WO2010026344A2 - Materiau a architecture multicouche, dedie a une mise en contact avec du silicium liquide - Google Patents
Materiau a architecture multicouche, dedie a une mise en contact avec du silicium liquide Download PDFInfo
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- WO2010026344A2 WO2010026344A2 PCT/FR2009/051668 FR2009051668W WO2010026344A2 WO 2010026344 A2 WO2010026344 A2 WO 2010026344A2 FR 2009051668 W FR2009051668 W FR 2009051668W WO 2010026344 A2 WO2010026344 A2 WO 2010026344A2
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Definitions
- the present invention aims at proposing new materials that can be used in silicon melting and solidification processes and in particular dedicated to photovoltaic applications. It also relates to a process for preparing these materials.
- Photovoltaic cells are essentially made from mono- or poly-crystalline silicon, obtained from the solidification of liquid silicon in crucibles. It is the platelets cut in the ingot formed in the crucible which serve as a basis for the manufacture of the cells.
- the growth of the ingot is generally carried out in silica crucibles, coated with a layer of silicon nitride to prevent adhesion of the ingot to the crucible after solidification.
- silica crucible is not reusable.
- Such crucibles are used in particular for the melting of silicon in metallurgical silicon purification processes.
- a layer of silicon carbide is formed by reaction at the interface.
- the reaction continues until a sealed barrier layer is interposed between the carbonaceous material and the liquid silicon.
- the silicon infiltrates into the carbon matrix, to a depth that depends mainly on the porosity of this matrix. For example, on extruded graphite type materials, centimeter depths are often reached, whereas they are of the order of one millimeter for fine-grained graphites.
- the vitreous carbon no noticeable infiltration is observed, only the barrier layer is formed by reaction at the interface
- Silicidation of graphite in the gas phase is also possible.
- the company Toyotanso sells under the trademark PERJVIA KOTE ® a graphite coated with SiC by the CVD technique (3).
- the thicknesses of SiC can be relatively large, of the order of 100 microns, but the layer is never perfectly dense and may cause sealing problems.
- the infiltration of silicon into the porosities and the contact with unreacted graphite can destroy the carbide layer due to the change in volume associated with the siliciding reaction.
- the protection provided by the SiC barrier layer is not sustainable. Two mechanisms contribute to the consumption of this layer.
- the system tends to evolve towards an equilibrium state where the liquid saturates with carbon by dissolving the SiC layer.
- the oxidation of SiC will also have the effect of reducing the thickness of the layer.
- the purpose of the present invention is precisely to propose a novel silicon carbide / graphite composite structure which makes it possible to significantly increase the service life of materials intended to be heated to very high temperatures, particularly in the case of crucibles intended to receive silicon in the form of fusion.
- the present invention also aims to propose a new type of crucibles suitable for reuse.
- the present invention aims in particular to provide a new type of crucibles particularly advantageous in terms of non-adhesion with respect to silicon.
- the present invention further aims to provide a preparation method useful for the preparation of such parts. More precisely, the present invention relates, according to one of its aspects, to a piece of material, in particular dedicated to contact with liquid silicon, having a multilayer architecture formed of at least one so-called “support” layer based on carbon, a so-called “surface” silicon carbide layer, and a so-called “intermediate” layer interposed between said support and surface layers characterized in that said intermediate layer is formed of a matrix of silicon carbide containing at least one carbon nodule.
- the surface and intermediate layers have less than 5%, especially less than 1% by volume of solid silicon, and in particular are totally devoid of solid silicon.
- the intermediate layer it is characterized by a homogeneity in terms of composition throughout its thickness.
- the matrix of silicon carbide forming the intermediate layer comprises at least 30% by volume of nodule (s) of carbon, in particular at least 40% by volume advantageously uniformly distributed in the thickness of the intermediate layer.
- this intermediate layer has a SiC volume fraction at least 1.8 times higher than the volume fraction of the graphite porosity of the so-called carbon-based support layer, representative of the composition of the surface of the surface. origin of the material before treatment according to the invention.
- the piece of material according to the invention has a surface layer of silicon carbide having a thickness of at least 5 microns, in particular ranging from 15 microns to 20 microns.
- the piece of material according to the invention has an intermediate layer having a thickness of at least 300 ⁇ m, in particular greater than 400 ⁇ m and in particular ranging from 500 to 2000 ⁇ m.
