CN105112993B - A kind of device and method for adjusting micro- drop-down crystal growth thermal gradient - Google Patents
A kind of device and method for adjusting micro- drop-down crystal growth thermal gradient Download PDFInfo
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- CN105112993B CN105112993B CN201510655669.9A CN201510655669A CN105112993B CN 105112993 B CN105112993 B CN 105112993B CN 201510655669 A CN201510655669 A CN 201510655669A CN 105112993 B CN105112993 B CN 105112993B
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Abstract
The present invention relates to a kind of device for adjusting micro- drop-down crystal growth thermal gradient, the device is made of graphite, molybdenum or tungsten material, solid liquid interface area installed in micro- drop-down crystal growing apparatus is between low-temperature space, the device includes tubulose heater and fixed seat, fixed seat is fixedly installed on tubulose heating external surface, thermal field distribution required during different crystal Material growth can be directed to, design is corresponding abnormally-structured, can be generated heat under electromagnetic induction.Compared with existing micro- lower pull technology, the device can effectively realize that nearby thermograde is fine-tuned and optimized solid liquid interface, the device is made using materials such as cheap graphite, molybdenum, tungsten, material source is extensive, cost is low, it is simple in construction, its Axial Temperature Distribution to Wen Ti areas plays positive adjustment effect, most appropriate temperature gradient distribution is provided for the growth of high quality single crystal, so as to improve crystal mass and yield rate.
Description
Technical field
The present invention relates to a kind of device and method for adjusting micro- drop-down crystal growth thermal gradient, belong to crystal growth equipment
And technical field.
Background technology
Micro- drop-down (micro-pulling-down, μ-PD) crystal technique belongs to one kind of melt method, compared to tradition
Czochralski method, with advantages such as materials are few, crystal growth cycles are short, crystal pro cessing utilization rate height, is particularly suitable for use in new material exploration
And the industrialized mass production of ripe crystal.In the time of nearly twenties years, the technology is in Japan, France, Italy, U.S. etc.
Numerous research institutions be widely used and develop, can prepare including laser, flicker, non-linear, piezoelectricity ferro,
And a variety of artificial lens including superstructure material etc..
Micro- drop-down can be using the mode of heating of electromagnetic induction or resistance heating come melt raw material, while realizing solid liquid interface
Control, crystal is grown by downward traction in whole process, and the foundation of its thermal field generally comprises crucible heater, refractory material and protected
Warm structure and support pedestal etc..The growth of high quality single crystal needs suitable thermo parameters method, so as to ensure crystalline component and light
The uniformity of quality is learned, it is generally axial symmetry distribution, using single or multiple lift zirconium oxide, aluminum oxide insulating tube, coordinates crucible
A heat-insulation system that can flexibly assemble is constituted with after-heater.
Melt high-temperature region, solid liquid interface area and low-temperature space constitute the axially temperature ladder of micro- drop-down, in order to ensure crystal mass
Axial uniformity, the defect such as while reducing the thermal stress of crystals, prevent from dissociating, ftracture, conventional method is generally using platinum
Spun gold (Journal of Applied Physics, 2008,104,103114) or conventional resistive silk adjust the hair in Wen Ti areas
Heat, to optimize the Axial Temperature Distribution in Wen Ti areas.But this method needs external dc power to supply heating, and assembling is complicated,
And heating wire is yielding, service life is shorter.And for the Temperature Distribution near solid liquid interface, traditional micro- glass tube down-drawing is relied primarily on
Becket post-heater adjusts (Shaped Crystals:Growth by Micro-Pullling-Down Technique,
2007, Springer), using precious metal alloys such as the iraurite consistent with crucible material, platinums, post-heater diameter and crucible are straight
Footpath is identical, and general appearance size is relatively fixed；Larger, whole processing and making is lost in special-shaped make of the noble metal device simultaneously
Cost is very high, therefore this method is very limited for the adjustment effect of temperature ladder distribution near solid liquid interface.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of device for adjusting micro- drop-down crystal growth thermal gradient, should
Device can effectively realize that nearby thermograde is fine-tuned and optimized solid liquid interface, and the device (compared using cheap
The noble metals such as platinum, iraurite) the material such as graphite, molybdenum, tungsten be made, material source is extensive, cost is low, simple in construction, its
Positive adjustment effect is risen to the Axial Temperature Distribution in Wen Ti areas, most appropriate thermograde is provided for the growth of high quality single crystal
Distribution, so as to improve crystal mass and yield rate.
