CN110592664A - Process method for prolonging service life of quartz crucible for silicon single crystal - Google Patents

Process method for prolonging service life of quartz crucible for silicon single crystal Download PDF

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Publication number
CN110592664A
CN110592664A CN201910966327.7A CN201910966327A CN110592664A CN 110592664 A CN110592664 A CN 110592664A CN 201910966327 A CN201910966327 A CN 201910966327A CN 110592664 A CN110592664 A CN 110592664A
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CN
China
Prior art keywords
quartz crucible
aluminum hydroxide
single crystal
silicon single
silicon
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Pending
Application number
CN201910966327.7A
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Chinese (zh)
Inventor
赵国伟
徐强
高润飞
王林
谷守伟
***
周泽
杨志
吴树飞
刘振宇
王鑫
刘学
皇甫亚楠
杨瑞峰
郭志荣
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Inner Mongolia Zhonghuan Solar Material Co Ltd
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Inner Mongolia Zhonghuan Solar Material Co Ltd
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Priority to CN201910966327.7A priority Critical patent/CN110592664A/en
Publication of CN110592664A publication Critical patent/CN110592664A/en
Pending legal-status Critical Current

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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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  • Chemical & Material Sciences (AREA)
  • 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 provides a process method for prolonging the service life of a quartz crucible for silicon single crystals. The method has the advantages of adding the aluminum hydroxide, accelerating the conversion of the quartz crucible to a stable alpha-cristobalite structure, supplementing the fallen crystallization layer, reducing the corrosion of a silicon solution to the quartz crucible, prolonging the service life of the quartz crucible, and reducing cost and improving efficiency.