- the piece of material is a crucible or a mold, intended in particular to be brought into contact with a material brought to a very high temperature such as for example liquid silicon.
- crucibles according to the invention are more suitable than their counterparts in graphite for several reasons.
- the holding of the release layer S1 3 N 4 is better on SiC substrate than on graphite substrate, because it is possible to anneal the nitride release deposit at higher temperature.
- the pieces of material according to the invention are thus compatible with a use at a temperature of up to 1600 ° C.
- the present invention aims at providing a method for preparing a piece of material having a multilayer architecture composed of at least one so-called “support” layer based on carbon, a so-called layer “ of silicon carbide and a so-called “intermediate” layer interposed between the two previous layers and formed of at least one silicon carbide matrix containing at least one carbon nodule, said method comprising at least the steps of at :
- the temperature of step (3) can be advantageously adjusted between the melting point of silicon, namely from about 1410 ° C. to about 1500 ° C., advantageously about 1410 ° C. 0 C to about 1450 0 C.
- Figures la and Ib are schematic cross-sectional representations of a crucible before and after treatment according to a method according to the invention.
- FIG. 2 is a schematic cross-sectional representation of a detail of the interior portion of a crucible according to the invention and on which the SiC surface layer and the structure of the composite zone forming the intermediate layer are shown.
- FIG. 3 is a photograph (optical microscope, magnification * 10 3 ) of the intermediate composite structure obtained during step 3 of the process according to the invention, after 2 minutes of infiltration at 1460 ° C. of liquid silicon on a graphite Carbone Lorraine 2020.
- the graphite matrix is in dark gray, the silicon carbide in light gray and the unreacted silicon appears in white in the pores.
- FIG. 4 is a scanning electron microscope photograph of the material obtained from a POCO AX2-5Q graphite material at the end of step 4 of a method according to the invention.
- the graphite nodules appear in dark gray, the SiC matrix in light gray. There is no more unreacted silicon visible in the pores.
- the piece of material according to the invention has at least one carbonaceous support layer, a so-called surface layer formed essentially of silicon carbide and a layer said intermediate, interposed between the two previous layers and formed of a composite zone having an SiC structure containing at least one and preferably several graphite nodules.
- the volume fraction of the SiC structure can vary from 45 to 70%.
- the volume fraction of the SiC in the composite zone is equal to the volume fraction of the graphite porosity forming the original piece of material, that is to say before treatment according to the invention, multiplied by at least 1.2, preferably at least 1.5 and more preferably 1.8.
- the thickness of the layer "surface” and the “intermediate” layer combined is advantageously greater than 300 microns, and preferably from 500 to 2000 microns.
- the support layer it is preferably carbonaceous.
- a layer based on a carbonaceous material is represented by a material formed, essentially, of carbon atoms. More specifically, a carbon material is, for the purposes of the invention, a material whose carbon atoms content is greater than 95%, in particular greater than 99% by weight relative to its total weight.
- This carbonaceous material has an open porosity.
- its open pore volume varies from 25% to 40%, preferably from 30% to 35%.
- This porosity can be characterized by the mercury porosimetry method.
- its structure is moreover constituted by graphite grains of micrometric dimensions varying from 1 to 10 ⁇ m, advantageously from 1 to 5 ⁇ m and preferably spaced a few microns apart, in particular from 1 to 10 ⁇ m, advantageously from 1 to 5 ⁇ m. .mu.m.
- the piece of material to be treated according to the invention has on the surface a carbonaceous layer having a grain size compatible with siliciding over a millimeter depth and with a reaction rate sufficient for the structure final is composed of graphite nodules dispersed in a matrix of silicon carbide. Its carbonaceous structure has an open porosity as defined above.
- step (2) of the process according to the invention is brought into contact with liquid silicon, for example by immersion in a molten silicon bath.
- Its thickness is in particular greater than 1 mm.
- a volume balance taking into account the change in volume associated with the Si + C -> SiC reaction shows that the SiC volume fraction in the composite is equal to the fraction volume of initial porosity of graphite multiplied by 1.8.
- the method according to the invention therefore comprises at least the steps consisting in disposing a piece of material, comprising at least on the surface a carbonaceous layer, to put said piece in contact with liquid silicon, and to bring it to a first temperature level conducive to the infiltration of molten silicon into the graphite until the clogging of the pores.
- This temperature is at least equal to the melting temperature of the silicon.
