CN109112613B - Preparation process of quartz crucible - Google Patents

Preparation process of quartz crucible Download PDF

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CN109112613B
CN109112613B CN201710483566.8A CN201710483566A CN109112613B CN 109112613 B CN109112613 B CN 109112613B CN 201710483566 A CN201710483566 A CN 201710483566A CN 109112613 B CN109112613 B CN 109112613B
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melting
layer
crucible
bubble
quartz crucible
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CN109112613A (en
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杜兴林
祝立君
于宏宇
章北铭
刘应龙
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Inner Mongolia Ojing Quartz Co ltd
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Inner Mongolia Ojing Quartz Co ltd
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    • 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)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a novel quartz crucible preparation process, which comprises the following steps: (1) preparing raw materials, (2) debugging before prefabrication, (3) prefabricating, (4) debugging before melting, and (5) melting. The invention has the advantages that by controlling the opening and closing of the vacuum valve and the melting condition in the melting process, the bubble composite layer with more micro-bubble content is clamped between the transparent layer with less micro-bubble content and the thin bubble outer layer, thereby not only ensuring the uniform radiation of a heat source of the quartz crucible during the crystal pulling work, but also ensuring that the bubbles in the bubble composite layer do not expand and crack in the crystal pulling process, reducing the reaction between the bubbles on the outer surface of the quartz crucible and the graphite crucible after expansion and cracking during the long-time crystal pulling work, delaying the time of forming a crystallization layer after the reaction of the bubbles and the graphite crucible, prolonging the service life of the quartz crucible, increasing the service life of the quartz crucible to 190 hours, prolonging the service life of the quartz crucible by more than 90 hours compared with the service life of a conventional quartz crucible, and meeting the crystal pulling process.

Description

Preparation process of quartz crucible
The technical field is as follows:
the invention relates to a preparation process of a quartz crucible, in particular to a novel preparation process of a quartz crucible.
Background art:
the quartz crucible is essential basic equipment in the pulling process of monocrystalline silicon, the conventional arc quartz crucible for pulling the monocrystalline consists of an inner layer and an outer layer, the inner layer is a transparent layer, the proportion of the thickness of the inner layer in the wall thickness of the crucible is about 1/3, and the content of bubbles is lower; the outer layer is a bubble composite layer, the ratio of the thickness of the bubble composite layer in the crucible wall thickness is about 2/3, the bubble content is high, and the bubble composite layer is a part for supporting the deformation strength of the crucible and ensuring the uniform radiation of a heat source.
The single crystal silicon melting and drawing are carried out in a graphite thermal field, the temperature of the graphite thermal field is as high as 1600 ℃, bubbles at the outer layer of the quartz crucible can expand and crack in the process of long-time and high-temperature use, liquid and other impurities released in the cracked bubbles and the inner surface of the quartz crucible generate chemical reaction, so that a crystallization layer is formed on the outer wall of the quartz crucible, the crystallization layer gradually becomes thicker along with the increase of crystal pulling time, the crystallization layer becomes thicker along with the increase of the crystal pulling time, the deformation resistance and the heat radiation efficiency of the quartz crucible are gradually reduced, and finally the abnormal rate of crystal pulling is increased and the crystallization rate is reduced. At present, the service life of a conventional quartz crucible can only be controlled to be less than or equal to 100 hours, only 1 to 2 single crystal rods can be pulled, and the requirement of a crystal pulling process for pulling at least 3 to 4 single crystal rods cannot be met.
At present, in order to prevent the reduction of the deformation resistance and the heat radiation efficiency of the quartz crucible caused by the expansion and the rupture of bubbles of a bubble composite layer of the quartz crucible in the crystal pulling working process, and finally the increase of the abnormal rate and the reduction of the crystal forming rate of crystal pulling, the inner wall and the outer wall of the quartz crucible are generally provided with coatings to prevent the bubbles from escaping and reacting with the inner surface of the quartz crucible, and the deformation resistance and the heat radiation efficiency of the quartz crucible are improved; however, in the process of transporting and loading silicon materials, the coating is easy to peel off under the action of external force, the using effect is not good, and simultaneously the crystal pulling quality is easy to be influenced.
