WO2010105617A2 - Creuset pour fondre et cristalliser un métal, un semi-conducteur ou un alliage métallique, composant pour un corps de base d'un creuset et procédé de fabrication d'un creuset - Google Patents
Creuset pour fondre et cristalliser un métal, un semi-conducteur ou un alliage métallique, composant pour un corps de base d'un creuset et procédé de fabrication d'un creuset Download PDFInfo
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- WO2010105617A2 WO2010105617A2 PCT/DE2010/000338 DE2010000338W WO2010105617A2 WO 2010105617 A2 WO2010105617 A2 WO 2010105617A2 DE 2010000338 W DE2010000338 W DE 2010000338W WO 2010105617 A2 WO2010105617 A2 WO 2010105617A2
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- crucible
- silicon nitride
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- melting
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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Definitions
- the invention relates to technologies in the field of crucibles for melting and crystallizing a metal, a semiconductor or a metal alloy, as well as their production and use.
- Such crucibles are used, for example, to melt silicon and then crystallize. Silicon melt proves to be extremely corrosive to almost all crucible materials. Only crucibles made of graphite, silicon carbide, silicon nitride, silicon dioxide and boron nitride resist the corrosive attack for a long time. Furthermore, crystalline silicon must be present in very high purity for many applications (in particular electronic components and photovoltaics), so that the penetration of traces of impurities from the crucible into the melt must also be avoided. Therefore, in practice, for all crystallization processes of silicon, the requirement has arisen that only materials which exclusively contain Si, O, N, C and H as elements may be brought into contact with liquid silicon. For the cultivation of single crystals according to the Czochralski principle, melting crucibles made of the purest SiO 2 have therefore long prevailed.
- the wafers need not necessarily be present as single crystals.
- multicrystalline solidification in large cuboid blocks with edge lengths on the dm scale has also been established over time (see Khattak et al., "Silicon Processing for Photovoltaics II”). , Elseviewer Science Publishers 1987, pp. 153-182).
- the silicon is solidified here in corresponding, called molds, open-topped crucibles with parallelepipedic cavity by heat dissipation directed primarily over the crucible bottom from bottom to top.
- the melting of the silicon can be carried out in the crystallization crucible itself or in a separate crucible.
- pure SiO 2 is not suitable as a crucible material, since the resulting crystal adheres to the crucible wall and on cooling in usually by the forces occurring, caused by different expansion coefficients of crucible and crystal, is destroyed.
- silicon is widely used today in large molds made of SiO 2 quartz (an optically opaque, because not completely sintered quartz glass) melted and crystallized, because these crucibles apparently represent the most cost-effective variant.
- Si 3 N 4 powder they are virtually coated as a release agent in order to prevent the crystallizing silicon from adhering and to ensure that the block can be readily removed after the end of the process.
- EP 0 268 166 B1 describes a crucible material consisting of silicon nitride, silicon oxynitride and silicon dioxide which has been added by curing a silica sol, to which silicon nitride, silicon dioxide and elemental silicon have been added as further components, with subsequent nitridation at temperatures of more than 1400 ° C. Crucibles is formed.
- the object of the invention is to provide improved technologies in the field of crucibles for melting and crystallizing a metal, a semiconductor or a metal alloy, as well as their production and use, with which the applications for such crucibles are extended and improved.
- a crucible for melting and crystallizing a metal, a semiconductor material or a metal alloy, wherein a crucible wall of a crucible body is at least partially composed of a crucible material comprising silicon nitride and silicon dioxide in a weight ratio between about 1:10 and about 1: 1 (Si 3 N 4 : SiO 2 ).
- a crucible body crucible main body for melting and crystallizing a metal, a semiconductor material or a metal alloy, wherein a component portion is at least partially composed of a crucible material comprising silicon nitride and silicon dioxide in a weight ratio between about 1:10 and about 1: 1 (Si 3 N 4 : SiO 2 ).
