CN102787350A - Device and method of growing 500-1000mm long bismuth germanate crystals by descent method - Google Patents
Device and method of growing 500-1000mm long bismuth germanate crystals by descent method Download PDFInfo
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- CN102787350A CN102787350A CN2012103222194A CN201210322219A CN102787350A CN 102787350 A CN102787350 A CN 102787350A CN 2012103222194 A CN2012103222194 A CN 2012103222194A CN 201210322219 A CN201210322219 A CN 201210322219A CN 102787350 A CN102787350 A CN 102787350A
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Abstract
The invention provides a device and a method of growing 500-1000mm long bismuth germanate crystals by descent method. The device of growing bismuth germanate crystals includes a furnace structure system and an auxiliary heating system. According to the invention, by means of the furnace structure system and the auxiliary heating system, the temperature in the corresponding gradient region and auxiliary heating region of the crystal growth device is simultaneously controlled and regulated to insure that the whole growth device is provided with the best temperature field. According to the invention, the height of the high temperature region of the growth device and the height of the auxiliary heating system can be regulated by a ratio of 1:1 according to the length of the grown crystals, in addition, a long-size platinum crucible and alumina lead-down crucible are designed, a suitable temperature gradient and descent speed are obtained, and long-size and high-quality bismuth germanate scintillation crystals are prepared efficiently.
Description
Technical field
The invention belongs to the crystal technique field, be specifically related to the apparatus and method of the long bismuth-germanium-oxide crystal of a kind of descent method for growing 500-1000mm.
Technical background
Inorganic scintillation crystal is to survey one type of light functional crystal material of various microcosmic particles of nuclear physics and particle physics field or ray.It is the hi-tech device of Application Areass such as nuclear physics, high energy physics, space physics, nuclear medicine, industrial nondestructive testing, Homeland Security, environment measuring, the core material of equipment, belongs to the hi-tech material.Material is the basis and the breach of hi-tech, generation material one generation technique, and it is the most outstanding that this embodies aspect the inorganic scintillation crystal material.
Bismuth germanium oxide (BGO) crystal is the flash detection material of excellent combination property.Series of advantages such as the e/ gamma energy resolving power that its density is big, tool is excellent, specific refractory power height, no hygroscopicity, physicochemical property are stable, processing characteristics is good are widely used in various fields: high energy physics, nuclear physics, space physics, nuclear medicine, safety inspection, environmental monitoring, food inspection and oil well logging or the like.
BGO is a high-density flash detection material.High-density, large size, high quality scintillation crystal are the difficult points of technology of preparing always, do not make substantial breakthroughs for a long time to have caused making slow progress of relevant device research and development and application.Bismuth-germanium-oxide crystal became the crystalline material of the first-selection of dark matter particle space exploration method (electromagnetic calorimeter), and demand is of a size of 500-1000mm along with the deepening continuously and promoting of dark spatial material particle detection study and application in nearly 2 years.
Long in the world for a long time size BGO crystal all is to adopt Czochralski grown, and because the limitation of crystal pulling method preparation facilities, and it is size-constrained to grow crystalline, only reaches below the 400mm like Russia and Crystal Is Inc. of Saint-Gobain crystalline maximum available dimensions length.China mainly adopts descent method for growing BGO crystal, although aspect batch process, unique advantage is arranged, because restrictions such as preparation facilities size of burner hearth and growth techniques, the long bismuth-germanium-oxide crystal of preparation 500-1000mm has great difficulty.Therefore, the public reported of length greater than the bismuth-germanium-oxide crystal of 400mm do not arranged so far in the world as yet.
Summary of the invention
The present invention is intended to break through the technical bottleneck that existing growth apparatus and growth method etc. exist, and has increased auxiliary heating system, the device of the long bismuth-germanium-oxide crystal of a kind of descent method for growing is provided, and has prepared the long bismuth-germanium-oxide crystal of 500-1000mm.
On the one hand, the present invention provides a kind of descent method for growing 500-1000mm the device of long bismuth-germanium-oxide crystal, and said device comprises furnace binding system and auxiliary heating system.