The invention content is as follows:
the invention aims to provide a novel quartz crucible preparation process which has long service life and can ensure the crystal pulling quality.
The invention is implemented by the following technical scheme: the novel quartz crucible preparation process comprises the following steps: (1) preparing raw materials, (2) debugging before prefabrication, (3) prefabricating, (4) debugging before melting, and (5) melting; through controlling the opening and closing of the vacuum valve of the melting furnace and the melting conditions in the melting process in step (5), the novel quartz crucible prepared after the melting process in step (5) sequentially comprises a composite inner layer and a thin bubble outer layer from inside to outside, the composite inner layer sequentially comprises a transparent layer and a bubble composite layer from inside to outside, and the content of micro bubbles contained in the transparent layer and the thin bubble outer layer is smaller than that of the bubble composite layer.
Further, the bubble content of the transparent layer and the outer layer of the thin bubbles is less than that of the bubble composite layer, and the number of the microbubbles contained in the transparent layer is 11-15/mm3The micro-bubbles contained in the bubble composite layer are 35-55/mm3The outer layer of the thin bubble contains 10-12 micro-bubbles/mm3。
Further, the method comprises the following steps:
preparing raw materials: weighing quartz sand which is qualified in quality inspection, meets production requirements and has specified quality;
debugging before prefabrication (2): after the raw material preparation is finished, mounting a crucible mold and an outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position where an included angle between an axis of the crucible mold and a horizontal plane is 60-95 degrees, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 55-130 r/min;
the step (3) is carried out: after debugging is finished before prefabrication in the step (2), placing the quartz sand in the crucible mold, and prefabricating a pot blank by using a forming rod according with the material layer radius of the quartz sand;
and (4) debugging before melting: after the prefabrication in the step (3) is finished, adjusting the crucible mold filled with the quartz sand to a position where the included angle between the axis of the crucible mold and the horizontal direction is 96-100 degrees, and placing the crucible mold into a melting furnace so that the crucible mold is positioned below the three high-purity graphite electrodes and is coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to enable the distance between a heat insulation plate of the heat insulation system and a mold opening of the crucible mold to be 50-250 mm; then, respectively installing clamps on the three high-purity graphite electrodes in the melting furnace, and adjusting the positions of the high-purity graphite electrodes to enable the distance between the lower end of each high-purity graphite electrode and the die opening to be 5-275 mm; finally, switching on a power supply of the melting furnace to generate plasma arcs among the lower ends of the three high-purity graphite electrodes;
the melting method (5) specifically comprises the following steps:
step A, melting an inner layer: opening the vacuum valve of the melting furnace to enable the vacuum degree in the melting furnace to be-0.03 Mpa to-0.09 Mpa, and melting for 1-9 min at the power of 300 KW-2000 KW;
b, melting the intermediate layer: after the melting of the inner layer is finished, closing the vacuum valve, and melting for 4-20 min at the power of 350-1850 KW;
step C, outer layer melting: and B, after the melting of the middle layer is finished, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.052 Mpa to-0.076 Mpa, and finishing the melting for 1-12 min by using 380-1800 KW power to obtain the novel quartz crucible.
Furthermore, the total content of impurities in the natural quartz sand is less than or equal to 20ppm, and the quartz sand with the particle size of less than or equal to 150 mu m in unit weight accounts for 15%.
The invention has the advantages that: the novel quartz crucible is of a three-layer structure by controlling the opening and closing of a vacuum valve and the melting conditions in the melting process, and a bubble composite layer with high micro-bubble content is clamped between a transparent layer with low micro-bubble content and a thin bubble outer layer, so that the uniform radiation of a heat source of the quartz crucible during crystal pulling work is ensured, the normal operation of crystal pulling is ensured, and the quality of pulled monocrystalline silicon is stable; the method also ensures that the bubbles in the bubble composite layer do not expand and crack in the crystal pulling process, reduces the reaction between the outer surface of the quartz crucible and the graphite crucible after the bubbles expand and crack during long-time crystal pulling work, delays the time for forming a crystallization layer after the reaction between the outer surface of the quartz crucible and the graphite crucible, prolongs the service life of the quartz crucible, increases the service life of the quartz crucible to 190 hours, prolongs the service life of the quartz crucible by more than 90 hours compared with the service life of the conventional quartz crucible, and can meet the crystal pulling process requirement of pulling at least 3-4 single crystal rods.
