the section of the inductor 6 is chosen so as to best concentrate the repulsion forces on the meniscus 12.
  • An exemplary embodiment of the device implements an inductor 6 concentrating the currents at about 5 mm from the meniscus 12.
  • This inductor allows the retention in the crucible of a silicon height of 5 cm, when it is traversed by a current of 900 A to a frequency of 30Khz.
  • the slot 4 has a width of 75mm and a height of 3mm.
  • the inductor 6 also causes a stirring effect of the material in the liquid phase 5 close to the slot 4. It creates recirculation loops of the material in the liquid phase 5, which entrain the impurities originating from the solidification interface in the entire material in the liquid phase 5.
  • the accumulation of impurities near the solid phase is also reduced compared to the prior art due to the presence of a broader solidification front.
  • the stirring effect is favored by the use of a current in the inductor in the low frequency range, for example, of the order of 50 Hz.
  • the device therefore preferably comprises means for superimposing at a frequency of between 1 kHz and 300 kHz a frequency favoring stirring in the material in the liquid phase 5.
  • two inductors 6 are provided, respectively, traversed by currents of different frequencies.
  • a first inductor is then powered by a current having a frequency to ensure the mixing of the material in the liquid phase 5, preferably in the low frequency range, of the order of 50Hz.
  • the other inductor is traversed by a current having a frequency between 1OkHz and 300 kHz to ensure the repulsion of the material in the liquid phase 5.
  • This simultaneous action can also be performed by a single inductor, for example, by a frequency modulation , amplitude over-modulation, etc.
  • the plate 8 of crystalline material consists exclusively of solid phase. Indeed, the material in the liquid phase 5 is pushed back inside the crucible 1 by the inductor 6. The plate 8 is then self-supporting from the outlet of the crucible.
  • the material in the liquid phase 5 is brought into contact with a crystallization seed when starting the solidification.
  • the crystallization seed is preferably brought into contact with the meniscus 12 to allow the start of crystallization according to predetermined orientations.
  • Nucleation / germination centers for example, consisting of localized cold spots, can be added at the interface between the bottom 2 of the crucible 1 and the liquid phase material 5 to facilitate the start of crystallization.
  • a treatment device 13 in particular a thermal device, is coupled to the crucible 1 at the exit of the slot 4.
  • This device allows the monitoring of a predefined profile of the cooling kinetics of the plate 8. This profile makes it possible to reduce the mechanical stresses and the density of crystalline defects.
  • the device 13 can be used to preheat the crystallization seed used at the start of the solidification.

Abstract

The invention relates to a device for making a plate (8) of a crystalline material by the directed crystallisation of a liquid-phase material (5), that comprises at least one crucible (1) with a bottom (2), side walls (3) and at least one horizontal outlet slot (4) provided on a lower portion of a side wall (3). The crucible (1) comprises, on its outer surface and in the immediate vicinity of the slot (4), electromagnetic means (6) for generating, at least at the slot (4), magnetic repulsion forces on the liquid-phase material (5). An alternating current with a frequency between 10kHz and 300kHz flows through the electromagnetic means (6). In order to promote the agitation of the liquid-phase material (5), a low frequency can be superimposed to the former.

Description

Dispositif et procédé de fabrication de plaques autosupportées de silicium ou autres matériaux cristallins Device and method for manufacturing self-supporting plates of silicon or other crystalline materials
Domaine technique de l'inventionTechnical field of the invention
L'invention concerne un dispositif de fabrication d'une plaque de matériau cristallin par cristallisation dirigée d'un matériau en phase liquide dans un creuset muni d'un fond, de parois latérales et d'au moins une fente de sortie de plaque, ladite fente étant horizontale et formée dans une partie inférieure d'une paroi latérale.The invention relates to a device for producing a plate of crystalline material by directed crystallization of a liquid phase material in a crucible provided with a bottom, side walls and at least one plate outlet slot, said slot being horizontal and formed in a lower part of a side wall.