- this step can be carried out at temperatures varying between the melting point of the silicon, namely from about 1410 ° C. to about 1500 ° C., advantageously from about 1410 ° C. to about 1450 ° C.
- the duration of this first stage can vary between 10 minutes and one hour, advantageously between 20 minutes and 40 minutes.
- this third step the piece of material whose external surface is formed to a certain depth, greater than 300 ⁇ m, of a graphite matrix containing SiC nodules and silicon is subjected to a second level of temperature.
- the temperature of this second bearing makes it possible to homogenize the microstructure of the outer layer and in particular to complete the consumption of the infiltrated silicon.
- This step can be performed at temperatures ranging between 1500 0 C and 1700 0 C, preferably between 1500 0 C and 1600 0 C.
- the duration of this second stage may vary between one hour and eight hours, preferably between three hours and six hours. In all cases, this time is sufficient to allow the further processing of graphite into a silicon carbide structure incorporating graphite nodules and the substantially total elimination of residual silicon.
- the third and fourth stages of the process can be carried out at variable pressure, generally at atmospheric pressure or lower pressure.
- a vacuum embodiment advantageously allows by gas phase pre-siliciding in the graphite grains, better penetration of liquid silicon during the second step.
- the infiltration can then be carried out at a thickness of 15% to 20% greater than the thickness obtained at atmospheric pressure.
- the shade tested is a plate of POCO AXZ-5Q graphite material (length 10 cm, width 10 cm, thickness 1 cm), 32% volume porosity and grain size of the order of 1 ⁇ m.
- the material is heated under an atmosphere of neutral gas (Argon) in an induction furnace.
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
Claims
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
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JP2011525599A JP5497041B2 (ja) | 2008-09-05 | 2009-09-03 | 多層構造を持ちかつ液状シリコンと接触させるための材料 |
CN2009801349498A CN102186795B (zh) | 2008-09-05 | 2009-09-03 | 具有多层结构并用于与液态硅接触的材料 |
RU2011107881/03A RU2494999C2 (ru) | 2008-09-05 | 2009-09-03 | Материал, обладающий многослойной структурой и предназначенный для контакта с жидким кремнием |
ES09741365.2T ES2619321T3 (es) | 2008-09-05 | 2009-09-03 | Material de arquitectura multicapa, dedicado a ser puesto en contacto con silicio líquido |
EP09741365.2A EP2326607B1 (fr) | 2008-09-05 | 2009-09-03 | Materiau a architecture multicouche, dedie a une mise en contact avec du silicium liquide |
BRPI0918153A BRPI0918153B1 (pt) | 2008-09-05 | 2009-09-03 | peça de material e processo útil para a preparação de uma peça de material |
US13/062,472 US9145339B2 (en) | 2008-09-05 | 2009-09-03 | Material having a multilayer architecture and intended for being contacted with liquid silicon |
KR1020117007594A KR101426015B1 (ko) | 2008-09-05 | 2009-09-03 | 다층 아키텍쳐를 구비하고 액체 실리콘과 접촉하기 위한 물질 |
Applications Claiming Priority (2)
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FR0855972A FR2935636B1 (fr) | 2008-09-05 | 2008-09-05 | Materiau a architecture multicouche, dedie a une mise en contact avec du silicium liquide |
FR0855972 | 2008-09-05 |
Publications (2)
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WO2010026344A2 true WO2010026344A2 (fr) | 2010-03-11 |
WO2010026344A3 WO2010026344A3 (fr) | 2010-12-02 |
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PCT/FR2009/051668 WO2010026344A2 (fr) | 2008-09-05 | 2009-09-03 | Materiau a architecture multicouche, dedie a une mise en contact avec du silicium liquide |
Country Status (10)
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US (1) | US9145339B2 (fr) |
EP (1) | EP2326607B1 (fr) |
JP (1) | JP5497041B2 (fr) |
KR (1) | KR101426015B1 (fr) |
CN (1) | CN102186795B (fr) |
BR (1) | BRPI0918153B1 (fr) |