Description of the drawings:
FIG. 1 is a schematic view showing the structure of a novel quartz crucible of the present invention.
The composite inner layer 1, the transparent layer 1-1, the bubble composite layer 1-2 and the thin bubble outer layer 2.
The specific implementation mode is as follows:
example 1:
as shown in FIG. 1, the novel quartz crucible preparation process, which prepares a novel quartz crucible with a size of 20 inches, specifically comprises the following steps:
(1) preparing raw materials: weighing 20.5kg of quartz sand which is qualified in quality inspection and meets the production requirement, wherein the sum of the impurity contents of the natural quartz sand is less than or equal to 20ppm, and the quartz sand with the particle size of less than or equal to 150 mu m in unit weight accounts for 15 percent;
(2) debugging before prefabrication: (1) after the preparation of the raw materials is finished, mounting the crucible mold and the outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position with an included angle of 60 degrees between the axis of the crucible mold and the horizontal plane, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 82 r/min;
(3) prefabrication: (2) after debugging is finished before prefabrication, quartz sand is placed in a crucible mold, a molding rod which is in accordance with the radius of a material layer of the quartz sand is used, the radius of the molding rod is 235mm, and a pot blank is prefabricated by the quartz sand;
(4) debugging before melting: (3) after prefabrication, adjusting a crucible mold filled with quartz sand to a position where the included angle between the axis of the crucible mold and the horizontal direction is 96 degrees, and putting the crucible mold into a melting furnace, so that the crucible mold is positioned below the three high-purity graphite electrodes and is coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to ensure that the distance between the heat insulation plate of the heat insulation system and the mold opening of the crucible mold is 50 mm; then, respectively installing the clamps on three high-purity graphite electrodes in the melting furnace, and adjusting the positions of the high-purity graphite electrodes to enable the distance between the lower end of each high-purity graphite electrode and the opening of the die to be 5 mm; finally, a power supply of the melting furnace is switched on, so that plasma arcs are generated among the lower ends of the three high-purity graphite electrodes;
(5) the melting method specifically comprises the following steps:
step A, melting an inner layer: opening a vacuum valve of the melting furnace to enable the vacuum degree in the melting furnace to be-0.03 Mpa, and melting for 1min at the power of 300 KW;
b, melting the intermediate layer: step A, after the inner layer is melted, closing a vacuum valve, and melting for 4min at 350KW power;
step C, outer layer melting: and B, after the melting of the middle layer is finished, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.052 Mpa, and finishing the melting for 1min at 600KW to obtain the novel quartz crucible.
Controlling the opening and closing of a vacuum valve of a melting furnace in the melting process and the melting conditions in step (5), so that the novel quartz crucible prepared after the melting process in step (5) sequentially comprises a composite inner layer 1 and a thin bubble outer layer 2 from inside to outside, the composite inner layer 1 sequentially comprises a transparent layer 1-1 and a bubble composite layer 1-2 from inside to outside, and microbubbles contained in the transparent layer 1-1 are 11/mm3The bubble composite layer 1-2 contains microbubbles of35 pieces/mm3The thin bubble outer layer 2 contains 10 micro bubbles/mm3The content of micro bubbles in the transparent layer 1-1 and the thin bubble outer layer 2 is less than that in the bubble composite layer 1-2, and the thickness of the thin bubble outer layer 2 is 0.5 mm.
