CN113510824A - Preparation method of composite quartz crucible and composite quartz crucible - Google Patents

Preparation method of composite quartz crucible and composite quartz crucible Download PDF

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Publication number
CN113510824A
CN113510824A CN202010275959.1A CN202010275959A CN113510824A CN 113510824 A CN113510824 A CN 113510824A CN 202010275959 A CN202010275959 A CN 202010275959A CN 113510824 A CN113510824 A CN 113510824A
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quartz sand
sand layer
layer
crucible
quartz
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CN113510824B (en
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韩东
郭华盈
刘攀
刘阳
王征
周俊祥
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Longi Green Energy Technology Co Ltd
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Longi Green Energy Technology Co Ltd
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Priority to PCT/CN2020/133623 priority patent/WO2021203723A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/20—Producing shaped prefabricated articles from the material by centrifugal or rotational casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/04—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/40—Moulds; Cores; Mandrels characterised by means for modifying the properties of the moulding material
    • B28B7/44—Moulds; Cores; Mandrels characterised by means for modifying the properties of the moulding material for treating with gases or degassing, e.g. for de-aerating
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/14—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 based on silica
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/653—Processes involving a melting step
    • C04B35/657—Processes involving a melting step for manufacturing refractories
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • 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
    • C30B15/10—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
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

The invention provides a preparation method of a composite quartz crucible and the composite quartz crucible, which comprises the following steps: sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer with sequentially reduced median grain sizes along the inner side surface of the crucible mold to obtain a blank of the composite quartz crucible; and performing arc melting on the blank to obtain a composite quartz crucible, wherein the composite quartz crucible comprises a bubble layer, a first transparent layer and a second transparent layer, the bubble content of which is reduced from the outer side surface to the inner side surface in sequence. In the invention, as the median particle diameters of the first quartz sand layer to the third quartz sand layer in the blank are sequentially reduced, the bubble contents from the bubble layer to the second transparent layer in the composite quartz crucible prepared by using the blank are sequentially reduced, so that the content of microbubbles close to the surface layer on the inner side surface of the quartz crucible is effectively reduced, the influence of the breakage of the microbubbles on the growing monocrystalline silicon is reduced in the process of preparing the monocrystalline silicon by using the quartz crucible, and the quality and the crystallization rate of the monocrystalline silicon are improved.

Description

Preparation method of composite quartz crucible and composite quartz crucible
Technical Field
The invention relates to the technical field of monocrystalline silicon, in particular to a preparation method of a composite quartz crucible and the composite quartz crucible.
Background
With the continuous consumption of traditional energy and the increasingly serious negative impact on the environment, the function of the crystalline silicon solar cell in the aspects of changing the energy structure, relieving the environmental pressure and the like is increasingly prominent, and the monocrystalline silicon as one of the important basic materials of the crystalline silicon solar cell has wide market demand.
In the prior art, in the process of preparing monocrystalline silicon by the czochralski method, a commonly used quartz crucible is a quartz crucible obtained by molding quartz sand with a single median diameter to obtain a blank, then the blank is melted to obtain the quartz crucible, and the finally obtained quartz crucible comprises a bubble composite layer and a transparent layer from outside to inside through vacuumizing in the melting process, wherein the bubble content of the bubble composite layer is high, a radiation heat source provided by a heater can be uniformly radiated, so that the radiation heat source provided by the uniform radiation heater of the quartz crucible in a thermal field is ensured, the bubble content of the transparent layer is low, and the quantity of micro bubbles and quartz micro particles released to silicon liquid can be reduced.
However, in the prior art, the quartz crucible prepared by arc melting the blank still contains a large amount of microbubbles in the transparent layer of the quartz crucible, so that the microbubbles in the transparent layer of the quartz crucible are broken during the process of preparing the monocrystalline silicon by using the quartz crucible, thereby causing dislocation of the growing monocrystalline silicon and reducing the quality and the crystal forming rate of the monocrystalline silicon.
Disclosure of Invention
The invention provides a preparation method of a composite quartz crucible and the composite quartz crucible, aiming at reducing the possibility of breaking micro bubbles in a transparent layer of the quartz crucible in the process of preparing monocrystalline silicon by using the quartz crucible, thereby reducing the influence on the quality and the crystallization rate of the monocrystalline silicon.
In a first aspect, an embodiment of the present invention provides a method for preparing a composite quartz crucible, where the method includes:
sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the axis of the crucible mold facing the inner side of the crucible mold to obtain a blank of the composite quartz crucible, wherein the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced;
and arc melting is carried out on the blank of the composite quartz crucible to obtain the composite quartz crucible, the composite quartz crucible comprises a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content of the bubble layer, the first transparent layer and the second transparent layer is sequentially reduced.
Optionally, before the step of arc melting the blank of the composite quartz crucible to obtain the composite quartz crucible, the method further includes:
and carrying out vacuumizing operation on the outer side of the crucible mold, so that a vacuum environment with a preset vacuum degree is formed and maintained in the outer side of the crucible mold within a preset time, the third quartz sand layer is transferred to the second quartz sand layer, a transition layer between the second quartz sand layer and the third quartz sand layer is formed, and a blank of the composite quartz crucible comprising the transition layer is obtained.
Optionally, the step of performing arc melting on the blank of the composite quartz crucible to obtain the composite quartz crucible includes:
and arc melting the blank of the composite quartz crucible comprising the transition layer so that the transition layer and the third quartz sand layer form the second transparent layer.
Optionally, the preset time ranges from 0 minute to 10 minutes, and the preset vacuum degree ranges from 40 kpa to 75 kpa.
Optionally, the step of sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the inner side surface of the crucible mold towards the axis of the crucible mold to obtain a blank of the composite quartz crucible comprises:
respectively preparing a straight wall section of the first quartz sand layer and an arc-shaped part and a bottom part of the first quartz sand layer on the inner side of the crucible mold by using a first molding rod, wherein the straight wall section of the first quartz sand layer is mutually connected with the arc-shaped part and the bottom part of the first quartz sand layer to form the first quartz sand layer;
respectively preparing a straight wall section of the second quartz sand layer and an arc-shaped part and a bottom part of the second quartz sand layer on the inner side of the first quartz sand layer by using a second forming rod, wherein the straight wall section of the second quartz sand layer is mutually connected with the arc-shaped part and the bottom part of the second quartz sand layer to form the second quartz sand layer;
respectively preparing a straight wall section of the third quartz sand layer and an arc-shaped part and a bottom part of the third quartz sand layer on the inner side of the second quartz sand layer by using a third forming rod, wherein the straight wall section of the third quartz sand layer is mutually connected with the arc-shaped part and the bottom part of the third quartz sand layer to form the third quartz sand layer;
wherein the first to third forming bars are sequentially reduced in profile size.
