CN108531980B - Improved quartz crucible and method for making same - Google Patents
Improved quartz crucible and method for making same Download PDFInfo
- Publication number
- CN108531980B CN108531980B CN201810526785.4A CN201810526785A CN108531980B CN 108531980 B CN108531980 B CN 108531980B CN 201810526785 A CN201810526785 A CN 201810526785A CN 108531980 B CN108531980 B CN 108531980B
- Authority
- CN
- China
- Prior art keywords
- quartz crucible
- crucible
- quartz
- barium hydroxide
- spraying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5024—Silicates
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to an improved quartz crucible and a manufacturing method thereof, belonging to the technical field of monocrystalline silicon manufacturing equipment, and the invention can increase the contact porosity of the quartz crucible and a graphite crucible by increasing the roughness of the outer surface of the quartz crucible, when the quartz crucible reacts with the graphite crucible at high temperature to generate gas, the gas can be led out through the pore between the quartz crucible and the graphite crucible, thereby avoiding the deformation of the quartz crucible, spraying barium hydroxide solution on the inner surface of the quartz crucible to react barium hydroxide with carbon dioxide in the air to generate barium carbonate, reacting the barium carbonate with the quartz crucible to generate barium silicate, inducing the inner surface of the quartz crucible by the barium silicate to generate a compact crystal cristobalite layer, because the crystal cristobalite has no softening point and high strength, the strength of the inner wall of the quartz crucible is improved, and the quartz crucible is prevented from deforming. The method can effectively reduce the deformation of the quartz crucible at high temperature, and is convenient to operate.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon manufacturing equipment, and particularly relates to an improved quartz crucible and a manufacturing method thereof.
Background
As one method for growing a silicon single crystal, a pulling method typified by a Czochralski method (CZ method) is generally used. The apparatus used herein generally has a quartz crucible for holding a raw material silicon melt, wherein the crucible is surrounded by a graphite crucible having an inner shape for supporting the quartz crucible and achieving uniform heating, and a heater for heating is disposed outside thereof. Both quartz and graphite crucibles are generally shaped to comprise a side wall of approximately cylindrical shape and a suitably radially chamfered bottom.
In the CZ method, a silicon raw material in a quartz crucible is heated and melted. Since the melting point of silicon is approximately 1420 ℃, heating must first be carried out to reach the melting point. In this case, the temperature of the heater must be increased to about 1700 ℃. Due to this heating process, both the graphite crucible and the quartz crucible are heated to the melting point of silicon or higher. The quartz starts to soften and deform when it exceeds about 1200 c, and the quartz crucible is almost completely in close contact with the graphite crucible supporting the outside of the quartz crucible due to the load of the molten silicon in the quartz crucible.
As shown in the following equation, a known problem of the CZ method is that at the melting temperature of silicon, SiC solid and CO gas are generated by the reaction between the outer surface of the quartz crucible and the inner surface of the graphite crucible, and the specific reaction equation is: SiO 22+3C = = SiC +2CO, and the thermal expansion coefficient of the produced SiC is significantly different from that of the graphite crucible, and therefore SiC becomes a cause of breakage or the like during the cooling/heating cycle of the graphite crucible, and its service life is limited in terms of safety or the like. Furthermore, the generated CO gas thus exerts pressure on the quartz crucible, causing deformation thereof.
The method for reducing the deformation of the quartz crucible is commonly used at present, the quartz crucible is made into a double-layer structure, and a shaping device is arranged outside the graphite crucible, so that the graphite crucible and the quartz crucible are fixedly lifted, and the deformation of the quartz crucible is reduced. However, the process is complicated and the effect of preventing the deformation of the quartz crucible is poor.
Disclosure of Invention
In view of the above, there is a need for an improved quartz crucible that can effectively reduce high temperature deformation of the quartz crucible.
There is also a need for an improved method of making a quartz crucible.
An improved quartz crucible, the roughness of the outer surface of the quartz crucible is 200 um-2000 um, and the inner surface of the quartz crucible is coated with a crystal cristobalite coating.
A manufacturing method of an improved quartz crucible comprises the following steps:
increasing the roughness of the outer surface of the quartz crucible: selecting stone sand with the granularity of 0.1-2 mm to perform sand blasting treatment on the outer surface of the quartz crucible, so that the roughness of the outer surface of the quartz crucible reaches 200-2000 um;
spraying a coating on the inner surface of the quartz crucible: spraying barium hydroxide solution to the inner surface of the quartz crucible.