In one embodiment of the present invention, said furnace binding system comprises heating element (6), temperature-controlled tube (5), high-temperature zone (4), go up at a distance from brick (7), gradient zones (8), down at a distance from brick (10), flame-proof thermal insulation material (3), cold zone (9), insulating cotton (2) and furnace shell (1).
In one embodiment of the present invention, said auxiliary heating system comprises lagging material (11), boosting heating element (12,13), boosting district (14) and side hot baffle (15,16).
In the present invention, the height of the high-temperature zone of said furnace binding (4) can be regulated according to the length of growing crystal.And the height in the boosting district (14) of said auxiliary heating system also can be regulated according to the length of growing crystal.
In one embodiment of the present invention, the heating element of said auxiliary heating system (12,13) is globars or Si-Mo rod.
In preferred implementation of the present invention, the size of said side hot baffle (15,16) is adjustable.
On the other hand, the present invention provides the device that adopts the long bismuth-germanium-oxide crystal of said descent method for growing 500-1000mm to prepare the method for bismuth-germanium-oxide crystal, and said method comprises:
(1) the bismuth germanium oxide raw material metallic crucible of packing into is placed on aluminum oxide and draws down in the crucible;
(2) aluminum oxide is drawn following crucible and move in the device of the long bismuth-germanium-oxide crystal of said descent method for growing 500-1000mm, according to the descent method for growing bismuth-germanium-oxide crystal;
Wherein, simultaneously said device is carried out temperature control and adjusting through the heating element (6) of furnace binding system and the boosting heating element (12,13) of auxiliary heating system.
In one embodiment of the present invention, aluminum oxide draw down the lowering speed of crucible be the 0.8-2.0 millimeter/hour.
In one embodiment of the present invention, the longitudinal temperature gradient of the gradient zones of furnace binding system (8) is 30-60 Kelvin/centimetre (K/cm).
In one embodiment of the present invention, said metallic crucible is the platinum crucible, and length is 600-1100mm.
In one embodiment of the present invention, the length of crucible was 520-1020mm under said aluminum oxide drew.
In the present invention, according to the axial distribution of reactors, burner hearth is divided into high-temperature zone, gradient zones, cold zone and boosting district.Among the present invention, the height of high-temperature zone can be regulated along with the variation of growing crystal length.In the crystalline process of growth, raw material melts in the high-temperature zone, and crystal is in cold zone and the insulation of boosting district, in the gradient zones crystallization.Designed to the invention property auxiliary heating system; Utilize Si-Mo rod or globars to be heating member; Part through to the bottom advantages of good crystallization of long crystal is carried out boosting, and in the side hot baffle of auxiliary heating system setting lagging material is housed, thereby has avoided heat radiation to make the thermograde of gradient zones unstable and influence the crystalline crystallization; Effectively suppress the generation of growth defect (inclusion and striation), improved the growth quality of long bismuth-germanium-oxide crystal widely.In addition, be incubated to reduce the crystalline cracking through the part crystal of auxiliary heating system advantages of good crystallization.
In the present invention; The height in the height of said high-temperature zone and boosting district is adjustable (both height are regulated according to the ratio of 1:1) according to crystalline length needs; To satisfy the needs of longer bismuth-germanium-oxide crystal growth, the preparation of long crystal becomes possibility thereby make more.
Among the present invention; The method of the long bismuth-germanium-oxide crystal of a kind of descent method for growing 500-1000mm comprises the raw material metallic crucible of packing into is placed on aluminum oxide and draws down in the crucible and move in the device of descent method for growing bismuth-germanium-oxide crystal; Intensification and the inoculation of insulation back, the vertical fall off rate of crucible and the thermograde of crystal growth interface under control is drawn.In order to satisfy the needs of 500-1000 long crystal growth, the Al of the platinum crucible of the overlength placement raw material of design and use coupling and the placement buffering thermal stresses of overlength
2O
3The aluminum oxide of powder filler draws crucible down.In the process of crystal growth; Simultaneously the corresponding section of whole device is carried out temperature control and adjusting through the heating element of furnace binding system and the boosting heating element of auxiliary heating system; Wherein the scope of the heating element temperature control of furnace binding system is between 1200-1400 ℃; The heating element temperature control scope of auxiliary heating system is between 300-600 ℃; Thereby the temperature field that makes whole device is more suitable for crystal growth, guarantees that the best crystallization gradient of gradient zones is 30-60 Kelvin/centimetre (K/cm), the crystalline crystallization velocity can be increased to the 0.8-2.0 millimeter/hour.