- a further aspect of the invention relates to a method for producing a component for a crucible base body of a crucible for melting and crystallizing a metal, a crucible A semiconductor material or a metal alloy, wherein a component portion is at least partially formed of a crucible material containing silicon nitride and silicon dioxide in a weight ratio of about 1: 10 to about 1: 1 (Si 3 N 4 : SiO 2 )
- Another aspect of the invention relates to the use of such a crucible for melting and crystallizing silicon in a multicrystalline block.
- the applications of crucibles are extended, which can be used to melt and crystallize a metal, a semiconductor material or a metal alloy.
- the proposed crucible material is resistant to materials to be processed, attack the known crucible materials or even make their use impossible, and moreover can be used as material for the crucible base body of the crucible. This applies, for example, in particular in connection with silicon melts. Such melts are of particular importance in connection with photovoltaic applications, for example.
- the technologies proposed here allow the melting and crystallization of silicon into multicrystalline blocks.
- the crucible material of the crucible base body has a low thermal resistance. Contamination of the melt of silicon or other material by foreign substances are largely avoided.
- the proposed technologies can be used with extensive retention of established processes such as preparation, melting and crystallization processes.
- a preferred embodiment of the invention provides that the at least partially consisting of the crucible material crucible wall is formed at least in the crucible bottom of the crucible body.
- the at least partial use of the crucible material in the crucible bottom such a design can be provided for the crucible side walls of the crucible base body.
- the entire crucible wall of the crucible base body can be made using the crucible material.
- crucible bottom and side walls are at least partially made of different materials.
- a crucible side wall of the crucible base body consists at least partially of SiO 2 with a purity of at least 99%.
- An advantageous embodiment of the invention provides that the at least partially consisting of the crucible material crucible wall of the crucible base body is at least partially provided with an inside and / or outside coating.
- the crucible base body inside and / or outside is provided partially or completely with a wall coating, which preferably consists of a different material from the crucible material.
- the crucible wall of the crucible body is at least partially formed entirely from the crucible material.
- portions of the crucible wall are completely made of the crucible material, that is, they consist of the crucible material.
- a preferred embodiment of the invention provides that on the crucible wall of the crucible base body at least in sections has an inner lining, which is arranged on the inside.
- a lining is characterized in that, after the production of a crucible wall basic element of the crucible base body, it is arranged thereon, be it in the process of producing a base crucible or a base crucible component.
- the liner may be of the crucible material or other material.
- a development of the invention can provide that the crucible wall of the crucible base body is formed with a plurality of joined wall components.
- the joining of the wall components can be non-positively, materially and / or positively.
- the term joining techniques according to DIN 8593 summarizes those methods in which two or more bodies of the same or different material are assembled and joined together to form a new body. By joining the cohesion between the previously separate workpieces locally - ie created at the joints - and brought about a change in shape of the newly formed part.
- joining techniques in particular the material connection (compound two bodies by atomic forces due to common material), the positive engagement (mesh) and the adhesion (connection by pressing together with externally applied forces) in question.
- a preferred embodiment of the invention provides that the crucible wall of the crucible base body is formed at least in sections with a property gradient.
- a gradient of the thermal conductivity may be formed in the crucible wall, for example with a heat conductivity of the crucible material which increases from the upper edge of the crucible to the crucible bottom of the crucible base body.
- the silicon nitride and / or the silicon dioxide in the crucible material have a particle size between about 1 ⁇ m and about 500 ⁇ m.
- the principle of directional solidification may be provided to realize the bottom and side walls of the crucible body of materials of different thermal conductivity:
- the side walls would then be conventional fused silica low thermal conductivity, crucible bottom of the mixed ceramic with higher thermal conductivity.
- the production of such functional crucibles by construction of individual plates is simple, but also the one-piece production of crucibles with a bottom of higher thermal conductivity via slip casting or dry pressing is possible, as well as the realization of property gradients, for example one in the side walls from top to bottom to bottom of the crucible increasing thermal conductivity.
- a preferred embodiment of the invention provides the following steps: preparing a suspension in silicon nitride and silicon dioxide in a weight ratio between about 1:10 and about 1: 1, producing one or more green compacts by slip casting into a casting mold with subsequent drying and sintering of one or the plurality of green compacts by heating to temperatures between about 1000 ° C and 1300 ° C.
