CN103266294A - Method of repeatedly using molybdenum crucible in HEM crystal growth - Google Patents
Method of repeatedly using molybdenum crucible in HEM crystal growth Download PDFInfo
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- CN103266294A CN103266294A CN2013100733506A CN201310073350A CN103266294A CN 103266294 A CN103266294 A CN 103266294A CN 2013100733506 A CN2013100733506 A CN 2013100733506A CN 201310073350 A CN201310073350 A CN 201310073350A CN 103266294 A CN103266294 A CN 103266294A
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- molybdenum crucible
- molybdenum
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Abstract
The invention discloses a method of repeatedly using a molybdenum crucible in HEM crystal growth, which comprises the following steps: (1) sandblasting the molybdenum crucible by a sand blasting machine to remove a coating surface of the molybdenum crucible; (2) washing and drying the molybdenum crucible after sandblasting; (3) spraying the molybdenum crucible; (4) polishing after spraying; (5) heating after completion of crystal growth, taking the crystal out by the thermal expansion and cool contraction principle, and repeating the above steps. The beneficial effects of the present invention are that: tungsten alloy and carbon spraying technology are used for forming a protective layer on the surface of the molybdenum crucible, the coating is removed by sandblasting after the crucible is used, then the spray coating is performed again for using, while the use of tungsten molybdenum alloy or carbon material for spraying achieves the purpose of repeated use of the molybdenum crucible, the production costs are reduced, while the pollution problems of sapphire are eliminated, and the yield of the crystal is improved.
Description
Technical field
The present invention relates to a kind of method of in the HEM crystal growth, reusing molybdenum crucible, belong to HEM crystal production technical field.
Background technology
Because high-melting-point (fusing point the is 2610 ℃) characteristic of molybdenum crucible, it has been widely used in the production of LED saphire substrate material.But because the rate of utilization of its fancy price and single, serious restriction the development of lokav jewelry industry.
As long as the molybdenum crucible shortcoming of using in the existing HEM crystal growth be embodied in following some:
1, domestic molybdenum crucible manufacturing technology is immature: the molybdenum crucible that domestic sapphire industry is used all is to adopt rotating-expressing type to be shaped, but this technology is grasped abroad in the staff, thereby having caused domestic 90% crucible all is import, finally cause it expensive, restricted the development of domestic sapphire crystal technology and production.
2, molybdenum easily reacts with graphite: molybdenum crucible in the HEM heat-exchanging method can be compositions such as MoC because can contact with graphite dust by reaction at 1100-1200 ℃, and molybdenum is reacted easily, and reaction product MoC pollutes sapphire easily simultaneously.
3, parasitic nucleation and pollution: since molybdenum element at the segregation coefficient in the sapphire liquation near 1, in crystal orientation can process, be not easy to discharge, cause sapphire to pollute.Simultaneously, because existing crucible inwall quality in the process of growth, forms parasitic nuclear from sidewall or bottom easily on backboard, cause the sapphire single-crystal that grows bad.
4, can not reuse: because the molybdenum crucible is added the reaction of molybdenum and carbon thermal insulation layer and graphite heating body for a long time under the condition of high temperature, cause crucible very crisp in crystal growth intact back change, cause crucible can not repeat the problem of usefulness.Simultaneously, for A to sapphire crystal growth, its crystal coefficient of expansion anisotropy, crystal should not take off pot.
Summary of the invention
The object of the present invention is to provide a kind of method of in the HEM crystal growth, reusing molybdenum crucible, can allow expensive molybdenum crucible can repeat repeatedly to use, reduce production cost, stop sapphire pollution problem simultaneously.
The objective of the invention is to be achieved through the following technical solutions: a kind of method of in the HEM crystal growth, reusing molybdenum crucible, it comprises following steps:
(1), utilize sandblast machine that molybdenum crucible is carried out sandblasting, remove the coating on molybdenum crucible surface;
(2), handle after, with the molybdenum crucible cleaning, drying;
(3), molybdenum crucible is carried out meltallizing, use lance driving device molybdenum crucible to be sprayed as spray material with miramint silk or the carbon dust of metal tungsten powder, tungsten filament, content 35% tungsten, forming a layer thickness until the molybdenum crucible surface is the coating of 0.1-1mm;
(4), polish behind the meltallizing, make the molybdenum crucible surfaceness reach 3.2;
(5), after crystal growth finishes, utilize the rising-heat contracting-cold principle, crystal is taken out in the heating back, repeats above step.
Described lance driving device comprises hydrogen spray gun, direct current plasma spray gun, AC plasma spray gun and radio frequency plasma spray gun.
Described bruting process adopts No. 1000 sand paper to polish.
Beneficial effect of the present invention is: use tungstenalloy and carbon meltallizing technology to form protective layer on the molybdenum crucible surface; crucible use the back by sandblast with coating removal; and then carry out spray-on coating and continue to use; adopt miramint or carbon material to spray simultaneously and realized that molybdenum crucible can repeat nonexpondable purpose; reduced production cost; stop sapphire pollution problem simultaneously, improved the yield rate of crystal.
Embodiment
Further describe technical scheme of the present invention below in conjunction with embodiment, but that claimed scope is not limited to is described.
