CN102787350B - The apparatus and method of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm - Google Patents
The apparatus and method of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm Download PDFInfo
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- CN102787350B CN102787350B CN201210322219.4A CN201210322219A CN102787350B CN 102787350 B CN102787350 B CN 102787350B CN 201210322219 A CN201210322219 A CN 201210322219A CN 102787350 B CN102787350 B CN 102787350B
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Abstract
The invention provides the apparatus and method of the long bismuth-germanium-oxide crystal of a kind of descent method for growing 500-1000mm.The device of described growth bismuth-germanium-oxide crystal comprises furnace structure system and auxiliary heating system.In the present invention, simultaneously by furnace structure system and auxiliary heating system the corresponding gradient zones of crystal growing apparatus and boosting district carried out temperature control and regulated, ensureing that whole growing apparatus has best temperature field.The present invention can also according to the length of growing crystal according to the height of proportion adjustment growing apparatus high-temperature zone of 1:1 and the height of auxiliary heating system, and design the platinum crucible of long size and aluminum oxide draws lower crucible, adjust suitable thermograde and lowering speed, prepare long size, high-quality bismuth germanium oxide scintillation crystal expeditiously.
Description
Technical field
The invention belongs to technical field of crystal growth, 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 a class light functional crystal material that can detect the various microcosmic particle of nuclear physics and particle physics field or ray.It is the hi-tech device of Application Areas, the core materials of equipment such as nuclear physics, high energy physics, space physics, nuclear medicine, industrial nondestructive testing, Homeland Security, environment measuring, belongs to High-tech Material.Material is basis and the breach of hi-tech, generation material one generation technique, and it is the most outstanding that this embodies in inorganic scintillation crystal material.
Bismuth germanium oxide (BGO) crystal is the flash detection material of excellent combination property.The series of advantages such as the e/ gamma energy resolving power that its density is large, tool is excellent, specific refractory power are high, no hygroscopicity, physicochemical property 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 etc.
BGO is 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 result in relevant device research and development and application make slow progress.Nearly 2 years deepening continuously and promotion along with space dark matter particle detection research and apply, bismuth-germanium-oxide crystal becomes the crystalline material of the first-selection of dark matter particles spatial detection method (electromagnetic calorimeter), and demand is of a size of 500-1000mm.
Long size BGO crystal is all adopt Czochralski grown in the world for a long time, and due to the limitation of crystal pulling method preparation facilities, grows the size-constrained of crystal, and the maximum available dimensions length as Russia and Crystal Is Inc. of Saint-Gobain crystal only reaches below 400mm.China mainly adopts descent method for growing BGO crystal, although have unique advantage in batch production, due to 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, length is not yet had to be greater than the open report of the bismuth-germanium-oxide crystal of 400mm so far in the world.
Summary of the invention
The present invention is intended to the technical bottleneck breaking through the existence such as existing growth apparatus and growth method, adds auxiliary heating system, provides the device of the long bismuth-germanium-oxide crystal of a kind of descent method for growing, and prepares the long bismuth-germanium-oxide crystal of 500-1000mm.
On the one hand, the invention provides the device of the long bismuth-germanium-oxide crystal of a kind of descent method for growing 500-1000mm, described device comprises furnace structure system and auxiliary heating system.
In one embodiment of the present invention, described furnace structure system comprise heating element (6), temperature-controlled tube (5), high-temperature zone (4), on every brick (7), gradient zones (8), under every 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, described auxiliary heating system comprises lagging material (11), boosting heating element (12,13), boosting district (14) and side block hot plate (15,16).
In the present invention, the height of the high-temperature zone (4) of described furnace binding can regulate according to the length of growing crystal.And the height in the boosting district (14) of described auxiliary heating system also can regulate according to the length of growing crystal.
In one embodiment of the present invention, the heating element (12,13) of described auxiliary heating system is globars or Si-Mo rod.
In a preferred embodiment of the invention, the size of described side block hot plate (15,16) is adjustable.
