CN106480493B - A kind of heating device for crystal growth - Google Patents
A kind of heating device for crystal growth Download PDFInfo
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- CN106480493B CN106480493B CN201510536016.9A CN201510536016A CN106480493B CN 106480493 B CN106480493 B CN 106480493B CN 201510536016 A CN201510536016 A CN 201510536016A CN 106480493 B CN106480493 B CN 106480493B
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Abstract
The present invention relates to a kind of New Heatings for crystal growth, outward successively include: crucible, heater, thermal insulation material and induction coil from center, wherein the crucible is used to accommodate the melt of growth crystal and does not have heating function；The heater is spaced with the crucible, and receives the signal of the induction coil to generate heat and heat source as crystal growth.The present invention has not only broken the traditional method that can only passively construct thermal field by adjusting thermal insulation material using crucible as heater, can actively construct suitable thermal field by the shape and size of regulation heating body；Furthermore it is also possible to which the mode of induction heating is applied in Bridgman method crystal growth, the use scope of Bridgman method has been widened.
Description
Technical field
The present invention relates to a kind of New Heatings for crystal growth, and in particular to is applied to crystal growth to a kind of
The heating device that suitable temperature field can effectively be established in furnace for a long time, belongs to technical field of crystal growth.
Background technique
Artificial crystal material is able to achieve conversion between the different forms energy such as electricity, light, sound, thermal and magnetic, power and mutually because of it
Effect, becomes critical function material indispensable in new and high technology, is widely used in communication, computer, medical treatment, core object
The civil fields such as reason, detection, electronic equipment.In recent years, with the continuous development of new and high technology, the artificial lens demand in market pair
Sustainable growth mainly develops towards high-quality, low cost and extensive direction.
The preparation method of artificial lens has very much, be broadly divided into room temperature solwution method, pyrosol/melt method, vapor phase method and
Solid phase method etc..Wherein using pyrosol/melt method for crystal growth necessarily by raw material heating fusing then in suitable temperature
It crystallizes off field；Vapor phase method need for raw material to be heated to after sublimation point to condense under suitable temperature field and airflow field effect and
At.It is now generally used for that the mode that raw material heats mainly is had to the modes such as resistance-type, induction type and laser heating.
Resistance heating uses electric current to pass through the materials such as resistance wire, Elema, Si-Mo rod, tungsten, molybdenum generally to generate heat.Its
Middle resistance wire, Elema and Si-Mo rod only up to be used due to temperature limiting to 1700 DEG C, but use for a long time can become
Shape is easy failure.And induction heating is then to generate vortex by the way that heater to be placed in alternating magnetic field, and heat generating member is caused to generate heat,
Its heater can be the materials such as cast iron, platinum, iraurite, graphite and molybdenum.This heating method maximum operation (service) temperature is by heater
Fusing point determine, can use for a long time, and heat quickly, efficiently, be widely used in Metal Melting, welding, heat preservation and
In the equipment such as crystal growth.
Different from other fields, the induction heating mode for crystal growth is other than providing basic heating function, also
It must play the role of constructing temperature field, and this is vital for growing high quality crystal.Because of crystal growth
The temperature field of system will affect the temperature gradient at growth solid liquid interface, will directly determine that can crystal growth go on smoothly and brilliant
The superiority and inferiority (the defects of control crystal) of the quality of body.
The temperature field that different crystal needs is not also identical, and big temperature gradient is conducive to crystal growth under normal circumstances, can
To improve rate of crystalline growth, but big stress can be generated in crystal, so as to cause crystal cleavage.In addition, thermal field also shadow
The solid-liquid interface shape for ringing crystal growth under general condition, is intended to obtain planar interface (or dimpling) to improve crystal quality,
Inhibit crystal defect.In short, the temperature field that design construction is different is needed according to different crystal types, to meet growth Gao Pin
The needs of matter crystal.
If crystal growth system is to directly adopt during constructing temperature field using induction heating mode
Crucible is limited because of the shape and size of crucible by the shape and size of grown crystal again as heater, cannot
Free variation, so its effect for adjusting temperature field is very weak.In view of the foregoing, traditional induction heating mode is all mainly
Temperature field is adjusted by the shape and size for adjusting thermal insulation material.Although under the conditions of major part, can expire to a certain extent
Sufficient crystal growth needs, but changes the very time-consuming effort of shape and size of thermal insulation material, and the life for crystal
Length will not be able to satisfy actual use needs.
