CN111778557A - Crucible for preparing sapphire single crystal - Google Patents

Crucible for preparing sapphire single crystal Download PDF

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Publication number
CN111778557A
CN111778557A CN202010567992.1A CN202010567992A CN111778557A CN 111778557 A CN111778557 A CN 111778557A CN 202010567992 A CN202010567992 A CN 202010567992A CN 111778557 A CN111778557 A CN 111778557A
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CN
China
Prior art keywords
crucible
coating
tungsten
sapphire single
single crystal
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.)
Pending
Application number
CN202010567992.1A
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Chinese (zh)
Inventor
张玉亮
宋旭波
李树新
王健
魏超
杜迎虎
吴庆华
王志岭
宋渤
曹学玲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Xinsheng Optoelectronic Technolog Co ltd
Original Assignee
Shandong Xinsheng Optoelectronic Technolog Co ltd
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Filing date
Publication date
Application filed by Shandong Xinsheng Optoelectronic Technolog Co ltd filed Critical Shandong Xinsheng Optoelectronic Technolog Co ltd
Priority to CN202010567992.1A priority Critical patent/CN111778557A/en
Publication of CN111778557A publication Critical patent/CN111778557A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/20Aluminium oxides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002Crucibles or containers for supporting the melt

Abstract

The invention relates to the technical field of devices for sapphire single crystals, in particular to a crucible for preparing sapphire single crystals, which is a tungsten crucible, wherein a convex rib is arranged outside the crucible and used for decomposing the stress effect of heating and cooling of the crucible, so that the durability and the strength of the crucible are enhanced, the thickness of the crucible is 5-100mm, the material cost of the crucible is reduced, the thickness of the crucible is reduced, the heat transfer effect is also provided on the premise of ensuring the quality, the heating and cooling efficiency is improved, in addition, a coating is arranged inside the tungsten crucible, the thickness of the coating is 50-150 microns, the coating is made of a composite material of tungsten, tantalum and molybdenum, the enhancement effect is achieved, and the growth quality of crystals is also improved.