État de la techniqueState of the art
La fabrication de plaques de matériau cristallin par cristallisation dirigée au moyen d'un creuset muni d'une fente permet d'obtenir des rubans directement à partir de la matière première liquide, sans nécessiter, après cristallisation d'un lingot, d'étapes supplémentaires d'écroûtage du lingot, de débitage du lingot écroûté en brique et de découpe des briques en plaquettes par sciage. Cependant, pour être intégré dans des cellules photovoltaïques, les plaquettes doivent présenter des joints de grains perpendiculaires aux jonctions P/N utilisées et donc perpendiculaires à la surface de la plaquette.The manufacture of crystalline material plates by directed crystallization by means of a crucible provided with a slit makes it possible to obtain ribbons directly from the liquid raw material, without requiring, after crystallization of an ingot, additional steps. ingot removal of the ingot, debiting of the brick-encrusted ingot and cutting of slab bricks by sawing. However, to be integrated in photovoltaic cells, the platelets must have grain boundaries perpendicular to the P / N junctions used and therefore perpendicular to the surface of the wafer.
La principale difficulté rencontrée actuellement par ce type de dispositif tient dans le contrôle du gradient thermique vertical dans la zone de solidification au sein du creuset. Il a été proposé dans la demande de brevet international PCT/FR2006/002349 (déposé le 19 octobre 2006), un dispositif dans lequel l'interface de solidification séparant la phase solide et la phase liquide se trouve au niveau de la fente latérale du creuset. En effet, ce dispositif est difficile à mettre en œuvre et présente certains inconvénients. En effet, la solidification au sein du creuset est limitée à une faible surface. De même, le brassage dans la phase liquide n'est pas suffisant pour que les impuretés aient la possibilité de migrer dans le bain. Elles peuvent alors se retrouver dans la phase solide avec l'avancée du front de solidification. Ces impuretés sont alors préjudiciables aux cellules photovoltaïques à intégrer.The main difficulty currently encountered by this type of device is in the control of the vertical thermal gradient in the solidification zone within the crucible. It has been proposed in the international patent application PCT / FR2006 / 002349 (filed October 19, 2006), a device in which the solidification interface separating the solid phase and the liquid phase is at the level of the lateral slot of the crucible . Indeed, this device is difficult to implement and has some disadvantages. Indeed, the solidification within the crucible is limited to a small area. Similarly, stirring in the liquid phase is not sufficient for the impurities have the opportunity to migrate into the bath. They can then be in the solid phase with the advance of the solidification front. These impurities are then detrimental to the photovoltaic cells to integrate.
Les articles de Hide et al (« Cast Ribbon for Low Cost Solar CeIIs » 0160- 8371/88/0000-1400, 1988 IEEE 26 septembre 1988) et de Suzuki et al (« Growth of Polycrystalline Silicon Sheet by Hoxan Cast Ribbon Process » Journal of crystal growth, Elsevier, vol 104, n°1 1 juillet 1990) présentent un autre procédé de cristallisation dirigée au moyen d'une filière. Le silicium est fondu à l'intérieur d'un creuset et s'écoule sous pression au sein d'une fente située au centre du fond du creuset. La chaussette et le moule coudé qui suivent le creuset forment alors dans la section finale un canal étroit et allongé. Dans cette portion, le gradient thermique vertical imposé entraîne une cristallisation dirigée et verticale de l'ensemble de la matière. Cette dernière est alors incapable, au vu de la dimension de la filière de rejeter hors de la phase solide les impuretés présentes en phase liquide.The articles of Hide et al ("Cast Ribbon for Low Cost Solar CeIIs" 0160- 8371/88 / 0000-1400, 1988 IEEE 26 September 1988) and Suzuki et al ("Growth of Polycrystalline Silicone Sheet by Hoxan Cast Ribbon Process" Journal of crystal growth, Elsevier, vol. 104, No. 11, July 1990) discloses another spin-directed crystallization method. The silicon is melted inside a crucible and flows under pressure in a slot in the center of the bottom of the crucible. The sock and the bent mold which follow the crucible then form in the final section a narrow and elongated channel. In this portion, the imposed vertical thermal gradient causes a directed and vertical crystallization of the whole material. The latter is then unable, given the size of the die to reject out of the solid phase impurities present in the liquid phase.