Optionally, the step of preparing the straight wall section specifically includes:
the crucible mould is in order to predetermine the rotational speed, follows the axis of crucible mould is rotatory under the condition as the rotation center line, prepare straight wall section, just the contained angle between the axis of crucible mould and the horizontal plane is 30 degrees to 75 degrees, the scope of predetermineeing the rotational speed is 35 revolutions per minute to 75 revolutions per minute.
Optionally, the step of preparing the arc-shaped portion and the bottom portion specifically includes:
the crucible mould is in order to predetermine the rotational speed, follows under the condition that the axis of crucible mould rotated for the rotation axis, preparation arc portion and bottom, just contained angle between the axis of crucible mould and the horizontal plane is 90 degrees, the scope of predetermineeing the rotational speed is 35 commentaries on classics/minute to 75 commentaries on classics/minute.
Optionally, the mass percentage of the first quartz sand layer ranges from 0% to 70%, the mass percentage of the second quartz sand layer ranges from 10% to 95%, and the mass percentage of the third quartz sand layer ranges from 5% to 40%.
Optionally, the median grain size of the first quartz sand layer ranges from 240 micrometers to 295 micrometers, the median grain size of the second quartz sand layer ranges from 173 micrometers to 270 micrometers, and the median grain size of the third quartz sand layer ranges from 131 micrometers to 173 micrometers.
In a second aspect, an embodiment of the present invention provides a composite quartz crucible, where the composite quartz crucible includes a bubble layer, a first transparent layer and a second transparent layer, which are sequentially arranged, where the bubble layer is far away from an axis of the composite quartz crucible, and the second transparent layer is close to the axis of the composite quartz crucible;
the bubble content of the bubble layer, the first transparent layer and the second transparent layer is reduced in sequence;
the composite quartz crucible is prepared by arc melting of a blank of the composite quartz crucible, the blank of the composite quartz crucible comprises a first quartz sand layer, a second quartz sand layer and a third quartz sand layer which are sequentially arranged along the inner side surface of a crucible mold towards the axis of the crucible mold, and the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced.
Based on the preparation method of the composite quartz crucible and the composite quartz crucible, the preparation method has the following beneficial effects:
the utility model provides a material embryo of composite quartz crucible includes first quartz sand layer, second quartz sand layer and the third quartz sand layer that sets gradually towards the axis of crucible mould along the inboard of crucible mould, and the meso position particle diameter of first quartz sand layer to third quartz sand layer reduces in proper order, therefore will the composite quartz crucible that the material embryo obtained through electric arc melting, it is corresponding, have the bubble layer, first stratum lucidum and the second stratum lucidum that set gradually, wherein, the axis of composite quartz crucible is kept away from to the bubble layer, the axis that the second stratum lucidum is close to composite quartz crucible, and the bubble content of bubble layer to second stratum lucidum reduces in proper order, thereby the effectual microbubble content that reduces the nearly top layer of quartz crucible medial surface, and then also reduced the gathering of microbubble near the top layer of quartz crucible medial surface, lead to the possibility that the growth breaks after the microbubble volume increases to certain degree, in the process of preparing the monocrystalline silicon by using the quartz crucible, the influence of the breakage of the micro bubbles in the transparent layer of the quartz crucible on the growing monocrystalline silicon is reduced, so that the quality and the crystal forming rate of the monocrystalline silicon are improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments of the present invention will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without inventive labor.
FIG. 1 is a flow chart showing the steps of a method for manufacturing a composite quartz crucible according to a first embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating a process for preparing a preform according to a first embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a preform according to a first embodiment of the present invention;
FIG. 4 is a schematic structural view showing a composite quartz crucible according to a first embodiment of the present invention;
FIG. 5 is a schematic diagram illustrating another blank manufacturing process according to the first embodiment of the present invention;
FIG. 6 is a flow chart showing the steps of a method for manufacturing a composite quartz crucible according to a second embodiment of the present invention;
FIG. 7 is a schematic view showing a process for preparing a preform according to the second embodiment of the present invention;
FIG. 8 is a schematic view showing another process for preparing a preform according to example II of the present invention;
FIG. 9 is a schematic view showing another process for preparing a preform according to example two of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, fig. 1 is a flow chart showing steps of a method for manufacturing a composite quartz crucible according to a first embodiment of the present invention. The method may comprise the steps of:
101, sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the inner side surface of a crucible mold towards the axis of the crucible mold to obtain a blank of the composite quartz crucible, wherein the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced.
In this step, a first quartz sand layer, a second quartz sand layer and a third quartz sand layer may be sequentially formed along an inner side surface of the crucible mold toward an axis of the crucible mold, thereby obtaining a blank of the composite quartz crucible, wherein median particle diameters of the first quartz sand layer to the third quartz sand layer are sequentially reduced.
Referring to fig. 2, fig. 2 is a schematic view showing a process for preparing a preform according to a first embodiment of the present invention, and the process for preparing a composite quartz crucible preform may be a process for sequentially forming a first quartz sand layer 10, a second quartz sand layer 20 and a third quartz sand layer 30 inside a crucible mold 40 having a desired size and shape.
Specifically, the quartz sand with the first mass percent and the first median particle size may be uniformly laid on the inner side of the crucible mold 40, and preformed to obtain the first quartz sand layer 10, then the quartz sand with the second mass percent and the second median particle size may be uniformly laid on the inner side of the first quartz sand layer 10, and preformed to obtain the second quartz sand layer 20, and then the quartz sand with the third mass percent and the third median particle size may be uniformly laid on the inner side of the second quartz sand layer 20, and preformed to obtain the third quartz sand layer 30, so as to obtain the first quartz sand layer 10, the second quartz sand layer 20, and the third quartz sand layer 30 sequentially arranged along the outer side surface and the inner side surface of the crucible mold 40, and obtain the blank of the composite quartz crucible.
Optionally, the mass percentage of the first quartz sand layer, that is, the range of the first mass percentage, is 0% to 70%, the mass percentage of the second quartz sand layer, that is, the range of the second mass percentage, is 10% to 95%, and the mass percentage of the third quartz sand layer, that is, the range of the third mass percentage, is 5% to 40%, and when the mass percentage ranges meet the above-mentioned specifications, the sum of the first mass percentage, the second mass percentage, and the third mass percentage is 100%, so that the mass percentages of the first quartz sand layer, the second quartz sand layer, and the third quartz sand layer may be determined, and the mass percentages of the quartz sand respectively used when the first quartz sand layer, the second quartz sand layer, and the third quartz sand layer are prepared may be determined.