Description

Process method for prolonging service life of quartz crucible for silicon single crystal
Technical Field
The invention belongs to the technical field of photovoltaics, and particularly relates to a process method for prolonging the service life of a quartz crucible for silicon single crystals.
Background
The prior quartz crucible for silicon single crystal can only pull 2-3 single crystals generally, has short service life and can not meet the requirement of continuously using the pulling sheet.
Since silicon has high chemical activity in a molten state, it reacts with the quartz crucible, i.e., SiO2+ Si → 2SiO, and irreversibly damages the transparent layer of the quartz crucible, affecting the service life of the quartz crucible.
In the prior art, barium carbonate aqueous solution is sprayed on the inner wall of a crucible to accelerate the crystallization of the crucible, the crystallization of the crucible is serious in the later period of operation of the method, cristobalite on the inner wall can fall off, so that silicon single crystals are difficult to crystallize, the service life is short, and the use requirement cannot be met.
Disclosure of Invention
In view of the above problems, the present invention provides a process for prolonging the service life of a quartz crucible for silicon single crystal, which is applied to the process of pulling the silicon single crystal, wherein aluminum hydroxide is added to accelerate the transformation of the quartz crucible to a stable alpha-cristobalite structure, supplement a dropped crystallization layer, reduce the corrosion of silicon solution to the quartz crucible, prolong the service life of the quartz crucible, and reduce the cost and improve the effect.
In order to solve the technical problems, the invention adopts the technical scheme that: a process for prolonging the service life of a quartz crucible for silicon single crystal comprises adding a certain amount of aluminum hydroxide to the crucible during charging of Czochralski single crystal to promote the transformation of the crucible to an alpha-cristobalite structure.
Further, the amount of aluminum hydroxide is 0.1g to 1 g.
Further, the calculation of the dosage of the aluminum hydroxide comprises the following steps:
determining the mole fraction of aluminum oxide;
calculating the number of silicon atoms;
calculating the mole number of silicon atoms;
calculating the molar mass of the aluminum hydroxide;
the mass of the aluminum hydroxide was calculated.
Further, the mole fraction of the aluminum oxide is determined according to the liquid phase immiscible glass phase of the aluminum oxide system, and the mole fraction of the aluminum oxide is 15%.
Further, the number of silicon atoms is calculated by multiplying the thickness of the alpha-cristobalite by the number of atoms per unit area of nanometers.
Further, the thickness of the alpha-cristobalite is 30 to 200 nm.
Further, the number of moles of silicon atoms in the number of moles of silicon atoms is calculated to be naThen, then
Wherein n is avogalois constant, n is 6.02 × 1023。
Further, the molar mass of aluminum hydroxide in the molar mass of aluminum hydroxide is calculated to be nbThen, then
According to
The molar mass of the aluminium hydroxide is calculated.
Further, the mass of the aluminum hydroxide is calculated as the molar mass of the aluminum hydroxide multiplied by the relative molecular mass of the aluminum hydroxide.
By adopting the technical scheme, aluminum hydroxide powder is added in the charging process, and aluminum oxide generated at high temperature can be used as a nucleating agent, so that the conversion of the quartz crucible to a stable alpha-cristobalite structure is accelerated, the fallen crystallization layers are supplemented, and finally the quartz crucible meets the requirement of pulling a plurality of single crystals, the crystallization rate of the quartz crucible can be accelerated, the corrosion of silicon solution to the quartz crucible is reduced, the service life of the quartz crucible is prolonged, the pulling of the single crystals is prevented from being influenced after the quartz crucible is corroded, the number of the single-furnace silicon single crystal pulling of the quartz crucible is increased, and the cost reduction and the efficiency improvement are realized.
Detailed Description
The present invention will be further described with reference to the following examples.
The embodiment relates to a method for prolonging the service life of a quartz crucible for monocrystalline silicon, which is applied to the process of pulling the monocrystalline silicon, aluminum hydroxide is added in the charging process of the monocrystalline silicon, the nucleating agent is prepared according to the characteristic that the aluminum hydroxide can be decomposed into aluminum oxide at high temperature, and under the action of the nucleating agent, alpha-cristobalite separated from the inner wall of the quartz crucible in the process of pulling the monocrystalline silicon is supplemented, so that the density of the contact part of the inner wall of the quartz crucible and a silicon solution is increased, the corrosion resistance of the crucible is improved, and the service life of the quartz crucible is prolonged.
In the Czochralski single crystal pulling, a certain amount of aluminum hydroxide is added during charging to promote the conversion of the quartz crucible to the α -cristobalite structure, that is, at the beginning of charging of the Czochralski single crystal, a certain amount of aluminum hydroxide is charged into the quartz crucible along with the silicon raw material, the aluminum hydroxide is a white amorphous powder, hardly soluble in water, and is decomposed by heating, and the reaction is as follows:
as can be seen from the above reaction, the aluminum hydroxide forms γ -Al at 140 deg.C2O3；
