CN110093661A - The growing method of crystal - Google Patents
The growing method of crystal Download PDFInfo
- Publication number
- CN110093661A CN110093661A CN201910360867.0A CN201910360867A CN110093661A CN 110093661 A CN110093661 A CN 110093661A CN 201910360867 A CN201910360867 A CN 201910360867A CN 110093661 A CN110093661 A CN 110093661A
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- Prior art keywords
- crystal
- oxygen
- growing method
- growing
- oxide
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Classifications
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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
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/34—Silicates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of growing method of crystal, which includes shove charge, heating, lifting process, in shove charge by the addition of appropriate pyrolytic oxide among thermal field.The growing method of this crystal, the existing long crystallization of lifting is improved, without being filled with oxygen into crystal growing furnace, next oxygen is decomposited during 400 DEG C or more of heating and long crystalline substance to maintain the partial pressure of oxygen in furnace by added pyrolytic oxide, improves the quality of grown crystal.
Description
Technical field
The present invention relates to the preparation field of crystal more particularly to a kind of growing methods of crystal.
Background technique
Czochralski method is a kind of method that crystal is grown from melt, has the speed of growth fast, easy observation, crystal quality height etc.
Advantage is widely used in the growth of silicon, germanium, sapphire, laser crystal, scintillation crystal.
Medium frequency induction czochralski method is acted on using the induction heating of intermediate frequency coil, melts original using inductive crucible heater
Material, the method to complete crystal growth.Medium frequency induction czochralski method has many advantages, such as that pollution is small, capacity usage ratio is high, is current oxygen
One of the main method of compound crystal growth, is widely used in the crystalline substances such as garnet, Yttrium Orthovanadate, yttrium luetcium silicate, lithium niobate, lithium tantalate
The production of body.
The growth of refractory oxide crystal (fusing point is more than 1500 DEG C) is limited by crucible material, can generally be selected
The metals such as iridium, tungsten, molybdenum make crucible.In induction czochralski method, iridium is the crucible material of most common refractory oxide crystal.
Since iridium is expensive, generally when growing crystal, iridium oxidational losses at high temperature is avoided using inert atmosphere.But indifferent gas
Atmosphere will lead to refractory oxide crystal and generate Lacking oxygen during the growth process, influence the performance of crystal.
Currently, most technical solutions maintain crystal growth using certain density oxygen is filled in crystal growing process
Partial pressure of oxygen in atmosphere.But due to the presence of crystal growing thermal field, environment relative closure around crystal, crystal ambient oxygen is dense
Spend the partial pressure of oxygen being extremely difficult in furnace chamber.In addition, being filled with quantitative oxygen in crystal growth equipment, accurate gas stream is needed
The devices such as meter increase the cost and long brilliant cost of crystal growth equipment.
Thus, it is necessary to design a kind of growing method of improved crystal to solve the above technical problems.
Summary of the invention
It is an object of the invention to propose a kind of growing method of improved crystal.
To realize foregoing purpose, the present invention adopts the following technical scheme: a kind of growing method of crystal, the growing method packet
Shove charge, heating, lifting process are included, in shove charge by the addition of appropriate pyrolytic oxide among thermal field.
As a further improvement of the present invention, the pyrolytic oxide 400 DEG C or more temperature-rise period and lifted
Cheng Zhonghui decomposites oxygen.
As a further improvement of the present invention, which is metal oxide.
As a further improvement of the present invention, the pyrolytic oxide and its decomposition product will not volatilize.
As a further improvement of the present invention, which includes gallium oxide, calper calcium peroxide, in peromag
At least one.
As a further improvement of the present invention, which decomposes the oxygen of release for crystal growing furnace completely
Furnace chamber in oxygen concentration maintain between 0.01% ~ 0.5%.
The growing method of this crystal is improved the existing long crystallization of lifting, without being filled with into crystal growing furnace
Oxygen decomposites the oxygen come during 400 DEG C or more of heating and long crystalline substance by added pyrolytic oxide
To maintain the partial pressure of oxygen in furnace, the quality of the grown crystal of raising.
Specific embodiment
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention proposes a kind of growing method of crystal, which includes shove charge, heating, lifting process, in shove charge
When by appropriate pyrolytic oxide addition among thermal field.The growing method of this crystal is one kind to the existing long crystallization of lifting
It improves.
As a further improvement of the present invention, the pyrolytic oxide 400 DEG C or more temperature-rise period and lifted
Cheng Zhonghui decomposites oxygen.