Strengthening the inner coating of the quartz crucible: heating the quartz crucible with the inner surface sprayed with the barium hydroxide solution to 800-1200 ℃, and inducing the silicon dioxide in the inner layer of the quartz crucible to be converted into crystal cristobalite by the inner coating to obtain the improved quartz crucible.
Preferably, the stone sand consists of pomegranate sand particles with different particle sizes, specifically, 10-30% by mass of the pomegranate sand particles with the particle size of less than 0.5mm, 50-75% by mass of the pomegranate sand particles with the particle size of 0.5-1.2 mm and 10-35% by mass of the pomegranate sand particles with the particle size of 1.2-2 mm, the sand blasting pressure is 0.4-0.6 Mpa, the rotation frequency of the quartz crucible on a rotating platform is 20Hz, and the sand blasting time is 60-300 seconds.
By adopting the technical scheme, the invention has the beneficial effects that: the invention reduces the deformation of the quartz crucible at high temperature by increasing the roughness of the outer surface of the quartz crucible and arranging the coating on the inner surface of the quartz crucible, can increase the contact porosity of the quartz crucible and the graphite crucible by increasing the roughness of the outer surface of the quartz crucible, can lead out gas through the pores between the quartz crucible and the graphite crucible when the quartz crucible reacts with the graphite crucible at high temperature to generate gas, thereby avoiding the deformation of the quartz crucible, in addition, the barium hydroxide solution is sprayed on the inner surface of the quartz crucible to generate barium carbonate by the reaction of the barium hydroxide and carbon dioxide in the air, then barium silicate is generated by the reaction of the barium carbonate and the quartz crucible, the barium silicate induces the inner surface of the quartz crucible to generate a compact crystal cristobalite layer, and the strength of the inner wall of the quartz crucible is improved because the crystal cristobalite has no softening point and high strength, thereby preventing the quartz crucible from being deformed.
The method can effectively reduce the deformation of the quartz crucible at high temperature, and is convenient to operate.
Detailed Description
The embodiment of the invention provides an improved quartz crucible capable of effectively reducing high-temperature deformation of the quartz crucible.
There is also a need for an improved method of making a quartz crucible.
An improved quartz crucible, the roughness of the outer surface of the quartz crucible is 200 um-2000 um, and the inner surface of the quartz crucible is coated with a crystal cristobalite coating.
A manufacturing method of an improved quartz crucible comprises the following steps:
increasing the roughness of the outer surface of the quartz crucible: selecting stone sand with the granularity of 0.1-2 mm to carry out sand blasting treatment on the outer surface of the quartz crucible, wherein the stone sand consists of pomegranate sand particles with different particle sizes, specifically 10-30% of the pomegranate sand particles with the particle size of less than 0.5mm, 50-75% of the pomegranate sand particles with the particle size of 0.5-1.2 mm and 10-35% of the pomegranate sand particles with the particle size of 1.2-2 mm, the sand blasting pressure is 0.4-0.6 MPa, the rotation frequency of the quartz crucible on a rotating platform is 20Hz, the sand blasting time is 60-300 seconds, and the roughness of the outer surface of the quartz crucible reaches 200-2000 um; the porosity of the quartz crucible in contact with the graphite crucible can be improved by increasing the roughness of the outer surface of the quartz crucible, so that gas generated by high-temperature reaction of the quartz crucible and the graphite crucible is easy to discharge, and the deformation of the quartz crucible is reduced;
spraying a coating on the inner surface of the quartz crucible: firstly, placing a quartz crucible with the outer surface subjected to sand blasting treatment in a cleaning pool, cleaning the quartz crucible with hydrofluoric acid, wherein the volume concentration of the hydrofluoric acid is 15-20%, removing metal impurities in the quartz crucible by acid cleaning, placing the quartz crucible after acid cleaning into deionized water for cleaning so as to clean residual acid on the quartz crucible, and then placing the quartz crucible into an infrared drying instrument for drying until no moisture exists on the surface of the quartz crucible; the infrared oven is used for drying the quartz crucible, so that new impurities adhered to the quartz crucible due to contact with an instrument can be reduced.