On the other hand, the invention provides the method adopting the device of the long bismuth-germanium-oxide crystal of described descent method for growing 500-1000mm to prepare bismuth-germanium-oxide crystal, described method comprises:
(1) bismuth germanium oxide raw material loading metallic crucible being placed on aluminum oxide draws in lower crucible;
(2) aluminum oxide being drawn lower crucible moves in the device of the long bismuth-germanium-oxide crystal of described descent method for growing 500-1000mm, according to descent method for growing bismuth-germanium-oxide crystal;
Wherein, temperature control and adjustment are carried out to described device by the heating element (6) of furnace structure system and the boosting heating element (12,13) of auxiliary heating system simultaneously.
In one embodiment of the present invention, the lowering speed that aluminum oxide draws lower crucible is 0.8-2.0 milli m/h.
In one embodiment of the present invention, the longitudinal temperature gradient of the gradient zones (8) of furnace structure system is 30-60 Kelvin/centimetre (K/cm).
In one embodiment of the present invention, described metallic crucible is platinum crucible, and length is 600-1100mm.
In one embodiment of the present invention, the length that described aluminum oxide draws lower crucible is 520-1020mm.
In the present invention, according to the axial distribution of growth furnace, burner hearth is divided into high-temperature zone, gradient zones, cold zone and boosting district.In the present invention, the height of high-temperature zone can regulate along with the change of growing crystal length.In the process of growth of crystal, raw material melts in high-temperature zone, and crystal is incubated, in gradient zones crystallization in cold zone and boosting district.The present invention creatively devises auxiliary heating system, Si-Mo rod or globars is utilized to be heating member, boosting is carried out by the part of the bottom advantages of good crystallization to long crystal, and the side block hot plate that auxiliary heating system is arranged is built with lagging material, thus avoid heat radiation and make the thermograde of gradient zones unstable and the crystallization that affects crystal, the generation of effective Developing restraint defect (inclusion and striation), greatly increases the growth quality of long bismuth-germanium-oxide crystal.In addition, be incubated by the partial crystals of auxiliary heating system to advantages of good crystallization the cracking reducing crystal.
In the present invention, the height of described high-temperature zone and the height in boosting district need to be adjustable (both height regulate according to the ratio of 1:1) according to the length of crystal, to meet the needs of longer bismuth-germanium-oxide crystal growth, thus the preparation of more long crystal is made to become possibility.
In the present invention, the method of the long bismuth-germanium-oxide crystal of a kind of descent method for growing 500-1000mm comprises and raw material is loaded metallic crucible and be placed on aluminum oxide and draw in lower crucible and to move in the device of descent method for growing bismuth-germanium-oxide crystal, heat up and be incubated rear inoculation, controlling to draw the vertical fall off rate of lower crucible and the thermograde of crystal growth interface.In order to the needs of 500-1000 long crystal growth can be met, design and use the overlength of coupling to place the Al of the platinum crucible of raw material and the placement buffering thermal stresses of overlength
2o
3the aluminum oxide of powder filler draws lower crucible.In the process of crystal growth, simultaneously by the heating element of furnace structure system and the boosting heating element of auxiliary heating system the corresponding section of whole device is carried out temperature control and regulated, wherein the scope of the heating element temperature control of furnace structure system is between 1200-1400 DEG C, the heating element temperature control scope of auxiliary heating system is between 300-600 DEG C, thus make the warm field of whole device be more suitable for crystal growth, the best crystallization gradient of guarantee gradient zones is 30-60 Kelvin/centimetre (K/cm), and the crystallization velocity of crystal can be increased to 0.8-2.0 milli m/h.
Meanwhile, can according to the difference of practical application to crystal shape and dimensional requirement, in growing apparatus, lay one or many crucibles, batch grows superior in quality long bismuth-germanium-oxide crystal.
