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CN108609864B - Film-coated heat-insulation reflective quartz heat shield and preparation method thereof - Google Patents

Film-coated heat-insulation reflective quartz heat shield and preparation method thereof Download PDF

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Publication number
CN108609864B
CN108609864B CN201611139837.XA CN201611139837A CN108609864B CN 108609864 B CN108609864 B CN 108609864B CN 201611139837 A CN201611139837 A CN 201611139837A CN 108609864 B CN108609864 B CN 108609864B
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Prior art keywords
quartz
film layer
heat shield
heat
lining
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CN201611139837.XA
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CN108609864A (en
Inventor
贾祯
梁永生
冉瑞应
栗宁
张立平
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Yinchuan Longi Silicon Materials Co ltd
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Yinchuan Longi Silicon Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3605Coatings of the type glass/metal/inorganic compound
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3642Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating containing a metal layer
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3644Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3686Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating being used for ovens
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method

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  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Laminated Bodies (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a film-coated heat-insulation reflective quartz heat shield which comprises a quartz substrate and a silver film layer plated on the inner surface of the quartz substrate, wherein the silver film layer is completely attached with a quartz lining. The invention also discloses a preparation method of the film-coated heat-insulation reflective quartz heat shield, which comprises the following steps: preparing a quartz substrate; carrying out silver plating treatment on the inner surface of the quartz substrate; and (3) paving the fused quartz on the silver film layer for cooling to obtain the quartz heat shield. According to the preparation method of the film-coated heat-insulation reflective quartz heat shield, high-purity quartz is melted at high temperature to prepare the quartz substrate, then the inner surface of the quartz substrate is subjected to silver plating, and the quartz in a melting state is laid on the silver film layer to be cooled to obtain the quartz heat shield.