The present invention also provides a kind of device using the micro- drop-down crystal growth thermal gradient of above-mentioned regulation and carries out Temperature Distribution
The method of regulation.
The present invention also provides a kind of installation method for the device for adjusting micro- drop-down crystal growth thermal gradient.
Technical scheme is as follows：
A kind of device for adjusting micro- drop-down crystal growth thermal gradient, the device is made of graphite, molybdenum or tungsten material, pacified
Solid liquid interface area mounted in micro- drop-down crystal growing apparatus is between low-temperature space, and the device includes tubulose heater and fixed seat,
Fixed seat is fixedly installed on tubulose heating external surface, and the top of tubulose heater is close to micro- crucible for pulling down crystal growing apparatus
Bottom；In the refractory material pedestal of the micro- drop-down crystal growing apparatus of edge insertion of fixed seat.
It is currently preferred, the through hole of the refractory material base central of the micro- drop-down crystal growing apparatus of tubulose heater insertion
Interior, the top of tubulose heater is less than crucible bottom nozzle.
It is further preferred that the distance of the top of tubulose heater and crucible bottom nozzle is 5-10mm.Such a design pair
The temperature adjustment effect of solid liquid interface is obvious.
Currently preferred, fixed seat is arranged on the top of tubulose heater.Such a design major regulatory low-temperature space thermal field
Distribution, the adjustable length of tubulose heater.
Currently preferred, described tubulose heater includes upper tubular heater and lower tubular heater, fixed
Seat is fixedly installed between upper tubular heater and lower tubular heater.Such a design can regulate and control crucible bottom solid-liquid simultaneously
Interface area and the Temperature Distribution of low-temperature space.
It is further preferred that described tubulose heater is selected from following one of which or two or more combinations：
Upper tubular heater and lower tubular heating body length are identical or different；
Upper tubular heater is identical with the internal-and external diameter of lower tubular heater,
Upper tubular heater is identical with the internal diameter of lower tubular heater, and external diameter is different,
To be abnormally-structured at the top of the upper end of upper tubular heater.
Still more preferably, it is described abnormally-structured for any shapes such as arcs of recesses, concavo-convex alternate shapes or zigzag.For
The situation that crucible bottom nozzle heat is concentrated, arcs of recesses adjustable structure thermoisopleth is close to level；Carried if desired for heat-generating pipe top
For small heat, then it can be realized by zigzag structure.
The device of the present invention can be according to requirement of the target crystal material for temperature ladder near solid liquid interface, and design is suitable
Abnormally-structured tubulose heater, you can to change thickness, length, end shape, top end diameter size or adjustment perforate size
With shape etc..
It is currently preferred, offer peep hole on the side wall of lower tubular heater, described peep hole for it is square,
Any shapes such as rectangle, circle or ellipse.
Currently preferred, described fixed seat is annular or side's annular, it is preferred that fixed seat is annular.Annulus
Shape fixed seat can be such that the device hangs on refractory material pedestal.
Currently preferred, the tubulose heater internal diameter is 8-12mm.
The device of the present invention produces heat by electromagnetic induction, and the top of tubulose heater, can be direct close to crucible bottom
Regulate and control the heat distribution near solid liquid interface, different tubulose heater diameters and thickness are designed according to the distribution of target thermal field.
The present invention can design corresponding diameter, thickness and length according to the distribution of target thermal field, so as to optimize caloric value.
The structure is generated heat under electromagnetic induction, can be compensated and be adjusted solid liquid interface thermal field nearby, also can adjust whole crystal growth
Axial temperature field, is proved by many experiments, device of the invention finally can optimization be adapted to the thermal field distribution of aimed crystal growth,
It is final to improve crystal mass and yield rate.
A kind of method that Temperature Distribution is adjusted in device using the micro- drop-down crystal growth thermal gradient of above-mentioned regulation, bag
Include step as follows：
In the through hole that said apparatus is fixed on to the refractory material base central of micro- drop-down crystal growing apparatus, the device exists
Generated heat under electromagnetic induction, for compensating and adjusting thermal field near solid liquid interface, or adjust the axial temperature field of whole crystal growth.
Corresponding regulating and controlling temperature scope can be set according to different crystal using the device of the present invention.
The installation method of the above-mentioned micro- drop-down crystal growth thermal gradient device of regulation is expensive with carrying by the device during shove charge
The refractory material pedestal of metallic crucible and after-heater is engaged, and noble metal after-heater and crucible, heat-insulation and heat-preservation are then combined successively
Material, fills protective gas and carries out crystal growth.