γ-Al2O3At high temperature of about 1200 ℃, alpha-Al can be formed2O3The reaction process is as follows:
it can thus be concluded that gamma-Al can be utilized2O3Formation of alpha-Al by crystal orientation transformation at high temperature2O3，α-Al2O3The crystallization of the quartz crucible is promoted, the quartz crucible is promoted to be converted to a stable alpha-cristobalite structure, the fallen alpha-cristobalite is filled, the alpha-cristobalite is compact and strong in corrosion resistance, the contact of a silicon solution on the inner wall of the quartz crucible is reduced, and the service life of the quartz crucible is prolonged.
The amount of the aluminum hydroxide is 0.1-1g, and is selected according to actual calculation results.
The calculation of the dosage of the aluminum hydroxide comprises the following steps:
determining the mole fraction of aluminum oxide:
the mole fraction of the aluminum oxide is determined according to the immiscible glass phase of the liquid phase of the aluminum oxide system, and the mole fraction of the aluminum oxide is 15 percent according to the immiscible glass phase of the liquid phase of the aluminum oxide system.
Calculating the number of silicon atoms:
the number of silicon atoms is calculated according to the thickness of the alpha-cristobalite multiplied by the number of atoms in unit nanometer area, the thickness of the alpha-cristobalite is 30-200nm, and the alpha-cristobalite is selected according to actual requirements without specific requirements. For example:
setting the thickness of alpha-cristobalite as h and the number of atoms per nano area as nNumber of atoms per unit of nanometerThen number of silicon atoms
nNumber of silicon atoms＝h×nNumber of atoms per unit of nanometer
Wherein n isNumber of atoms per unit of nanometer＝7.79×1019And h is the thickness of alpha-cristobalite and is 30-200nm, and is selected according to actual requirements.
Calculating the mole number of silicon atoms:
when the number of moles of silicon atoms (the amount of substance of silicon atoms) is calculated, the number of moles of silicon atoms is set to naThen, then
Wherein n is avogalois constant, n is 6.02 × 1023。
Calculating the molar mass of aluminum hydroxide:
when calculating the molar mass of aluminum hydroxide, the molar mass of aluminum hydroxide is set to nbThen according to
Calculating the molar mass of the aluminum hydroxide, the molar mass of the aluminum hydroxide is
Calculating the mass of the aluminum hydroxide:
the mass of the aluminum hydroxide is calculated as the molar mass of the aluminum hydroxide multiplied by the relative molecular mass of the aluminum hydroxide, i.e., assuming that the mass of the aluminum hydroxide is m, m ═ nb×M。
The thickness of α -cristobalite is 100nm as an example.
Determining the mole fraction of aluminum oxide:
the mole fraction of the aluminum oxide is determined according to the immiscible glass phase of the liquid phase of the aluminum oxide system, and the mole fraction of the aluminum oxide is 15 percent according to the immiscible glass phase of the liquid phase of the aluminum oxide system.
Calculating the number of silicon atoms:
when the number of silicon atoms is calculated, the thickness of the alpha-cristobalite is set to be 100nm according to the thickness of the alpha-cristobalite multiplied by the number of atoms per unit nanometer areaHas a thickness of h and a number of atoms per unit area of nanometers of nNumber of atoms per unit of nanometerThen number of silicon atoms
nNumber of silicon atoms＝h×nNumber of atoms per unit of nanometer
Wherein n isNumber of atoms per unit of nanometer＝7.79×1019And h is 100, then
nNumber of silicon atoms＝h×nNumber of atoms per unit of nanometer＝7.79×1019×100＝7.79×1021An
That is, when the thickness of the α -cristobalite was 100nm, the number of silicon atoms was 7.79 × 1021And (4) respectively.
Calculating the mole number of silicon atoms:
in calculating the number of moles of silicon atoms, the number of moles of silicon atoms is set to naThen, then
Wherein n is avogalois constant, n is 6.02 × 1023。
From the above step, the number of silicon atoms was 7.79X1021The number of moles of silicon atoms (i.e., the amount of silicon atom species) is
Calculating the molar mass of aluminum hydroxide:
when calculating the molar mass of aluminum hydroxide, the molar mass of aluminum hydroxide is set to nbThen according to
Calculating the molar mass of the aluminum hydroxide, wherein the molar mass of the aluminum hydroxide is
Then the process of the first step is carried out,
that is, the molar mass of aluminum hydroxide is 2.27X10-3。
Calculating the mass of the aluminum hydroxide:
the mass of the aluminum hydroxide is calculated as the molar mass of the aluminum hydroxide multiplied by the relative molecular mass of the aluminum hydroxide, i.e., assuming that the mass of the aluminum hydroxide is m, m ═ nbX M, the molar mass of the aluminium hydroxide is known from the previous step, the mass of the aluminium hydroxide is calculated:
m＝nb×M＝1.76×10-3×78＝0.14g
by adopting the technical scheme, aluminum hydroxide powder is added in the charging process, and the aluminum oxide generated at high temperature can be used as a nucleating agent, so that the conversion of the quartz crucible to a stable alpha-cristobalite structure is accelerated, the fallen crystallization layers are supplemented, and finally the quartz crucible meets the requirement of pulling a plurality of single crystals, the crystallization rate of the quartz crucible can be accelerated, the corrosion of silicon solution to the quartz crucible is reduced, the service life of the quartz crucible is prolonged, the single crystal pulling is prevented from being influenced after the quartz crucible is corroded, the number of the single-furnace silicon single crystal pulling of the quartz crucible is increased, and the cost reduction and the efficiency improvement are realized.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (9)