For example, boracic acid oxygen calcium yttrium crystal (YCa4B3O10, following shorthand is at YCOB) and it is a kind of very important nonlinear optical
Crystalline material is learned, is had a wide range of applications in ultra-intense laser field, but its premise that can obtain application must have greatly
Size (bore is greater than 200mm × 200mm), high-quality (the defects of no inclusion enclave, bubble).Currently, the small size of open report
The growing method of YCOB crystal mainly have Bridgman method (referring to Materials research bulletin 2012,47:
2689-2691) and czochralski method (referring to Journal of crystal growth 2014,401:160-163), but its maximum ruler
Very little only 100mm, is unable to reach application requirement.Its reason is analyzed, mainly Czochralski grown large scale YCOB crystal cannot have
The defects of effect control crystal, and its crystal internal stress is big, is easy cracking, causes finally obtain large size and high quality crystalline substance
Body；However, although Bridgman method can grow high quality YCOB crystal, when growing large-size YCOB crystal, growth
Period is more than 30 days；And YCOB crystalline melting point is 1510 DEG C, in addition growth needs certain temperature gradient, so growth furnace
Temperature has reached 1600 DEG C, and the growth conditions of so harshness has all reached the growth limit of Bridgman method substantially.Experiment is also demonstrate,proved
Bright existing Bridgman method is unable to satisfy this requirement, and heating element Si-Mo rod is grow into 15~25 days will be because
For deformation is excessive and is broken.It solves the above problems and just necessarily changes the heating method of Bridgman method.In existing technology
Under the conditions of, although although the temperature of YCOB crystal growth can be competent at as the Bridgman method of heater using tungsten, molybdenum,
It is YCOB is oxide crystal, and tungsten, molybdenum cannot be used in oxidation environment, so cannot use.
In conclusion field of crystal growth very meets the growth need of different crystal there is an urgent need to novel heating method
It wants.
Summary of the invention
The purpose of the present invention is to provide a kind of Novel heating modes that can be used for crystal growth, are not only able to satisfy tradition
Heating function, also having the function of can be with flexible modulation crystal growth temperature-field.Shape, the size of heater are carried out appropriate
Adjustment can be suitable for growing different types of crystal, be used in Bridgman method that Bridgman method will can be widened
Use scope.
Here, the present invention provides a kind of heating device for crystal growth, the heating device from center outward successively
It include: crucible, heater, thermal insulation material and induction coil, wherein
The crucible is used to accommodate the melt of growth crystal and does not have heating function；
The heater is spaced with the crucible, and receives the signal of the induction coil to generate heat and raw as crystal
Long heat source.
Heating device of the invention has abandoned traditional induction type crystal growing furnace and has directlyed adopt crucible as heater
Heating method, use independent heater instead as heating element, crucible made no longer to have the function of calandria.The present invention is not
The traditional method that can only passively construct thermal field by adjusting thermal insulation material using crucible as heater, Ke Yitong are only broken
The shape and size of heater are overregulated actively to construct suitable thermal field；Furthermore it is also possible to by the mode application of induction heating
In Bridgman method crystal growth, the use scope of Bridgman method has been widened.The present invention is simple and practical, does not need to original
Growing system carry out large-scale redevelopment, that is, implementable, suitable for all systems for carrying out crystal growth using induction heating mode
In, especially suitable in high temperature Bridgman method crystal growth system.
Preferably, the heating device further includes the filled media between the crucible and the heater.
Preferably, the shape and size of the crucible are determined according to the shape and size of the crystal grown.
Preferably, the material of the crucible is determined according to the type of the crystal grown and growth atmosphere.
Preferably, by adjusting the shape and size of the heater come temperature field needed for obtaining crystal growth.
Preferably, the material of the heater is the material that can receive induction heating, and according to the crystal grown
Type determines.
Preferably, assisting constructing temperature field by adjusting the shape and size of the thermal insulation material.
Preferably, assisting constructing temperature field by adjusting the shape and size of the filled media.
Preferably, the heating device is felt for czochralski method, Bridgman method, kyropoulos, vapor transportation and other use
The method for answering heating method to carry out crystal growth.
The present invention also provides a kind of crystal growing furnaces for having the above-mentioned heating device for crystal growth.
