CN206814880U - The adjustable crystal growing apparatus of thermal field - Google Patents
The adjustable crystal growing apparatus of thermal field Download PDFInfo
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- CN206814880U CN206814880U CN201720669049.5U CN201720669049U CN206814880U CN 206814880 U CN206814880 U CN 206814880U CN 201720669049 U CN201720669049 U CN 201720669049U CN 206814880 U CN206814880 U CN 206814880U
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Abstract
The utility model provides a kind of adjustable crystal growing apparatus of thermal field, and the device includes bell, heat-insulation layer, furnace tubing, resistance wire, corundum hollow circular-tube, insulation powder, thermocouple and temperature controller.The device uses a kind of adjustable dimension, readily replaceable adiabator layer, and only needs one-part form to heat, and turns and platform rise and fall system without crystalline substance.By adjusting the size of adiabator layer, stove thermal field is set to be suitable for the growth of lanthanum bromide cerium crystal.The utility model carries out crystal growth using the fairly static method of without motion mechanism.It is high to descending system precision requirement to overcome conventional Bridgman-Stockbarger method, the shortcomings of differ greatly bad batch duplicating between stove, and space-consuming is big.Lanthanum bromide cerium crystal easily realizes that sequencing grows, extremely advantageous to the control of lanthanum bromide cerium crystal aufwuchsplate, and growing environment is stable, can effectively avoid crystal defect.And the making of crystal growing apparatus is simple, cleaning is maintained easily.
Description
Technical field
The utility model belongs to rare earth material field of deep, specifically, is related to a kind of adjustable crystal growth of thermal field
Device.
Background technology
Scintillation crystal can make detector, in high-energy physics, nuclear physics, nuclear medical imaging diagnosis, geological prospecting, astronomy
There is huge application prospect in Space Physics and safety random check field.With nuclear science technology and other correlation techniques
Rapid development, its application field constantly widening.Different application field it is also proposed more higher to inorganic scintillator
It is required that.Traditional NaI:The scintillation crystals such as TI, BGO can not meet the particular/special requirement of new application field.
Mix cerium lanthanum bromide crystal (LaBr3:Ce after) being found from 1999, ground because its excellent scintillation properties has started
The upsurge studied carefully.Cerium lanthanum bromide light output is mixed up to 78000Ph/MeV, and its die-away time reaches 30ns soon, and its density is 5.1g/cm3,
NaI is significantly stronger than to the absorbability of high-performance ray：Tl crystal, and the risk of its environmental pollution is far smaller than NaI：Tl, because
This LaBr3:Ce crystal has turned into the representative of light output height, the fast scintillation crystal of decay at present, and the crystal is expected to substitute NaI comprehensively：
Tl crystal, so as to be used widely in fields such as Medical Instruments, safety inspection and oil well detections.But LaBr3:Ce crystal growths
Difficulty, component seriously volatilize, and are very easy to react with oxygen, water；And crystal is very easy to cracking.Such as lanthanum bromide is along a axles
Thermal coefficient of expansion be along 5-6 times of C direction of principal axis, it is so very easy in crystal growth and follow-up machine cuts, polishing process
In cracking and crush, therefore LaBr3:The device yield of Ce crystal is very low, and production large-size crystals device is particularly difficult, price
It is extremely expensive.
For LaBr3:The halide crystals such as Ce are typically grown using Bridgman Method (Bridgman-Stockbarger method).Its base
Present principles are by the relative movement between crucible and melt, form certain temperature field, provide growth driving force for crystal, make
Crystal growth.Crystal raw material is placed in crucible, the temperature of high-temperature region is slightly above the fusing point of melt by heater, it is low
The temperature of warm area is slightly below the freezing point of crystal, then crucible is passed slowly with certain temperature gradient by lowering means
Region:High-temperature region, temperature gradient zone and low-temperature space.Melt starts to grow crystal by temperature gradient zone, as crucible is continuous
Decline, crystal is persistently grown up, and is also referred to as Bridgman-Stockbarger method in this way.But traditional Bridgman-Stockbarge method for growing bromination
Lanthanum crystal has following several shortcomings：(1) it is related to a whole set of accurate descending system, it is easy to influenceed, need by external environment
The maintenance of specialty is wanted, and solid liquid interface because decline process constantly produces disturbance, generates interior during crystal decline
Stress；(2) because growth furnace is totally-enclosed structure, once thermal field should not adjust after the completion of building, it is impossible to and preferably matching is different
The crystal of size；(3) space-consuming is big, and maintenance is extremely inconvenient.