In the embodiment of the invention, the first median particle size of the quartz sand required for preparing the first quartz sand layer is smaller than the second median particle size of the quartz sand required for preparing the second quartz sand layer, and meanwhile, the second median particle size of the quartz sand required for preparing the second quartz sand layer is smaller than the third median particle size of the quartz sand required for preparing the third quartz sand layer, so that the median particle sizes of the corresponding quartz sand layers are sequentially reduced along the outer side surface and the inner side surface of the blank of the prepared composite quartz crucible with the multilayer composite structure.
Referring to fig. 3, fig. 3 shows a structural schematic diagram of a preform in a first embodiment of the invention, wherein the preform of the composite quartz crucible comprises a first quartz sand layer 10, a second quartz sand layer 20 and a third quartz sand layer 30 which are sequentially arranged along an axis 41 facing a crucible mold 40 from the outer side of the preform, wherein median grain sizes of the first quartz sand layer 10 to the third quartz sand layer 30 are sequentially reduced.
102, arc melting is carried out on the blank of the composite quartz crucible to obtain the composite quartz crucible, the composite quartz crucible comprises a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content of the bubble layer, the bubble content of the first transparent layer and the bubble content of the second transparent layer are sequentially reduced.
Wherein the second quartz sand layer comprises a first part close to the first quartz sand layer, a second part located at the middle position of the second quartz sand layer and a third part close to the third quartz sand layer, the bubble layer is generated by the first quartz sand layer and the first part, the first transparent layer is generated by the second part, the second transparent layer is generated by the third part and the third quartz sand layer, the bubble layer, the first transparent layer and the second transparent layer are sequentially arranged along the outer side surface and the inner side surface of the composite quartz crucible, the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content from the bubble layer to the second transparent layer is sequentially reduced.
In the step, the blank of the composite quartz crucible is subjected to arc melting, each quartz sand layer in the blank is rapidly melted and formed into the composite quartz crucible under the action of the electric arc of the electrode, referring to fig. 4, fig. 4 shows a structural schematic diagram of the composite quartz crucible in the first embodiment of the invention, the composite quartz crucible obtained after the blank of the composite quartz crucible is subjected to arc melting comprises a bubble layer 60, a first transparent layer 70 and a second transparent layer 80 which are sequentially arranged, wherein the bubble layer 60 is far away from the axis 100 of the composite quartz crucible, the second transparent layer is close to the axis 100 of the composite quartz crucible, and the bubble content of the bubble layer 60 to the second transparent layer 80 is sequentially reduced.
Specifically, the distance between the inner side surface of the straight wall portion of the bubble layer 60 and the axis 100 of the composite quartz crucible is R1, the distance between the inner side surface of the straight wall portion of the first transparent layer 70 and the axis 100 of the composite quartz crucible is R2, and the distance between the inner side surface of the straight wall portion of the second transparent layer 80 and the axis 100 of the composite quartz crucible is R3, wherein R1 > R2 > R3.
Specifically, referring to fig. 5, fig. 5 is a schematic diagram illustrating a preparation process of another preform in the first embodiment of the invention, in the process of arc melting the preform of the composite quartz crucible, a part a quartz sand layer is formed by a first part 21 of the first quartz sand layer 10 and a second quartz sand layer 20, which is close to the first quartz sand layer 10, and is rapidly melted and formed into a bubble layer in the composite quartz crucible under the action of an arc; the second part 22 positioned in the middle of the second quartz sand layer 20 forms a B quartz sand layer, and is rapidly melted and formed into a first transparent layer in the composite quartz crucible under the action of electric arc; and a third part 23 of the second quartz sand layer 20, which is close to the third quartz sand layer 30, and a part C quartz sand layer which is formed by the third quartz sand layer 30 together are rapidly melted and formed into a second transparent layer in the composite quartz crucible under the action of electric arc.
Because in the material embryo of compound quartz crucible, follow the lateral surface of material embryo is to the medial surface, and the meso position particle diameter of first quartz sand layer to third quartz sand layer reduces in proper order, and the space between the quartz sand reduces in proper order, and is corresponding, utilizes the compound quartz crucible that the material embryo preparation obtained follows the lateral surface of compound quartz crucible is to the medial surface, and the bubble content of bubble layer to the second stratum lucidum reduces in proper order to the effectual microbubble content that has reduced the nearly top layer of quartz crucible medial surface, and has restrained the microbubble and has taken place to grow up the possibility of breaking.
In an embodiment of the invention, a preparation method of a composite quartz crucible comprises the following steps: sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the axis of the inner side surface of the crucible mold facing the crucible mold to obtain a blank of the composite quartz crucible, wherein the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced; and arc melting is carried out on the blank of the composite quartz crucible to obtain the composite quartz crucible, the composite quartz crucible comprises a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content of the bubble layer, the first transparent layer and the second transparent layer is sequentially reduced. In the application, utilize the material embryo of the compound quartz crucible that has multilayer composite structure, prepare and obtain compound quartz crucible, because the material embryo includes first quartz sand layer, second quartz sand layer and the third quartz sand layer that sets gradually towards the axis of crucible mould along the inboard of crucible mould, and the median particle size of first quartz sand layer to third quartz sand layer reduces in proper order, therefore will the compound quartz crucible that the material embryo obtained through electric arc melting, it is corresponding, have bubble layer, first stratum lucidum and the second stratum lucidum that sets gradually, wherein, the axis of compound quartz crucible is kept away from to the bubble layer, the axis that the second stratum lucidum is close to compound quartz crucible, and the bubble content of bubble layer to second stratum lucidum reduces in proper order to the effectual microbubble content that has reduced the near surface layer of quartz crucible medial surface, and restrained the possibility that the microbubble takes place to grow up and break, in the process of preparing the monocrystalline silicon by using the quartz crucible, the influence of the breakage of the micro bubbles in the transparent layer of the quartz crucible on the growing monocrystalline silicon is reduced, so that the quality and the crystal forming rate of the monocrystalline silicon are improved.
Example two
Referring to fig. 6, there is shown a flow chart of the steps of a method for manufacturing a composite quartz crucible according to a second embodiment of the present invention, which may include the steps of:
step 201, respectively preparing a straight wall section of the first quartz sand layer and an arc-shaped part and a bottom part of the first quartz sand layer on the inner side of the crucible mold by using a first molding rod, wherein the straight wall section of the first quartz sand layer is connected with the arc-shaped part and the bottom part of the first quartz sand layer to form the first quartz sand layer.