New Heating provided by the invention not only has significant improvement in terms of adjusting temperature field, makes adjustable parameter
Become more, and also relatively easily fast implement, and the mode of induction heating can be extended in Bridgman method crystal growth, opens up
The wide use scope of Bridgman method.
Detailed description of the invention
Fig. 1 is the schematic diagram of the heating device for crystal growth of an example of the present invention, wherein 1- crucible, 2- are filled out
Filling medium, 3- heater, 4- thermal insulation material, 5- induction coil；
Fig. 2 is the shape of two kinds of typical heaters.
Specific embodiment
Hereinafter, referring to attached drawing, and the present invention is further illustrated with the following embodiments.It should be understood that these attached drawings and implementation
Mode is merely to illustrate the present invention, rather than the limitation present invention.
The present invention provides a kind of New Heating of crystal growth, and specifically a kind of be applied in crystal growing furnace can be with
The heating device of suitable temperature field is effectively established for a long time.
Fig. 1 shows the schematic diagram of the heating device for crystal growth of an example of the present invention.As shown in Figure 1, described
Heating device may include: crucible 1, filled media 2, heater 3, thermal insulation material 4 and induction coil 5 from center outward.
The crucible 1 is mainly used for containing melt, and compared with traditional heating method, the crucible in the present invention does not have
The function of heater only undertakes the function of container.
The shape and size of crucible can be corresponding to do according to the shape of the different crystal of different growing methods, growth
Adjustment.For example, being used to can be made circle when Czochralski grown crystal, size grows the size of crystal as needed to design really
It is fixed；In Bridgman method, crucible shape and size are consistent with the shape and size of the crystal grown, can be it is round,
Rectangular and other irregular shapes etc..
The material of crucible can correspond to selection according to the difference of the growth atmosphere of grown crystal, comprising: platinum, iraurite,
The materials such as graphite, quartz.
That is, the shape of crucible, size and material can design determination according to the crystalline material type of growth, and
It is little with temperature field relationship needed for crystal growth.For example, its shape can be designed according to the shape of grown crystal, can be
Round, rectangular and irregular shape etc.；Platinum, iraurite, quartz, graphite used by its material can be crystal growth usually etc.
Material, but its selection must be according to the crystalline grown come reasonable selection.Such as: platinum crucible can be used in various gas
It in atmosphere, but is limited, only up to be used to 1600 DEG C by its fusing point；Iridium Crucible can only be useful in inert atmosphere or micro-
The atmosphere kind of oxygen, cannot directly be useful in oxygen atmosphere；Silica crucible is limited in 1000 DEG C also because its fusing point is low
It is used below；Graphite crucible only can be used in reduction or inert atmosphere, cannot be with the presence of some oxygen.
Filled media 2 between crucible 1 and heater 3 is mainly used to that crucible 1 and heater 3 is isolated.But Ying Li
Solution, the present invention can not also include filling material 2, i.e., between crucible 1 and heater 3 can also directly be spaced and be not filled with
Medium (being growth atmosphere i.e. between crucible 1 and heater 3).When being not provided with filling material 2, between crucible 1 and heater 3
Spacing distance can requirement according to the crystal grown to temperature field design determination, may be, for example, 1~10mm.
In addition filled media 2 also functions to the effect that auxiliary constructs temperature field, shape, size and material can be according to crucibles
It is selected with temperature field requirement.Specifically, its shape, size can match with shape, the size of crucible.Its material, thickness
Degree and whether there is or not can requirement according to the crystal grown to temperature field design determination.For example, its thickness can be 1~20mm.
Its material includes but is not limited to select the common thermal insulation material such as aluminium oxide, zirconium oxide, carbon felt, asbestos and its derived product.
Heater 3 is mainly used to the signal of induction receiving coil 5 to generate heat, is the heat source of crystal growth, therefore its
Shape, size will directly affect the temperature field of crystal growth system.It can be obtained in the present invention by adjusting its shape and size
Obtain the ideal temperature field of crystal growth.
That is, the shape of heater 3, size and material are set according to the crystalline material and its required temperature field that are grown
Meter determines.Its shape can be consistent substantially with the shape of the crystal grown, but can also be different, and objective is exactly
Construct suitable temperature field, such as can be round, rectangular and irregular shape etc..That is, its shape and size may be used also
To be determined according to the shape and size of crucible, preferably match with the shape and size of crucible.