Utility model content
The purpose of this utility model is overcome the deficiencies in the prior art, there is provided a kind of thermal field is adjustable, whole static side
Method carries out the crystal growing apparatus of lanthanum bromide cerium crystal growth, and the adjustable characteristic of thermal field can meet the life of different sized crystals
It is long, overcome the adaptation issues that Bridgman-Stockbarger method is directed to different sized crystals.
In order to realize the utility model purpose, a kind of adjustable crystal growing apparatus of new thermal field of the present utility model,
Including bell, heat-insulation layer, furnace tubing, resistance wire, corundum hollow circular-tube, insulation powder, thermocouple and temperature controller.
Wherein, the heat-insulation layer is the circular lamination knot from top to bottom stacked by multilayer aluminum silicate insulation material
Structure, orlop are solid base plate, total number of plies N=10-30 of the heat-insulation layer, and N-1 layers insulation material is the annulus of central hollow
Shape structure；Every layer of thickness is 5-10cm, external diameter 50cm-100cm, internal diameter 10-30cm.
Heat-insulation layer described in the utility model is enclosed on the outside of the furnace tubing；The bottom of the furnace tubing and heat-insulation layer
Contacts baseplate.
Corundum hollow circular-tube described in the utility model is enclosed on the inner side of the furnace tubing, and forms a cavity body structure,
Filled with insulation powder in the cavity body structure.
Resistance wire described in the utility model is wrapped on the outside of furnace tubing.
Thermocouple described in the utility model is located at every layer of insulation material immediate vicinity, and the temperature controller is connected by binding post
Outside body of heater.
Bell described in the utility model is located at the top end opening of the furnace tubing.
Preferably, furnace tubing described in the utility model is ceramic boiler tube, and its external diameter is adapted to the internal diameter of above-mentioned heat-insulation layer,
Boiler tube wall thickness is 10mm.
The internal diameter of corundum hollow circular-tube described in the utility model is 80-140mm, wall thickness 3mm.
Insulation powder described in the utility model is zirconium oxide, particle size 0.3mm.The thermal conductivity of zirconium oxide is 800-
1000 DEG C, 2.09W/ (mK).
The utility model prepares lanthanum bromide cerium crystal using high-temperature melting method, and lanthanum bromide cerium crystalline substance is prepared using said apparatus
Body, comprise the following steps：
1) appropriate seed crystal is taken to be put into crucible bottom of the tube as seed crystal from the material for not being brominated lanthanum melting at high temperature；
2) cerium lanthanum bromide crystal raw material will be mixed to add in the above-mentioned crucible pipe containing seed crystal, crucible pipe is blocked with quartz wedge
Mouthful, and seal crucible tube opening end with resin；
3) packaged crucible pipe is placed in the center of the insulation powder of the adjustable crystal growing apparatus of the thermal field, heating
Melt, a period of time is incubated after the completion of material, room temperature is then gradually drop, produces lanthanum bromide cerium crystal.
Wherein, step 2) operates in the glove box for fill high pure nitrogen.
Foregoing method, the step 1) seed crystal are quartz crystal.
Foregoing method, step 2) is described mix cerium lanthanum bromide crystal raw material by anhydrous lanthanum bromide and the mixing of anhydrous bromination cerium and
Into, wherein the doping mol ratio of anhydrous bromination cerium is m, 0.0001<m<0.1.