Compared with the apparatus and method of existing growth bismuth-germanium-oxide crystal, the advantage of apparatus of the present invention and method is:
1) in simple growth furnace body structure system-based, creatively devise auxiliary heating system, Si-Mo rod or globars is utilized to be heating member, boosting is carried out by the part of the bottom advantages of good crystallization to long crystal, prevent it in atmosphere exposed and the heat of melt in diffusion hearth, ensure that the growth quality of long bismuth-germanium-oxide crystal also can avoid the cracking of crystal simultaneously;
2) because the height in high-temperature zone and boosting district can regulate according to growing crystal length needs, the change of the height in high-temperature zone and boosting district regulates in 1:1 ratio, therefore can prepare the bismuth-germanium-oxide crystal of the even longer size of 500-1000mm;
3) auxiliary heating system is provided with side block hot plate, and lagging material is equipped with in inside, and its effect prevents the air of temperature convection from entering burner hearth, the better effect ensureing boosting;
4) heating element of furnace structure system and the boosting heating element of auxiliary heating system carry out temperature control to the corresponding section of described device and regulate simultaneously, make the warm field of whole device be more suitable for crystal growth, ensure that gradient zones is at best crystallization gradient 30-60 Kelvin/centimetre (K/cm);
5) design and use the overlength platinum crucible of applicable 500-1000mm crystal growth needs and overlength aluminum oxide to draw lower crucible.
Accompanying drawing explanation
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, described device comprises furnace structure system and auxiliary heating system; Wherein:
1-furnace shell; 2-insulating cotton; 3-flame-proof thermal insulation material; 4-high-temperature zone; 5-temperature-controlled tube;
6-heating element; 7-is upper every brick; 8-gradient zones; 9-cold zone; Every brick under 10-; 17-platinum crucible; 18-aluminum oxide draws lower crucible.
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:
11-lagging material, 12 and 13-boosting heating element, 14-boosting district, 15 and 16-side block hot plate.
Fig. 3 is the long bismuth-germanium-oxide crystal of 600mm adopting the apparatus and method of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm of the present invention to prepare.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.It should be noted that content of the present invention is not limited to these concrete embodiments.Under the prerequisite not deviating from background of the present invention and spirit, those skilled in the art can carry out equivalencing and amendment on the basis of reading content of the present invention, and its content is also included within the scope of protection of 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 structure system and auxiliary heating system.
In described furnace binding, 1 is furnace shell, and 2 is insulating cotton, and 3 is flame-proof thermal insulation material, and 4 is high-temperature zone, and 5 is temperature-controlled tube, and 6 is heating element, 7 be on every brick, 8 is gradient zones, and 9 is cold zone, 10 be under every brick, 17 is platinum crucible; 18 draw lower crucible for aluminum oxide; In described auxiliary heating system, 11 is shell, and 12 is lagging material, and 13 is boosting heating element, and 14 is boosting district, and 15,16 is side block hot plate (as shown in Figure 1).
In equipment of the present invention, according to the axial distribution of growth furnace, burner hearth is divided into high-temperature zone 4, gradient zones 8, cold zone 9 and boosting district 14.High-temperature zone 4 be on every the region of brick more than 7, and the height of high-temperature zone 4 can increase along with the increase of crystal length, and heating element 6 adopts Si-Mo rod to heat, and is positioned on brick 7, and the heating temperatures of burner hearth can be made to 1230-1280 DEG C; Cold zone 9 be on every brick 7 under region between brick 10.
In equipment of the present invention, boosting district 14 is auxiliary heating system region, and the thermograde in high-temperature zone 4, cold zone 9 and boosting district 14 is all less, gradient zones 8 be near brick 7, its thermograde is larger.In the process of growth of crystal, raw material melts in high-temperature zone 4, and crystal is incubated, in gradient zones 8 crystallization in cold zone 9 and boosting district 14.When the partial denudation of the bottom advantages of good crystallization of long crystal is in air, heating element 12,13 Si-Mo rod of boosting can provide boosting for it, the lagging material 11 be filled with around Si-Mo rod, and the hot baffle 15,16 of auxiliary heating system can prevent the air of convection current from entering burner hearth, thus make the gradient stabilization of gradient zones, greatly increase the growth quality of long bismuth-germanium-oxide crystal.
In the present invention, when the crystalline size of required growth increases, can by increasing the height of high-temperature zone, increase the height in boosting district according to the ratio of 1:1 simultaneously, avoid the exposed heat radiation in atmosphere of the long crystal of descent method for growing affect crystal structure and cause the problems such as crystal cleavage, thus make high quality prepare 500-1000mm even more long crystal become possibility.