Description

Crucible for preparing sapphire single crystal
Technical Field
The invention relates to the technical field of devices for sapphire single crystals, in particular to a crucible for preparing sapphire single crystals.
Background
The sapphire single crystal comprises alumina as chemical component, and has chemical formula (α -Al)2O3) The aluminum alloy is formed by combining three oxygen atoms and two aluminum atoms in a covalent bond mode, and the crystal structure of the aluminum alloy is a hexagonal lattice structure.
The manufacturing process of the artificial sapphire comprises the following steps: preparing raw materials → filling raw materials and erecting seed crystals → vacuumizing the furnace body → heating the furnace body (adding a molybdenum heat shield and a tungsten heat shield in the furnace body) → melting the raw materials → welding seed crystals → growing crystal necks → growing crystals → separating the crystals from a crucible → cooling → taking out the crystals.
In the growth process of sapphire single crystal, a crucible is a key and necessary component, the crucible is used for containing raw materials and is always in a high-temperature environment in the growth process of the single crystal, a tungsten crucible, a molybdenum crucible and the like are commonly used, and the structure, the material and the coating of the crucible have very key influences on the growth quality of the single crystal, the crystal utilization rate and the like.
Therefore, the research on a crucible with reasonable structure and durable material quality has great significance for the growth of sapphire.
Disclosure of Invention
The invention provides a high-quality crucible with reasonable structure and durable material, which is a tungsten crucible, the durability and the strength of the crucible are enhanced by arranging a convex rib outside the crucible for decomposing the stress effect of heating and cooling of the crucible, the thickness of the crucible is 5-100mm, the material cost of the crucible is reduced on the premise of ensuring the quality, the thickness is reduced, the heat transfer effect is simultaneously provided, the heating efficiency and the cooling efficiency are both improved, in addition, a coating is arranged inside the tungsten crucible, the thickness of the coating is 50-150 microns, and the coating is made of a composite material of tungsten, tantalum and molybdenum, so that the effect of enhancement is achieved, and the growth quality of crystals is also improved.
The technical scheme of the invention is as follows:
a crucible for preparing sapphire single crystal is a cylinder at the upper part, and the bottom of the crucible is in a spherical crown shape; a plurality of convex ribs are arranged on the outer side wall of the crucible, and the cross section of each convex rib is semicircular; the crucible main body is made of tungsten, a coating is arranged in the crucible, the thickness of the coating is 50-150 microns, and the coating is made of a composite material of tungsten, tantalum and molybdenum.
Furthermore, the convex rib is located the middle-upper portion of crucible, and upper portion adopts the cylinder structure in this crucible, is convenient for stress dispersion after setting up the convex rib, and intensity is improved reduces the fracture phenomenon.
Furthermore, the convex ribs are 2-4 and are uniformly arranged on the middle upper part of the crucible, so that the uniform distribution and the uniform stress are realized.
Furthermore, the thickness of the crucible is 5-100mm, on the premise of ensuring the quality, the material cost of the crucible is reduced, the thickness is reduced, the heat transfer effect is provided, and the heating efficiency and the cooling efficiency are improved.
Further, the weight ratio of tungsten, tantalum and molybdenum in the coating is 70: (1-5) and (5-10), the addition of tantalum and molybdenum can improve the heat resistance of the crucible and is beneficial to improving the growth quality of crystals.
Further, the weight ratio of tungsten, tantalum and molybdenum in the coating is 70: (2-3) (6-8), the addition of tantalum and molybdenum can improve the heat resistance of the crucible and is beneficial to improving the crystal growth quality.
Furthermore, the coating also contains alumina, so that the crystal growth quality is further improved.
The beneficial effect of the invention is that,
the crucible is a tungsten crucible, the convex ribs are arranged outside the crucible and used for decomposing the stress effect of heating and cooling of the crucible, the durability and the strength of the crucible are enhanced, the thickness of the crucible is 5-100mm, the material cost of the crucible is reduced on the premise of ensuring the quality, the thickness is reduced, the heat transfer effect is submitted, the heating efficiency and the cooling efficiency are improved, in addition, the coating is arranged inside the tungsten crucible, the thickness of the coating is 50-150 micrometers, the coating is made of a composite material of tungsten, tantalum and molybdenum, the enhancing effect is achieved, the growth quality of crystals is improved, aluminum oxide is further compounded, and the growth quality of the crystals is further improved.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic view of the structure of the crucible of the present invention;
wherein, 1-convex rib.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A crucible for preparing sapphire single crystal is a cylinder at the upper part, and the bottom of the crucible is in a spherical crown shape; 4 convex ribs are arranged on the outer side wall of the crucible, the convex ribs are positioned at the middle upper part of the crucible, and the cross section of each convex rib is semicircular; crucible main part material is tungsten, sets up the coating in the inside of crucible, and the coating thickness is 50 microns, and the material of coating is tungsten, tantalum, molybdenum's combined material, and the well tungsten of coating, tantalum, molybdenum's weight ratio is 70: 5:5.
The thickness of crucible is 50mm, under the prerequisite of guaranteeing the quality, reduces the material cost of crucible, reduces thickness, submits the heat transfer effect simultaneously, and heating and cooling efficiency all improve.
Example 2
A crucible for preparing sapphire single crystal is a cylinder at the upper part, and the bottom of the crucible is in a spherical crown shape; 2 convex ribs are arranged on the outer side wall of the crucible, and the cross section of each convex rib is semicircular; crucible main part material is tungsten, sets up the coating in the inside of crucible, and the coating thickness is 150 microns, and the material of coating is tungsten, tantalum, molybdenum's combined material, and the well tungsten of coating, tantalum, molybdenum's weight ratio is 70: 1:10.
The thickness of crucible is 100mm, under the prerequisite of guaranteeing the quality, reduces the material cost of crucible, reduces thickness, submits the heat transfer effect simultaneously, and heating and cooling efficiency all improve.
Example 3
A crucible for preparing sapphire single crystal is a cylinder at the upper part, and the bottom of the crucible is in a spherical crown shape; 3 convex ribs are arranged on the outer side wall of the crucible, and the cross section of each convex rib is semicircular; crucible main part material is tungsten, sets up the coating in the inside of crucible, and the coating thickness is 70 microns, and the material of coating is tungsten, tantalum, molybdenum's combined material, and the well tungsten of coating, tantalum, molybdenum, the weight proportion of aluminium oxide is 70: 4:8: and 10, the addition of tantalum and molybdenum can improve the heat resistance of the crucible and is beneficial to improving the crystal growth quality. .
Further, the thickness of crucible is 5mm, under the prerequisite of guaranteeing the quality, reduces the material cost of crucible, reduces thickness, submits the heat transfer effect simultaneously, and heating and cooling efficiency all improve.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (7)

1. A crucible for preparing sapphire single crystal is characterized in that the crucible is a cylinder at the upper part, and the bottom of the crucible is in a spherical crown shape; a plurality of convex ribs are arranged on the outer side wall of the crucible, and the cross section of each convex rib is semicircular; the crucible main body is made of tungsten, a coating is arranged in the crucible, the thickness of the coating is 50-150 microns, and the coating is made of a composite material of tungsten, tantalum and molybdenum.
2. The crucible for preparing a sapphire single crystal as set forth in claim 1, wherein the rib is located at a middle-upper portion of the crucible.
3. The crucible for preparing a sapphire single crystal as set forth in claim 1, wherein the number of the ribs is 2 to 4 and the ribs are arranged uniformly in the middle-upper portion of the crucible.
4. The crucible for preparing a sapphire single crystal as set forth in claim 1, wherein the crucible has a thickness of 5 to 100 mm.
5. The crucible for preparing a sapphire single crystal as set forth in claim 1, wherein the coating layer contains tungsten, tantalum and molybdenum in a weight ratio of 70: (1-5):(5-10).
6. The crucible for preparing a sapphire single crystal as set forth in claim 1, wherein the coating layer contains tungsten, tantalum and molybdenum in a weight ratio of 70: (2-3):(6-8).
7. The method of claim 1, wherein the coating further comprises alumina.
CN202010567992.1A 2020-06-19 2020-06-19 Crucible for preparing sapphire single crystal Pending CN111778557A (en)