- one or more excipients are used in the preparation of the suspension.
- auxiliaries can be used: dispersing and liquefying aids such as synthetic Polyelekt- rolytes and / or carboxylic acid esters, antifoams such as hydrocarbons, fatty acid derivatives and / or Alkypolyalkylenglykolether, temporary binders such as polymer dispersion, polyvinyl alcohol, polyethylene glycol, acrylate, polysaccharides and / or waxes, suspension stabilizers such as polyammonium derivatives , Drainage aids such as polyammonium derivatives and / or polyamines, temporary pressing aids such as acrylate dispersion, wax emulsion and / or polyethylene.
- dispersing and liquefying aids such as synthetic Polyelekt- rolytes and / or carboxylic acid esters, antifoams such as hydrocarbons, fatty acid derivatives and / or Alkypolyalkylenglykolether, temporary binders such as polymer dispersion, polyvinyl
- An advantageous embodiment of the invention provides the following steps: providing the crucible material with silicon nitride and silicon dioxide in a weight ratio between about 1:10 and about 1: 1 as drying starting material, producing one or more green bodies from the drying starting material by means of compression in a mold and sintering of the one or more green compacts by heating to temperatures between about 1000 o C and l300 ° C.
- a development of the invention provides the following steps: preparing a suspension in water containing silicon nitride and silicon dioxide in a weight ratio between about 1:10 and about 1: 1, preparing spray-dried particles by spray-drying the suspension, producing one or more green compacts by means of compression of the Spray-dried particles in a mold and producing one or more green compacts by heating to temperatures between 1000 ° C and 1300 ° C.
- silicon nitride and silica are used in powder form.
- a development of the invention may provide that silicon nitride and / or silicon dioxide having a particle size of between about 1 ⁇ m and about 500 ⁇ m are used.
- a preferred embodiment of the invention provides that the Tie gel is made body in one piece.
- terms that may be relevant to one or more aspects of the invention will be further described in terms of their understanding as used herein.
- the crucible is formed with a crucible base body, which optionally can be provided with a coating, at least in partial sections, which may be located inside and / or outside.
- the coating can be carried out in one or more layers.
- a section-wise or complete lining of the crucible base body can be provided.
- Crucible base body can be built in one piece or in several parts composed of floor and side walls.
- a block is a solid, one-piece solid, which is in cylindrical or polyhedral, preferably cuboidal shape and whose dimensions in all three spatial directions have a respective ratio of not less than 1:10.
- Semiconductor materials or semiconductors are materials that contain at least one element of the 3rd, 4th and 5th group of the periodic table, as well as their connections to one another and their mixtures. These materials can be present as a solid, as a melt and as a powder or powder mixture. Ceramics are understood as meaning, in particular, nonmetallic, inorganic solids which are formed at ambient temperature from finely divided raw materials possibly with the addition of liquids such as water and then dried and sintered using elevated temperatures.
- powder refers to a solid which is present in separate or only loosely agglomerated particles of sizes of less than 1 mm.
- Granules are solids which are present in separate or only loosely agglomerated particles of sizes above 1 mm and below a few cm.
- Spray drying refers in particular to the technique customary in industrial powder treatment, a solution or suspension of a solid through special nozzles into a gas (possibly. in countercurrent) to spray and thereby dry, so that ultimately a powder or granules is formed.
- Slip casting refers to a shaping process used in ceramic processing in which a suspension of ceramic particles in a suitable liquid is poured into a mold, the walls of which are porous and largely absorb the liquid phase from the suspension, thus forming a layer of agglomerated material Solid particles stick to the mold wall. This can be taken intact from the mold as a so-called green body and further processed for their further use.
- Spray drying here means the disappearance of volatile liquid constituents (for example water) of a liquid-solid mixture by evaporation or evaporation at ambient temperature or elevated temperature below 250 ° C.
- Spray drying is a process for extracting the solids content of a suspension in granular or powder form with defined grain sizes. In this case, the suspension is injected under pressure through a nozzle into a drying gas atmosphere, where the liquid fraction evaporates while still in flight and the solid fraction precipitates as a conditioned particle.