In this step, since the first quartz sand layer, the second quartz sand layer and the third quartz sand layer need to be sequentially arranged along the inner side surface of the crucible mold towards the axis of the crucible mold, so that the blank of the composite quartz crucible can be finally obtained, the first quartz sand layer can be firstly molded on the inner side of the crucible mold.
Specifically, a straight wall section of the first quartz sand layer and an arc-shaped part and a bottom part of the first quartz sand layer may be respectively prepared inside the crucible mold by using a first forming rod, wherein the straight wall section of the first quartz sand layer and the arc-shaped part and the bottom part of the first quartz sand layer are connected with each other to jointly form the first quartz sand layer.
In the embodiment of the invention, in the process of preparing the first quartz sand layer on the inner side of the crucible mold, quartz sand with a first mass percentage and a first median particle size can be uniformly laid on the inner side of the crucible mold by scraping by using the first forming rod.
Optionally, the first mass percentage, i.e., the mass percentage of the first silica sand layer, may range from 0% to 70%, and the first median particle size, i.e., the median particle size of the first silica sand layer, may range from 240 micrometers to 295 micrometers.
In an embodiment of the present invention, the first quartz sand layer may include a straight wall section, an arc-shaped portion and a bottom portion, and the straight wall section of the first quartz sand layer and the arc-shaped portion and the bottom portion of the first quartz sand layer are connected to each other to form the first quartz sand layer, and therefore, the step of preparing the first quartz sand layer may specifically include:
substep 2011 of preparing a straight wall segment of the first quartz sand layer.
In this step, in order to allow the silica sand constituting the first silica sand layer to adhere to the inner wall of the mold during the preparation of the straight wall section of the first silica sand layer, the crucible mold may be rotated along the axis of the crucible mold as a rotation center line at a first predetermined rotation speed, so that the straight wall section of the first silica sand layer is prepared using the first molding rod while the crucible mold is rotated along the axis of the crucible mold as a rotation center line at the first predetermined rotation speed, an included angle between the axis of the crucible mold and a horizontal plane may be 30 to 75 degrees, and the first predetermined rotation speed may be in a range of 35 to 75 revolutions per minute.
The first preset rotating speed can be obtained by calculating the relationship between the friction force between the quartz sand and the mold and the gravity of the quartz sand, and because it is required to ensure that the quartz sand can be successfully attached to the inner wall of the mold in the process of preparing the first quartz sand layer, it is required to ensure that the upward friction force is greater than or equal to the downward gravity in the process of making circular motion of the mold, so that the range of the rotating speed of the mold, namely the range of the first preset rotating speed, is finally determined, and the specific calculation process is as follows:
Figure BDA0002444791970000091
Figure BDA0002444791970000092
wherein, FMassage 1The friction force of the quartz sand in the first quartz sand layer in the mold is Newton;
Fto 1The centrifugal force, Newton, of the quartz sand in the first quartz sand layer upwards in the mould is adopted;
μ1the coefficient of friction between the quartz sand in the first quartz sand layer and the mould is 1.333 +/-0.1;
m1the weight of the quartz sand in the first quartz sand layer is kilogram;
r1the outer diameter of the first quartz sand layer is meter;
t is the period of circular motion, second;
n1is the first preset speed, rpm.
For example, for a 28-inch composite quartz crucible, the inner diameter of the mold is 0.716 m, the thickness of the first quartz sand layer is 0.016 m, and the outer diameter r of the first quartz sand layer10.358 m, the friction coefficient mu between the quartz sand and the mould in the first quartz sand layer1Is 1.333 + -0.1, so that the rotation speed of the die, i.e. the first preset rotation speed n, can be calculated1Not less than 44.995 rpm.
Substep 2012, preparing the arc portion and the bottom portion of the first quartz sand layer.
In this step, in order to allow the silica sand constituting the first silica sand layer to adhere to the inner wall of the mold during the preparation of the arc portion and the bottom portion of the first silica sand layer, the crucible mold may be rotated along the axis of the crucible mold as a rotation center line at a first preset rotation speed, so that the arc portion and the bottom portion of the first silica sand layer are prepared using the first molding rod in a state where the crucible mold is rotated along the axis of the crucible mold as a rotation center line at the first preset rotation speed, an included angle between the axis of the crucible mold and a horizontal plane may be 90 degrees, and the first preset rotation speed may range from 35 rpm to 75 rpm.
Step 202, utilizing a second forming rod to respectively prepare a straight wall section of the second quartz sand layer and an arc-shaped part and a bottom part of the second quartz sand layer on the inner side of the first quartz sand layer, wherein the straight wall section of the second quartz sand layer is connected with the arc-shaped part and the bottom part of the second quartz sand layer to form the second quartz sand layer.
In the step, because the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are required to be sequentially formed on the inner side of the crucible mold, so that the blank of the composite quartz crucible can be finally obtained, and after the first quartz sand layer is prepared, the second quartz sand layer can be formed on the inner side of the first quartz sand layer.
Specifically, a straight wall section of the second quartz sand layer and an arc-shaped part and a bottom part of the second quartz sand layer may be respectively prepared on the inner side of the first quartz sand layer by using a second forming rod, wherein the straight wall section of the second quartz sand layer and the arc-shaped part and the bottom part of the second quartz sand layer are connected with each other to jointly form the second quartz sand layer.
In the embodiment of the invention, in the process of preparing the second quartz sand layer on the inner side of the first quartz sand layer, quartz sand with a second mass percentage and a second median particle size can be uniformly paved on the inner side of the first quartz sand layer by scraping by using the second forming rod.
Optionally, the second mass percentage, i.e., the mass percentage of the second silica sand layer, may be in a range of 10% to 95%, and the second median diameter, i.e., the median diameter of the second silica sand layer, may be in a range of 173 micrometers to 270 micrometers.
In an embodiment of the present invention, the second quartz sand layer may include a straight wall section, an arc-shaped portion and a bottom portion, and the straight wall section of the second quartz sand layer and the arc-shaped portion and the bottom portion of the second quartz sand layer are connected to each other to form the second quartz sand layer, and therefore, the step of preparing the second quartz sand layer may specifically include:
substep 2021, preparing a straight wall section of the second silica sand layer.