Objet de l'inventionObject of the invention
L'objet de l'invention a pour but de remédier à ces inconvénients et en particulier de fournir un dispositif et un procédé de fabrication de plaques de matériau cristallin par cristallisation dirigée, qui soit plus facile à mettre en œuvre et dont le rejet des impuretés dans la phase liquide soit plus important.The purpose of the invention is to overcome these drawbacks and in particular to provide a device and a method for manufacturing crystalline material plates by directed crystallization, which is easier to implement and whose rejection of impurities in the liquid phase is more important.
Ce but est atteint par le fait que le creuset présente, sur sa surface extérieure, à proximité immédiate de la fente de sortie de plaque, des moyens électromagnétiques de création, au moins au niveau de la fente de sortie de plaque, de forces de répulsion magnétiques sur le matériau en phase liquide, lesdits moyens électromagnétiques étant parcouru par un courant alternatif dont la fréquence est comprise entre 1OkHz et 30OkHz.This object is achieved by the fact that the crucible has, on its outer surface, in the immediate vicinity of the plate exit slot, electromagnetic means of creation, at least at the level of the slot of plate outlet, magnetic repulsion forces on the liquid phase material, said electromagnetic means being traversed by an alternating current whose frequency is between 1OkHz and 30OkHz.
Description sommaire des dessinsBrief description of the drawings
D'autres avantages et caractéristiques ressortiront plus clairement de la description qui va suivre de modes particuliers de réalisation de l'invention donnés à titre d'exemples non limitatifs et représentés aux dessins annexés, dans lesquels :Other advantages and features will emerge more clearly from the following description of particular embodiments of the invention given by way of non-limiting example and represented in the accompanying drawings, in which:
- la figure 1 représente une vue schématique, en coupe, d'un mode de réalisation particulier du dispositif selon l'invention.- Figure 1 shows a schematic sectional view of a particular embodiment of the device according to the invention.
- la figure 2 représente une vue de face de la fente du dispositif selon la figure 1.- Figure 2 shows a front view of the slot of the device according to Figure 1.
- la figure 3 représente une vue schématique, en coupe, d'un autre mode de réalisation particulier du dispositif selon l'invention.- Figure 3 shows a schematic sectional view of another particular embodiment of the device according to the invention.
- la figure 4 représente un agrandissement de la figure 3, centrée sur la fente et les moyens électromagnétiques de création de forces magnétiques.- Figure 4 shows an enlargement of Figure 3, centered on the slot and the magnetic means for creating magnetic forces.
Description d'un mode préférentiel de l'inventionDescription of a preferred embodiment of the invention
Comme dans la demande PCT/FR2006/002349, le dispositif représenté sur les figure 1 et 2, comporte un creuset 1 ayant un fond 2 et des parois latérales 3. Le creuset 1 comporte une fente de sortie 4 latérale disposée horizontalement en partie inférieure de la paroi latérale 3 de droite sur la figure 1. Le creuset 1 est partiellement rempli d'un matériau en phase liquide 5. La fente de sortie 4 est en communication avec l'atmosphère 7 entourant le creuset 1 , généralement constituée par un gaz neutre, comme l'argon. Une plaque 8 de matériau cristallin, obtenue par cristallisation dirigée du matériau au sein du creuset 1 , est tirée à travers la fente 4.As in application PCT / FR2006 / 002349, the device represented in FIGS. 1 and 2 comprises a crucible 1 having a bottom 2 and side walls 3. The crucible 1 has a lateral outlet slot 4 arranged horizontally in the lower part of the the right side wall 3 in FIG. 1. The crucible 1 is partially filled with a material in the liquid phase 5. The exit slot 4 is in communication with the surrounding atmosphere 7 the crucible 1, generally consisting of a neutral gas, such as argon. A plate 8 of crystalline material, obtained by directed crystallization of the material in the crucible 1, is drawn through the slot 4.
