CN1067933A - Metal twin crystal and three crystalline growing technology and devices - Google Patents
Metal twin crystal and three crystalline growing technology and devices Download PDFInfo
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Abstract
Metal twin crystal of the present invention and three crystalline growing technology and devices.
The present invention is that the technology and the device of a kind of Bridgmen method growing metal twin crystal and three crystalline substances comprises feedstock production, crystal growth and annealing, use the 5N raw material, clean rear impurity content is lower than 100PPM, annealing temperature is 800～1000 ℃, and 10～12 hours time, motionless of crucible moves the temperature field when it is characterized in that growing, longitudinal temperature degree of the passing 15～20%/cm of temperature field, translational speed is 0.5～2 mm/min.
Implement equipment therefor of the present invention and comprise transmission rig, temperature-controlling mechanism, heat preservation mechanism and crucible.It is characterized in that used crucible is to be combined by different function structural parts.Have easy to usely, the life-span is long, and young brilliant and crystal is easy to load and unload, the crystallographic parameter of twin crystal and three crystalline substances is easy to advantages such as control.
Description
The present invention relates to the growth method and the device of Metallic Solids, relate in particular to the growth of Brdgman method and the used crucible of metal twin crystal and three crystalline substances.
Single crystal is well-known a kind of solid material, and its function and character that is better than polycrystalline material is applied in various fields, and especially the application at the top science and front subject is more extensive.Yet single crystal still all has certain difficulty in practical application area in technology of preparing, and costs an arm and a leg.Polycrystalline material, people are seen everywhere in actual life, but because the existence of chaotic crystal boundary and other defective, the technical indicator and the physical and chemical performance of material have been influenced, France (C.Rey in 1985, P.Mussot, A.M.Vroux and A.Zaoui, J.Physique46(1985) (4-645) reported the preparation work of copper three crystalline substances, but do not give the grain boundary structure of copper three crystalline substances, and technology of preparing and use crucible, this shows that the control of crystal boundary orientation does not reach requirement, Japanese scientist thinks can not be considered as directed copper three crystalline substances.The preparation work of orientation three crystalline substances of refractory metal still is not reported, and the development work of directed metal three crystalline substances that grain boundary structure that hence one can see that is accurately controlled still is in initial period.Therefore, finding out influences the polycrystalline material performance factor, takes suitable approach to overcome or compensates the influence that is caused by chaotic crystal boundary and other defective, has become the direction that current physics worker makes great efforts.The metal twin crystal of using directed growth and three crystal research grain boundary structure and be current in the world about interface science and engineering to effect of material performance, crystal boundary design, the important content of crystal boundary modified and surface physics research.
The objective of the invention is in order to overcome the crystal habit that exists in metal twin crystal and three crystal growths strong, it is wayward to grow, impurity effect is remarkable, many nucleation centres make to have the complete substructure of influence, Small angle grain boundary in the crystal, lattice distortion, and introduce other simple substance element and easily in crystal, form defectives such as two second phase particles, grow good twin crystal of grain boundary structure integrity and three crystal, obtain the crystal boundary face of predefined crystallographic parameter.
Vertical Bridgman method is adopted in the preparation of directed metal twin crystal of the present invention and three crystalline substances, is to be positioned in the plumbago crucible of special shape having the young crystalline substance of determining orientation, puts into the metallic substance that will grow again.Crucible places high vacuum silica tube (generally charging into casual gas again), the outside adds a temperature field with certain temperature gradient, crucible bottom is by crucible lever bracket water (or other heat-eliminating mediums) cooling, make the young brilliant fusing of starting material and part, then with certain speed body of heater that moves up, the deposite metal is promptly along young brilliant direction crystallographic orientation, and by the relation of the relative orientation between young crystalline substance formation twin crystal or three crystalline substances, its crystal boundary orientation is measured with the X-X-ray goniometer X.