A kind of method of in the HEM crystal growth, reusing molybdenum crucible, it comprises following steps:
(1), utilize sandblast machine that molybdenum crucible is carried out sandblasting, remove the coating on molybdenum crucible surface;
(2), handle after, with the molybdenum crucible cleaning, drying;
(3), molybdenum crucible is carried out meltallizing, use lance driving device molybdenum crucible to be sprayed as spray material with miramint silk or the carbon dust of metal tungsten powder, tungsten filament, content 35% tungsten, forming a layer thickness until the molybdenum crucible surface is the coating of 0.1-1mm;
(4), polish behind the meltallizing, make the molybdenum crucible surfaceness reach 3.2;
(5), after crystal growth finishes, utilize the rising-heat contracting-cold principle, crystal is taken out in the heating back, and repeating step (1) is realized the recycling of molybdenum crucible to step (5).
Described lance driving device comprises hydrogen spray gun, direct current plasma spray gun, AC plasma spray gun and radio frequency plasma spray gun.
Described bruting process adopts No. 1000 sand paper to polish.
The tungsten coating of the present invention's spraying, the reaction that can well completely cut off molybdenum crucible and C, stop the molybdenum crucible and finish the problem that becomes fragile at sapphire crystal growth, also stop Mo and C reaction generation MoC and polluted sapphire problem, the tungsten coatingsurface is smooth simultaneously, in the sapphire crystal growth process, be not easy to form parasitic nuclear in crucible interior and bottom, improve the monocrystalline of the blue precious crystal of growth, the final yield rate that improves sapphire crystal, after crystal growth is intact, the miramint coating comes off from the molybdenum crucible easily, thereby finally can successfully solve the problem of the sticking pot of sapphire crystal, finally can realize the effect that the molybdenum crucible is repeatedly used.
In addition, the segregation coefficient of tungsten in the sapphire liquation is much smaller than 1, and it is discharged to crystal top easily in crystal growing process, reduces the pollution of metallic element.
Claims (3)
1. method of in the HEM crystal growth, reusing molybdenum crucible, it is characterized in that: it comprises following steps:
(1), utilize sandblast machine that molybdenum crucible is carried out sandblasting, remove the coating on molybdenum crucible surface;
(2), handle after, with the molybdenum crucible cleaning, drying;
(3), molybdenum crucible is carried out meltallizing, use lance driving device molybdenum crucible to be sprayed as spray material with miramint silk or the carbon dust of metal tungsten powder, tungsten filament, content 35% tungsten, forming a layer thickness until the molybdenum crucible surface is the coating of 0.1-1mm;
(4), polish behind the meltallizing, make the molybdenum crucible surfaceness reach 3.2;
(5), after crystal growth finishes, utilize the rising-heat contracting-cold principle, crystal is taken out in the heating back, repeats above step.
2. the method for reusing molybdenum crucible in the HEM crystal growth according to claim 1, it is characterized in that: described lance driving device comprises hydrogen spray gun, direct current plasma spray gun, AC plasma spray gun and radio frequency plasma spray gun.
3. the method for reusing molybdenum crucible in the HEM crystal growth according to claim 1, it is characterized in that: described bruting process adopts No. 1000 sand paper to polish.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100733506A CN103266294A (en) | 2013-03-07 | 2013-03-07 | Method of repeatedly using molybdenum crucible in HEM crystal growth |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100733506A CN103266294A (en) | 2013-03-07 | 2013-03-07 | Method of repeatedly using molybdenum crucible in HEM crystal growth |
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| CN103266294A true CN103266294A (en) | 2013-08-28 |
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| CN2013100733506A Pending CN103266294A (en) | 2013-03-07 | 2013-03-07 | Method of repeatedly using molybdenum crucible in HEM crystal growth |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458631A (en) * | 2013-09-22 | 2015-03-25 | 贵州航天精工制造有限公司 | Method for determining carbon and sulfur in material through repeatedly using crucible |
| 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 (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040110016A1 (en) * | 2002-11-20 | 2004-06-10 | Noriaki Hamaya | Heat resistant coated member, making method, and treatment using the same |
| CN101774583A (en) * | 2009-04-01 | 2010-07-14 | 北京京运通科技股份有限公司 | Crucible device for polycrystalline silicon growth process |
| JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
| CN102304751A (en) * | 2011-09-15 | 2012-01-04 | 江苏华盛天龙光电设备股份有限公司 | Composite crucible for growth of sapphire crystals |
| WO2013020153A1 (en) * | 2011-08-05 | 2013-02-14 | Plansee Se | Crucible for growing crystals |
-
2013
- 2013-03-07 CN CN2013100733506A patent/CN103266294A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040110016A1 (en) * | 2002-11-20 | 2004-06-10 | Noriaki Hamaya | Heat resistant coated member, making method, and treatment using the same |
| CN101774583A (en) * | 2009-04-01 | 2010-07-14 | 北京京运通科技股份有限公司 | Crucible device for polycrystalline silicon growth process |
| JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
| WO2013020153A1 (en) * | 2011-08-05 | 2013-02-14 | Plansee Se | Crucible for growing crystals |
| CN102304751A (en) * | 2011-09-15 | 2012-01-04 | 江苏华盛天龙光电设备股份有限公司 | Composite crucible for growth of sapphire crystals |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458631A (en) * | 2013-09-22 | 2015-03-25 | 贵州航天精工制造有限公司 | Method for determining carbon and sulfur in material through repeatedly using crucible |
| 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: 20130828 |