Compared with the conventional quartz crucible, the structure, the thickness, the impurity content and the like of the transparent layer 1-1 part of the quartz crucible are not changed, and the sum of the thicknesses of the bubble composite layer 1-2 and the thin bubble outer layer 2 is equivalent to the thickness of the bubble composite layer 1-2 of the conventional quartz crucible; in the process of pulling the single crystal, the inner surfaces of the transparent layers 1-1 of the quartz crucible and the conventional quartz crucible are in direct contact with the silicon liquid, so that the pulling process of the embodiment is the same as that of the conventional quartz crucible, the pulling operation can be normally carried out, and the quality of the pulled monocrystalline silicon is consistent with that of the monocrystalline silicon pulled by the conventional quartz crucible. Meanwhile, the bubble composite layer 1-2 with more micro-bubble content is clamped between the transparent layer 1-1 with less micro-bubble content and the thin bubble outer layer 2, so that the uniform radiation of a heat source during the crystal pulling work of the embodiment is ensured, the bubbles in the bubble composite layer 1-2 are prevented from expanding and cracking during the crystal pulling process, the reaction between the bubbles on the outer surface of the embodiment and a graphite crucible after expansion and cracking during the long-time crystal pulling work is reduced, the time for forming a crystallization layer after the reaction between the bubbles and the graphite crucible is delayed, the service life of the embodiment is prolonged to 190 hours, the service life of the embodiment is prolonged by more than 90 hours compared with that of a conventional quartz crucible, and the crystal pulling process requirement for pulling at least 3.
Example 2:
as shown in FIG. 1, the novel quartz crucible preparation process, which prepares a novel quartz crucible with a size of 22 inches, comprises the following steps:
(1) preparing raw materials: weighing 29.5kg of quartz sand which is qualified in quality inspection and meets production requirements, wherein the sum of the impurity contents of the natural quartz sand is less than or equal to 20ppm, and the quartz sand with the particle size of less than or equal to 150 mu m in unit weight accounts for 15%;
(2) debugging before prefabrication: (1) after the preparation of the raw materials is finished, mounting the crucible mold and the outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position with an included angle of 72 degrees between the axis of the crucible mold and the horizontal plane, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 80 r/min;
(3) prefabrication: (2) after debugging is finished before prefabrication, quartz sand is placed in a crucible mold, a molding rod which is in accordance with the radius of a material layer of the quartz sand is used, the radius of the molding rod is 260mm, and a pot blank is prefabricated by the quartz sand;
(4) debugging before melting: (3) after prefabrication, adjusting a crucible mold filled with quartz sand to a position where an included angle between the axis of the crucible mold and the horizontal direction is 97 degrees, and putting the crucible mold into a melting furnace to enable the crucible mold to be positioned below the three high-purity graphite electrodes and to be coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to ensure that the distance between the heat insulation plate of the heat insulation system and the mold opening of the crucible mold is 100 mm; then, respectively installing the clamps on three high-purity graphite electrodes in the melting furnace, and adjusting the positions of the high-purity graphite electrodes to enable the distance between the lower end of each high-purity graphite electrode and the opening of the die to be 80 mm; finally, a power supply of the melting furnace is switched on, so that plasma arcs are generated among the lower ends of the three high-purity graphite electrodes;
(5) the melting method specifically comprises the following steps:
step A, melting an inner layer: opening a vacuum valve of the melting furnace to enable the vacuum degree in the melting furnace to be-0.05 Mpa, and melting for 3min at the power of 800 KW;
b, melting the intermediate layer: step A, after the inner layer is melted, closing a vacuum valve, and melting for 8min at the power of 1000 KW;
step C, outer layer melting: and step B, after the melting of the middle layer is finished, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.059 Mpa, and finishing the melting for 4min at 700KW to obtain the novel quartz crucible.