Growing technology of the present invention and device, can satisfy molten point and be the metal below 1200 ℃ and the twin crystal of other solid materials and the preparation of three crystalline substances and require:
Maximum operating temperature: 1250 ℃, temperature-controlled precision: ± 1.0 ℃
Thermograde: 15-20 ℃/cm, heating power: 8KW
Body of heater miles of relative movement: 400mm(automatically+manually)
Movement velocity: (0.1-5) mm/min, precision: low speed jerking motion 0.005mm
Vacuum tightness: 5 * 10
-5Torr
Crystalline orientation control accuracy: ± 0.5 °
The diameter of each column monocrystalline: 20mm in twin crystal and three crystalline substances
Crystal length: greater than 50mm
The present invention is by frame and conducting system; Body of heater, heating and temperature controlling system; The crystalline growth velocity Controlling System: torque motor adds harmonic reduction, control power supply, vacuum system: silica tube vacuum chamber and fine pumping unit; Crucible system: plumbago crucible and crucible pole and holder.
Accompanying drawing 1 is a crystal growing apparatus host computer system of the present invention, and accompanying drawing 2 is complete machine controlling party block diagrams, and accompanying drawing 3 is speed control circuit skeleton diagrams.
Major technique of the present invention is summarized as follows:
1, growing apparatus
Growing apparatus of the present invention is by frame, body of heater, and heating source and temperature control system, crystalline growth velocity Controlling System, vacuum system, crucible waits composition.
A, frame see that accompanying drawing 1 is to add 2, two main silks of 1, four leading post of harmonic reduction by the moment unit to shoulder 3, guide pin bushing 4 is paid guide pillar 5, pays leading screw 6, vacuum chamber holder 7, body of heater 8, silica tube vacuum chamber 9, crucible pole 10, globars 11, crucible 12, counterweight 13, stove holder 14, shockproof lower margin 15 is formed, guide pin bushing 4 is a matrix material, and adjustable gaps has self-lubricating and self-damping performance.
B, body of heater, heating source and temperature control system
The physical dimension of heating furnace body is φ 500 * 700mm, with 8 globarss as thermal source.The temperature field is controlled and is regulated by asymmetric heating element and stove internal cooling water pipe in the stove.Lagging material is that precision temperature controller is used in Lay mineral wool, power given and temperature control for high purity aluminium oxide refractory brick and polycrystalline.
C, crystalline growth velocity Controlling System
Speed of growth control is one of key problem in technology of twin crystal and three crystals growths.Crystal growth of the present invention is controlled by mobile body of heater.Use the mariages thick stick, the motion of four guide pillars guiding body of heater has very high stationarity, the speed control system circuit block diagram as shown in Figure 2, crystalline growth velocity control is made up of permanent magnet dc motor, velodyne and velocity control system.This system is that the electric signal that will import is directly changed into the needed slow speed of revolution of load and enough big moment, and directly be connected with load, need not by retarding mechanisms such as gears, therefore, the speed stability height, dynamic property is good, the operation balance, pilot circuit adopts indifference system, has negative velocity feedback and Current Negative Three-Point Capacitance, can guarantee the stability and the rigidity of system.Rotating speed adopts numeral to show, and is visual and clear.Pulse width modulated mode is adopted in the adjusting of output rating, the present invention utilizes powerful on-off action the direct supply voltage transitions to be become the square-wave voltage of certain frequency, the electricity that is added to direct-current motor cashier's office in a shop, by control to the square-wave pulse width, change the average voltage on the armature, thereby regulate the rotating speed of torque motor, (seeing accompanying drawing 3).
D, vacuum system
Vacuum chamber is that silica tube, the silica tube lower end flange of last end closure is fastened in the vacuum chamber holder by the tetrafluoroethylene screw rod.Crucible pole is a double wall tube, can really connect with heat-eliminating medium to cool off crucible tray, and water coolant flow to outer tube by interior pipe, so there is not oscillation phenomenon.After vacuum tightness reaches necessary requirement, charge into the high-purity inert shielding gas of low pressure.