In this step, in order to allow the quartz sand constituting the second quartz sand layer to adhere to the inner wall of the first quartz sand layer during the preparation of the straight wall section of the second quartz sand layer, the crucible mold may be rotated along the axis of the crucible mold as the rotation center line at a second predetermined rotation speed, so that the straight wall section of the second quartz sand layer is prepared using the second forming rod in a case where the crucible mold is rotated along the axis of the crucible mold as the rotation center line at the second predetermined rotation speed, an included angle between the axis of the crucible mold and a horizontal plane may be 30 to 75 degrees, and the second predetermined rotation speed may be 35 to 75 revolutions per minute.
The second preset rotating speed can be calculated through a relation between the friction force between the quartz sand in the second quartz sand layer and the quartz sand in the first quartz sand layer and the gravity of the quartz sand in the second quartz sand layer, and because it is required to ensure that the quartz sand in the second quartz sand layer can be successfully attached to the inner wall of the first quartz sand layer in the process of preparing the second quartz sand layer, it is required to ensure that the upward friction force is greater than or equal to the downward gravity in the process of making the circular motion of the mold by the quartz sand in the second quartz sand layer, so that the range of the rotating speed of the mold is finally determined, namely the range of the second preset rotating speed, and the specific calculation process is as follows:
Figure BDA0002444791970000111
Figure BDA0002444791970000121
wherein, FMassage 2The upward friction force, Newton, of the quartz sand in the second quartz sand layer in the first quartz sand layer;
Fto 2The centrifugal force, Newton, of the quartz sand in the second quartz sand layer upwards in the first quartz sand layer;
μ2the friction coefficient between the quartz sand in the second quartz sand layer and the first quartz sand layer is 1.729 +/-0.1;
m2the weight of the quartz sand in the second quartz sand layer is kilogram;
r2the outer diameter of the second quartz sand layer is meter;
t is the period of circular motion, second;
n2at a second predetermined speed, rpm.
For example, for a composite quartz crucible of 28 inches, the inner diameter of the mold is 0.716 meters, the thickness of the first quartz sand layer is 0.016 meters, and the outer diameter r of the second quartz sand layer20.342 m, and the friction coefficient mu between the quartz sand in the second quartz sand layer and the first quartz sand layer21.729 + -0.1, so that the rotational speed of the mold, i.e. the second predetermined rotational speed n, can be calculated2Not less than 40.002 rpm.
Therefore, the first preset rotation speed n is comprehensively considered1Not less than 44.995 rpm and a second preset rotation speed n240.002 revolutions per minute or more can be finally determined to meet the requirement on the rotating speed of the mold in the preparation process of the first quartz sand layer and the second quartz sand layer, for example, the rotating speed of the mold can be determined, namely the preset rotating speed is n 45 revolutions per minute or more, so that the requirement on the rotating speed of the mold in the preparation process of the first quartz sand layer and the second quartz sand layer can be met simultaneously.
Substep 2022, preparing the arc portion and the bottom of the second quartz sand layer.
In this step, in order to allow the quartz sand constituting the second quartz sand layer to be attached to the inner wall of the first quartz sand layer in the process of preparing the arc portion and the bottom portion of the second quartz sand layer, the crucible mold may be rotated along the axis of the crucible mold as the rotation center line at a second predetermined rotation speed, so that the arc portion and the bottom portion of the second quartz sand layer are prepared using the second forming rod in a state where the crucible mold is rotated along the axis of the crucible mold as the rotation center line at the second predetermined rotation speed, an included angle between the axis of the crucible mold and a horizontal plane may be 90 degrees, and the second predetermined rotation speed may range from 35 rpm to 75 rpm.
Step 203, respectively preparing a straight wall section of the third quartz sand layer and an arc-shaped part and a bottom part of the third quartz sand layer on the inner side of the second quartz sand layer by using a third forming rod, wherein the straight wall section of the third quartz sand layer is mutually connected with the arc-shaped part and the bottom part of the third quartz sand layer to form the third quartz sand layer.
In the step, because the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are required to be sequentially formed on the inner side of the crucible mold, the blank of the composite quartz crucible can be finally obtained, and therefore, after the second quartz sand layer is prepared, the third quartz sand layer can be formed on the inner side of the second quartz sand layer.
In addition, since the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially arranged on the inner side of the crucible mold, the profile sizes of the first forming rod to the third forming rod are sequentially reduced.
Specifically, a straight wall section of the third silica sand layer and an arc-shaped part and a bottom part of the third silica sand layer may be respectively prepared inside the second silica sand layer by using a third forming rod, wherein the straight wall section of the third silica sand layer and the arc-shaped part and the bottom part of the third silica sand layer are connected with each other to jointly form the third silica sand layer.
In the embodiment of the invention, in the process of preparing the third quartz sand layer on the inner side of the second quartz sand layer, quartz sand with a third mass percent and a third median particle size can be uniformly paved on the inner side of the second quartz sand layer by scraping by using a third forming rod.
Optionally, the third mass percentage, that is, the mass percentage of the third silica sand layer may range from 5% to 40%, and the third median diameter, that is, the median diameter of the third silica sand layer may range from 131 micrometers to 173 micrometers.
In an embodiment of the present invention, the third silica sand layer may include a straight wall section, an arc-shaped portion and a bottom portion, and the straight wall section of the third silica sand layer and the arc-shaped portion and the bottom portion of the third silica sand layer are connected to each other to form the third silica sand layer, and therefore, the step of preparing the third silica sand layer may specifically include:
substep 2031, preparing a straight wall segment of the third silica sand layer.
In this step, in order to allow the quartz sand constituting the third quartz sand layer to adhere to the inner wall of the second quartz sand layer during the preparation of the straight wall section of the third quartz sand layer, the crucible mold may be rotated along the axis of the crucible mold as the rotation center line at a third predetermined rotation speed, so that the straight wall section of the third quartz sand layer is prepared using a third molding rod in a case where the crucible mold is rotated along the axis of the crucible mold as the rotation center line at the third predetermined rotation speed, an included angle between the axis of the crucible mold and a horizontal plane may be 30 to 75 degrees, and the third predetermined rotation speed may be in a range of 35 to 75 revolutions per minute.