Controlling the opening and closing of a vacuum valve of a melting furnace in the melting process and the melting conditions in step (5), so that the novel quartz crucible prepared after the melting process in step (5) sequentially comprises a composite inner layer 1 and a thin bubble outer layer 2 from inside to outside, the composite inner layer 1 sequentially comprises a transparent layer 1-1 and a bubble composite layer 1-2 from inside to outside, and microbubbles contained in the transparent layer 1-1 are 13/mm3The number of micro bubbles contained in the bubble composite layer 1-2 is 39/mm3The outer layer 2 of thin bubbles contains 11 micro bubbles/mm3Is transparentThe micro-bubble content of the layer 1-1 and the thin bubble outer layer 2 is less than that of the bubble composite layer 1-2, and the thickness of the thin bubble outer layer 2 is 1 mm.
Compared with the conventional quartz crucible, the structure, the thickness, the impurity content and the like of the transparent layer 1-1 part of the quartz crucible are not changed, and the sum of the thicknesses of the bubble composite layer 1-2 and the thin bubble outer layer 2 is equivalent to the thickness of the bubble composite layer 1-2 of the conventional quartz crucible; in the process of pulling the single crystal, the inner surfaces of the transparent layers 1-1 of the quartz crucible and the conventional quartz crucible are in direct contact with the silicon liquid, so that the pulling process of the embodiment is the same as that of the conventional quartz crucible, the pulling operation can be normally carried out, and the quality of the pulled monocrystalline silicon is consistent with that of the monocrystalline silicon pulled by the conventional quartz crucible. Meanwhile, the bubble composite layer 1-2 with more micro-bubble content is clamped between the transparent layer 1-1 with less micro-bubble content and the thin bubble outer layer 2, so that the uniform radiation of a heat source during the crystal pulling work of the embodiment is ensured, the bubbles in the bubble composite layer 1-2 are prevented from expanding and cracking during the crystal pulling process, the reaction between the bubbles on the outer surface of the embodiment and a graphite crucible after expansion and cracking during the long-time crystal pulling work is reduced, the time for forming a crystallization layer after the reaction between the bubbles and the graphite crucible is delayed, the service life of the embodiment is prolonged to 190 hours, the service life of the embodiment is prolonged by more than 90 hours compared with that of a conventional quartz crucible, and the crystal pulling process requirement for pulling at least 3.
Example 3:
as shown in FIG. 1, the novel quartz crucible preparation process, which prepares a novel quartz crucible with a size of 24 inches, comprises the following steps:
(1) preparing raw materials: weighing 37.5kg of quartz sand which is qualified in quality inspection and meets production requirements, wherein the sum of the impurity contents of the natural quartz sand is less than or equal to 20ppm, and the quartz sand with the particle size of less than or equal to 150 mu m in unit weight accounts for 15%;
(2) debugging before prefabrication: (1) after the preparation of the raw materials is finished, mounting the crucible mold and the outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position with an included angle of 84 degrees between the axis of the crucible mold and the horizontal plane, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 76 r/min;
(3) prefabrication: (2) after debugging is completed before prefabrication, quartz sand is placed in a crucible mold, a molding rod which is in accordance with the radius of a material layer of the quartz sand is used, the radius of the molding rod is 285mm, and a pot blank is prefabricated by the quartz sand;
(4) debugging before melting: (3) after prefabrication is finished, adjusting a crucible mold filled with quartz sand to a position where an included angle between the axis of the crucible mold and the horizontal direction is 99 degrees, and putting the crucible mold into a melting furnace to enable the crucible mold to be positioned below the three high-purity graphite electrodes and to be coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to ensure that the distance between the heat insulation plate of the heat insulation system and the mold opening of the crucible mold is 140 mm; then, respectively installing the clamps on three high-purity graphite electrodes in the melting furnace, and adjusting the positions of the high-purity graphite electrodes to enable the distance between the lower end of each high-purity graphite electrode and the opening of the die to be 192 mm; finally, a power supply of the melting furnace is switched on, so that plasma arcs are generated among the lower ends of the three high-purity graphite electrodes;
(5) the melting method specifically comprises the following steps:
step A, melting an inner layer: opening a vacuum valve of the melting furnace to enable the vacuum degree in the melting furnace to be-0.07 Mpa, and melting for 7min at 1500KW power;
b, melting the intermediate layer: step A, after the inner layer is melted, closing a vacuum valve, and melting for 16min at 1350KW power;
step C, outer layer melting: and step B, after the melting of the middle layer is finished, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.064 Mpa, and finishing the melting for 8min at 800KW to obtain the novel quartz crucible.