As a further improvement of the present invention, which is metal oxide.In the present invention, thermal field material
Material is using materials such as high-temperature oxides, such as zirconium oxide, aluminium oxide, magnesia, mullite.Metal oxygen is added in thermal field material
Compound can react to avoid with thermal field material, will not influence the stability of thermal field.
As a further improvement of the present invention, the pyrolytic oxide and its decomposition product will not volatilize.Crystal growth
Raw material be mostly high pure raw material.It, can be to avoid the pyrolytic oxide of addition using the pyrolytic oxide that will not be volatilized
And decomposition product volatilization pollution raw material.
As a further improvement of the present invention, pyrolytic oxide includes gallium oxide, calper calcium peroxide, in peromag
It is at least one.Gallium oxide can decompose one two galliums of oxidation of generation and oxygen at high temperature.Generation oxygen can be decomposed under calper calcium peroxide high temperature
Change calcium and oxygen.It can be decomposed under peromag high temperature and generate magnesia and oxygen.These oxides and its decomposition product are nontoxic
Harmless, stability is good at high temperature for decomposition product, does not chemically react with thermal field material.
As a further improvement of the present invention, which decomposes the oxygen of release for crystal growing furnace completely
Furnace chamber in oxygen concentration maintain between 0.01% ~ 0.5%.During temperature-rise period and lifting, in 400 DEG C or more of high temperature
Under, pyrolytic oxide slowly decomposes, and gradually releases oxygen, and crystal growth is maintained to have reasonable partial pressure of oxygen, reduces brilliant
The Lacking oxygen quantity that body generates when growing improves crystal quality.Under 0.01% ~ 0.5% oxygen concentration, iridium earthenware can also be avoided
Crucible oxidational losses.It is understood that the additive amount of pyrolytic oxide and the furnace chamber volume of crystal growing furnace are positively correlated.
Pyrolytic oxide can be with accurate weighing, relative to being quantitatively filled with oxygen, it is easier to control, also not need precision
The devices such as gas flowmeter, therefore use this method, long brilliant cost can be reduced.
The preparation-obtained crystal of this method without cracking, bubble, be mingled with, scatter the defects of.
Embodiment 1.
18kg cerium dopping yttrium luetcium silicate raw material is fitted into iridium crucible, it is 1m that iridium crucible, which is placed in furnace chamber volume,3Crystal
In growth furnace, 0.64g calper calcium peroxide is filled between the thermal field around crucible.In crystal growing process, 0.64g calper calcium peroxide is slow
It is slow to decompose, 0.14g oxygen is generated, the partial pressure of oxygen in crystal oven is maintained to reach 0.01%, until long crystalline substance terminates.
It is colourless using the preparation-obtained crystal of above-mentioned growing method, crystal diameter 80mm, length 200mm, crystal
No cracking, the defects of bubble, being mingled with, scattering.
Embodiment 2.
9kg cerium dopping gadolinium gallium-aluminum garnet raw material is fitted into inductive crucible, it is 1.2m that iridium crucible, which is placed in furnace chamber volume,3
Crystal growing furnace in, 10g gallium oxide is filled between the thermal field around crucible.In crystal growing process, 10g gallium oxide is slow
It decomposes, generates 1.7g oxygen, the partial pressure of oxygen in crystal oven is maintained to reach 0.1%, until long crystalline substance terminates.
Use the preparation-obtained crystal of above-mentioned growing method for yellow, crystal diameter 60mm, length 200mm are brilliant
Body without cracking, bubble, be mingled with, scatter the defects of.
Embodiment 3.
27kg neodymium doped yttrium aluminum garnet raw material is fitted into inductive crucible, it is 0.8m that iridium crucible, which is placed in furnace chamber volume,3
Crystal growing furnace in, 20g peromag is filled between the thermal field around crucible.In crystal growing process, 20g peromag
It slowly decomposes, generates 5.7g oxygen, maintaining the partial pressure of oxygen in crystal oven is 0.5%, until long crystalline substance terminates.
Use the preparation-obtained crystal of above-mentioned growing method for purple, crystal diameter 100mm, length 200mm are brilliant
Body without cracking, bubble, be mingled with, scatter the defects of.
The growing method of this crystal is improved the existing long crystallization of lifting, without being filled with into crystal growing furnace
Oxygen decomposites the oxygen come during 400 DEG C or more of heating and long crystalline substance by added pyrolytic oxide
To maintain the partial pressure of oxygen in furnace, the quality of the grown crystal of raising.