Simultaneously, can in growing apparatus, lay one or many crucibles, grow superior in quality long bismuth-germanium-oxide crystal in batches according to practical application different to crystal shape and dimensional requirement.
Compare with the apparatus and method of existing growth bismuth-germanium-oxide crystal, the advantage of apparatus of the present invention and method is:
1) on simple reactors body structure system-based; Creatively designed auxiliary heating system; Utilize Si-Mo rod or globars to be heating member; Part through to the bottom advantages of good crystallization of long crystal is carried out boosting, prevents that it from exposing the heat of melt in air and in the diffusion burner hearth, guaranteed that the growth quality of long bismuth-germanium-oxide crystal also can be avoided the crystalline cracking simultaneously;
2) because the height in high-temperature zone and boosting district is to regulate according to growing crystal length needs; The variation of the height in high-temperature zone and boosting district is regulated in the 1:1 ratio, therefore can prepare the bismuth-germanium-oxide crystal of 500-1000mm even longer size;
3) auxiliary heating system is provided with the side hot baffle, and lagging material is equipped with in inside, and its effect is the air admission burner hearth that prevents temperature convection, better guarantees the effect of boosting;
4) the boosting heating element of the heating element of furnace binding system and auxiliary heating system carries out temperature control to the corresponding section of described device simultaneously and regulates; Make the temperature field of whole device be more suitable for crystal growth, guarantee that gradient zones is at best crystallization gradient 30-60 Kelvin/centimetre (K/cm);
5) the overlength platinum crucible of design and the suitable 500-1000mm crystal growth needs of use and overlength aluminum oxide draw crucible down.
Description of drawings
Fig. 1 is the front view of the long bismuth-germanium-oxide crystal device of descent method for growing 500-1000mm of the present invention, and wherein, said device comprises furnace binding system and auxiliary heating system; Wherein:
The 1-furnace shell; The 2-insulating cotton; The 3-flame-proof thermal insulation material; The 4-high-temperature zone; The 5-temperature-controlled tube;
The 6-heating element; 7-is last at a distance from brick; The 8-gradient zones; The 9-cold zone; 10-is down at a distance from brick; 17-platinum crucible; The 18-aluminum oxide draws crucible down.
Fig. 2 is the sectional view of auxiliary heating system in the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm of the present invention; Wherein:
The 11-lagging material, 12 with 13-boosting heating element, 14-boosting district, 15 with 16-side hot baffle.
Fig. 3 is the long bismuth-germanium-oxide crystal of 600mm that the apparatus and method of the long bismuth-germanium-oxide crystal of employing descent method for growing 500-1000mm of the present invention are prepared.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further explain.It should be noted that content of the present invention is not limited to these concrete embodiments.Under the prerequisite that does not deviate from background of the present invention and spirit, those skilled in the art can carry out the equivalence replacement and revise on the basis of reading content of the present invention, and its content is also included within the scope of requirement protection of the present invention.
Fig. 1 is the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm of the present invention, and it comprises furnace binding system and auxiliary heating system.
In said furnace binding, 1 is furnace shell, and 2 is insulating cotton, and 3 is flame-proof thermal insulation material, and 4 is the high-temperature zone, and 5 is temperature-controlled tube, and 6 is heating element, and 7 is last separated brick, and 8 is gradient zones, and 9 is cold zone, and 10 are down separated brick, and 17 is the platinum crucible; 18 draw down crucible for aluminum oxide; In the said auxiliary heating system, 11 is shell, and 12 is lagging material, and 13 is the boosting heating element, and 14 is the boosting district, and 15,16 is side hot baffle (as shown in Figure 1).