The third preset rotating speed can be calculated through a relation between the frictional force between the quartz sand in the third quartz sand layer and the quartz sand in the second quartz sand layer and the gravity of the quartz sand in the third quartz sand layer, and because it is required to ensure that the quartz sand in the third quartz sand layer can be successfully attached to the inner wall of the second quartz sand layer in the process of preparing the third quartz sand layer, it is required to ensure that the upward frictional force is greater than or equal to the downward gravity in the process of making the circular motion of the mold by the quartz sand in the third quartz sand layer, so that the range of the rotating speed of the mold is finally determined, namely the range of the third preset rotating speed, and the specific calculation process is as follows:
Figure BDA0002444791970000141
Figure BDA0002444791970000142
wherein, FMassage 3The upward friction force, Newton, of the quartz sand in the third quartz sand layer in the second quartz sand layer;
Fto 3The centrifugal force, Newton, of the quartz sand in the third quartz sand layer upwards in the second quartz sand layer;
μ3the friction coefficient between the quartz sand in the third quartz sand layer and the second quartz sand layer is 1.729 +/-0.1;
m3the weight of the quartz sand in the third quartz sand layer is kilogram;
r3the outer diameter of the third quartz sand layer is meter;
t is the period of circular motion, second;
n3at a third predetermined speed, rpm.
For example, for a 32-inch composite quartz crucible, the inner diameter of the mold is 0.823 m, the thickness of the first quartz sand layer is 0.016 m, and the thickness of the second quartz sand layer is 0.033 m, the firstOuter diameter r of three quartz sand layers20.3625 m, the coefficient of friction between the quartz sand in the third quartz sand layer and the second quartz sand layer is mu31.729 + -0.1, so that the rotational speed of the mold, i.e. the third predetermined rotational speed n, can be calculated3Not less than 38.071 rpm, the first preset rotation speed n1Not less than 41.968 rpm.
Therefore, the first preset rotation speed n is comprehensively considered1Not less than 41.968 rpm and a third preset rotation speed n338.071 revolutions per minute or more can be finally determined to meet the requirement on the rotating speed of the mold in the preparation process of the first quartz sand layer and the third quartz sand layer, for example, the rotating speed of the mold can be determined, namely the preset rotating speed n is 42 revolutions per minute or more, so that the requirement on the rotating speed of the mold in the preparation process of the first quartz sand layer and the third quartz sand layer can be met simultaneously.
Substep 2032, preparing the arc part and the bottom of the third silica sand layer.
In this step, in order to allow the quartz sand constituting the third quartz sand layer to adhere to the inner wall of the second quartz sand layer in the process of preparing the arc portion and the bottom portion of the third quartz sand layer, the crucible mold may be rotated at a third preset rotation speed along the axis of the crucible mold as the rotation center line, so that the arc portion and the bottom portion of the third quartz sand layer are prepared using a third molding rod in a case where the crucible mold is rotated at the third preset rotation speed along the axis of the crucible mold as the rotation center line, an included angle between the axis of the crucible mold and a horizontal plane may be 90 degrees, and the third preset rotation speed may range from 35 rpm to 75 rpm.
And 204, performing vacuumizing operation on the outer side of the crucible mold, so that a vacuum environment with a preset vacuum degree is formed and maintained on the outer side of the crucible mold within a preset time, and the third quartz sand layer is transferred to the second quartz sand layer to form a transition layer between the second quartz sand layer and the third quartz sand layer, so as to obtain a blank of the composite quartz crucible comprising the transition layer.
In this step, after the blank of the composite quartz crucible is prepared, a vacuum pumping operation may be performed on the outer side of the crucible mold, so that a vacuum environment having a predetermined vacuum degree is formed and maintained in the outer side of the crucible mold within a predetermined time.
Specifically, a certain vacuum degree can be formed in a cavity between the crucible mold and the water cooling jacket by starting a vacuum system.
Optionally, the preset time is in a range of 0 minute to 10 minutes, and the preset vacuum degree is in a range of 40 kilopascals to 75 kilopascals.
Further, under the action of the vacuum environment, the third quartz sand layer migrates to the second quartz sand layer to form a transition layer, and a blank of the composite quartz crucible comprising the transition layer is obtained.
In the step, the blank of the composite quartz crucible is in a vacuum environment, and because the outside of the crucible mold forms and maintains the vacuum environment with the preset vacuum degree within the preset time, the quartz sand in the blank can be subjected to the vacuum pressure along the direction of the inner side surface of the blank to the outer side surface, therefore, the third quartz sand layer in the blank can migrate to the outer side surface of the blank under the action of vacuum pressure to obtain the blank of the composite quartz crucible comprising the transition layer, because the median particle size of the third quartz sand layer is smaller than that of the second quartz sand layer, the pores among the quartz sand in the second quartz sand layer are larger, and in the migration process of the quartz sand in the third quartz sand layer, will migrate into the pores of the second quartz sand layer to form a transition layer mixed with the third quartz sand layer and the second quartz sand layer, the bulk density of the quartz sand in the transition layer is higher, and the pores among the quartz sand are further reduced relative to the pores in the second quartz sand layer.
It should be noted that, in the process of preparing the blank of the composite quartz crucible including the transition layer, since each quartz sand layer moves circularly along with the mold, the quartz sand in the third quartz sand layer may migrate to the second quartz sand layer under the action of centrifugal force to form the transition layer.
In this step, the position of the transition layer formed in the blank is different according to the difference between the preset time and the preset vacuum degree of the vacuum environment, and the following specific conditions may be included:
substep 2041, in the case where the preset time is 3 minutes and the preset vacuum degree is 50 kpa.
Specifically, referring to fig. 7, which is a schematic diagram illustrating a preparation process of a preform in the second embodiment of the present invention, when a material layer thickness is 42 mm, a vacuum degree of a cavity between a crucible mold and a water cooling jacket, i.e., a preset vacuum degree, is 50 kpa, and a vacuum pumping time, i.e., a preset time is 3 minutes, under the action of a vacuum pressure, a part of quartz sand in the third quartz sand layer 30 migrates to the second quartz sand layer 20 to form a transition layer 90, and the transition layer 90 is located between the second quartz sand layer 20 and the third quartz sand layer 30.
Substep 2042, in the case where the preset time is 7 minutes and the preset vacuum degree is 50 kpa.
Referring to fig. 8, which is a schematic diagram illustrating a preparation process of another preform in the second embodiment of the present invention, when a thickness of a material layer is 42 mm, a vacuum degree of a cavity between a crucible mold and a water cooling jacket, i.e., a preset vacuum degree, is 50 kpa, and a vacuum pumping time, i.e., a preset time is 7 minutes, under a vacuum pressure, all quartz sand in a third quartz sand layer migrates to a second quartz sand layer 20, and completely overlaps with the second quartz sand layer 20 to form a transition layer 90, the second quartz sand layer 20 is not exposed to form an inner surface of the crucible, the third quartz sand layer disappears, and the transition layer 90 is located on an inner side surface of the second quartz sand layer 20, i.e., an inner side surface of the preform.