Foregoing method, step 3) are specially：Packaged crucible pipe is placed in described device, with 50-100 DEG C/h liters
Temperature is to 800 DEG C -850 DEG C (preferably 800 DEG C), and in the melting sources stage, material temperature is not higher than quartz crystal fusing point；Material is completed
Afterwards, 24h-48h (preferably 24h) is incubated, is first cooled using 0.3-0.6 DEG C/h (preferably 0.3 DEG C/h) rate of temperature fall, lanthanum bromide cerium
Melt makes crystal eliminate out the seed crystal toward the growth of C direction of principal axis, continued with 0.10-0.15 DEG C/h (preferably in the presence of seed crystal
0.15 DEG C/h) rate of temperature fall be down to room temperature.
The utility model also provides the lanthanum bromide cerium crystal prepared according to the method described above.The chemical composition of the crystal is
Cex:La(1-x)Br3, wherein x be Ce displacement La mol ratio, 0.0001<x<0.1.The crystal grown using this method, crystal
Quality conformance is high, is advantageous to mass production, and mechanical component is few needed for growth furnace, and growing environment is stable, reduces crystal
Defect.
In an embodiment of the present utility model, static lanthanum bromide cerium crystal growing method that thermal field is adjustable, bag
Include following steps：
(1) the thermal field adjusting stage：Heat-insulation layer internal diameter size is designed according to crucible size, insulation will be filled up in hollow alundum tube
Powder, 800 DEG C then are risen to 50-100 DEG C/h, then cooled with 100C/h rate of temperature fall, each section of heat-insulation layer is tested every 1h
Temperature.After being down to room temperature, thermal field curve is drawn with the temperature data measured.Thermal field figure during 783 DEG C of the curve is compared again
The temperature lowering curve of conventional crucible descent method, each heat-insulation layer size is repaired, is repeated the above steps, until the drop of the crystal growing apparatus
The temperature curve that warm curve declines stove with the size conventional crucible coincide substantially.
(2) the raw material preparatory stage：The material for not being brominated lanthanum melting at high temperature is first selected as seed crystal such as quartz-crystal
Body, it is put into silica crucible tip bottom.Further according to formula Cex:La(1-x)Br3, suitable x is first selected, then by corresponding mole
Percentage weighs required super dry anhydrous bromination cerium in glove box, lanthanum bromide raw material, uniformly loads special quartz after mixing
In crucible, the silica crucible mouth of pipe is blocked with quartz wedge, then seals the silica crucible mouth of pipe with epoxy resin, by the stone equipped with raw material
English crucible takes out glove box (filling high pure nitrogen), is sealed the mouth of pipe fusing of silica crucible using oxyhydrogen flame.
(3) the material stage：Packaged quartz ampoule is fitted into crystal growing apparatus, is at the interposition of device
Put, then will rise to 800 DEG C with 50-100 DEG C/h, quartz crystal fusing point is not higher than in the staged material temperature degree of melting sources.Material
After the completion of, it is incubated 24h.
(4) crystal growth phase：First cooled using 0.3 DEG C/h rate of temperature fall, effect of the lanthanum bromide cerium melt in seed crystal
Under, crystal is eliminated out the seed crystal toward the growth of C direction of principal axis, continue the rate of temperature fall cooling with 0.15 DEG C/h, until room temperature is down to,
Single crystallization is completed, and crystal growth finishes.Finally take out silica crucible.
The utility model has advantages below：
The adjustable crystal growing apparatus of thermal field provided by the utility model, the change of thermograde is produced by adjusting thermal field
Change, in this, as crystal growth driving force.Compared with conventional crucible descent method, reduce growth furnace and rise, decline, crystalline substance turn waits dynamic
Force system, growth course keep fairly static, the characteristic of without motion mechanism, make crystal growing process solid liquid interface stable, reduce
Crystal internal stress, is very beneficial for the big crystal of growth diameter.The adjustable crystal growth dress of thermal field provided by the utility model
Put, various sizes of crystal can be adapted to, simple in construction, maintaining is convenient, is advantageous to mass production, to lanthanum bromide cerium crystal
Industrialization is extremely advantageous.
Brief description of the drawings
Fig. 1 is the adjustable crystal growing apparatus profile of thermal field in the utility model embodiment 1；Wherein, 1- bells, 2- add
Hot stove pipe, 3- resistance wires, 4- heat-insulation layers, 5- thermocouples, 6- corundum hollow circular-tubes, 7- crucibles pipe (are equipped with and mix cerium lanthanum bromide crystal
Raw material), 8- insulation powders.
Stove thermal field figure declines stove with conventional crucible when Fig. 2 is 783 DEG C of crystal growing apparatus in the utility model embodiment 1
Temperature lowering curve figure；Wherein, ordinate represents the height of whole stove heat-insulation layer.