Above-mentioned micro- drop-down crystal growing apparatus is prior art, and it is (artificial brilliant that domestic equipment and technology for details, reference can be made to document
Body journal, 2014,43,1317-1322), overseas equipment and technology for details, reference can be made to works (Shaped Crystals:Growth
by Micro-Pullling-Down Technique,2007,Springer)。
The device and method for the micro- drop-down crystal growth temperature ladder of regulation that the present invention is provided, with the body phase of generating heat such as existing platinum wire
Than with advantages below：
(1) thermal field near more effective regulation solid liquid interface：Traditional micro- drop-down generally uses platinum wire, Aludirome
Resistance wire etc., is generated heat by way of direct current, and which only allows part of the resistance wire below insulation material pedestal
Use, therefore very little is contributed for the thermal field of crystal growth solid liquid interface.The present invention is made using high-melting-point conductor material, can be led to
The mode for crossing electromagnetic induction produces heat, therefore the device can be placed near crucible bottom nozzle, directly effectively adjust solid-liquid
The thermal field of near interface.
(2) special-shaped processing is easily realized, thermal field regulation is trickleer：The micro- pull-down device in part is using noble metals such as platinum, iraurites
Pipe designs thermal field, but the processing of these objectss made from precious metals is present that difficulty is big, the shortcomings of be lost many, therefore can not realize trickle different
Type structure fabrication, can not more realize large-scale promotion and use.Apparatus of the present invention are made using graphite or molybdenum pure metals, raw material
Source is relatively extensive, and the processing characteristics such as hardness is moderate, and the special-shaped processing of this device can be achieved in general unit, makes and is processed into
This is relatively low, therefore this method universality is very strong.
Brief description of the drawings
Fig. 1 is that the device of the micro- drop-down crystal growth thermal gradient of regulation of the present invention is fixed on micro- drop-down crystal growing apparatus
In structural representation；
Wherein 1 is crucible, 2 is melt, 3 is crucible bottom nozzle, 4 be solid liquid interface area, and 5 be upper tubular heater, 6
It is lower tubular heater for fixed seat, 7,8 be the crystal grown out, and 9 be micro- refractory material for pulling down crystal growing apparatus
Pedestal.
Fig. 2 is that the device fixed seat of the present invention is arranged on the structural representation at the top of tubulose heater, is mainly used in regulation
The thermograde of axial low-temperature space；
Wherein a figures are the shorter structural representation of tubulose heater, and b figures are the longer structural representation of tubulose heater, c
Figure is the structural representation that circular peep hole is provided with tubulose heater, and d figures are that rectangle observation is provided with tubulose heater
The structural representation in hole.
In figure, 6 be fixed seat, and 10 be tubulose heater, and 11 be peep hole.
Fig. 3 is to include the structural representation of upper tubular heater and lower tubular heater, top for tubulose heater
Tubulose heater, is distributed for adjusting thermal field near crucible bottom solid liquid interface；
Wherein a figures are the structural representation that lower tubular heating body length is more than upper tubular heater, and b figures are upper tube
The top of shape heater is the structural representation of concavo-convex interphase structure, and it is arcs of recesses knot at the top of upper tubular heater that c figures, which are,
Structure schematic diagram, d figures are that upper tubular heater is identical with the internal diameter of lower tubular heater, the different structural representation of external diameter；
In figure, 5 be upper tubular heater, and 7 be lower tubular heater.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
Embodiment 1
A kind of device for adjusting micro- drop-down crystal growth thermal gradient, the device is made of graphite, installed in micro- drop-down
The solid liquid interface area of crystal growing apparatus is between low-temperature space, and the device includes tubulose heater 10 and fixed seat 6, fixed seat 6
The outer surface of tubulose heater 10 is fixedly installed on, tubulose heater 10 inserts the refractory material pedestal of micro- drop-down crystal growing apparatus
In the through hole at 9 centers, the top of tubulose heater 10 is close to micro- crucible bottom for pulling down crystal growing apparatus；The side of fixed seat 6
In the refractory material base 9 of the micro- drop-down crystal growing apparatus of edge insertion, the top of tubulose heater 10 is less than crucible bottom nozzle 3,
The top of tubulose heater 10 is 6mm with the distance of crucible bottom nozzle 3.Fixed seat 6 is annular, and annular fixed seat can make
The device is hung on refractory material pedestal.The internal diameter of tubulose heater 10 is 10mm.