In order to measure the temperature variation of crystal growing process in real time, temperature-controlled tube 5 adopts platinum rhodium thermocouple to be temperature element, is placed in alumina ceramic tube by temperature thermocouple.
Below the method for the long bismuth-germanium-oxide crystal of descent method for growing 500-800mm of the present invention is further detailed.
Embodiment 1
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is as follows:
Being the bismuthous oxide bismuth trioxide of more than 4N and germanium dioxide by purity is placed in platinum crucible according to stoichiometric ratio 2:3 mixing of weighing, be warming up to more than melting temperature and be incubated about 10-60 minute, raw material is melted completely, injects mould fast, cooling obtains polycrystal ingot.
Be that to make cross section be 30 × 30mm for 3 layers of platinum sheet of 0.16mm by thickness
2, the long rectangular parallelepiped crucible for 700mm.
Selection thickness is 8mm, outer cross section is 80 × 90mm
2, the long rectangular parallelepiped aluminum oxide for 620mm draws lower crucible; And select to be of a size of 60 × 30 × 70mm
3bismuth-germanium-oxide crystal, through cutting, grind and as seed crystal after cleaning.
Seed crystal and ready raw material are loaded in the top of long 700mm, the platinum crucible of end both ends open or the platinum crucible of bottom seal.Aluminum oxide platinum crucible being placed in long 620mm after sealing (by curling for port platinum sheet folding, forming sealing) draws lower crucible.The sectional dimension that aluminum oxide draws lower crucible is greater than the sectional dimension of platinum crucible, draw between lower crucible at four thoughtful aluminum oxide of platinum crucible and fill up powdery lagging material, then aluminum oxide being drawn lower crucible moves in the device (as shown in Figure 1) of the long bismuth-germanium-oxide crystal of descent method for growing, the vertical position of lower crucible in burner hearth is drawn in adjustment, be warming up to more than 1050 DEG C, be incubated 48 hours and all melt rear inoculation to polycrystal ingot or crystal block raw material, in the process of crystal growth, simultaneously by the heating element of furnace structure system and the boosting heating element of auxiliary heating system the corresponding section of described device is carried out temperature control and regulated, wherein furnace structure system heating element temperature control at about 1320 DEG C, the heating element temperature control of auxiliary heating system is at about 500 DEG C, the warm field of whole device is made to be best suited for the growth of crystal, the thermograde controlling crystal growth interface is 50 Kelvins/centimetre (K/cm), the vertical fall off rate that aluminum oxide draws lower crucible is 1.2 millis m/h.
After growth terminates, stop declining.Temperature is down to room temperature.Cut off the electricity supply, take out platinum crucible, the crystal in crucible is stripped out, prepares described bismuth-germanium-oxide crystal (as Fig. 3).
Embodiment 2
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is as follows:
Select ready-made bismuth-germanium-oxide crystal, through cutting, grind to form required size and dimension, as the crystal block of growth raw material after cleaning.
Other steps of embodiment 2 as described in Example 1, finally obtain the long bismuth-germanium-oxide crystal of described 600mm (as Fig. 3).
Embodiment 3
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is as follows:
Control furnace structure system heating element temperature control at about 1280 DEG C, the heating element temperature control of auxiliary heating system is at about 480 DEG C, make the warm field of whole device be best suited for the growth of crystal, and the thermograde that the vertical fall off rate that controlled oxidization aluminium draws lower crucible is 1.0 millis m/h and crystal growth interface is 40 Kelvins/centimetre (K/cm).
Other steps of embodiment 3, as described in embodiment 1 or 2, finally obtain described wide plate shape bismuth-germanium-oxide crystal (as Fig. 3).
Embodiment 4
The long bismuth-germanium-oxide crystal of preparation 600mm, concrete preparation method is as follows:
Control furnace structure system heating element temperature control at about 1360 DEG C, the heating element temperature control of auxiliary heating system is at about 560 DEG C, make the warm field of whole device be best suited for the growth of crystal, and the thermograde that the vertical fall off rate that controlled oxidization aluminium draws lower crucible is 1.6 millis m/h and crystal growth interface is 60 Kelvins/centimetre (K/cm).