E, crucible
The shape of crucible and structure are that can decision prepare one of important determinative of perfect crystal.Can grow the twin crystal or three crystal of the grain boundary structure that requires, how to control the structure of crystal boundary easily, the structure and the shape that depend on crucible, the present invention studies successful twin crystal and three spar China ink crucible is exactly to design for this reason, see that accompanying drawing 2, accompanying drawing 3, twin crystal and three brilliant crucibles all are by young brilliant cover, young crystal cup, the growth zone of transition, different pieces such as vitellarium and shell combine.
Below in conjunction with description of drawings it
In the accompanying drawing 2,3: the 1st, the cylinder at the band end, the 2nd, seed crystal cover, the 3rd, seed crystal block set, the 4th, shouldering district, the 5, the 6th, vitellarium
The seed crystal block set 3 of twin crystal crucible as shown in Figure 3, be to combine by two 180 ° of symmetric semicolumns, centre bit at each cylinder is equipped with a round tube hole 8 that parallels with the cylinder axis, the external diameter 9(of through hole internal diameter and seed crystal cover sees accompanying drawing 4) equate that the seed crystal cover can freely be placed inside.
The seed crystal cover is seen accompanying drawing 4, also is that 180 ° of symmetric two semicolumns are formed, its upper end five/part is a cylinder (being the seeded growth district), it is the rounding platform of π/6 that the cylinder lower end connects the inclination angle, and a rounding platform lower end and a cross section are that foursquare rectangular parallelepiped joins, and are used for fixing the seed crystal district.180 ° of planes of symmetry are the plane that square diagonal lines constitutes.
Crystal growth district and shouldering district are all 180 ° of symmetric two semicolumns and form, see accompanying drawing 5, its external diameter is identical with the internal diameter of shell 7 in the accompanying drawing 1, it is crystal boundary face position that the equal-diameter part in crystal growth district is completed a business transaction the plane that two intersections of generation constitute by two isometrical cylinders, because completing a business transaction the district is a spire structure, therefore can retrain the growth of crystal boundary, the lower end in isometrical district is shouldering district 9, be to be that two rounding platforms of π/6 constitute by the inclination angle that end face intersects, the lower end of rounding platform be one with the isometrical seeded growth district of seed crystal set upper side cylinder, 180 ° of planes of symmetry are the plane that two cylinder axis constitute.
The seed crystal block set of three brilliant crucibles is to combine by 120 ° symmetric three, see shown in the accompanying drawing 6, the seed crystal cover is seen accompanying drawing 7, its shouldering district and vitellarium also are 120 ° symmetric three, wherein the shouldering district is that the tangent rounding platform in π/6 bases constitutes by the inclination angle, the vitellarium also is that three isometrical cylinders are completed a business transaction formation mutually, completes a business transaction into three class top steps, sees accompanying drawing 8.All the other structures are identical with the twin crystal crucible.
The used crucible of the present invention has easy to use, life-span is long, seed crystal and crystal are easy to loading and unloading, the crystallographic parameter of twin crystal and three crystalline substances (comprising crystalline orientation and crystal boundary planar orientation) is easy to advantages such as control, and crucible of the present invention also can be used for the twin crystal and three crystalline substances of other high-melting point metal materials or functional materials.
Characteristics of the present invention are:
1, adopts the high stability motor system
Because the quality of crystal growth equipment motor system stability, directly influence the quality of growing crystal.To twin crystal and three crystals growths, the crystal boundary that can obtain preestablishing crystallographic parameter is a final purpose.Reach this purpose, require twin crystal and three crystalline substances solid-liquid interface in process of growth to pass on balance and stability ground, if motor system is stable bad, to destroy this solid-liquid system balance, make the growth appearance of the single column single crystal in twin crystal and three crystal inconsistent, thereby break the stable balance that forms of crystal boundary; On the other hand, because crystal boundary is the artificial defective of introducing, its stability of structure only is in metastable state when the equilibrium state of system, in case the balance of growth mechanism is broken, crystal boundary certainly will form the trap of other defective, and catches other simple substance element and compound, form bigger defective, thereby destroy predefined grain boundary structure, the crystal boundary face of the crystallographic parameter that can not get wanting, crystal growth promptly fails.Therefore, the motor system of high stability is for being primary conditions with bridgman method growing metal twin crystal and three crystal.