Controlling the opening and closing of a vacuum valve of a melting furnace in the melting process and the melting conditions in step (5), so that the novel quartz crucible prepared after the melting process in step (5) sequentially comprises a composite inner layer 1 and a thin bubble outer layer 2 from inside to outside, the composite inner layer 1 sequentially comprises a transparent layer 1-1 and a bubble composite layer 1-2 from inside to outside, and microbubbles contained in the transparent layer 1-1 are 14/mm3The number of microbubbles contained in the bubble composite layer 1-2 is 42/mm3The thin bubble outer layer 2 contains 14 micro bubbles/mm3The content of micro bubbles in the transparent layer 1-1 and the thin bubble outer layer 2 is less than that in the bubble composite layer 1-2, and the thin bubblesThe thickness of the outer layer 2 is 2 mm.
Compared with the conventional quartz crucible, the structure, the thickness, the impurity content and the like of the transparent layer 1-1 part of the quartz crucible are not changed, and the sum of the thicknesses of the bubble composite layer 1-2 and the thin bubble outer layer 2 is equivalent to the thickness of the bubble composite layer 1-2 of the conventional quartz crucible; in the process of pulling the single crystal, the inner surfaces of the transparent layers 1-1 of the quartz crucible and the conventional quartz crucible are in direct contact with the silicon liquid, so that the pulling process of the embodiment is the same as that of the conventional quartz crucible, the pulling operation can be normally carried out, and the quality of the pulled monocrystalline silicon is consistent with that of the monocrystalline silicon pulled by the conventional quartz crucible. Meanwhile, the bubble composite layer 1-2 with more micro-bubble content is clamped between the transparent layer 1-1 with less micro-bubble content and the thin bubble outer layer 2, so that the uniform radiation of a heat source during the crystal pulling work of the embodiment is ensured, the bubbles in the bubble composite layer 1-2 are prevented from expanding and cracking during the crystal pulling process, the reaction between the bubbles on the outer surface of the embodiment and a graphite crucible after expansion and cracking during the long-time crystal pulling work is reduced, the time for forming a crystallization layer after the reaction between the bubbles and the graphite crucible is delayed, the service life of the embodiment is prolonged to 190 hours, the service life of the embodiment is prolonged by more than 90 hours compared with that of a conventional quartz crucible, and the crystal pulling process requirement for pulling at least 3.
Example 4:
as shown in FIG. 1, the novel quartz crucible preparation process, which prepares a novel quartz crucible with a size of 26 inches, comprises the following steps:
(1) preparing raw materials: weighing 45.5kg of quartz sand which is qualified in quality inspection and meets production requirements, wherein the sum of the impurity contents of the natural quartz sand is less than or equal to 20ppm, and the quartz sand with the particle size of less than or equal to 150 mu m in unit weight accounts for 15%;
(2) debugging before prefabrication: (1) after the preparation of the raw materials is finished, mounting the crucible mold and the outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position with an included angle of 95 degrees between the axis of the crucible mold and the horizontal plane, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 72 r/min;
(3) prefabrication: (2) after debugging is finished before prefabrication, quartz sand is placed in a crucible mold, a molding rod which is in accordance with the radius of a material layer of the quartz sand is used, the radius of the molding rod is 310mm, and a pot blank is prefabricated by the quartz sand;
(4) debugging before melting: (3) after prefabrication is finished, adjusting a crucible mold filled with quartz sand to a position where an included angle between the axis of the crucible mold and the horizontal direction is 100 degrees, and putting the crucible mold into a melting furnace to enable the crucible mold to be positioned below the three high-purity graphite electrodes and to be coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to enable the distance between the heat insulation plate of the heat insulation system and the mold opening of the crucible mold to be 250 mm; then, the clamps are respectively arranged on three high-purity graphite electrodes in the melting furnace, and the positions of the high-purity graphite electrodes are adjusted to ensure that the distance between the lower end of each high-purity graphite electrode and the opening of the die is 275 mm; finally, a power supply of the melting furnace is switched on, so that plasma arcs are generated among the lower ends of the three high-purity graphite electrodes;
(5) the melting method specifically comprises the following steps:
step A, melting an inner layer: starting a vacuum valve of the melting furnace to ensure that the vacuum degree in the melting furnace is-0.09 Mpa, and melting for 9min at the power of 2000 KW;
b, melting the intermediate layer: step A, after the melting of the inner layer is finished, closing a vacuum valve, and melting for 20min at 1850KW power;
step C, outer layer melting: b, after the melting of the middle layer is finished, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.076 Mpa, and finishing the melting for 12min at 900KW to obtain a novel quartz crucible;
controlling the opening and closing of a vacuum valve of a melting furnace in the melting process and the melting conditions in step (5), so that the novel quartz crucible prepared after the melting process in step (5) sequentially comprises a composite inner layer 1 and a thin bubble outer layer 2 from inside to outside, the composite inner layer 1 sequentially comprises a transparent layer 1-1 and a bubble composite layer 1-2 from inside to outside, and microbubbles contained in the transparent layer 1-1 are 15/mm3The number of micro bubbles contained in the bubble composite layer 1-2 is 55/mm3The thin bubble outer layer 2 contains 15 micro bubbles/mm3The content of micro bubbles in the transparent layer 1-1 and the thin bubble outer layer 2 is less than that in the bubble composite layer 1-2, and the thickness of the thin bubble outer layer 2 is 3 mm.
Compared with the conventional quartz crucible, the structure, the thickness, the impurity content and the like of the transparent layer 1-1 part of the quartz crucible are not changed, and the sum of the thicknesses of the bubble composite layer 1-2 and the thin bubble outer layer 2 is equivalent to the thickness of the bubble composite layer 1-2 of the conventional quartz crucible; in the process of pulling the single crystal, the inner surfaces of the transparent layers 1-1 of the quartz crucible and the conventional quartz crucible are in direct contact with the silicon liquid, so that the pulling process of the embodiment is the same as that of the conventional quartz crucible, the pulling operation can be normally carried out, and the quality of the pulled monocrystalline silicon is consistent with that of the monocrystalline silicon pulled by the conventional quartz crucible. Meanwhile, the bubble composite layer 1-2 with more micro-bubble content is clamped between the transparent layer 1-1 with less micro-bubble content and the thin bubble outer layer 2, so that the uniform radiation of a heat source during the crystal pulling work of the embodiment is ensured, the bubbles in the bubble composite layer 1-2 are prevented from expanding and cracking during the crystal pulling process, the reaction between the bubbles on the outer surface of the embodiment and a graphite crucible after expansion and cracking during the long-time crystal pulling work is reduced, the time for forming a crystallization layer after the reaction between the bubbles and the graphite crucible is delayed, the service life of the embodiment is prolonged to 190 hours, the service life of the embodiment is prolonged by more than 90 hours compared with that of a conventional quartz crucible, and the crystal pulling process requirement for pulling at least 3.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (3)

1. The preparation method of the quartz crucible comprises the following steps: (1) preparing raw materials, (2) debugging before prefabrication, (3) prefabricating, (4) debugging before melting, and (5) melting; the method is characterized in that the opening and closing of a vacuum valve of a melting furnace in the melting process (5) and the melting conditions are controlled, so that the quartz crucible prepared after the melting process (5) sequentially comprises a composite inner layer and a thin bubble outer layer from inside to outside, the composite inner layer sequentially comprises a transparent layer and a bubble composite layer from inside to outside, the content of micro bubbles contained in the transparent layer and the thin bubble outer layer is less than that of the bubble composite layer, and the number of the micro bubbles contained in the transparent layer is 11-15/mm3The micro-bubbles contained in the bubble composite layer are 35-55/mm3The outer layer of the thin bubble contains 10-12 micro-bubbles/mm3；
The melting method (5) specifically comprises the following steps:
step A, melting an inner layer: opening the vacuum valve of the melting furnace to enable the vacuum degree in the melting furnace to be-0.03 Mpa to-0.09 Mpa, and melting for 1-9 min at the power of 300 KW-2000 KW;
b, melting the intermediate layer: after the melting of the inner layer is finished, closing the vacuum valve, and melting for 4-20 min at the power of 350-1850 KW;
step C, outer layer melting: and B, after the middle layer is melted, opening the vacuum valve again to enable the vacuum degree in the melting furnace to be-0.052 Mpa to-0.076 Mpa, and melting for 1-12 min at 380-1800 KW to obtain the quartz crucible.