Le matériau cristallin est, par exemple du silicium, du germanium, de l'arséniure de gallium... Classiquement, le gradient thermique à l'intérieur du creuset 1 est vertical, la température diminuant du haut du creuset 1 vers le fond 2. Ainsi, la solidification du matériau à l'intérieur du creuset 1 entraîne la formation de joints de grains perpendiculaires à la plaque 8 de matériau en phase solide. Cette configuration est avantageuse pour une utilisation dans des dispositifs photovoltaïques.The crystalline material is, for example silicon, germanium, gallium arsenide ... Conventionally, the thermal gradient inside the crucible 1 is vertical, the temperature decreasing from the top of the crucible 1 to the bottom 2. Thus, the solidification of the material inside the crucible 1 causes the formation of grain boundaries perpendicular to the plate 8 of solid phase material. This configuration is advantageous for use in photovoltaic devices.
La cristallisation dirigée du matériau à lieu préférentiellement au niveau du fond 2 du creuset 1 et le matériau en phase solide formant la plaque 8 est retiré du bain à travers la fente de sortie 4, au fur et à mesure de sa solidification par tout moyen de préhension approprié non représenté sur la figure 1.The directed crystallization of the material preferably takes place at the bottom 2 of the crucible 1 and the solid phase material forming the plate 8 is withdrawn from the bath through the outlet slot 4, as and when it is solidified by any means of appropriate grip not shown in Figure 1.
La régulation thermique au sein du creuset 1 , est réalisée par tout moyen connu de façon à maintenir, stable et vertical, le gradient thermique au sein du creuset 1.The thermal regulation within the crucible 1 is carried out by any means known to maintain, stable and vertical, the thermal gradient in the crucible 1.
Comme illustré sur la figure 3, le creuset 1 peut être avantageusement couplé à un système de chauffage 9, situé préférentiellement au-dessus du creuset 1 , et à un système d'extraction de calories 10, situé préférentiellement sous le creuset 1 , afin de maintenir le gradient thermique sensiblement vertical. Le gradient thermique est, dans le creuset 1 , sensiblement perpendiculaire à l'interface de solidification. Le système d'extraction de calories 10 régule le flux de chaleur extrait sous le matériau en cours de solidification et la répartition du flux de chaleur selon la distance à la fente 4. Le système d'extraction de calories 10 est, par exemple, un transfert de chaleur par rayonnement à travers un fond 2, transparent, du creuset 1.As illustrated in FIG. 3, the crucible 1 may advantageously be coupled to a heating system 9, preferably situated above the crucible 1, and to a calorie extraction system 10, preferably located under the crucible 1, in order to maintain the temperature gradient substantially vertical. The thermal gradient is, in the crucible 1, substantially perpendicular to the solidification interface. The calorie extraction system 10 regulates the heat flux extracted under the material being solidified and the distribution of the heat flow according to the distance to the slot 4. The calorie extraction system 10 is, for example, a radiative heat transfer through a transparent bottom 2 of the crucible 1.
Comme illustré sur la figure 3, les parois latérales 3 du creuset 1 sont avantageusement couplées à un isolant thermique 11. Cet isolant thermique 11 est préférentiellement placé à l'extérieur du creuset 1 sur toute la surface délimitée par les parois latérales 3. De cette façon, il n'y a pas de perte de chaleur sur les parois latérales 3 et le gradient thermique est maintenu sensiblement vertical.As illustrated in FIG. 3, the side walls 3 of the crucible 1 are advantageously coupled to a thermal insulator 11. This thermal insulator 11 is preferably placed outside the crucible 1 over the entire surface delimited by the side walls 3. way, there is no heat loss on the side walls 3 and the thermal gradient is maintained substantially vertical.
L'interface de solidification du matériau, sensiblement perpendiculaire au gradient thermique, se situe dans la partie inférieure du creuset 1 , préférentiellement à proximité du fond 2 du creuset 1. Cette position est ajustée au moyen du gradient thermique au sein du creuset 1. L'épaisseur de la plaque 8 ainsi obtenue est essentiellement définie par la répartition thermique au sein du creuset 1 et par la vitesse de tirage de la plaque 8 hors du creuset 1. La vitesse de tirage de la plaque 8 est située, de préférence, dans la gamme 0,5 - 10 mètres/minute.The solidification interface of the material, substantially perpendicular to the thermal gradient, is located in the lower part of the crucible 1, preferably near the bottom 2 of the crucible 1. This position is adjusted by means of the thermal gradient in the crucible 1. The thickness of the plate 8 thus obtained is essentially defined by the thermal distribution in the crucible 1 and the drawing speed of the plate 8 out of the crucible 1. The drawing speed of the plate 8 is preferably located in the range 0.5 - 10 meters / minute.