The motor system of crystal growth of the present invention sees that accompanying drawing 1 adopts four guide pillars, and double lead and moment of torsion are big, and the torque motor that stability is high drives, and retarding mechanism adopts shockproof harmonic speed reducer, and guidance system adopts the little self-lubricating composite of frictional damping.Body of heater uses shockproof and damping with the balance mode counterweight.Therefore the speed of creeping of motor system is less than 1 μ, and the shake of the motor system that motor movement causes is less than 0.5 μ, and these parameters are than high 1～2 order of magnitude of homemade single crystal pulling equipment.
2, crucible is motionless, moves the temperature field
The stability of solid-liquid interface is growing high-quality crystalline essential condition.For the growth of metal twin crystal and three crystalline substances, the balance of solid-liquid system is particularly important.The crystal boundary face of the crystalline orientation that is designed in advance just must make twin crystal or three crystal solid-liquid interface in growth steadily pass.
The present invention adopts fixedly crucible, moves the method for temperature field, has so both avoided the stable influence to growth interface by machine system, has also reduced to cause owing to the random variation of temperature simultaneously the fluctuation of growth interface.
3, built-up type high-repetition-rate plumbago crucible
Can grow the twin crystal or three crystal of the grain boundary structure that requires, how control the structure of crystal boundary easily, depend on the structure and the shape of crucible, the present invention studies successful twin crystal and three spar China ink crucible is exactly to design for this reason.
4, the strict seed crystal of selecting, the accurately crystal parameter of definite crystal boundary.Seed size: 5 * 5 * 50mm
Crystal is in process of growth, and it is continuities of defective in the seed crystal that many defectives are arranged, as dislocation, Small angle grain boundary etc., twin crystal and three crystal will obtain the crystal boundary that perfect crystal is learned structural approach owing to adopt two seed crystals and three seeded growths, the selection of seed crystal is extremely important, and its practice is:
A, the strict son's crystalline substance of selecting are accurately set the crystal boundary orientation;
Seed crystal should be selected good uniformity, and the measured monocrystalline of matter partly cuts, to guarantee no above-mentioned defective in the crystal seed.Because twin crystal or three crystalline substances are taked two young brilliant or three young crystals growths, and the orientation of crystal boundary face depends on the orientation of the crystal boundary face of seed crystal, thus accurately set the orientation at young Jingjing interface, for the growth of twin crystal and three crystalline substances, most important.We require the direction of crystal seed and the two young crystalline substance that sets, the crystalline orientation errors of three young crystal boundary kinds to spend less than 0.3.
The processing of b, seed crystal, differing materials crystalline seed crystal, the treatment temp difference, as copper crystal:
In 550 ℃ of long-time (24 hours-72 hours) anneal of low temperature, eliminate structural stress, and the other defect that produces therefrom; High temperature can be eliminated thermal stresses 900 ℃ of annealing down, re-uses after strict clean.The so-called cleaning promptly earlier peelled off zone of oxidation with acid or alkaline solution, cleans with ethanol or acetone again, handles with deionized water at last.
5, reliable and stable temperature field
Because metal twin crystal and three crystalline substances are in process of growth, spontaneous crystallization speed is difficult to control, and this brings very big difficulty for the twin crystal and three crystals growths of growth (obtaining) complete grain boundary structure.And reliable and stable temperature field is the effective means of control crystal spontaneous crystallization.Because twin crystal and three crystalline substances only mobile temperature field in process of growth, so adopt the body of heater of big thermal capacity, make heating power constant, make temperature very blunt with respect to the random variation of heating power, temperature control element is selected in strictness in addition, makes that the variation of heating power is as much as possible little, and this just causes a reliable and stable temperature field, according to 15～20 ℃/cm of thermograde of temperature and the needs of the growth of twin crystal and three Jingjings circle, the crystalline growth velocity that we select is 1mm/min.