Substep 2043, in the case where said preset time is 10 minutes and said preset vacuum degree is 50 kpa.
Referring to fig. 9, which is a schematic diagram illustrating a preparation process of another preform in the second embodiment of the present invention, when a thickness of a material layer is 42 mm, a vacuum degree of a cavity between a crucible mold and a water cooling jacket, i.e., a preset vacuum degree, is 50 kpa, and a vacuum pumping time, i.e., a preset time is 10 minutes, under a vacuum pressure, all quartz sand in a third quartz sand layer migrates to the second quartz sand layer 20, and completely overlaps with the second quartz sand layer 20 to form a transition layer 90, and a part of the second quartz sand layer 20 is exposed to form an inner surface of the crucible, the third quartz sand layer disappears, and the transition layer 90 is located between the second portion 22 and the third portion 23 of the second quartz sand layer 20.
Step 205, performing arc melting on the blank of the composite quartz crucible including the transition layer, so that the transition layer and the third quartz sand layer form the second transparent layer.
In the step, the blank of the composite quartz crucible including the transition layer prepared in the above way is subjected to arc melting, and finally the composite quartz crucible including the bubble layer, the first transparent layer and the second transparent layer is obtained.
Specifically, the composite quartz crucible obtained after arc melting is different according to different blanks prepared in the above steps, and the method specifically includes the following conditions:
substep 2051, in the case where said preset time is 3 minutes and said preset vacuum is 50 kpa.
Specifically, referring to fig. 7, in the process of arc melting the blank of the composite quartz crucible, a first part 21 of the first quartz sand layer 10 and the second quartz sand layer 20, which is close to the first quartz sand layer 10, jointly forms a part a quartz sand layer, and under the action of the arc, the part a quartz sand layer is rapidly melted and formed into a bubble layer in the composite quartz crucible; the middle part and the second part 22 of the second quartz sand layer 20 form a B quartz sand layer, and the B quartz sand layer is rapidly melted and formed into a first transparent layer in the composite quartz crucible under the action of electric arc; the transition layer 90 and the third quartz sand layer 30 together form a part C quartz sand layer, and the part C quartz sand layer is rapidly melted and formed into a second transparent layer in the composite quartz crucible under the action of electric arc.
Substep 2052, in the case where said preset time is 7 minutes and said preset vacuum degree is 50 kpa.
Referring to fig. 8, in the process of arc melting the blank of the composite quartz crucible, a first part 21 of the first quartz sand layer 10 and the second quartz sand layer 20, which is close to the first quartz sand layer 10, jointly forms a part a quartz sand layer, and under the action of the arc, the part a quartz sand layer is rapidly melted and formed into a bubble layer in the composite quartz crucible; the middle part and the second part 22 of the second quartz sand layer 20 form a B quartz sand layer, and the B quartz sand layer is rapidly melted and formed into a first transparent layer in the composite quartz crucible under the action of electric arc; the transition layer 90 is rapidly melted and formed into a second transparent layer in the composite quartz crucible under the action of the electric arc.
Substep 2053, in the case where said preset time is 10 minutes and said preset vacuum is 50 kpa.
Referring to fig. 9, in the process of arc melting the blank of the composite quartz crucible, a first part 21 of the first quartz sand layer 10 and the second quartz sand layer 20, which is close to the first quartz sand layer 10, jointly forms a part a quartz sand layer, and under the action of the arc, the part a quartz sand layer is rapidly melted and formed into a bubble layer in the composite quartz crucible; the middle part and the second part 22 of the second quartz sand layer 20 form a B quartz sand layer, and the B quartz sand layer is rapidly melted and formed into a first transparent layer in the composite quartz crucible under the action of electric arc; the transition layer 90 and the second quartz sand layer 20 are exposed to form a third part 23 forming the inner surface of the crucible, and the quartz sand layer of the part C which is formed together is rapidly melted and formed into a second transparent layer in the composite quartz crucible under the action of electric arc.
Because in the material embryo of compound quartz crucible, follow the outside of material embryo is to the medial surface, and the gradient that the meso position particle diameter of quartz sand layer reduces further reduces, first quartz sand layer to transition layer, and the meso position particle diameter of arriving the third quartz sand layer reduces in proper order again, and the space between the quartz sand reduces in proper order, and is corresponding, utilizes the compound quartz crucible that the material embryo preparation obtained follows compound quartz crucible's outside is to the medial surface, and the bubble content of bubble layer to the second stratum lucidum reduces in proper order to the effectual microbubble content that has reduced the nearly top layer of quartz crucible medial surface, and has restrained the possibility that the microbubble takes place to grow up and break.
Step 206, preparing a coating on the inner side surface of the composite quartz crucible, wherein the coating comprises: any one of a barium hydroxide coating, a silicon nitride coating, a silicon dioxide coating, and a barium carbonate coating.
In this step, a coating may be prepared on the inner side of the composite quartz crucible obtained by arc melting, the coating comprising: any one of the barium hydroxide coating, the silicon nitride coating, the silicon dioxide coating and the barium carbonate coating, thereby greatly prolonging the service life and the crystallization rate of the quartz crucible.
For example, the quartz crucible wall is coated with a layer of barium hydroxide (ba (oh)2.8H2O) (saturated aqueous barium hydroxide solution) containing water of crystallization, which reacts with carbon dioxide in air to form barium carbonate. When the quartz crucible is heated on a single crystal furnace in the process of preparing the monocrystalline silicon, barium carbonate is decomposed to form barium oxide, and a layer of compact and tiny cristobalite crystals are formed on the wall of the quartz crucible along with the barium oxide and the quartz crucible reacting to form barium silicate, and the tiny cristobalite crystals are difficult to be penetrated into the solution and peeled off and can be dissolved by the solution quickly even if the small cristobalite crystals are peeled off, so that the service life and the crystal growth yield of the quartz crucible can be greatly improved, the strength of the quartz crucible can be increased, and the high-temperature softening phenomenon can be reduced.
In the embodiment of the invention, the blank of the composite quartz crucible comprises a first quartz sand layer, a second quartz sand layer and a third quartz sand layer which are sequentially arranged along the inner side of the crucible mold facing to the axis of the crucible mold, and the median particle sizes of the first quartz sand layer to the third quartz sand layer are sequentially reduced, so that the blank is subjected to arc melting to obtain the composite quartz crucible, correspondingly, the composite quartz crucible is provided with a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, wherein the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content of the bubble layer to the second transparent layer is sequentially reduced, thereby effectively reducing the content of microbubbles close to the surface layer on the inner side surface of the quartz crucible, inhibiting the possibility of the microbubbles from growing up and breaking, reducing the influence of the microbubbles in the transparent layer of the quartz crucible on the growing monocrystalline silicon in the process of preparing the monocrystalline silicon by using the quartz crucible, thereby improving the quality and the crystal forming rate of the monocrystalline silicon.