In the equipment of the present invention, according to the axial distribution of reactors, burner hearth is divided into high-temperature zone 4, gradient zones 8, cold zone 9 and boosting district 14.High-temperature zone 4 is to go up at a distance from the zone of brick 7 or more, and the height of high-temperature zone 4 can increase along with the increase of crystal length, and heating element 6 adopts the Si-Mo rods heating, is positioned on the separated brick 7, can make the temperature of burner hearth be heated to 1230-1280 ℃; Cold zone 9 is last zone between brick 7 to down separated brick 10.
In the equipment of the present invention, boosting district 14 is the auxiliary heating system zone, and the thermograde in high-temperature zone 4, cold zone 9 and boosting district 14 is all less, and gradient zones 8 is last at a distance near the brick 7, and its thermograde is bigger.In the crystalline process of growth, raw material is 4 fusings in the high-temperature zone, and crystal is in cold zone 9 and 14 insulations of boosting district, in gradient zones 8 crystallizations.When the part of the bottom of long crystal advantages of good crystallization is exposed in the air; Heating element 12,13 Si-Mo rods of boosting can provide boosting for it; The lagging material 11 that is filled with around the Si-Mo rod; And the hot baffle 15,16 of auxiliary heating system can prevent the air admission burner hearth of convection current, thereby makes the gradient of gradient zones stable, has improved the growth quality of long bismuth-germanium-oxide crystal widely.
In the present invention; When the crystalline size of required growth increases; Can be through increasing the height of high-temperature zone; Increase simultaneously the height in boosting district according to the ratio of 1:1, having avoided the long crystal of descent method for growing to expose in air heat radiation influence crystal structure and causes problem such as crystal cleavage, thus make high quality prepare 500-1000mm in addition more long crystal become possibility.
In order to measure the temperature variation of crystal growing process in real time, it is temperature element that temperature-controlled tube 5 adopts platinum rhodium thermocouple, and temperature thermocouple is placed in the alumina ceramic tube.
Further explain in the face of the method for the long bismuth-germanium-oxide crystal of descent method for growing 500-800mm of the present invention down.
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is following:
With purity is that bismuthous oxide bismuth trioxide and germanium dioxide more than the 4N weighed to mix according to stoichiometric ratio 2:3 and be placed in the platinum crucible; It is above and be incubated about 10-60 minute to be warming up to melting temperature; Raw material is melted fully, inject mould fast, cooling obtains the polycrystal ingot.
With thickness is that to process the cross section be 30 * 30mm for 3 layers of platinum sheet of 0.16mm
2, long be the rectangular parallelepiped crucible of 700mm.
Selection thickness is that 8mm, outer cross section are 80 * 90mm
2, long draw time crucible for the rectangular parallelepiped aluminum oxide of 620mm; And selection is of a size of 60 * 30 * 70mm
3Bismuth-germanium-oxide crystal, through cutting, grind and clean the back and be used as seed crystal.
Seed crystal and ready raw material are packed in the platinum crucible of platinum crucible or bottom seal of top, end both ends open of long 700mm.Place the aluminum oxide of long 620mm to draw crucible down platinum crucible after sealing (it is folding that port platinum sheet is curled, and forms and seal).The sectional dimension of crucible was greater than the sectional dimension of platinum crucible under aluminum oxide drew; Fill up the powdery lagging material in drawing to aluminum oxide down of platinum crucible between the crucible all around; Crucible moves in the device (as shown in Figure 1) of the long bismuth-germanium-oxide crystal of descent method for growing under then aluminum oxide being drawn, and the vertical position of crucible in burner hearth down drawn in adjustment, is warming up to more than 1050 ℃; Be incubated 48 hours and all melt the back inoculation to polycrystal ingot or crystal block raw material; In the process of crystal growth, the heating element through the furnace binding system and the boosting heating element of auxiliary heating system carry out temperature control to the corresponding section of described device simultaneously and regulate, wherein the heating element temperature control of furnace binding system about 1320 ℃; The heating element temperature control of auxiliary heating system is about 500 ℃; Make the temperature field of whole device be suitable for the crystalline growth most, the thermograde of control crystal growth interface is 50 Kelvins/centimetre (K/cm), and the vertical fall off rate of crucible was 1.2 millimeters/hour under aluminum oxide drew.