- sintering is meant here the temperature treatment used in the production of ceramic bodies for their solidification, wherein macroscopically no liquid phase occurs.
- Microscopically in the sintering process, touching, formerly separate particles grow together by rearrangement of atoms to form a coherent, usually initially porous, more solid mass with increasing sintering time.
- a body with a graded property is one such body in which the corresponding property changes in volume. This can happen continuously-steadily, but also unsteadily-leaps and bounds. The same fact is also described by the term property gradient. In this case, the material composition of the material can be graded.
- the so-called slip adjusted to a liter weight of 1900 ⁇ 20 g / l and a solids content of 60-75%, at room temperature and normal atmospheric conditions, in a plaster mold with a square base area of 120 * 120 mm 2 , an inner height of the cavity of 60 mm and a wall thickness of 12 mm. cast according to the Vollguss270.
- the mold was filled with uniform, not too fast flow without interruption. Due to the capillary-active plaster mold, the body formation takes place as a diffusion process of the water. After a life of 40 min. has formed a broken piece of 10 mm thickness and the residual slip can be removed.
- the plaster mold absorbs water from the slurry mass so that drying of the cast body takes place in the plaster mold. After 2 hours, dry the cast body at room temperature the fragments are detached from the plaster mold wall and can be removed from the core by means of light sliding.
- the cast body was dried in a drying chamber at a temperature of 70 0 C to 0% residual moisture and then fired at temperatures between 1100-1300 ° C in an oxidic atmosphere and sintered.
- the result was dimensionally stable, crack-free crucible bodies made from a Si 3 N 4 -SiO 2 mixed ceramic, which can be used in the usual silicon block crystallization process.
- Embodiment 2 is a diagrammatic representation of Embodiment 1:
- the suspension prepared according to Example 1 was, with the same formulation, solids content and weight per liter, but with other organic additions and polyethylene glycol as a binder, polyvinyl alcohol as a temporary binder and a non-ionic wax dispersion as a binding, pressing and sliding aid through a 1 mm nozzle and sprayed under a pressure of 30 bar in a chamber with a circulating air temperature of 400 ° C and thereby spray-dried.
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Silicon Compounds (AREA)
- Ceramic Products (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
L'invention concerne un creuset pour fondre et cristalliser un métal, un matériau semi-conducteur ou un alliage métallique, une paroi d'un corps de base de creuset étant au moins partiellement composée d'un matériau de creuset contenant du nitrure de silicium et du dioxyde de silicium dans un rapport massique de 1:10 à 1:1 environ (Si3N4 : SiO2). L'invention concerne également un composant pour un corps de base d'un creuset pour fondre et cristalliser un métal, un matériau semi-conducteur ou un alliage métallique, une partie du composant étant au moins partiellement composée d'un matériau de creuset contenant du nitrure de silicium et du dioxyde de silicium dans un rapport massique de 1:10 à 1:1 environ (Si3N4 : SiO2), et un procédé de fabrication d'un composant pour un corps de base d'un creuset pour fondre et cristalliser un métal, un matériau semi-conducteur ou un alliage métallique, une partie du composant étant au moins partiellement composée d'un matériau de creuset contenant du nitrure de silicium et du dioxyde de silicium dans un rapport massique de 1:10 à 1:1 environ (Si3N4 : SiO2).