La hauteur de la fente 4 est choisie supérieure à l'épaisseur de la plaque 8, de façon à éviter tout accrochage mécanique et toute solidification parasite lors de la sortie de la plaque 8 à travers la fente 4.The height of the slot 4 is chosen to be greater than the thickness of the plate 8, so as to avoid any mechanical catching and any parasitic solidification during the exit of the plate 8 through the slot 4.
Le dispositif comporte, de plus, au moins un inducteur 6 à l'extérieur du creuset 1 , contre la paroi latérale 3, à proximité immédiate de la fente de sortie 4. L'inducteur 6 constitue un mode de réalisation préférentiel de moyens électromagnétiques de création de forces magnétiques 6. L'inducteur 6 est parcouru par un courant alternatif ayant une fréquence comprise entre 1OkHz et 30OkHz et une intensité, de préférence, comprise entre 100A et 3000A. l'inducteur 6 créé ainsi des forces de répulsion magnétiques sur le matériau en phase liquide 5. L'inducteur 6 peut être disposé au-dessus ou au-dessous de la fente 4. Dans le mode particulier de réalisation de la figure 1 , deux inducteurs 6 sont disposés de part et d'autre de la fente 4.The device further comprises at least one inductor 6 outside the crucible 1, against the side wall 3, in the immediate vicinity of the exit slot 4. The inductor 6 constitutes a preferred embodiment of the electromagnetic means of 6. The inductor 6 is traversed by an alternating current having a frequency of between 10kHz and 30OkHz and an intensity, preferably between 100A and 3000A. the inductor 6 thus creates magnetic repulsion forces on the material in the liquid phase 5. The inductor 6 may be arranged above or below the slot 4. In the particular embodiment of FIG. 1, two inductors 6 are arranged on either side of the slot 4.
Comme illustré plus en détail sur la figure 4, l'interface entre le matériau en phase liquide 5 et l'atmosphère 7 a la forme d'un ménisque 12. Les forces de répulsion magnétiques produites par l'inducteur 6, n'ayant d'effet que sur le matériau en phase liquide 5, l'inducteur 6 permet de contrôler la position du ménisque 12. Ce dernier est préférentiellement situé à l'intérieur de la fente 4, de façon à interdire toute sortie du matériau en phase liquide 5 à travers la fente 4 sans perturber la cristallisation du matériau en phase liquide 5 à l'intérieur du creuset 1.As illustrated in more detail in FIG. 4, the interface between the liquid phase material 5 and the atmosphere 7 is in the form of a meniscus 12. The magnetic repulsion forces produced by the inductor 6, having no the effect that on the material in the liquid phase 5, the inductor 6 makes it possible to control the position of the meniscus 12. The latter is preferably situated inside the slot 4, so as to prohibit any exit of the material in the liquid phase. through the slot 4 without disturbing the crystallization of the material in the liquid phase 5 inside the crucible 1.
Les forces de répulsion magnétiques créées par l'inducteur 6 sont ajustées de sorte que la répulsion du matériau en phase liquide 5 ait lieu au niveau de la fente de sortie 4, au-dessus de la plaque 8. Des forces de répulsion agissent également entre les bords de la plaque 8 et chaque extrémité latérale. Le matériau en phase liquide 5 est ainsi maintenu à l'intérieur du creuset 1. L'amplitude du courant dans l'inducteur 6 est déterminée en fonction de la pression hydrostatique du matériau en phase liquide 5 dans le creuset 1 et de la distance entre l'inducteur 6 et le ménisque 12. La section de l'inducteur 6 est choisie de manière à concentrer au mieux les forces de répulsion sur le ménisque 12.The magnetic repulsion forces created by the inductor 6 are adjusted so that the repulsion of the liquid phase material 5 takes place at the exit slot 4, above the plate 8. Repulsion forces also act between the edges of the plate 8 and each lateral end. The material in the liquid phase 5 is thus kept inside the crucible 1. The amplitude of the current in the inductor 6 is determined as a function of the hydrostatic pressure of the liquid-phase material 5 in the crucible 1 and the distance between the inductor 6 and the meniscus 12. The section of the inductor 6 is chosen so as to best concentrate the repulsion forces on the meniscus 12.