1. A process for prolonging the service life of a quartz crucible for silicon single crystal is characterized in that: during the charging process of pulling up a single crystal, a certain amount of aluminum hydroxide is added to promote the conversion of the quartz crucible to an alpha-cristobalite structure.
2. The process for prolonging the life of a quartz crucible for a silicon single crystal according to claim 1, wherein: the dosage of the aluminum hydroxide is 0.1g-1 g.
3. The process for improving the lifetime of a quartz crucible for a silicon single crystal according to claim 1 or 2, wherein: the calculation of the dosage of the aluminum hydroxide comprises the following steps:
determining the mole fraction of aluminum oxide;
calculating the number of silicon atoms;
calculating the mole number of silicon atoms;
calculating the molar mass of the aluminum hydroxide;
the mass of the aluminum hydroxide was calculated.
4. The process for prolonging the life of a quartz crucible for a silicon single crystal according to claim 3, wherein: the determined mole fraction of the aluminum oxide is determined according to the liquid-phase immiscible glass phase of an aluminum oxide system, and the mole fraction of the aluminum oxide is 15%.
5. The process for prolonging the life of a quartz crucible for a silicon single crystal according to claim 4, wherein: and the number of the silicon atoms is calculated by multiplying the thickness of the alpha-cristobalite by the number of atoms in unit nanometer area.
6. The process for prolonging the life of a quartz crucible for a silicon single crystal according to claim 5, wherein: the thickness of the alpha-cristobalite is 30-200 nm.
7. The process for improving the lifetime of a quartz crucible for a silicon single crystal according to claim 5 or 6, wherein: the number of moles of silicon atoms in the calculated number of moles of silicon atoms is naThen, then
Wherein n is avogalois constant, n is 6.02 × 1023。
8. The process for improving the life of a quartz crucible for a silicon single crystal according to claim 7, wherein: the molar mass of the aluminum hydroxide in the calculated molar mass of the aluminum hydroxide is nbThen according to
Calculating the molar mass of the aluminum hydroxide.
9. The process for improving the life of a quartz crucible for a silicon single crystal according to claim 8, wherein: the calculated mass of aluminum hydroxide is the molar mass of the aluminum hydroxide multiplied by the relative molecular mass of the aluminum hydroxide.
CN201910966327.7A 2019-10-12 2019-10-12 Process method for prolonging service life of quartz crucible for silicon single crystal Pending CN110592664A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3621282B2 (en) * 1999-02-25 2005-02-16 東芝セラミックス株式会社 Quartz glass crucible and method for producing the same
CN101316953A (en) * 2005-11-29 2008-12-03 日本超精石英株式会社 Quartz glass crucible, process for producing the same, and use
EP2817269A1 (en) * 2012-02-22 2014-12-31 Schott Ag Transparent low-colour lithium aluminium silicate glass ceramic and the use thereof
CN109154102A (en) * 2016-03-23 2019-01-04 莫门蒂夫性能材料股份有限公司 Devitrification agent for quartz glass crucibles crystal growth technique
CN111320393A (en) * 2018-12-13 2020-06-23 阔斯泰公司 Quartz glass crucible and method for producing same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3621282B2 (en) * 1999-02-25 2005-02-16 東芝セラミックス株式会社 Quartz glass crucible and method for producing the same
CN101316953A (en) * 2005-11-29 2008-12-03 日本超精石英株式会社 Quartz glass crucible, process for producing the same, and use
EP2817269A1 (en) * 2012-02-22 2014-12-31 Schott Ag Transparent low-colour lithium aluminium silicate glass ceramic and the use thereof
CN109154102A (en) * 2016-03-23 2019-01-04 莫门蒂夫性能材料股份有限公司 Devitrification agent for quartz glass crucibles crystal growth technique
CN111320393A (en) * 2018-12-13 2020-06-23 阔斯泰公司 Quartz glass crucible and method for producing same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马世昌等: "《化学物质辞典》", 30 April 1999 *

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