6, the recovery again of grain boundary structure: metal twin crystal or three crystal are in process of growth, because it is difficult to control from crystallization rate, so the structure of formed crystal boundary face generally is unfavorable, can think from microcosmic angle, the atom at crystal boundary place, some is not in balance and stability with the end of crystal growth state is necessary to handle again, and experiment shows that the crystalline substance before and after handling is the difference of the order of magnitude before the emission of dislocation and the anneal at the interface.
The crystal that the present invention finishes growth is high temperature annealing under near the temperature of crystalline melting point again, stablize straight through twin crystal and three crystalline crystal boundary faces that anneal obtains, no matter the stable of this structure is the structural experiment that is used for the interface, still use mechanical test, final crystal boundary face all is stable.
List the twin crystal and the three crystal growth embodiment of zinc, aluminium, three kinds of metallic substance of copper below:
Material zinc (Zn) aluminium (Ae) copper (Cu)
Raw material is selected particle or the bar-like raw material of purity more than 99.999% for use
The direction of growth＜0001〉＜110＜110,＜100
Crystal boundary planar orientation＜10T1〉＜100＜100,＜1T0 〉
Single crystal growing growth high-quality oriented single crystal body is selected for use for seed crystal
Seed crystal chooses＜and 0001〉＜110＜110,＜100〉high-quality monocrystalline
Determine grain boundary structure selection crystal boundary planar orientation with definite symmetrical crystal boundary, or twist boundaries
480 ℃ 760 ℃ 1200 ℃ of growth temperatures
Growth velocity 0.2 mm/min 0.8 mm/min 1 mm/min
Recover to stablize/12 hours 640 degree of crystal boundary 380 degree and spent/24 hours in/12 hours 1050
Annealing temperature
Twin crystal size 20 * 40 * 80mm 20 * 40 * 80mm 20 * 40 * 80mm
Three brilliant size 35 * 40 * 60mm 35 * 40 * 80mm 35 * 40 * 80mm
Claims (7)
1, the technology of a kind of Bridgman method growing metal twin crystal or three crystalline substances comprises feedstock production, growth and annealing, wherein, uses the 5N raw material, and clean rear impurity content is lower than 100PPM; The crystal annealing temperature is 800～1000 ℃, 10～12 hours time, it is characterized in that:
A, the strict son's crystalline substance of selecting are accurately set the crystal boundary orientation;
B (seed crystal being carried out anneal at low temperature 550 ℃ long-time (24～72 hours)) annealing temperature is the high-temperature zone near crystalline melting point.
C, peel off the outer zone of oxidation of seed crystal, clean, handle with deionized water at last with ethanol or acetone again with acid or alkaline solution.
Crucible is motionless when d, twin crystal or three crystals growths, only moves temperature, a temperature longitudinal temperature gradient be 15～20 degree/centimetre, translational speed is the 0.5-5 mm/min.
2, the growing technology of metal twin crystal according to claim 1 or three crystalline substances is characterized in that, seed crystal cleans and is of a size of 5 * 5 * 50Cm;
3, the growing technology of metal twin crystal according to claim 1 or three crystalline substances is characterized in that, the translational speed of temperature field is 0.5～5 mm/min.
4, the growing technology of metal twin crystal according to claim 1 or three crystalline substances is characterized in that seed crystal is carried out anneal.
A, to the annealing temperature of zinc: 350～390 degree/10 hours;
B, to the annealing temperature of aluminium: 600～650 degree/12 hours;
C, to the annealing temperature of copper: 950～1000 degree/24 hours.