Embodiment 2
The side of Temperature Distribution is adjusted using the device of the micro- drop-down crystal growth thermal gradient of regulation described in embodiment 1
Method, step is as follows：
The device for adjusting micro- drop-down crystal growth thermal gradient is fixed on to the refractory material of micro- drop-down crystal growing apparatus
In the through hole at the center of pedestal 9, the device generates heat under electromagnetic induction, for compensating and adjusting thermal field near solid liquid interface, or adjusts
Save the axial temperature field of whole crystal growth.
Embodiment 3
The installation method of the micro- drop-down crystal growth thermal gradient device of regulation, during shove charge, by the device and carrying noble metal
The refractory material pedestal of crucible and after-heater is engaged, and noble metal after-heater and crucible, heat-insulating heat-preserving material are then combined successively,
Fill protective gas and carry out crystal growth.
The method that micro- drop-down growth crystal is carried out using apparatus and method of the present invention, step is as follows：
(1) according to the chemical constitution and thermal property of target crystal material, the graphite regulation of design and making high-purity is micro-
Pull down crystal growth thermal gradient device.
(2) prepare raw material, crucible, thermal field insulation material, seed crystal, the invention device is pressed with micro- drop-down crystal growing apparatus
Above-mentioned relation is used cooperatively, and sees Fig. 1.
(3) after shove charge is finished, 10Pa or so is evacuated to, protective atmosphere, power per liter is filled until melting sources, are sequentially passed through
Sow, shouldering, it is isometrical, carry it is de-, cooling Four processes, blow-on take out target crystal.
Embodiment 4
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 1, and difference is：
The device of the micro- drop-down crystal growth thermal gradient of regulation is made of simple substance molybdenum, it is considered to the difference of graphite and molybdenum simple substance
Electromagnetic induction performance, targetedly calculates and adjusts the electro-heat equipment.
Embodiment 5
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 1, and difference is：
The device of the micro- drop-down crystal growth thermal gradient of regulation is made of simple substance tungsten, it is considered to the difference of graphite and tungsten simple substance
Electromagnetic induction performance, targetedly calculates and adjusts the electro-heat equipment.
Embodiment 6
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 1, and difference is：
Fixed seat 6 is arranged on the top of tubulose heater 10, and this is designed primarily for the temperature ladder for adjusting axial low-temperature space
Degree, it can open up part peep hole according to demand on the side wall of tubulose heater 10, to record crystal in time in specific temperature
The quality condition of terraced position, is shown in that Fig. 2, Fig. 2 list the different situations that fixed seat 6 is arranged on the top of tubulose heater 10.
Embodiment 7
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 1, and difference is：
Tubulose heater 10 includes upper tubular heater 5 and lower tubular heater 7, and fixed seat 6 is fixedly installed on
Between portion's tubulose heater 5 and lower tubular heater 7, structure is as shown in fig. 1.
Embodiment 8
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 7, and difference is：
Upper tubular heater 5 is identical with the internal diameter of lower tubular heater 7, and external diameter is different, and structure is shown in Fig. 3 d figures institute
Show.
Embodiment 9
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 7, and difference is：
It is abnormally-structured at the top of the upper end of upper tubular heater, abnormally-structured is arcs of recesses or concavo-convex alternate shape, structure
See shown in Fig. 3 b, c figure.
Embodiment 10
The device of micro- drop-down crystal growth thermal gradient is adjusted as described in Example 1, and difference is：
Upper tubular heater is different from lower tubular heating body length, sees that Fig. 3, Fig. 3 list upper tubular heater
Several situations different from lower tubular heating body length.
The present invention is directed to propose a kind of device and method for adjusting micro- drop-down crystal growth thermal gradient, the program is applied to
All crystalline materials for meeting micro- drop-down growth conditions.Those of ordinary skill in the art may be to some technical characteristics of the invention
Modify, without departing from the connotation of technical solution of the present invention, these changes all should be covered claimed in the present invention
Within the scope of technical scheme.
Claims (10)
1. a kind of device for adjusting micro- drop-down crystal growth thermal gradient, the device is made of graphite, molybdenum or tungsten material, installed
In the solid liquid interface area of micro- drop-down crystal growing apparatus between low-temperature space, the device includes tubulose heater and fixed seat, Gu
Reservation is fixedly installed on tubulose heating external surface, and the top of tubulose heater is close to the crucible bottom of micro- drop-down crystal growing apparatus
Portion；In the refractory material pedestal of the micro- drop-down crystal growing apparatus of edge insertion of fixed seat.
2. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 1, it is characterised in that tubulose generates heat
In the through hole of the refractory material base central of the micro- drop-down crystal growing apparatus of body insertion, the top of tubulose heater is less than crucible bottom
Portion's nozzle.
3. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 1, it is characterised in that tubulose generates heat
The top of body is 5-10 mm with the distance of crucible bottom nozzle.
4. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 1, it is characterised in that fixed seat is set
Put at the top of tubulose heater.
5. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 1, it is characterised in that described pipe
Shape heater includes upper tubular heater and lower tubular heater, and fixed seat is fixedly installed on upper tubular heater with
Between portion's tubulose heater.
6. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 5, it is characterised in that described pipe
Shape heater is selected from following one of which or two or more combinations：
Upper tubular heater and lower tubular heating body length are identical or different,
Upper tubular heater is identical with the internal-and external diameter of lower tubular heater or internal diameter is identical, and external diameter is different,
To be abnormally-structured at the top of the upper end of upper tubular heater.
7. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 6, it is characterised in that the abnormal shape
Structure is arcs of recesses, concavo-convex alternate shape or zigzag.
8. the device of the micro- drop-down crystal growth thermal gradient of regulation according to claim 5, it is characterised in that in lower tube
Peep hole is offered on the side wall of shape heater, described fixed seat is annular or side's annular；Annular fixed seat can make this
Device is hung on refractory material pedestal, and the tubulose heater internal diameter is 8-12 mm.
9. Temperature Distribution is adjusted in a kind of device of the micro- drop-down crystal growth thermal gradient of regulation described in utilization claim 1
Method, including step is as follows：
In the through hole that said apparatus is fixed on to the refractory material base central of micro- drop-down crystal growing apparatus, the device is in electromagnetism
Sensing is lower to generate heat, and for compensating and adjusting thermal field near solid liquid interface, or adjusts the axial temperature field of whole crystal growth.
10. the installation method of the micro- drop-down crystal growth thermal gradient device of regulation described in claim 1, during shove charge, this is filled
Put and be engaged with the refractory material pedestal of carrying noble metal crucible and after-heater, noble metal after-heater and earthenware are then combined successively
Crucible, heat-insulating heat-preserving material, fill protective gas and carry out crystal growth.
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| CN105839176A (en) * | 2016-05-17 | 2016-08-10 | 中国科学院上海光学精密机械研究所 | Micro drop-down crystal growth device automatically controlled and automatic control method |
| CN109778308B (en) * | 2019-03-05 | 2020-10-30 | 山东大学 | Device and method for adjusting crystal growth temperature gradient of laser heating base |
| US11856678B2 (en) * | 2019-10-29 | 2023-12-26 | Senic Inc. | Method of measuring a graphite article, apparatus for a measurement, and ingot growing system |
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| JP3825127B2 (en) * | 1997-03-27 | 2006-09-20 | 日本碍子株式会社 | Single crystal growth method and apparatus |
| TW200510581A (en) * | 2003-07-17 | 2005-03-16 | Stella Chemifa Corp | Method for producing crystal of fluoride |
| JP2007197269A (en) * | 2006-01-27 | 2007-08-09 | Nec Tokin Corp | Crucible for growing crystal and method of growing single crystal |
| CN202865394U (en) * | 2012-09-25 | 2013-04-10 | 倪屹 | Three-dimensional sapphire crystal growing apparatus |
| JP5968198B2 (en) * | 2012-11-08 | 2016-08-10 | 国立大学法人東北大学 | Single crystal manufacturing method |
| CN103060891B (en) * | 2013-01-31 | 2015-04-29 | 长春理工大学 | Device and method for directionally growing fluoride single crystal via lifting small-gradient thermal field |
| CN104611764B (en) * | 2015-01-21 | 2017-10-31 | 华中科技大学 | A kind of micro- downward lifting crystal growing furnace |
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Effective date of registration: 20230411 Address after: 221100 West Floor 2, Building 3, Area A, Xuzhou Huaihai Biomedical Industrial Park, No. 10, the Pearl River East Road, Xuzhou High tech Industrial Development Zone, Xuzhou, Jiangsu Patentee after: Jiangsu Jingying Optoelectronic Technology Co.,Ltd. Address before: No. 27, mountain Dana Road, Ji'nan City, Shandong, Shandong Patentee before: SHANDONG University |