Embodiment
The utility model is further described below by embodiment.Raw material, examination used in following examples
Agent and instrument can be obtained by way of buying commercially available prod.
In description of the present utility model, unless otherwise indicated, the orientation or state relation of the instruction such as term " on ", " under "
It is for only for ease of description the utility model and simplifies and describe, rather than indicates or imply that signified device or element must have
Specific orientation, with specific azimuth configuration and operation, therefore it is not intended that to limitation of the present utility model.
Static lanthanum bromide cerium crystal growing method that the thermal field of embodiment 1 is adjustable
The adjustable crystal growing apparatus of thermal field (Fig. 1) is 5cm by 10 thickness degree in the present embodiment, and internal diameter is 10cm silicic acid
Aluminium heat insulation material is stacked and formed, and the external diameter of first layer is 40cm from top to bottom, and the external diameter of the second layer is 43cm, the external diameter of third layer
For 46cm, the 4th layer, the external diameter of layer 5 be 52cm, the external diameter of layer 6 is 46cm, and the external diameter of layer 7 is 43cm, the 8th layer
External diameter be 53cm, the 9th layer of external diameter is 55cm, and the tenth layer of external diameter is 60cm.Quartz crystal is first cut into edge during charging
The strip seed crystal of C axles, size are 3mm × 3mm × 15mm, and C direction of principal axis is parallel with length direction (15mm), is put into silica crucible
Bottom.Again by the anhydrous lanthanum bromide voluntarily synthesized, anhydrous bromination cerium mix to mix cerium lanthanum bromide crystal raw material (wherein anhydrous
298.5 grams of lanthanum bromide, anhydrous 1.5 grams of bromination cerium), load silica crucible pipe after uniformly being mixed in the glove box for fill high pure nitrogen
In, the crucible mouth of pipe then is blocked with quartz wedge, then seals the mouth of pipe with epoxy resin, takes out glove box, using oxyhydrogen flame by stone
The mouth of pipe fusing of English crucible seals.Silica crucible is put into crystal growing apparatus again and (is placed in the zirconium oxide that particle size is 0.3mm
Be incubated powder center) in temperature increasing for melting materials, be warming up to 800 DEG C with 50-100 DEG C/h；After the completion of 8-16h materials, 24h is incubated, then
First cooled using 0.3 DEG C/h rate of temperature fall, lanthanum bromide cerium melt is eliminated out crystal and given birth to toward C directions in the presence of seed crystal
Long seed crystal, continue the rate of temperature fall cooling with 0.15 DEG C/h, until being down to room temperature, single crystallization is completed, and crystal growth finishes.Most
After take out silica crucible.
Gained transparent single crystal size is 25 × 50mm of Φ3, cut and be packaged into 25 × 25mm of Φ3Scintillator, test the flicker
The scintillation detector that body is coupled into Bialkali photocathode photomultiplier, the photopeak energy resolution to radioactive source are 3.5%.Gained
The chemical composition of crystal is Cex:La(1-x)Br3, x=0.005.