Although for illustrative purposes, the preferred embodiment of the present invention is had been disclosed, but the ordinary skill people of this field
Member will realize without departing from the scope and spirit of the invention as disclosed by the appended claims, various to change
Into, increase and replace be possible.
Claims (6)
1. a kind of growing method of crystal, which includes shove charge, heating, lifting process, it is characterised in that: in shove charge
By the addition of appropriate pyrolytic oxide among thermal field.
2. the growing method of crystal according to claim 1, it is characterised in that: the pyrolytic oxide 400 DEG C with
On temperature-rise period and lifting during can decomposite oxygen.
3. the growing method of crystal according to claim 1, it is characterised in that: the pyrolytic oxide is metal oxidation
Object.
4. the growing method of crystal according to claim 1, it is characterised in that: the pyrolytic oxide and its decomposition produce
Object will not volatilize.
5. the growing method of crystal according to claim 1, it is characterised in that: the pyrolytic oxide includes oxidation
At least one of gallium, calper calcium peroxide, peromag.
6. the growing method of crystal according to claim 1, it is characterised in that: the pyrolytic oxide decomposes completely to be released
The oxygen put maintains the oxygen concentration in the furnace chamber of crystal growing furnace between 0.01% ~ 0.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910360867.0A CN110093661A (en) | 2019-04-30 | 2019-04-30 | The growing method of crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910360867.0A CN110093661A (en) | 2019-04-30 | 2019-04-30 | The growing method of crystal |
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| CN110093661A true CN110093661A (en) | 2019-08-06 |
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| CN201910360867.0A Pending CN110093661A (en) | 2019-04-30 | 2019-04-30 | The growing method of crystal |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6158885A (en) * | 1984-08-29 | 1986-03-26 | Nec Corp | Process for growing single crystal |
| CN1450208A (en) * | 2003-05-09 | 2003-10-22 | 中国科学院上海光学精密机械研究所 | Method for growing crystal of lithium aluminate and lithium gallate |
| CN102477580A (en) * | 2010-11-24 | 2012-05-30 | 美国西门子医疗解决公司 | Crystal growth atmosphere for oxyorthosilicate materials production |
| CN102671677A (en) * | 2012-04-27 | 2012-09-19 | 中国科学院福建物质结构研究所 | Annealing method for increasing visible light absorption of bismuth oxychloride photocatalyst |
| CN103046133A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院福建物质结构研究所 | Annealing method for increasing resistivity of ZnO single crystal |
| CN103255478A (en) * | 2012-04-06 | 2013-08-21 | 上海超硅半导体有限公司 | Improvement on structure of crystal growing furnace for pulling alumina single crystal and method for growing alumina single crystal |
-
2019
- 2019-04-30 CN CN201910360867.0A patent/CN110093661A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6158885A (en) * | 1984-08-29 | 1986-03-26 | Nec Corp | Process for growing single crystal |
| CN1450208A (en) * | 2003-05-09 | 2003-10-22 | 中国科学院上海光学精密机械研究所 | Method for growing crystal of lithium aluminate and lithium gallate |
| CN102477580A (en) * | 2010-11-24 | 2012-05-30 | 美国西门子医疗解决公司 | Crystal growth atmosphere for oxyorthosilicate materials production |
| CN103046133A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院福建物质结构研究所 | Annealing method for increasing resistivity of ZnO single crystal |
| CN103255478A (en) * | 2012-04-06 | 2013-08-21 | 上海超硅半导体有限公司 | Improvement on structure of crystal growing furnace for pulling alumina single crystal and method for growing alumina single crystal |
| CN102671677A (en) * | 2012-04-27 | 2012-09-19 | 中国科学院福建物质结构研究所 | Annealing method for increasing visible light absorption of bismuth oxychloride photocatalyst |
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Effective date of registration: 20200508 Address after: 239004 east of yongyang Road, west of Nanjing Road, north of Anqing road and south of Lu'an road in Langya Economic Development Zone, Langya District, Chuzhou City, Anhui Province Applicant after: Anhui Guangzhi Technology Co., Ltd Address before: 511517 Guangdong province Qingyuan Baijia Industrial Park 27-9B Applicant before: FIRST RARE MATERIALS Co.,Ltd. |
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Application publication date: 20190806 |
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