ES (1) | ES2619321T3 (fr) |
FR (1) | FR2935636B1 (fr) |
RU (1) | RU2494999C2 (fr) |
WO (1) | WO2010026344A2 (fr) |
Cited By (4)
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CN102219518A (zh) * | 2011-03-31 | 2011-10-19 | 浙江立泰复合材料有限公司 | 碳化硼碳化硅复相陶瓷及其制备方法 |
WO2016087549A1 (fr) | 2014-12-02 | 2016-06-09 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Creuset réutilisable pour la fabrication de matériau cristallin |
EP3330240A1 (fr) * | 2016-12-01 | 2018-06-06 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Procede pour la siliciuration surfacique de graphite |
FR3074908A1 (fr) * | 2017-12-13 | 2019-06-14 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Sonde acoustique destinee a etre utilisee dans un four de solidification du silicium et son procede de fabrication |
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US9352389B2 (en) | 2011-09-16 | 2016-05-31 | Silicor Materials, Inc. | Directional solidification system and method |
TWI643983B (zh) * | 2013-03-14 | 2018-12-11 | 美商希利柯爾材料股份有限公司 | 定向凝固系統及方法 |
CN107207373A (zh) * | 2015-01-29 | 2017-09-26 | 揖斐电株式会社 | SiC被覆碳复合材料 |
KR101712387B1 (ko) * | 2015-04-08 | 2017-03-07 | (주)제너코트 | 흑연 기판의 표면 특성 개질 방법 |
CN105523778A (zh) * | 2016-01-22 | 2016-04-27 | 青岛华杰硅碳科技有限公司 | 一种硅化石墨及其制备方法 |
EP3514128A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
EP3514129A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
EP3514130A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
EP3514257A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
EP3514127A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
EP3514259A1 (fr) | 2018-01-18 | 2019-07-24 | Heraeus GMSI LLC | Procédé de fabrication d'un corps revêtu de carbure de silicium |
GB2582379B (en) * | 2019-03-22 | 2021-12-08 | Tenmat Ltd | Method of coating carbon components |
US20210363069A1 (en) * | 2020-05-21 | 2021-11-25 | Raytheon Technologies Corporation | Method to produce dense ceramic matrix composites |
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2008
- 2008-09-05 FR FR0855972A patent/FR2935636B1/fr not_active Expired - Fee Related
-
2009
- 2009-09-03 US US13/062,472 patent/US9145339B2/en not_active Expired - Fee Related
- 2009-09-03 ES ES09741365.2T patent/ES2619321T3/es active Active
- 2009-09-03 CN CN2009801349498A patent/CN102186795B/zh not_active Expired - Fee Related
- 2009-09-03 JP JP2011525599A patent/JP5497041B2/ja not_active Expired - Fee Related
- 2009-09-03 WO PCT/FR2009/051668 patent/WO2010026344A2/fr active Application Filing
- 2009-09-03 RU RU2011107881/03A patent/RU2494999C2/ru active
- 2009-09-03 KR KR1020117007594A patent/KR101426015B1/ko active IP Right Grant
- 2009-09-03 BR BRPI0918153A patent/BRPI0918153B1/pt not_active IP Right Cessation
- 2009-09-03 EP EP09741365.2A patent/EP2326607B1/fr active Active
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WO2016087549A1 (fr) | 2014-12-02 | 2016-06-09 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Creuset réutilisable pour la fabrication de matériau cristallin |
EP3330240A1 (fr) * | 2016-12-01 | 2018-06-06 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Procede pour la siliciuration surfacique de graphite |
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Also Published As
Publication number | Publication date |
---|---|
BRPI0918153B1 (pt) | 2020-02-04 |
EP2326607A2 (fr) | 2011-06-01 |
BRPI0918153A8 (pt) | 2019-04-30 |
BRPI0918153A2 (pt) | 2015-12-01 |
CN102186795A (zh) | 2011-09-14 |
ES2619321T3 (es) | 2017-06-26 |
FR2935636B1 (fr) | 2011-06-24 |
JP2012501945A (ja) | 2012-01-26 |
JP5497041B2 (ja) | 2014-05-21 |
WO2010026344A3 (fr) | 2010-12-02 |
KR101426015B1 (ko) | 2014-08-06 |
US20120040139A1 (en) | 2012-02-16 |
US9145339B2 (en) | 2015-09-29 |
KR20110083614A (ko) | 2011-07-20 |
RU2011107881A (ru) | 2012-10-10 |
CN102186795B (zh) | 2013-09-18 |
FR2935636A1 (fr) | 2010-03-12 |
RU2494999C2 (ru) | 2013-10-10 |
EP2326607B1 (fr) | 2016-12-21 |
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