Static lanthanum bromide cerium crystal growing method that the thermal field of embodiment 2 is adjustable
The adjustable crystal growing apparatus of thermal field is 5cm by 11 thickness degree in the present embodiment, and the alumina silicate that internal diameter is 13cm is protected
Adiabator is stacked and formed, and the external diameter of first layer is 40cm from top to bottom, and the external diameter of the second layer is 44cm, and the external diameter of third layer is
47cm, the 4th layer, the external diameter of layer 5, layer 6 be 56cm, the external diameter of layer 7 is 46cm, and the 8th layer of external diameter is 51cm,
9th layer of external diameter is 59cm, and the tenth layer of external diameter is 65cm, and the external diameter of eleventh floor is 70cm.First by quartz crystal during charging
The strip seed crystal along C axles is cut into, size is 3mm × 3mm × 15mm, and C direction of principal axis is parallel with length direction (15mm), is put into
Silica crucible bottom.Again cerium lanthanum bromide crystal raw material is mixed by what the anhydrous lanthanum bromide voluntarily synthesized, anhydrous bromination cerium mixed
(wherein anhydrous 696.5 grams of lanthanum bromide, anhydrous 3.5 grams of bromination cerium), load after uniformly being mixed in the glove box for fill high pure nitrogen
In silica crucible pipe, the silica crucible mouth of pipe then is blocked with quartz wedge, then seals the mouth of pipe with epoxy resin, takes out glove box,
The mouth of pipe fusing of silica crucible is sealed using oxyhydrogen flame.Silica crucible is put into crystal growing apparatus again and (is placed in particle size
For 0.3mm zirconium oxide be incubated powder center) in temperature increasing for melting materials, be warming up to 800 DEG C with 50-100 DEG C/h；8-16h materials are completed
Afterwards, 24h is incubated, is then first cooled using 0.3 DEG C/h rate of temperature fall, lanthanum bromide melt washes in a pan crystal in the presence of seed crystal
The seed crystal toward the growth of C directions is eliminated out, continues the rate of temperature fall cooling with 0.1 DEG C/h, until being down to room temperature, single crystallization is completed, brilliant
Body growth finishes.Finally take out silica crucible.
Gained transparent single crystal size is 38 × 76mm of Φ3, cut and be packaged into 38 × 38mm of Φ3Scintillator, test the flicker
The scintillation detector that body is coupled into Bialkali photocathode photomultiplier, the photopeak energy resolution to radioactive source are 3.6%.Gained
The chemical composition of crystal is Cex:La(1-x)Br3, x=0.005.
Static lanthanum bromide cerium crystal growing method that the thermal field of embodiment 3 is adjustable
The adjustable crystal growing apparatus of thermal field is 5cm by 12 thickness degree in the present embodiment, and the alumina silicate that internal diameter is 15cm is protected
Adiabator is stacked and formed, and the external diameter of first layer is 40cm from top to bottom, and the external diameter of the second layer is 44cm, and the external diameter of third layer is
47cm, the 4th layer, the external diameter of layer 5, layer 6 be 58cm, the external diameter of layer 7 is 45cm, and the 8th layer of external diameter is 52cm,
9th layer of external diameter is 59cm, and the tenth layer of external diameter is 65cm, and the external diameter of eleventh floor is 70cm, and the external diameter of Floor 12 is
75cm.Quartz crystal is first cut into the strip seed crystal along C axles during charging, size is 3mm × 3mm × 15mm, C direction of principal axis with
Length direction (15mm) is parallel, is put into silica crucible bottom.Again by the anhydrous lanthanum bromide voluntarily synthesized, anhydrous bromination cerium mix and
Into mix cerium lanthanum bromide crystal raw material (wherein 995 grams of lanthanum bromide, 5 grams of bromination cerium), in the glove box for fill high pure nitrogen uniformly
It is fitted into after mixing in silica crucible pipe, then blocks the silica crucible mouth of pipe with quartz wedge, then seal the mouth of pipe with epoxy resin, take
Go out glove box, sealed the mouth of pipe fusing of silica crucible using oxyhydrogen flame.Silica crucible is put into crystal growing apparatus again (to be placed in
Particle size be 0.3mm zirconium oxide be incubated powder center) in temperature increasing for melting materials, be warming up to 800 DEG C with 50-100 DEG C/h；8-16h
After the completion of material, be incubated 48h, then first using 0.3 DEG C/h rate of temperature fall cool, lanthanum bromide melt in the presence of seed crystal,
Crystal is eliminated out the seed crystal toward the growth of C directions, continue the rate of temperature fall cooling with 0.1 DEG C/h, until being down to room temperature, single crystallization
Complete, crystal growth finishes.Finally take out silica crucible.
Gained transparent single crystal size is 52 × 105mm of Φ3, cut and be packaged into 52 × 52mm of Φ3Scintillator, test the sudden strain of a muscle
The scintillation detector that bright body is coupled into Bialkali photocathode photomultiplier, the photopeak energy resolution to radioactive source are 3.4%.Institute
The chemical composition for obtaining crystal is Cex:La(1-x)Br3, x=0.005.