Preparing a barium hydroxide solution, weighing barium hydroxide octahydrate solid powder, wherein the purity of the barium hydroxide octahydrate solid powder is 95% -99% of analytical purity, and dissolving the barium hydroxide octahydrate solid powder in deionized water at the temperature of 20-60 ℃ to form the barium hydroxide solution with the molar concentration of 0.2-2 mol/L;
spraying barium hydroxide solution to the inner surface of the quartz crucible, heating the quartz crucible in a high-temperature baking furnace to make the surface temperature of the quartz crucible reach 150-600 ℃, and spraying the prepared barium hydroxide solution through a spray gunThe barium hydroxide solution is sprayed on the inner surface of the quartz crucible and then reacts with carbon dioxide in the air rapidly to generate barium carbonate which is attached to the inner surface of the quartz crucible, and the specific reaction formula is as follows: ba (OH)2+CO2=BaCO3+H2O, controlling the concentration of the sprayed barium hydroxide solution within the range that the concentration of the barium carbonate coating formed on the inner surface of the quartz crucible is 60ug/cm2~300ug/cm2(ii) a Placing the quartz crucible after the barium hydroxide is sprayed in a high-temperature baking furnace at the temperature of 100-600 ℃ for heating for 2-10 minutes, taking out the quartz crucible, and cooling under natural conditions to obtain a quartz crucible with an inner coating; if the concentration of barium carbonate is too low, the cristobalite compact layer formed at high temperature is too thin, and has no great effect on enhancing the strength of the quartz crucible, and if the concentration of barium carbonate is too high, the cristobalite compact layer formed at high temperature is too thick, and is easy to peel off from the crucible substrate, so that the crystal pulling is stopped;
strengthening the inner coating of the quartz crucible: when the temperature of a quartz crucible with an inner coating is raised to 800-1200 ℃, a barium carbonate coating adhered to the inner surface of the quartz crucible reacts with silicon dioxide at high temperature to generate barium silicate, and the specific reaction formula is as follows: BaCO3+SiO2=BaSiO3+CO2And the barium silicate induces amorphous silicon dioxide in the inner layer of the quartz crucible to be converted into crystal cristobalite so as to obtain the high-strength quartz crucible, the crystal cristobalite has no softening point and high strength, and the strength of the inner wall of the quartz crucible is improved, so that the quartz crucible is prevented from deforming.
Example 1:
a manufacturing method of an improved quartz crucible comprises the following steps:
(1) placing a 24-inch quartz crucible on a rotary platform of a sand blasting machine, selecting pomegranate sand with the granularity specification of 0.1-2 mm, and comprising the following particles with different particle sizes in percentage by weight: 30% of particle size less than 0.5mm, 50% of particle size 0.5 mm-1.2 mm and 20% of particle size greater than 1.2mm, carrying out outer surface sand blasting treatment, wherein the sand blasting pressure is 0.4-0.6 Mpa, the workpiece rotation frequency is 20Hz, the sand blasting time is 60 seconds, and the roughness detection of the outer surface of the quartz crucible after spraying reaches 200 um-600 um.
(2) Cleaning the sand-blasted quartz crucible with pure water, placing the quartz crucible into an acid tank containing hydrofluoric acid for acid cleaning treatment, wherein the volume concentration of the hydrofluoric acid is 15%, and the acid cleaning time is 20 minutes, so that metal ions on the quartz crucible are removed, the influence on the crystal pulling quality of monocrystalline silicon is avoided, cleaning the acid-cleaned crucible with the deionized water for 3 minutes, and completely cleaning residual acid on the surface.
(3) Drying the cleaned quartz crucible in a clean room for 3 hours by infrared rays;
(4) 0.2mol of barium hydroxide octahydrate solid powder is weighed and dissolved in 1L of deionized water at 30 ℃ to form a barium hydroxide solution with the molar concentration of 0.2 mol/L.
(5) The quartz crucible is placed in a high-temperature baking furnace with the temperature of 400 ℃ and heated for 8 minutes, so that the surface temperature of the quartz crucible reaches 150 ℃.
(6) Placing the quartz crucible on a rotating platform, weighing 75g of the barium hydroxide solution prepared in the step (4), spraying the barium hydroxide solution by a spray gun to perform chemical reaction with carbon dioxide in the air to form barium carbonate, and uniformly attaching the barium carbonate to the inner surface of the quartz crucible to ensure that the concentration of the barium carbonate on the inner surface of the quartz crucible is 116ug/cm2。
(7) And (3) placing the quartz crucible sprayed with the barium hydroxide solution into a high-temperature baking furnace at the temperature of 200 ℃ to heat for 5 minutes, and taking out and naturally cooling.