Fig. 2 shows the shapes of two kinds of typical heaters.Wherein left figure is circle, and shape mainly includes three sizes,
Height H, Outside Dimensions Do and interior enclose dimension D i.Height H can be 50~100mm, and Outside Dimensions Do can be 50~100mm, inside enclose
Dimension D i can be 48~98mm.Right figure be it is rectangular, height can be 50~100mm, peripheral lengths can be 50~100mm, periphery
Width can be 48~98mm.
The material of heater 3 can determine that can select can receive induction heating according to the type of the crystal of growth
All materials, it is common to include but is not limited to: cast iron, platinum, iraurite, graphite, tungsten, molybdenum etc..
Thermal insulation material 4 primarily serves heat preservation and auxiliary constructs the effect of thermal field, in addition also functions to energy-saving effect.?
In traditional heating method, since crucible is heater, and shape and size all receive the limitation of grown crystal,
Effect in terms of adjusting temperature field is many smaller, so thermal insulation material just plays very important angle in terms of constructing temperature field
Color.Novel heating mode provided by the invention, because there is individual heater that can be used to adjust temperature field, thermal insulation material
The function of adjusting temperature field is weakened.Thermal insulation material 4 is preferably close together with heater 3.
Shape, the size of thermal insulation material 4 can design determination according to temperature field required for the crystalline material grown.Example
Such as, thickness can be 20~100mm.
The selection of the material of thermal insulation material 4 is only limited by the growth atmosphere and maximum growth temperature of the crystal grown, can
Common thermal insulation material, the including but not limited to materials such as aluminium oxide, zirconium oxide, carbon felt, asbestos are selected, also including these materials
Derived product, such as alumina hollow ball product, Zirconium oxide fibre.
Induction coil 5 mainly plays reception external power supply signal, is then passed to the function of heater.Its shape and size one
As can be determined according to the peripheral shape of thermal insulation material and size.The material of induction coil 5 is unlimited, can be had using any
The material of its function, such as hollow copper tubing etc..
The present invention also provides a kind of heating means, i.e., not using crucible as heating element, but with the fever independently of crucible
Body is heated as heating element, and constructs suitable temperature field by the shape and size of the adjusting heater.Separately
Outside, it can also assist constructing temperature field by adjusting the shape and size of the packing material and/or the thermal insulation material.
Heating device and heating means of the invention be suitable for czochralski method, Bridgman method, kyropoulos, vapor transportation and its
The method that it carries out crystal growth using induction heating mode.It is particularly applied in Bridgman method crystal growth, widens
The use scope of Bridgman method.
In traditional Bridgman method, crucible is constantly moved downward with being grown in for crystal, if using induction
The mode of heating, since crucible also has the function of heater simultaneously, then entire heater is not during growth all
It is disconnectedly mobile, it directly results in temperature and grows and constantly changing, so cannot use.But New Heating provided by the invention and
Heating means, crucible and heater be it is relatively independent, the growth of crystal will not influence temperature field, it is possible to using induction plus
Heat.
For example, in the system of Bridgman method growth YCOB crystal, if using New Heating of the invention and
Heating means, heater select platinum that will solve the problems, such as that original system Si-Mo rod cannot work long hours, raw for YCOB crystal
It is long that stable, efficient heating source is provided.
From the point of view of above-mentioned principle, New Heating and heating means provided by the invention are not only adjusting temperature field side
There is significant improvement in face, make adjustable parameter become it is more (such as can based on the shape and size of regulation heating body, with adjusting fill out
Supplemented by the shape and size of filling medium and/or thermal insulation material), and also relatively easily fast implement, and by the mode of induction heating
It is extended in Bridgman method crystal growth.
The present invention also provides a kind of crystal growing furnaces with above-mentioned heating device.The crystal growing furnace can also have it
Its device, such as seed rod, bonnet etc..It should be understood that there is no limit as long as do not influence this hair for other components of the crystal growing furnace
Bright purpose.When heating device of the invention is used for crystal growing furnace, do not need to carry out original growing system big
Scale transformation is i.e. implementable, suitable for all systems for carrying out crystal growth using induction heating mode, especially suitable for height
In warm Bridgman method crystal growth system.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Parameter is also only an example in OK range, i.e., those skilled in the art suitable model can be done by the explanation of this paper
Interior selection is enclosed, and does not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Structure is as shown in Figure 1, crucible is made of the round iraurite of Φ 100mm × 80mm × 2mm；Filled media is growth
Atmosphere (is equivalent to fill-media-free), with a thickness of 4mm；Heater is made of iraurite, and Outside Dimensions are Φ 112mm, is inside enclosed
It is highly 90mm having a size of Φ 108mm；Thermal insulation material selects aluminium oxide ceramic products, with a thickness of 40mm；Induction coil is using empty
Heart round copper pipe is made, internal diameter 200mm.This system is used for 2 inches of YCOB crystal of Czochralski grown, and the crystalline size of acquisition is
The defects of Φ 55mm × 120mm, crystal perfection, no scattering particles, inclusion enclave, bubble, can be used for cutting piezoelectricity and nonlinear optical
Element.