Other steps of embodiment 3, as described in embodiment 1 or 2, finally obtain described wide plate shape bismuth-germanium-oxide crystal (as Fig. 3).
Embodiment 5
The preparation of the long bismuth-germanium-oxide crystal of 800mm, concrete preparation method is as follows:
Bismuth germanium oxide polycrystal ingot or crystal block is provided as described in embodiment 1 and 2.
Be that to make cross section be 30 × 30mm for 3 layers of platinum sheet of 0.16mm by thickness
2, height is the rectangular parallelepiped crucible of 900mm.
Selection thickness is 8mm, outer cross section is 80 × 90mm
2, the long rectangular parallelepiped aluminum oxide for 820mm draws lower crucible.
Other is all by the processing condition described in any one of embodiment 1-4, controls growth time and 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 as follows:
Bismuth germanium oxide polycrystal ingot or crystal block is provided as described in embodiment 1 and 2.
Be that to make cross section be 30 × 30mm for 3 layers of platinum sheet of 0.16mm by thickness
2, height is the rectangular parallelepiped crucible of 1000mm.
Selection thickness is 8mm, outer cross section is 80 × 90mm
2, the long rectangular parallelepiped aluminum oxide for 920mm draws lower crucible.
Other is all by the processing condition described in embodiment 5, controls growth time and can obtain the long bismuth germanium oxide scintillation crystal of 900mm.
Anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (10)
1. a device for the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm, described device comprises furnace structure system and auxiliary heating system;
Described furnace structure system comprise heating element (6), temperature-controlled tube (5), high-temperature zone (4), on every brick (7), gradient zones (8), under every brick (10), flame-proof thermal insulation material (3), cold zone (9), insulating cotton (2) and furnace shell (1);
Described auxiliary heating system comprises lagging material (11), boosting heating element (12,13), boosting district (14) and side block hot plate (15,16);
Wherein, according to axial distribution, described device comprises high-temperature zone (4), gradient zones (8), cold zone (9) and boosting district (14) successively; Wherein, high-temperature zone (4) be on region on brick (7), gradient zones (8) upper near brick (7), cold zone (9) be on every brick (7) under region between brick (10), boosting district (14) be under region under brick (10).
2. 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 (4) of described furnace binding regulates according to the length of growing crystal.
3. the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm as claimed in claim 1, is characterised in that: the height in the boosting district (14) of described auxiliary heating system regulates according to the length of growing crystal.
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 heating element (12,13) of described auxiliary heating system is globars or Si-Mo rod.
5. 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 size of described side block hot plate (15,16) is adjustable.
6. adopt the device of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm described in any one of claim 1 to 5 to prepare the method for bismuth-germanium-oxide crystal, described method comprises:
(1) bismuth germanium oxide raw material loading metallic crucible being placed on aluminum oxide draws in lower crucible;
(2) aluminum oxide being drawn lower crucible moves in the device of the long bismuth-germanium-oxide crystal of described descent method for growing 500-1000mm, according to descent method for growing bismuth-germanium-oxide crystal;
Wherein, temperature control and adjustment are carried out to described device by the heating element (6) of furnace structure system and the boosting heating element (12,13) of auxiliary heating system simultaneously.
7. prepare the method for bismuth-germanium-oxide crystal as claimed in claim 6, it is characterized in that: in descent method, aluminum oxide draws the lowering speed of lower crucible is 0.8-2.0 milli m/h.
8. prepare the method for bismuth-germanium-oxide crystal as claimed in claim 6, it is characterized in that: in furnace structure system, the longitudinal temperature gradient of gradient zones (8) is 30-60K/cm.
9. prepare the method for bismuth-germanium-oxide crystal as claimed in claim 6, it is characterized in that: described metallic crucible is platinum crucible, length is 600-1100mm.
10. prepare the method for bismuth-germanium-oxide crystal as claimed in claim 6, be characterised in that: the length that described aluminum oxide draws lower crucible is 520-1020mm.
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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 |
| CN103255473B (en) * | 2013-04-25 | 2016-06-29 | 浙江晶盛机电股份有限公司 | A kind of assisted heating device for zone melting furnace and monocrystal rod heat preserving method thereof |
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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