Behind the growth ending, stop to descend.Temperature is reduced to room temperature.Cut off the electricity supply, take out platinum crucible, the crystal in the crucible is stripped out, prepare described bismuth-germanium-oxide crystal (like Fig. 3).
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is following:
Select ready-made bismuth-germanium-oxide crystal,, clean the crystal block of back as growth raw material through cutting, grind to form needed size and dimension.
Other steps such as the embodiment 1 of embodiment 2 are said, finally make the long bismuth-germanium-oxide crystal of said 600mm (like Fig. 3).
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is following:
The heating element temperature control of control furnace binding system about 1280 ℃; The heating element temperature control of auxiliary heating system is about 480 ℃; Make the temperature field of whole device be suitable for the crystalline growth most, and controlled oxidation aluminium to draw the vertical fall off rate of crucible down be that the thermograde of 1.0 millimeters/hour and crystal growth interface is 40 Kelvins/centimetre (K/cm).
Other steps of embodiment 3 such as embodiment 1 or 2 are said, finally make said wide plate shape bismuth-germanium-oxide crystal (like Fig. 3).
Embodiment 4
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is following:
The heating element temperature control of control furnace binding system about 1360 ℃; The heating element temperature control of auxiliary heating system is about 560 ℃; Make the temperature field of whole device be suitable for the crystalline growth most, and controlled oxidation aluminium to draw the vertical fall off rate of crucible down be that the thermograde of 1.6 millimeters/hour and crystal growth interface is 60 Kelvins/centimetre (K/cm).
Other steps of embodiment 3 such as embodiment 1 or 2 are said, finally make said wide plate shape bismuth-germanium-oxide crystal (like Fig. 3).
The preparation of the long bismuth-germanium-oxide crystal of 800mm, concrete preparation method is following:
Like embodiment 1 and 2 said bismuth germanium oxide polycrystal ingot or the crystal blocks of providing.
With thickness is that to process the cross section be 30 * 30mm for 3 layers of platinum sheet of 0.16mm
2, height is the rectangular parallelepiped crucible of 900mm.
Selection thickness is that 8mm, outer cross section are 80 * 90mm
2, long draw time crucible for the rectangular parallelepiped aluminum oxide of 820mm.
Other is all by each described processing condition of embodiment 1-4, and the control growing time can obtain the long bismuth germanium oxide scintillation crystal of 800mm.
Embodiment 6
The preparation of the long bismuth-germanium-oxide crystal of 900mm, concrete preparation method is following:
Like embodiment 1 and 2 said bismuth germanium oxide polycrystal ingot or the crystal blocks of providing.
With thickness is that to process the cross section be 30 * 30mm for 3 layers of platinum sheet of 0.16mm
2, height is the rectangular parallelepiped crucible of 1000mm.
Selection thickness is that 8mm, outer cross section are 80 * 90mm
2, long draw time crucible for the rectangular parallelepiped aluminum oxide of 920mm.
Other is all by embodiment 5 described processing condition, and the control growing time can obtain the long bismuth germanium oxide scintillation crystal of 900mm.
Any technician who is familiar with the present technique field is in the technical scope that the present invention discloses, and the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (12)
1. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm, said device comprises furnace binding system and auxiliary heating system.
2. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm according to claim 1 is characterized in that: said furnace binding system comprises heating element (6), temperature-controlled tube (5), high-temperature zone (4), go up at a distance from brick (7), gradient zones (8), down at a distance from brick (10), flame-proof thermal insulation material (3), cold zone (9), insulating cotton (2) and furnace shell (1).
3. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 1; It is characterized in that: said auxiliary heating system comprises lagging material (11), boosting heating element (12; 13), boosting district (14) and side hot baffle (15,16).
4. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 1 is characterized in that: the height of the high-temperature zone of said furnace binding (4) is regulated according to the length of growing crystal.
5. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 3 is characterised in that: the height in the boosting district (14) of said auxiliary heating system is regulated according to the length of growing crystal.
6. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 3 is characterized in that: the heating element of said auxiliary heating system (12,13) is globars or Si-Mo rod.
7. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 3 is characterized in that: the size of said side hot baffle (15,16) is adjustable.
8. the device of the long bismuth-germanium-oxide crystal of employing each said descent method for growing 500-1000mm of claim 1 to 7 prepares the method for bismuth-germanium-oxide crystal, and said method comprises:
(1) the bismuth germanium oxide raw material metallic crucible of packing into is placed on aluminum oxide and draws down in the crucible;
(2) aluminum oxide is drawn following crucible and move in the device of the long bismuth-germanium-oxide crystal of said descent method for growing 500-1000mm, according to the descent method for growing bismuth-germanium-oxide crystal;
Wherein, simultaneously said device is carried out temperature control and adjusting through the heating element (6) of furnace binding system and the boosting heating element (12,13) of auxiliary heating system.
9. like the said method for preparing bismuth-germanium-oxide crystal of claim 8, it is characterized in that: in the descent method aluminum oxide draw down the lowering speed of crucible be the 0.8-2.0 millimeter/hour.
10. like the said method for preparing bismuth-germanium-oxide crystal of claim 8, it is characterized in that: the longitudinal temperature gradient of gradient zones in the furnace binding system (8) is 30-60K/cm.
11. like the said method for preparing bismuth-germanium-oxide crystal of claim 8, it is characterized in that: said metallic crucible is the platinum crucible, length is 600-1100mm.
12. like the said method for preparing bismuth-germanium-oxide crystal of claim 8, be characterised in that: the length of crucible was 520-1020mm under said aluminum oxide drew.
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| CN103938266A (en) * | 2013-01-18 | 2014-07-23 | 广东先导稀材股份有限公司 | Composite crucible, preparation method thereof and method for bismuth germanate crystal growth using the crucible |
| WO2014172929A1 (en) * | 2013-04-25 | 2014-10-30 | 浙江晶盛机电股份有限公司 | Auxiliary heating device for float zone furnace and heat preservation method for single crystal rod thereof |
| CN105369344A (en) * | 2015-12-15 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and device used for preparing platy monocrystals via temperature field gradient vertical shifting method |
| CN105420809A (en) * | 2015-12-15 | 2016-03-23 | 河南西格马晶体科技有限公司 | Method and device for preparing platy monocrystal with temperature field vertical gradient moving method |
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| JPH02271989A (en) * | 1989-04-13 | 1990-11-06 | Shin Etsu Chem Co Ltd | Production of single crystal of bismuth germanate |
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| CN102206869A (en) * | 2011-05-11 | 2011-10-05 | 昆明沃特尔机电设备有限公司 | Mobile-furnace-body high-purity crystal grower |
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| JPH02271989A (en) * | 1989-04-13 | 1990-11-06 | Shin Etsu Chem Co Ltd | Production of single crystal of bismuth germanate |
| CN101323968A (en) * | 2008-07-24 | 2008-12-17 | 山东大学 | Multicomponent compounds infrared crystal growth apparatus |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103938266A (en) * | 2013-01-18 | 2014-07-23 | 广东先导稀材股份有限公司 | Composite crucible, preparation method thereof and method for bismuth germanate crystal growth using the crucible |
| WO2014172929A1 (en) * | 2013-04-25 | 2014-10-30 | 浙江晶盛机电股份有限公司 | Auxiliary heating device for float zone furnace and heat preservation method for single crystal rod thereof |
| US10138573B2 (en) | 2013-04-25 | 2018-11-27 | Zhejiang Jingsheng M & E Co., Ltd | Auxiliary heating device for zone melting furnace and heat preservation method for single crystal rod thereof |
| CN105369344A (en) * | 2015-12-15 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and device used for preparing platy monocrystals via temperature field gradient vertical shifting method |
| CN105420809A (en) * | 2015-12-15 | 2016-03-23 | 河南西格马晶体科技有限公司 | Method and device for preparing platy monocrystal with temperature field vertical gradient moving method |
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| CN102787350B (en) | 2016-04-06 |
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