Un exemple de réalisation du dispositif met en œuvre un inducteur 6 concentrant les courants à environ 5mm du ménisque 12. Cet inducteur permet la rétention dans le creuset d'une hauteur de silicium de 5cm, lorsqu'il est parcouru par un courant de 900A à une fréquence de 30Khz. La fente 4 présente une largeur de 75mm et une hauteur de 3mm. L'inducteur 6 provoque, de plus, un effet de brassage du matériau en phase liquide 5 près de la fente 4. Il créé des boucles de recirculation du matériau en phase liquide 5, qui entraînent les impuretés provenant de l'interface de solidification dans l'ensemble du matériau en phase liquide 5. L'accumulation des impuretés près de la phase solide est aussi réduite en comparaison à l'art antérieur dû à la présence d'un front de solidification plus étendu. L'effet de brassage est favorisé par l'utilisation d'un courant dans l'inducteur dans la gamme des basses fréquences, par exemple, de l'ordre de 50Hz. Le dispositif comporte donc, de préférence, des moyens pour superposer à la fréquence comprise entre 1 OkHz et 300Khz une fréquence favorisant le brassage dans le matériau en phase liquide 5.An exemplary embodiment of the device implements an inductor 6 concentrating the currents at about 5 mm from the meniscus 12. This inductor allows the retention in the crucible of a silicon height of 5 cm, when it is traversed by a current of 900 A to a frequency of 30Khz. The slot 4 has a width of 75mm and a height of 3mm. The inductor 6 also causes a stirring effect of the material in the liquid phase 5 close to the slot 4. It creates recirculation loops of the material in the liquid phase 5, which entrain the impurities originating from the solidification interface in the entire material in the liquid phase 5. The accumulation of impurities near the solid phase is also reduced compared to the prior art due to the presence of a broader solidification front. The stirring effect is favored by the use of a current in the inductor in the low frequency range, for example, of the order of 50 Hz. The device therefore preferably comprises means for superimposing at a frequency of between 1 kHz and 300 kHz a frequency favoring stirring in the material in the liquid phase 5.
Dans une variante de réalisation, deux inducteurs 6 sont prévus, respectivement, parcourus par des courants de fréquences différentes. Un premier inducteur est alors alimenté par un courant ayant une fréquence visant à assurer le brassage du matériau en phase liquide 5, préférentiellement dans la gamme de basses fréquences, de l'ordre de 50Hz. L'autre inducteur est parcouru par un courant ayant une fréquence comprise entre 1OkHz et 300 kHz pour assurer la répulsion du matériau en phase liquide 5. Cette action simultanée peut également être réalisée, par un seul inducteur, par exemple, par une modulation de fréquence, une surmodulation en amplitude etc.In an alternative embodiment, two inductors 6 are provided, respectively, traversed by currents of different frequencies. A first inductor is then powered by a current having a frequency to ensure the mixing of the material in the liquid phase 5, preferably in the low frequency range, of the order of 50Hz. The other inductor is traversed by a current having a frequency between 1OkHz and 300 kHz to ensure the repulsion of the material in the liquid phase 5. This simultaneous action can also be performed by a single inductor, for example, by a frequency modulation , amplitude over-modulation, etc.
A la sortie de la fente 4, la plaque 8 de matériau cristallin est constituée exclusivement de phase solide. En effet, le matériau en phase liquide 5 est repoussé à l'intérieur du creuset 1 par l'inducteur 6. La plaque 8 est alors autosupportée dès la sortie du creuset.At the exit of the slot 4, the plate 8 of crystalline material consists exclusively of solid phase. Indeed, the material in the liquid phase 5 is pushed back inside the crucible 1 by the inductor 6. The plate 8 is then self-supporting from the outlet of the crucible.