Description

Film-coated heat-insulation reflective quartz heat shield and preparation method thereof
Technical Field
The invention belongs to the technical field of single crystal manufacturing equipment, and particularly relates to a coated heat-insulating reflective quartz heat shield and a preparation method thereof.
Background
In the process of producing silicon single crystal by the Czochralski method, the brief process is that raw materials are firstly loaded into a quartz crucible in a single crystal furnace, protective gas is introduced after the furnace body is sealed, a material block is heated to about 1400 ℃ by a heater to be melted, the crystal pulling process is completed by the operations of seeding, shouldering, shoulder rotating, diameter equalizing, ending and the like, and finally the heater is closed and the furnace is shut down. Because the equal-diameter growth accounts for about 40 percent of the whole time in the whole single crystal preparation process, the improvement of the equal-diameter growth speed is particularly important for improving the single crystal production capacity of the Czochralski method and reducing the preparation cost of the Czochralski single crystal.
The growth speed of the equal diameter is closely related to the temperature gradient of a thermal field of the single crystal by the Czochralski method, the larger the temperature gradient of the thermal field is, the faster the growth speed of the equal diameter theoretically is, the smaller the temperature gradient of the thermal field is, the slower the growth speed of the equal diameter theoretically is, whether heat above a crystal boundary surface of the single crystal by the Czochralski method can be taken away in time or not can directly influence the growth speed of the equal diameter of the single crystal, if the heat can not be taken away in time, the growth speed of the equal diameter can be reduced, otherwise, the growth speed of the equal diameter is increased.
Disclosure of Invention
The invention aims to provide a film-coated heat-insulation reflective quartz heat shield which can effectively increase the temperature gradient and improve the growth speed of single crystals.
The invention also aims to provide a preparation method of the coated heat-insulation reflective quartz heat shield.
The invention adopts a technical scheme that: a film-coated heat-insulation reflective quartz heat shield comprises a quartz substrate and a silver film layer plated on the inner surface of the quartz substrate, wherein a quartz lining is completely attached to the silver film layer, and the shapes of the quartz substrate and the quartz lining are adapted to the shape of a graphite heat shield inner container in a single crystal furnace.
The present invention is also characterized in that,
the thickness of the quartz substrate and the quartz lining is 3mm-5 mm.
The thickness of the silver film layer is 0.03mm-0.06 mm.
The other technical scheme adopted by the invention is as follows: the preparation method of the coated heat-insulation reflective quartz heat shield comprises the following steps:
firstly, melting quartz sand at high temperature to prepare a transparent quartz substrate;
secondly, forming a silver film layer on the inner surface of the quartz substrate after silver plating the inner surface of the quartz substrate;
thirdly, melting the quartz sand at high temperature to a molten state, laying the quartz sand on the silver film layer, and cooling to form the quartz lining.
The present invention is also characterized in that,
in the third step, when bubbles appear between the quartz lining and the silver film layer during the cooling process of the quartz lining, the quartz lining is vacuumized to remove the bubbles.
The invention has the beneficial effects that: the invention relates to a preparation method of a film-coated heat-insulation reflective quartz heat shield, which comprises the steps of melting high-purity quartz at high temperature, respectively preparing quartz substrates, then carrying out silver plating treatment on the inner surfaces of the quartz substrates, laying the quartz in a molten state on a silver film layer, and cooling to obtain the film-coated heat-insulation reflective quartz heat shield.
Drawings
FIG. 1 is a schematic structural diagram of a coated heat-insulating reflective quartz heat shield according to the present invention.
In the figure, 1 is a quartz substrate, 2 is a quartz lining, and 3 is a silver film layer.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The structure of the film-coated heat-insulation reflective quartz heat shield is shown in figure 1, and comprises a quartz substrate 1 and a silver film layer 3 plated on the inner surface of the quartz substrate 1, wherein the silver film layer 3 is completely attached with a quartz lining 2, and the shapes of the quartz substrate 1 and the quartz lining 2 are adapted to the shape of a graphite heat shield inner container in a single crystal furnace.
Illustratively, the quartz substrate 1 and the quartz lining 2 have a thickness of 3mm to 5 mm. The thickness of the silver film layer 3 is 0.03mm-0.06 mm.
The invention also provides a preparation method of the film-coated heat-insulation reflective quartz heat shield, which comprises the following steps:
firstly, melting quartz sand at high temperature to prepare a transparent quartz substrate 1;
secondly, forming a silver film layer 3 on the inner surface of the quartz substrate 1 after silver plating the inner surface of the quartz substrate 1;
thirdly, melting the quartz sand at high temperature to a molten state, laying the quartz sand on the silver film layer 3, and cooling to form the quartz lining 2.
Preferably, in the third step, bubbles may occur between the quartz lining 2 and the silver film layer 3 in the cooling process of the quartz lining 2, and at this time, the space between the quartz lining 2 and the silver film layer 3 is vacuumized to remove the bubbles, so as to avoid the occurrence of cracking of the quartz lining 2 due to thermal expansion caused by the existence of the bubbles in the high temperature state during use.
When the coated heat-insulating reflective quartz heat shield is used, the coated heat-insulating reflective quartz heat shield is arranged at the lower part of a conventional graphite heat shield inner container in a single crystal furnace, the coated heat-insulating reflective quartz heat shield is provided with a silver film layer 3 inside and is of a double-sided reflective structure, the surfaces of a quartz substrate 1 and the silver film layer 3 on the same side of the quartz substrate mainly play a role in heat insulation and are used for isolating the temperature of a heater and a silicon melt interface, the surfaces of a quartz lining 2 and the silver film layer 3 on the same side of the quartz lining mainly play a role in reflecting heat released by a silicon rod, so that the heat is isolated and reflected to the top of the single crystal furnace and the silicon rod, the temperature gradient is effectively increased, and the crystal growth speed can be increased by 5mm/h through measurement; because the silver film layer 3 is wrapped by the quartz material, the raw material and the graphite heat shield cannot be polluted due to the diffusion of silver metal elements caused by high temperature.