(8) And heating the quartz crucible with the inner coating to 800-1200 ℃, and inducing the silica in the inner layer of the quartz crucible to be converted into cristobalite crystals by the inner coating to obtain the high-strength quartz crucible.
Example 2:
a method for effectively reducing high-temperature deformation of a quartz crucible comprises the following steps:
(1) placing a 24-inch quartz crucible on a rotary platform of a sand blasting machine, selecting pomegranate sand with the granularity specification of 0.1-2 mm, and comprising the following particles with different particle sizes in percentage by weight: 10% of particle size less than 0.5mm, 70% of particle size 0.5 mm-1.2 mm and 20% of particle size greater than 1.2mm, carrying out outer surface sand blasting treatment, wherein the sand blasting pressure is 0.4-0.6 Mpa, the workpiece rotation frequency is 20Hz, the sand blasting time is 60 seconds, and the roughness detection of the outer surface of the quartz crucible after spraying reaches 800 um-1200 um.
(2) Cleaning the sand-blasted quartz crucible with pure water, placing the quartz crucible into an acid tank containing hydrofluoric acid for acid cleaning treatment, wherein the volume concentration of the hydrofluoric acid is 20%, and the acid cleaning time is 40 minutes, so that metal ions on the quartz crucible are removed, the crystal pulling quality of monocrystalline silicon is prevented from being influenced, cleaning the acid-cleaned crucible with the deionized water for 3 minutes, and completely cleaning residual acid on the surface.
(3) Drying the cleaned quartz crucible in a clean room for 3 hours by infrared rays;
(4) weighing 2mol of barium hydroxide octahydrate solid powder, and dissolving the powder in 1L of deionized water at 20 ℃ to form a barium hydroxide solution with the molar concentration of 2 mol/L.
(5) The quartz crucible is placed in a high-temperature baking furnace with the temperature of 400 ℃ and heated for 8 minutes, so that the surface temperature of the quartz crucible reaches 600 ℃.
(6) Placing the quartz crucible on a rotating platform, weighing 94g of the barium hydroxide solution prepared in the step (4), spraying the barium hydroxide solution by a spray gun to perform chemical reaction with carbon dioxide in the air to form barium carbonate, and uniformly attaching the barium carbonate to the inner surface of the quartz crucible to ensure that the concentration of the barium carbonate on the inner surface of the quartz crucible is 195ug/cm2。
(7) And (3) placing the quartz crucible sprayed with the barium hydroxide solution into a high-temperature baking furnace at the temperature of 200 ℃ to heat for 5 minutes, and taking out and naturally cooling.
(8) And heating the quartz crucible with the inner coating to 800-1200 ℃, and inducing the silica in the inner layer of the quartz crucible to be converted into cristobalite crystals by the inner coating to obtain the high-strength quartz crucible.
Example 3:
a method for effectively reducing high-temperature deformation of a quartz crucible comprises the following steps:
(1) placing a 24-inch quartz crucible on a rotary platform of a sand blasting machine, selecting pomegranate sand with the granularity specification of 0.1-2 mm, and comprising the following particles with different particle sizes in percentage by weight: 10% of particle size less than 0.5mm, 68% of particle size 0.5 mm-1.2 mm and 22% of particle size greater than 1.2mm, carrying out outer surface sand blasting treatment, wherein the sand blasting pressure is 0.4-0.6 Mpa, the workpiece rotation frequency is 20Hz, the sand blasting time is 60 seconds, and the roughness detection of the outer surface of the quartz crucible after spraying reaches 1200 um-2000 um.
(2) Cleaning the sand-blasted quartz crucible with pure water, placing the quartz crucible into an acid tank containing hydrofluoric acid for acid cleaning treatment, wherein the volume concentration of the hydrofluoric acid is 18%, and the acid cleaning time is 20 minutes, so that metal ions on the quartz crucible are removed, the crystal pulling quality of monocrystalline silicon is prevented from being influenced, cleaning the acid-cleaned crucible with the deionized water for 3 minutes, and completely cleaning residual acid on the surface.