Priority Applications (1)

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CN202010567992.1A CN111778557A (en) 2020-06-19 2020-06-19 Crucible for preparing sapphire single crystal

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114574939A (en) * 2022-04-19 2022-06-03 北京通美晶体技术股份有限公司 Growth method of GaAs single crystal

Citations (13)

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CN2796900Y (en) * 2005-06-23 2006-07-19 重庆市机电设计研究院 Quantitative transfer device of molten magnesium alloy liquid
JP2011105572A (en) * 2009-11-20 2011-06-02 Asahi Glass Co Ltd Melting furnace of optical glass, and method for producing optical glass using the same
CN104152984A (en) * 2014-08-12 2014-11-19 杭州铸泰科技有限公司 Reusable crucible used in orientated growth of sapphire monocrystal
CN104213096A (en) * 2014-08-12 2014-12-17 厦门虹鹭钨钼工业有限公司 Preparation method of crucible with tungsten coating
CN104487618A (en) * 2012-04-17 2015-04-01 普兰西欧洲股份公司 Crucible for producing oxide ceramic monocrystals
CN204417656U (en) * 2015-01-16 2015-06-24 浙江理工大学 The hemisphere die bed crucible of sapphire growth furnace
CN105102648A (en) * 2013-03-21 2015-11-25 联合材料公司 Crucible for growing sapphire single crystal and method for growing sapphire single crystal
CN105220223A (en) * 2014-07-02 2016-01-06 攀时(上海)高性能材料有限公司 For the crucible that crystal is cultivated
CN205062235U (en) * 2015-10-10 2016-03-02 贵阳嘉瑜光电科技咨询中心 A double crucible that is used for heat exchange method growth jumbo size sapphire
CN105683425A (en) * 2013-10-30 2016-06-15 联合材料公司 Crucible and single crystal sapphire production method using same
CN206266721U (en) * 2016-12-09 2017-06-20 株洲硬质合金集团有限公司 A kind of molybdenum crucible
CN109174224A (en) * 2018-10-17 2019-01-11 北京铂阳顶荣光伏科技有限公司 Crucible device
CN209082031U (en) * 2018-09-10 2019-07-09 河南晶鸿光电科技有限公司 A kind of sapphire crystal growth crucible

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2796900Y (en) * 2005-06-23 2006-07-19 重庆市机电设计研究院 Quantitative transfer device of molten magnesium alloy liquid
JP2011105572A (en) * 2009-11-20 2011-06-02 Asahi Glass Co Ltd Melting furnace of optical glass, and method for producing optical glass using the same
CN104487618A (en) * 2012-04-17 2015-04-01 普兰西欧洲股份公司 Crucible for producing oxide ceramic monocrystals
CN105102648A (en) * 2013-03-21 2015-11-25 联合材料公司 Crucible for growing sapphire single crystal and method for growing sapphire single crystal
CN105683425A (en) * 2013-10-30 2016-06-15 联合材料公司 Crucible and single crystal sapphire production method using same
CN105220223A (en) * 2014-07-02 2016-01-06 攀时(上海)高性能材料有限公司 For the crucible that crystal is cultivated
CN104213096A (en) * 2014-08-12 2014-12-17 厦门虹鹭钨钼工业有限公司 Preparation method of crucible with tungsten coating
CN104152984A (en) * 2014-08-12 2014-11-19 杭州铸泰科技有限公司 Reusable crucible used in orientated growth of sapphire monocrystal
CN204417656U (en) * 2015-01-16 2015-06-24 浙江理工大学 The hemisphere die bed crucible of sapphire growth furnace
CN205062235U (en) * 2015-10-10 2016-03-02 贵阳嘉瑜光电科技咨询中心 A double crucible that is used for heat exchange method growth jumbo size sapphire
CN206266721U (en) * 2016-12-09 2017-06-20 株洲硬质合金集团有限公司 A kind of molybdenum crucible
CN209082031U (en) * 2018-09-10 2019-07-09 河南晶鸿光电科技有限公司 A kind of sapphire crystal growth crucible
CN109174224A (en) * 2018-10-17 2019-01-11 北京铂阳顶荣光伏科技有限公司 Crucible device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114574939A (en) * 2022-04-19 2022-06-03 北京通美晶体技术股份有限公司 Growth method of GaAs single crystal

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Application publication date: 20201016