The utility model uses a kind of adjustable dimension, readily replaceable adiabator layer, and only needs one-part form to heat,
Turn and platform rise and fall system without brilliant.By adjusting the size of adiabator layer, stove thermal field is set to be suitable for lanthanum bromide cerium
Crystal growth.The utility model carries out crystal growth using fairly static side of without motion mechanism.Conventional crucible is overcome to decline
The shortcomings of method is high to descending system precision requirement, and differ greatly bad batch duplicating between stove, and space-consuming is big.Lanthanum bromide
Cerium crystal easily realizes that sequencing grows, extremely advantageous to the control of lanthanum bromide cerium crystal aufwuchsplate, and growing environment is stable, can effectively keep away
Exempt from crystal defect.The making of crystal growing apparatus is simple, maintains easily cleaning.
Embodiment described above be only to absolutely prove preferred embodiment that the utility model is enumerated, it is of the present utility model
Protection domain not limited to this.The equivalent substitute or conversion that those skilled in the art are made on the basis of the utility model,
Within the scope of protection of the utility model.
Claims (4)
- A kind of 1. adjustable crystal growing apparatus of thermal field, it is characterised in that including bell, heat-insulation layer, furnace tubing, resistance wire, Corundum hollow circular-tube, insulation powder, thermocouple and temperature controller；Wherein, the heat-insulation layer is the circular laminated structure from top to bottom stacked by multilayer aluminum silicate insulation material, most Lower floor is solid base plate, total number of plies N=10-30 of the heat-insulation layer；Every layer of thickness is 5-10cm, external diameter 50cm-100cm, Internal diameter 10-30cm；The heat-insulation layer is enclosed on the outside of the furnace tubing；The bottom of the furnace tubing and heat-insulation layer contacts baseplate；The corundum hollow circular-tube is enclosed on the inner side of the furnace tubing, and forms a cavity body structure, in the cavity body structure In filled with insulation powder；The resistance wire is wrapped on the outside of furnace tubing；The thermocouple is located at every layer of insulation material immediate vicinity, and the temperature controller is connected to outside body of heater by binding post；The bell is located at the top end opening of the furnace tubing.
- 2. device according to claim 1, it is characterised in that the furnace tubing is ceramic boiler tube, its external diameter with it is above-mentioned The internal diameter adaptation of heat-insulation layer, boiler tube wall thickness is 10mm.
- 3. device according to claim 1, it is characterised in that the internal diameter of the corundum hollow circular-tube is 80-140mm, wall Thickness is 3mm.
- 4. device according to claim 1, it is characterised in that the insulation powder is zirconium oxide, and particle size is 0.3mm。
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| CN201720669049.5U CN206814880U (en) | 2017-06-09 | 2017-06-09 | The adjustable crystal growing apparatus of thermal field |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107119315A (en) * | 2017-06-09 | 2017-09-01 | 厦门中烁光电科技有限公司 | The method for preparing lanthanum bromide cerium crystal using the adjustable crystal growing apparatus of thermal field |
| CN114808108A (en) * | 2022-04-29 | 2022-07-29 | 中国科学院福建物质结构研究所 | Bridgman-Stockbarger method crystal growth device and application thereof |
-
2017
- 2017-06-09 CN CN201720669049.5U patent/CN206814880U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107119315A (en) * | 2017-06-09 | 2017-09-01 | 厦门中烁光电科技有限公司 | The method for preparing lanthanum bromide cerium crystal using the adjustable crystal growing apparatus of thermal field |
| CN107119315B (en) * | 2017-06-09 | 2018-05-08 | 厦门中烁光电科技有限公司 | The method for preparing lanthanum bromide cerium crystal using the adjustable crystal growing apparatus of thermal field |
| CN114808108A (en) * | 2022-04-29 | 2022-07-29 | 中国科学院福建物质结构研究所 | Bridgman-Stockbarger method crystal growth device and application thereof |
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| CB03 | Change of inventor or designer information |
Inventor after: Wei Jiande Inventor after: Fang Shenghao Inventor after: Zhang Zhicheng Inventor after: Ye Ning Inventor after: Wu Shaofan Inventor after: Long Xifa Inventor before: Wei Jiande Inventor before: Fang Shenghao Inventor before: Zhang Zhicheng Inventor before: Ye Ning Inventor before: Wu Shaofan Inventor before: Long Xifa |
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