Embodiment 2
Structure is as shown in Figure 1, crucible uses the rectangular of 80mm × 50 × 120mm × 0.2mm (length × width × height × thickness)
Platinum is made；Filled media is calcined oxide aloxite, with a thickness of 15mm；Heater is made of platinum, and Outside Dimensions are
100mm × 70mm is highly 60mm with a thickness of 2mm；Thermal insulation material selects zirconia ceramic product, with a thickness of 30mm；Induction
Coil is made of hollow side's copper pipe, inside encloses size 140mm × 110mm.This system grows 3 inches for Bridgman method
YCOB crystal, the crystalline size of acquisition are 80mm × 50mm × 120mm, crystal perfection, no scattering particles, inclusion enclave, bubble etc.
Defect can be used for cutting piezoelectricity and nonlinear optics element.
Although above having used general explanation, specific embodiment etc., the present invention is described in detail,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (7)
1. a kind of heating means for crystal growth, which is characterized in that grow crystal using Bridgman method, and use and add
Thermal carries out, the heating device from center outward successively include: crucible, heater, thermal insulation material and induction coil,
In,
The crucible is used to accommodate the melt of growth crystal and does not have heating function；
The heater is spaced with the crucible, and receive the signal of the induction coil come generate heat and as crystal growth
Heat source；
By adjusting the shape and size of the heater come temperature field needed for obtaining crystal growth.
2. the heating means according to claim 1 for crystal growth, which is characterized in that further include being located at the crucible
Filled media between the heater.
3. the heating means according to claim 1 for crystal growth, which is characterized in that the shape and ruler of the crucible
It is very little to be determined according to the shape and size of the crystal grown.
4. the heating means according to claim 1 for crystal growth, which is characterized in that the material of the crucible according to
The type of the crystal grown and growth atmosphere determine.
5. the heating means according to claim 1 for crystal growth, which is characterized in that the material of the heater is
The material of induction heating can be received, and is determined according to the type of the crystal grown.
6. the heating means according to claim 1 for crystal growth, which is characterized in that by adjusting the thermal insulating material
The shape and size of material assist constructing temperature field.
7. the heating means according to claim 1 for crystal growth, which is characterized in that by adjusting filling Jie
The shape and size of matter assist constructing temperature field.
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| CN107653487A (en) * | 2017-10-23 | 2018-02-02 | 安徽中晶光技术股份有限公司 | A kind of recycling bin for being used in crystal growing process reclaim iridium powder |
| CN108441938A (en) * | 2018-03-06 | 2018-08-24 | 同济大学 | Special-shaped thermal-field device suitable for crystal growth |
| CN108385160A (en) * | 2018-03-12 | 2018-08-10 | 安徽晶宸科技有限公司 | A kind of devices and methods therefor adjusting sensing heating method of crystal growth by crystal pulling thermal field gradient |
| CN113370591B (en) * | 2021-07-12 | 2022-12-23 | 成都东骏激光股份有限公司 | High-temperature volatilization inhibition device and method and application of device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257943A (en) * | 1999-12-16 | 2000-06-28 | 中国科学院上海光学精密机械研究所 | Equipment for growing high-temp oxide crystal |
| CN2571773Y (en) * | 2002-10-14 | 2003-09-10 | 德清华莹电子有限公司 | Thermal field device for crystal growth |
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| CN103180492B (en) * | 2010-10-13 | 2016-10-26 | Tdk株式会社 | The raw material used in LGS type oxide material, its manufacture method and this manufacture method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257943A (en) * | 1999-12-16 | 2000-06-28 | 中国科学院上海光学精密机械研究所 | Equipment for growing high-temp oxide crystal |
| CN2571773Y (en) * | 2002-10-14 | 2003-09-10 | 德清华莹电子有限公司 | Thermal field device for crystal growth |
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