(3) Drying the cleaned quartz crucible in a clean room for 3 hours by infrared rays;
(4) 1.85mol of barium hydroxide octahydrate solid powder is weighed and dissolved in 1L of deionized water at 60 ℃ to form a barium hydroxide solution with the molar concentration of 1.85 mol/L.
(5) The quartz crucible is placed in a high-temperature baking furnace with the temperature of 400 ℃ and heated for 8 minutes, so that the surface temperature of the quartz crucible reaches 600 ℃.
(6) Placing the quartz crucible on a rotating platform, weighing 95g of the barium hydroxide solution prepared in the step (4), spraying the barium hydroxide solution by a spray gun to perform chemical reaction with carbon dioxide in the air to form barium carbonate, and uniformly attaching the barium carbonate to the inner surface of the quartz crucible to ensure that the concentration of the barium carbonate on the inner surface of the quartz crucible is 255ug/cm2。
(7) And (3) placing the quartz crucible sprayed with the barium hydroxide solution into a high-temperature baking furnace at the temperature of 200 ℃ to heat for 5 minutes, and taking out and naturally cooling.
(8) And heating the quartz crucible with the inner coating to 800-1200 ℃, and inducing the silica in the inner layer of the quartz crucible to be converted into cristobalite crystals by the inner coating to obtain the high-strength quartz crucible.
Test results
The quartz crucibles of the specific preparation examples 1, 2 and 3 were pulled under the same conditions as the ordinary quartz crucibles, the loading amount of the quartz crucibles was 140kg, the melting time was about 12 hours, and the probability of deformation of the quartz crucibles after pulling was compared, and the data are as follows:
crucible type | Number of inputs | Number of figures | Deformation ratio% |
Common quartz crucible | 182 | 6 | 3.29 |
Example 1 Quartz crucible | 150 | 1 | 0.6 |
EXAMPLE 2 Quartz crucible | 150 | 0 | 0 |
Example 3 Quartz crucible | 148 | 0 | 0 |
From the data in the table, the probability of deformation is greatly reduced or basically no deformation occurs during the process of pulling the monocrystalline silicon by using the quartz crucible, and the quality of the quartz crucible is greatly improved.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (1)
1. An improved quartz crucible, characterized in that: the outer surface roughness of the quartz crucible is 200 um-2000 um, and the inner surface of the quartz crucible is coated with a crystal cristobalite coating, and the manufacturing method of the improved quartz crucible comprises the following steps:
increasing the roughness of the outer surface of the quartz crucible: selecting stone sand with the granularity of 0.1-2 mm to perform sand blasting treatment on the outer surface of the quartz crucible, so that the roughness of the outer surface of the quartz crucible reaches 200-2000 um;
spraying a coating on the inner surface of the quartz crucible: spraying a barium hydroxide solution to the inner surface of the quartz crucible;
strengthening the inner coating of the quartz crucible: heating the quartz crucible with the inner surface sprayed with the barium hydroxide solution to 800-1200 ℃, and inducing the silicon dioxide in the inner layer of the quartz crucible to be converted into crystal cristobalite by the inner coating to obtain an improved quartz crucible;
the stone sand consists of pomegranate sand particles with different particle sizes, specifically consists of 10-30% by mass of pomegranate sand particles with particle size smaller than 0.5mm, 50-75% by mass of pomegranate sand particles with particle size of 0.5-1.2 mm and 10-35% by mass of pomegranate sand particles with particle size of 1.2-2 mm, the sand blasting pressure is 0.4-0.6 Mpa, the rotation frequency of the quartz crucible on a rotating platform is 20Hz, and the sand blasting time is 60-300 seconds;
the step of spraying the coating on the inner surface of the quartz crucible comprises the following specific steps: and (2) placing the quartz crucible in a high-temperature baking furnace for heating to ensure that the surface temperature of the quartz crucible reaches 150-600 ℃, then spraying a barium hydroxide solution with the barium ion molar concentration of 0.2-2% onto the inner surface of the quartz crucible, and placing the quartz crucible after spraying the barium hydroxide in the high-temperature baking furnace for heating to obtain the quartz crucible with the inner coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810526785.4A CN108531980B (en) | 2018-05-29 | 2018-05-29 | Improved quartz crucible and method for making same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810526785.4A CN108531980B (en) | 2018-05-29 | 2018-05-29 | Improved quartz crucible and method for making same |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108531980A CN108531980A (en) | 2018-09-14 |