2. The method for producing a quartz crucible according to claim 1, characterized by comprising the steps of:
preparing raw materials: weighing quartz sand which is qualified in quality inspection, meets production requirements and has specified quality;
debugging before prefabrication (2): after the raw material preparation is finished, mounting a crucible mold and an outer sleeve thereof on a rotating shaft, enabling the crucible mold to be inclined to a position where an included angle between an axis of the crucible mold and a horizontal plane is 60-95 degrees, and then starting the rotating shaft to enable the rotating speed of the crucible mold to be 55-130 r/min;
the step (3) is carried out: after debugging is finished before prefabrication in the step (2), placing the quartz sand in the crucible mold, and prefabricating a pot blank by using a forming rod according with the material layer radius of the quartz sand;
and (4) debugging before melting: after the prefabrication in the step (3) is finished, adjusting the crucible mold filled with the quartz sand to a position where the included angle between the axis of the crucible mold and the horizontal direction is 96-100 degrees, and placing the crucible mold into a melting furnace so that the crucible mold is positioned below the three high-purity graphite electrodes and is coaxial with the three high-purity graphite electrodes; then, adjusting the distance between a heat insulation system of the melting furnace and the crucible mold to enable the distance between a heat insulation plate of the heat insulation system and a mold opening of the crucible mold to be 50-250 mm; then, respectively installing clamps on the three high-purity graphite electrodes in the melting furnace, and adjusting the positions of the high-purity graphite electrodes to enable the distance between the lower end of each high-purity graphite electrode and the die opening to be 5-275 mm; and finally, switching on a power supply of the melting furnace to generate plasma arcs among the lower ends of the three high-purity graphite electrodes.
3. The method of claim 2, wherein the natural silica sand has a total impurity content of 20ppm or less and a silica sand content of 15% or less having a particle size of 150 μm or less per unit weight.
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CN113735421A (en) * 2020-05-28 2021-12-03 隆基绿能科技股份有限公司 Quartz crucible manufacturing method and forming device
CN112144115B (en) * 2020-09-21 2022-02-08 无锡市尚领石英科技有限公司 Quartz crucible with long service life and low deformation rate and preparation method thereof
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CN115246704A (en) * 2021-04-27 2022-10-28 新沂市中鑫光电科技有限公司 Method for eliminating impurity elements in transparent layer of quartz crucible
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1162027A (en) * 1996-02-06 1997-10-15 三菱麻铁里亚尔硅材料株式会社 Single crystal drawing device
CN104150755A (en) * 2014-08-07 2014-11-19 南通路博石英材料有限公司 Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof
WO2016017055A1 (en) * 2014-07-31 2016-02-04 信越石英株式会社 Quartz glass crucible for single crystal silicon pulling and method for producing same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1162027A (en) * 1996-02-06 1997-10-15 三菱麻铁里亚尔硅材料株式会社 Single crystal drawing device
WO2016017055A1 (en) * 2014-07-31 2016-02-04 信越石英株式会社 Quartz glass crucible for single crystal silicon pulling and method for producing same
CN106574394A (en) * 2014-07-31 2017-04-19 信越石英株式会社 Quartz glass crucible for single crystal silicon pulling and method for producing same
CN104150755A (en) * 2014-08-07 2014-11-19 南通路博石英材料有限公司 Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof

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