Claims (3)

1. The film-coated heat-insulation reflective quartz heat shield is characterized by comprising a quartz substrate (1) and a silver film layer (3) plated on the inner surface of the quartz substrate (1), wherein the silver film layer (3) is completely attached with a quartz lining (2), and the shapes of the quartz substrate (1) and the quartz lining (2) are adapted to the shape of a graphite heat shield inner container in a single crystal furnace;
the preparation method of the coated heat-insulation reflective quartz heat shield comprises the following steps:
firstly, melting quartz sand at high temperature to prepare a transparent quartz substrate (1);
secondly, forming a silver film layer (3) on the inner surface of the quartz substrate (1) after silver plating treatment is carried out on the inner surface of the quartz substrate (1);
thirdly, melting the quartz sand at high temperature to a molten state, laying the quartz sand on the silver film layer (3), and cooling to form a quartz lining (2); when bubbles appear between the quartz lining (2) and the silver film layer (3) in the cooling process of the quartz lining (2), the quartz lining is vacuumized to remove the bubbles.
2. The coated heat-insulating reflective quartz heat shield according to claim 1, wherein the thickness of the quartz substrate (1) and the quartz lining (2) is 3mm to 5 mm.
3. The coated heat-insulating reflective quartz heat shield according to claim 1, wherein the thickness of the silver film layer (3) is 0.03mm to 0.06 mm.
CN201611139837.XA 2016-12-12 2016-12-12 Film-coated heat-insulation reflective quartz heat shield and preparation method thereof Active CN108609864B (en)

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CN108609864B true CN108609864B (en) 2022-01-14

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CN111022168B (en) * 2019-12-27 2020-12-25 东风汽车集团有限公司 Oxygen sensor heat insulation protection device

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JP2004224642A (en) * 2003-01-23 2004-08-12 Siltronic Japan Corp Single crystal manufacturing apparatus
CN101838841A (en) * 2010-02-23 2010-09-22 上海汉虹精密机械有限公司 Single crystal furnace device
CN102352530A (en) * 2011-11-09 2012-02-15 内蒙古中环光伏材料有限公司 Heat shield device for CZ-Si single crystal furnace
CN202766655U (en) * 2012-07-11 2013-03-06 银川隆基硅材料有限公司 Heat shield for Czochralski silicon single crystal furnace
CN103342362A (en) * 2013-07-12 2013-10-09 新特能源股份有限公司 Heat shield of polysilicon CVD (chemical vapor deposition) reactor
CN103882510A (en) * 2012-12-24 2014-06-25 九州方园新能源股份有限公司 Diversion cylinder for increasing single crystal silicon growth rate

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JPH0967187A (en) * 1995-08-25 1997-03-11 Mitsubishi Materials Corp Apparatus for producing single crystal
KR20090046301A (en) * 2007-11-05 2009-05-11 삼성전기주식회사 Manufacturing method of single crystal substrate and manufacturing method of solar cell using it
CN101565278A (en) * 2009-05-08 2009-10-28 浙江大学 Double-sided sputtering silvered device of barrel-type quartz crystal
CN202401161U (en) * 2011-12-31 2012-08-29 宁波科论太阳能有限公司 Continuous direct-pull single crystal furnace
CN203007477U (en) * 2012-12-13 2013-06-19 无锡鼎晶光电科技有限公司 Structure of single-crystal furnace thermal field for growth of sapphire crystal
CN104726931A (en) * 2015-03-30 2015-06-24 江苏盎华光伏工程技术研究中心有限公司 Single crystal furnace with annealing device and control method for single crystal furnace

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004224642A (en) * 2003-01-23 2004-08-12 Siltronic Japan Corp Single crystal manufacturing apparatus
CN101838841A (en) * 2010-02-23 2010-09-22 上海汉虹精密机械有限公司 Single crystal furnace device
CN102352530A (en) * 2011-11-09 2012-02-15 内蒙古中环光伏材料有限公司 Heat shield device for CZ-Si single crystal furnace
CN202766655U (en) * 2012-07-11 2013-03-06 银川隆基硅材料有限公司 Heat shield for Czochralski silicon single crystal furnace
CN103882510A (en) * 2012-12-24 2014-06-25 九州方园新能源股份有限公司 Diversion cylinder for increasing single crystal silicon growth rate
CN103342362A (en) * 2013-07-12 2013-10-09 新特能源股份有限公司 Heat shield of polysilicon CVD (chemical vapor deposition) reactor

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