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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DE102009013706.8 | 2009-03-20 | ||
DE102009013706 | 2009-03-20 | ||
DE102009048741A DE102009048741A1 (de) | 2009-03-20 | 2009-10-08 | Tiegel zum Schmelzen und Kristallisieren eines Metalls, eines Halbleiters oder einer Metalllegierung, Bauteil für einen Tiegelgrundkörper eines Tiegels und Verfahren zum Herstellen eines Bauteils |
DE102009048741.7 | 2009-10-08 |
Publications (4)
Publication Number | Publication Date |
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WO2010105617A2 true WO2010105617A2 (fr) | 2010-09-23 |
WO2010105617A8 WO2010105617A8 (fr) | 2010-11-25 |
WO2010105617A3 WO2010105617A3 (fr) | 2011-01-13 |
WO2010105617A4 WO2010105617A4 (fr) | 2011-03-10 |
Family
ID=42664191
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/DE2010/000338 WO2010105617A2 (fr) | 2009-03-20 | 2010-03-19 | Creuset pour fondre et cristalliser un métal, un semi-conducteur ou un alliage métallique, composant pour un corps de base d'un creuset et procédé de fabrication d'un creuset |
Country Status (2)
Country | Link |
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DE (1) | DE102009048741A1 (fr) |
WO (1) | WO2010105617A2 (fr) |
Cited By (6)
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CN103360077A (zh) * | 2012-04-01 | 2013-10-23 | 浙江昱辉阳光能源有限公司 | 一种氮化硅坩埚及其制备方法 |
FR3003272A1 (fr) * | 2013-03-14 | 2014-09-19 | Saint Gobain Ct Recherches | Creuset |
EP2799597A4 (fr) * | 2011-12-30 | 2015-08-19 | Sumco Corp | Creuset en verre de silice |
WO2015132399A1 (fr) * | 2014-03-06 | 2015-09-11 | Ald Vacuum Technologies Gmbh | Creuset hybride pour la cristallisation des matériaux |
CN107236987A (zh) * | 2017-07-12 | 2017-10-10 | 晶科能源有限公司 | 一种坩埚制备方法和多晶铸锭炉 |
DE102018006329B3 (de) | 2018-08-09 | 2019-03-21 | Faruk Savasci | Verfahren zur Herstellung von Schmelztiegeln durch Schichtenbildung mit thermischer Zerstörung der Tiegelpositive |
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Publication number | Priority date | Publication date | Assignee | Title |
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DE102012101214B4 (de) * | 2012-02-15 | 2016-09-01 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Wiederverwendbarer Tiegel aus einer Siliziumnitrid-Keramik, Verfahren zu dessen Herstellung, dessen Verwendung sowie Verfahren zur Herstellung eines mono- oder multikristallinen Halbmetall-Ingots oder Halbmetall-Körpers aus einer Schmelze |
DE102013109024B4 (de) | 2013-08-21 | 2019-12-05 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Wiederverwendbarer Tiegel aus einer Siliziumnitrid-Keramik, Verfahren zu dessen Herstellung, Verwendung des Tiegels, sowie Verfahren zur Herstellung eines mono- oder multikristallinen Silizium-Ingots und eines Silizium-Einkristalls aus einer Schmelze |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2799597A4 (fr) * | 2011-12-30 | 2015-08-19 | Sumco Corp | Creuset en verre de silice |
CN103360077A (zh) * | 2012-04-01 | 2013-10-23 | 浙江昱辉阳光能源有限公司 | 一种氮化硅坩埚及其制备方法 |
FR3003272A1 (fr) * | 2013-03-14 | 2014-09-19 | Saint Gobain Ct Recherches | Creuset |
WO2015132399A1 (fr) * | 2014-03-06 | 2015-09-11 | Ald Vacuum Technologies Gmbh | Creuset hybride pour la cristallisation des matériaux |
US10100427B2 (en) | 2014-03-06 | 2018-10-16 | Ald Vacuum Technologies Gmbh | Hybrid crucible for crystallizing materials |
TWI668339B (zh) * | 2014-03-06 | 2019-08-11 | 德商Ald真空工業股份有限公司 | 用於材料之結晶的混成坩鍋 |
CN107236987A (zh) * | 2017-07-12 | 2017-10-10 | 晶科能源有限公司 | 一种坩埚制备方法和多晶铸锭炉 |
DE102018006329B3 (de) | 2018-08-09 | 2019-03-21 | Faruk Savasci | Verfahren zur Herstellung von Schmelztiegeln durch Schichtenbildung mit thermischer Zerstörung der Tiegelpositive |
Also Published As
Publication number | Publication date |
---|---|
WO2010105617A3 (fr) | 2011-01-13 |
DE102009048741A1 (de) | 2010-09-30 |
WO2010105617A8 (fr) | 2010-11-25 |
WO2010105617A4 (fr) | 2011-03-10 |
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