Il est, de préférence, prévu une mise en contact du matériau en phase liquide 5 avec un germe de cristallisation lors du démarrage de la solidification. Le germe de cristallisation est, de préférence, mis en contact avec le ménisque 12 afin de permettre le démarrage de la cristallisation selon des orientations prédéterminées.It is preferably provided that the material in the liquid phase 5 is brought into contact with a crystallization seed when starting the solidification. The crystallization seed is preferably brought into contact with the meniscus 12 to allow the start of crystallization according to predetermined orientations.
Des centres de nucléations / germinations, par exemple, constitués par des points froids localisés, peuvent être ajoutés au niveau de l'interface entre le fond 2 du creuset 1 et le matériau en phase liquide 5 pour faciliter le début de la cristallisation.Nucleation / germination centers, for example, consisting of localized cold spots, can be added at the interface between the bottom 2 of the crucible 1 and the liquid phase material 5 to facilitate the start of crystallization.
Dans le mode de réalisation particulier représenté à la figure 3, un dispositif de traitement 13, notamment thermique, est couplé au creuset 1 au sortir de la fente 4. Ce dispositif autorise le suivi d'un profil prédéfini de la cinétique de refroidissement de la plaque 8. Ce profil permet une réduction des contraintes mécaniques et de la densité de défauts cristallins. De plus, le dispositif 13 peut servir à préchauffer le germe de cristallisation utilisé au démarrage de la solidification. In the particular embodiment shown in FIG. 3, a treatment device 13, in particular a thermal device, is coupled to the crucible 1 at the exit of the slot 4. This device allows the monitoring of a predefined profile of the cooling kinetics of the plate 8. This profile makes it possible to reduce the mechanical stresses and the density of crystalline defects. In addition, the device 13 can be used to preheat the crystallization seed used at the start of the solidification.

Claims

Revendications claims
1. Dispositif de fabrication d'une plaque (8) de matériau cristallin par cristallisation dirigée d'un matériau en phase liquide (5) dans un creuset (1) muni d'un fond (2), de parois latérales (3) et d'au moins une fente (4) de sortie de plaque, ladite fente étant horizontale et formée dans une partie inférieure d'une paroi latérale (3), dispositif caractérisé en ce que le creuset (1) présente, sur sa surface extérieure, à proximité immédiate de la fente (4) de sortie de plaque, des moyens électromagnétiques (6) de création, au moins au niveau de la fente (4) de sortie de plaque, de forces de répulsion magnétiques sur le matériau en phase liquide (5), lesdits moyens électromagnétiques (6) étant parcouru par un courant alternatif dont la fréquence est comprise entre 1OkHz et 30OkHz.Apparatus for producing a plate (8) of crystalline material by directed crystallisation of a liquid-phase material (5) in a crucible (1) provided with a bottom (2), side walls (3) and at least one plate outlet slot (4), said slot being horizontal and formed in a lower part of a side wall (3), characterized in that the crucible (1) has on its outer surface in the immediate vicinity of the plate exit slot (4), electromagnetic means (6) for creating, at least at the plate exit slot (4), magnetic repulsion forces on the liquid-phase material ( 5), said electromagnetic means (6) being traversed by an alternating current whose frequency is between 1OkHz and 30OkHz.
2. Dispositif selon la revendication 1 , caractérisé en ce que les moyens électromagnétiques de création de forces magnétiques (6) sont situés au- dessus de la fente (4).2. Device according to claim 1, characterized in that the electromagnetic means for creating magnetic forces (6) are located above the slot (4).
3. Dispositif selon les revendications 1 ou 2, caractérisé en ce que les moyens électromagnétiques de création de forces magnétiques (6) sont situés au-dessous de la fente (4).3. Device according to claims 1 or 2, characterized in that the electromagnetic means for creating magnetic forces (6) are located below the slot (4).
4. Dispositif selon l'une quelconque des revendications 1 à 3, caractérisé en ce que les moyens électromagnétiques de création de forces magnétiques (6) comportent au moins un inducteur.4. Device according to any one of claims 1 to 3, characterized in that the electromagnetic means for creating magnetic forces (6) comprise at least one inductor.
5. Dispositif selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'il comporte des moyens de superposition d'une fréquence favorisant le brassage du matériau en phase liquide (5). 5. Device according to any one of claims 1 to 4, characterized in that it comprises means for superposition of a frequency promoting the mixing of the material in the liquid phase (5).