CN108531980B true CN108531980B (en) | 2020-12-11 |
Family
ID=63473179
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810526785.4A Active CN108531980B (en) | 2018-05-29 | 2018-05-29 | Improved quartz crucible and method for making same |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108531980B (en) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10114698A1 (en) * | 2001-03-23 | 2002-09-26 | Heraeus Quarzglas | Component made from quartz glass e.g. crucible having high thermal stability comprises a mold, part of which is provided with a stabilizing layer having a higher softening temperature than quartz glass |
US20070084400A1 (en) * | 2005-10-19 | 2007-04-19 | General Electric Company | Quartz glass crucible and method for treating surface of quartz glass crucible |
JP5229778B2 (en) * | 2007-09-28 | 2013-07-03 | 株式会社Sumco | Method for producing quartz glass crucible for pulling silicon single crystal |
CN201506711U (en) * | 2009-09-30 | 2010-06-16 | 常州天合光能有限公司 | Crucible for casting ingot |
CN101696499A (en) * | 2009-09-30 | 2010-04-21 | 常州天合光能有限公司 | Treatment method for crucible for casting ingots |
CN201634794U (en) * | 2010-03-23 | 2010-11-17 | 扬州华尔光电子材料有限公司 | Coating quartz crucible for producing solar silicon single-crystal |
CN102260902B (en) * | 2011-07-15 | 2013-09-11 | 江苏晶鼎电子材料有限公司 | Method for preparing quartz crucible coating |
-
2018
- 2018-05-29 CN CN201810526785.4A patent/CN108531980B/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN108531980A (en) | 2018-09-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP1985593B1 (en) | Reinforced silica glass crucible | |
KR100408905B1 (en) | Surface-processing crucibles for improved zero potential performance | |
TW302499B (en) | ||
CN112144115B (en) | Quartz crucible with long service life and low deformation rate and preparation method thereof | |
CN101696514A (en) | Method for producing polycrystal ingot | |
JP4815003B2 (en) | Crucible for silicon crystal growth, crucible manufacturing method for silicon crystal growth, and silicon crystal growth method | |
WO1996021617A1 (en) | Silica gel, synthetic quartz glass powder, quartz glass molding, and processes for producing these | |
CN108531980B (en) | Improved quartz crucible and method for making same | |
JP5108803B2 (en) | Method for producing silica container | |
JP2001114590A (en) | Quartz glass crucible for pulling silicon single crystal | |
US8858706B2 (en) | Single-crystal manufacturing apparatus and single-crystal manufacturing method | |
CN103703171A (en) | Silica vessel for drawing up monocrystalline silicon and method for producing same | |
JP5487259B2 (en) | Silica container | |
CN101696499A (en) | Treatment method for crucible for casting ingots | |
CN111320393B (en) | Quartz glass crucible and method for producing same | |
JPS62100436A (en) | Production of high-purity quartz glass | |
TWI808756B (en) | Quartz glass crucible, manufacturing method thereof, and silicon single crystal manufacturing method | |
JPH1112091A (en) | Production of spherical single crystal silicon | |
CN116607205A (en) | Quartz crucible and preparation method and application thereof | |
WO2011156976A1 (en) | Method for polycrystalline silicon ingot casting | |
JP3875780B2 (en) | Manufacturing method of high purity powder | |
KR20170014115A (en) | Fabrication method of Zirconia(ZrO2) coated quartz crucible in situ fusion process | |
JPH06122549A (en) | Sintered compact of cristobalite and its production | |
TW202413741A (en) | Synthetic crucibles with rim coating | |
JPH1121662A (en) | Adhesion-preventive plate for film forming equipment, and its production |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CP01 | Change in the name or title of a patent holder |
Address after: 750021 No.23 Guangming West Road, Xixia District, Yinchuan City, Ningxia Hui Autonomous Region Patentee after: Ningxia dunyuan poly core semiconductor technology Co.,Ltd. Address before: 750021 No.23 Guangming West Road, Xixia District, Yinchuan City, Ningxia Hui Autonomous Region Patentee before: FERROTEC (NINGXIA) ADVANCED QUARTZ MATERIAL Co.,Ltd. |
|
CP01 | Change in the name or title of a patent holder |