In addition, before the blank is subjected to electric arc melting, the outer side of the crucible mold can be subjected to vacuum pumping operation, quartz sand in the third quartz sand layer migrates to the second quartz sand layer under the action of vacuum pressure to form a transition layer, and the blank of the composite quartz crucible comprising the transition layer is obtained.
It should be noted that, for simplicity of description, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will recognize that the embodiments are not limited by the order of acts described, as some steps may occur in other orders or concurrently depending on the embodiments. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the embodiments of the application.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
Through the above description of the embodiments, those skilled in the art will clearly understand that the method of the above embodiments can be implemented by software plus a necessary general hardware platform, and certainly can also be implemented by hardware, but in many cases, the former is a better implementation manner. Based on such understanding, the technical solutions of the present invention may be embodied in the form of a software product, which is stored in a storage medium (such as ROM/RAM, magnetic disk, optical disk) and includes instructions for enabling a terminal (such as a mobile phone, a computer, a server, an air conditioner, or a network device) to execute the method according to the embodiments of the present invention.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. A method for preparing a composite quartz crucible, comprising:
sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the axis of the crucible mold facing the inner side of the crucible mold to obtain a blank of the composite quartz crucible, wherein the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced;
and arc melting is carried out on the blank of the composite quartz crucible to obtain the composite quartz crucible, the composite quartz crucible comprises a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, the bubble layer is far away from the axis of the composite quartz crucible, the second transparent layer is close to the axis of the composite quartz crucible, and the bubble content of the bubble layer, the first transparent layer and the second transparent layer is sequentially reduced.
2. The method of claim 1, wherein prior to the step of arc melting the blank of the composite quartz crucible to obtain the composite quartz crucible, the method further comprises:
and carrying out vacuumizing operation on the outer side of the crucible mold, so that a vacuum environment with a preset vacuum degree is formed and maintained in the outer side of the crucible mold within a preset time, the third quartz sand layer is transferred to the second quartz sand layer, a transition layer between the second quartz sand layer and the third quartz sand layer is formed, and a blank of the composite quartz crucible comprising the transition layer is obtained.
3. The method of claim 2, wherein the step of arc melting the blank of the composite quartz crucible to obtain the composite quartz crucible comprises:
and arc melting the blank of the composite quartz crucible comprising the transition layer so that the transition layer and the third quartz sand layer form the second transparent layer.
4. The method of claim 2, wherein the preset time is in a range of 0 minutes to 10 minutes and the preset vacuum is in a range of 40 kilopascals to 75 kilopascals.
5. The method as claimed in claim 1, wherein the step of sequentially arranging a first quartz sand layer, a second quartz sand layer and a third quartz sand layer along the axis of the crucible mold facing the inside of the crucible mold to obtain the blank of the composite quartz crucible comprises:
sequentially molding a straight wall section of the first quartz sand layer and the arc-shaped part and the bottom of the first quartz sand layer on the inner side of the crucible mold by using a first molding rod, wherein the straight wall section of the first quartz sand layer is mutually connected with the arc-shaped part and the bottom of the first quartz sand layer to form the first quartz sand layer;
sequentially molding a straight wall section of the second quartz sand layer and an arc-shaped part and a bottom part of the second quartz sand layer on the inner side of the first quartz sand layer by using a second molding rod, wherein the straight wall section of the second quartz sand layer is mutually connected with the arc-shaped part and the bottom part of the second quartz sand layer to form the second quartz sand layer;
sequentially molding a straight wall section of the third quartz sand layer and the arc-shaped part and the bottom of the third quartz sand layer on the inner side of the second quartz sand layer by using a third molding rod, wherein the straight wall section of the third quartz sand layer is mutually connected with the arc-shaped part and the bottom of the third quartz sand layer to form the third quartz sand layer;
wherein the first to third forming bars are sequentially reduced in profile size.
6. The method according to claim 5, characterized in that said step of preparing said straight wall segments comprises in particular:
the crucible mould is in order to predetermine the rotational speed, follows the axis of crucible mould is rotatory under the condition as the rotation center line, prepare straight wall section, just the contained angle between the axis of crucible mould and the horizontal plane is 30 degrees to 75 degrees, the scope of predetermineeing the rotational speed is 35 revolutions per minute to 75 revolutions per minute.
7. The method according to claim 5, wherein the step of preparing the arc-shaped portion and the bottom portion comprises in particular:
the crucible mould is in order to predetermine the rotational speed, follows under the condition that the axis of crucible mould rotated for the rotation axis, preparation arc portion and bottom, just contained angle between the axis of crucible mould and the horizontal plane is 90 degrees, the scope of predetermineeing the rotational speed is 35 commentaries on classics/minute to 75 commentaries on classics/minute.
8. The method according to claim 1, wherein the first quartz sand layer ranges from 0% to 70% by mass, the second quartz sand layer ranges from 10% to 95% by mass, and the third quartz sand layer ranges from 5% to 40% by mass.
9. The method of claim 1, wherein the first silica sand layer has a median grain size in a range of 240 microns to 295 microns, the second silica sand layer has a median grain size in a range of 173 microns to 270 microns, and the third silica sand layer has a median grain size in a range of 131 microns to 173 microns.
10. The composite quartz crucible is characterized by comprising a bubble layer, a first transparent layer and a second transparent layer which are sequentially arranged, wherein the bubble layer is far away from the axis of the composite quartz crucible, and the second transparent layer is close to the axis of the composite quartz crucible;
the bubble content of the bubble layer, the first transparent layer and the second transparent layer is reduced in sequence;
the composite quartz crucible is prepared by arc melting of a blank of the composite quartz crucible, the blank of the composite quartz crucible comprises a first quartz sand layer, a second quartz sand layer and a third quartz sand layer which are sequentially arranged along the inner side surface of a crucible mold towards the axis of the crucible mold, and the median particle sizes of the first quartz sand layer, the second quartz sand layer and the third quartz sand layer are sequentially reduced.
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CN115110145B (en) * 2022-06-23 2023-09-29 宁夏盾源聚芯半导体科技股份有限公司 Oxygen increasing quartz crucible for crystal silicon lifting and preparation equipment and method thereof
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