6. Dispositif selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la fréquence favorisant le brassage est de l'ordre de 50Hz.6. Device according to any one of claims 1 to 5, characterized in that the frequency promoting the mixing is of the order of 50Hz.
7. Dispositif selon l'une quelconque des revendications 1 à 6, caractérisé en ce que les moyens électromagnétiques de création de forces magnétiques (6) sont parcourus par un courant dont l'intensité est comprise entre 10OA et 3000A.7. Device according to any one of claims 1 to 6, characterized in that the electromagnetic means for creating magnetic forces (6) are traversed by a current whose intensity is between 10OA and 3000A.
8. Dispositif selon l'une quelconque des revendications 1 à 7, caractérisé en ce qu'il comporte des moyens de production et de maintien d'un gradient thermique dans le matériau perpendiculairement au fond (2) du creuset (1 ).8. Device according to any one of claims 1 to 7, characterized in that it comprises means for producing and maintaining a thermal gradient in the material perpendicular to the bottom (2) of the crucible (1).
9. Procédé de fabrication d'une plaque (8) de matériau cristallin par cristallisation dirigée d'un matériau en phase liquide (5) dans un creuset (1) d'un dispositif selon l'une quelconque des revendications 1 à 8, caractérisé en ce que des forces magnétiques de répulsion sont appliquées, au niveau de la fente (4), sur le matériau en phase liquide (5), pour la solidification du matériau en phase liquide (5) ayant lieu sur le fond (2) du creuset (1 ), pour empêcher la fuite du matériau en phase liquide (5). 9. A process for producing a plate (8) of crystalline material by directed crystallization of a liquid phase material (5) in a crucible (1) of a device according to any one of claims 1 to 8, characterized in that magnetic repulsive forces are applied at the slit (4) to the liquid-phase material (5) for the solidification of the liquid-phase material (5) taking place on the bottom (2) of the crucible (1) to prevent leakage of the liquid phase material (5).
EP08775638A 2007-03-08 2008-03-07 Device and method for producing self-sustained plates of silicon or other crystalline materials Withdrawn EP2132366A2 (en)

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FR0701701A FR2913434B1 (en) 2007-03-08 2007-03-08 DEVICE AND METHOD FOR MANUFACTURING SELF-SUPPORTED PLATES OF SILICON OR OTHER CRYSTALLINE MATERIALS.
PCT/FR2008/000304 WO2008132323A2 (en) 2007-03-08 2008-03-07 Device and method for producing self-sustained plates of silicon or other crystalline materials

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FR2928641B1 (en) * 2008-03-14 2010-03-26 Centre Nat Rech Scient SILICON PURIFICATION PROCESS FOR PHOTOVOLTAIC APPLICATIONS
NL2004209C2 (en) * 2010-02-08 2011-08-09 Rgs Dev B V Apparatus and method for the production of semiconductor material foils.
KR101281033B1 (en) * 2011-05-19 2013-07-09 한국에너지기술연구원 Manufacturing apparatus of silicon substrate for solar cell using continuous casting with easiness of temperature control and manufacturing method of silicon substrate using the same
KR101483693B1 (en) * 2012-04-05 2015-01-19 한국에너지기술연구원 Apparatus for Manufacturing Silicon Substrate

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US4661200A (en) * 1980-01-07 1987-04-28 Sachs Emanuel M String stabilized ribbon growth
CA1169336A (en) * 1980-01-07 1984-06-19 Emanuel M. Sachs String stabilized ribbon growth method and apparatus
US4572279A (en) * 1984-02-27 1986-02-25 Olin Corporation Electromagnetic shaping of thin ribbon conductor strip cast onto a chill wheel
JPH0620601B2 (en) * 1985-06-26 1994-03-23 住友電気工業株式会社 Continuous casting method
FR2853913B1 (en) * 2003-04-17 2006-09-29 Apollon Solar CUTTER FOR A DEVICE FOR MANUFACTURING A BLOCK OF CRYSTALLINE MATERIAL AND METHOD OF MANUFACTURE
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FR2913434A1 (en) 2008-09-12
WO2008132323A2 (en) 2008-11-06

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