5, the growing technology of metal twin crystal according to claim 1 or three crystalline substances is characterized in that, the crystalline speed of growth: zinc is 0.2 mm/min, and aluminium is 0.8 mm/min, and copper is 1 mm/min.
6, the growing technology of metal twin crystal according to claim 1 or three crystalline substances is characterized in that the crystalline growth temperature: zinc is～500 ℃ of aluminium is～760 ℃, copper is～and 1200 ℃.
7, implement the metal twin crystal of claim 1-6 or the equipment of three crystals growth methods, comprise transmission rig, temperature controlling system, the crystalline growth velocity Controlling System, crucible, wherein transmission rig comprises four guide pillars, mariages power, torque motor and harmonic speed reducer, it is characterized in that: used crucible: a is combined by two 180 ° of symmetric semicolumns during (1) growing metal twin crystal, at each semicolumn center a round tube hole that parallels with the cylinder axis is arranged, the external diameter of through hole internal diameter and seed crystal cover equates; B, seed crystal cover also are made up of 180 ° of symmetric two semicolumns, its upper end five/part is a cylinder, it is the rounding platform of π/6 that the cylinder lower end connects the inclination angle, and a rounding platform lower end and a cross section are that foursquare rectangular parallelepiped joins, and 180 ° of planes of symmetry are the plane that square diagonal lines constitutes; C, crystal growth district and shouldering district all are that 180 ° of symmetric two semicolumns are formed, and its external diameter is identical with the internal diameter of shell.
When (2) growing metal three is brilliant, used crucible; A, combined by 120 ° of identical three cylinders bodies, three cylindrical center a round tube hole that parallels with the cylinder axis is arranged, the external diameter of through hole internal diameter and seed crystal cover equates;
B, seed crystal cover also are made up of 120 ° of identical three cylinders bodies, its upper end five/part is that connection inclination angle, a cylinder lower end is the tangent rounding platforms in π/6 bases, a rounding platform lower end and a cross section are that foursquare rectangular parallelepiped connects, 120 ° of three symmetric three semicolumn formed, and its external diameter is identical with the internal diameter of shell.
C, crystal growth district and shouldering district all be 120 ° three symmetric, three semicolumns are formed, its external diameter is identical with the internal diameter of shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92104638 CN1025633C (en) | 1992-06-19 | 1992-06-19 | Metallic bicrystal and tricrystal growth technology and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92104638 CN1025633C (en) | 1992-06-19 | 1992-06-19 | Metallic bicrystal and tricrystal growth technology and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1067933A true CN1067933A (en) | 1993-01-13 |
| CN1025633C CN1025633C (en) | 1994-08-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92104638 Expired - Fee Related CN1025633C (en) | 1992-06-19 | 1992-06-19 | Metallic bicrystal and tricrystal growth technology and device |
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| CN (1) | CN1025633C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334260C (en) * | 2001-08-13 | 2007-08-29 | 西门子公司 | Method for producing monocrystalline component, having complex moulded structure |
| CN102002752A (en) * | 2010-11-22 | 2011-04-06 | 福建福晶科技股份有限公司 | Process method for growing bismuth boronate crystals |
| CN102084037A (en) * | 2008-06-16 | 2011-06-01 | Gt太阳能公司 | Systems and methods for growing monocrystalline silicon ingots by directional solidification |
| CN104164699A (en) * | 2013-05-17 | 2014-11-26 | 中国科学院合肥物质科学研究院 | Crucible for growing metal bicrystal |
| CN105369361A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and apparatus for preparing sapphire single crystals by moving thermal field |
| CN107287657A (en) * | 2017-06-26 | 2017-10-24 | 北京中材人工晶体研究院有限公司 | The growing method and gained crystal of a kind of lanthanum bromide scintillation crystal |
| CN108048904A (en) * | 2017-11-30 | 2018-05-18 | 安徽省恒伟铋业有限公司 | A kind of bismuth crystal making apparatus |
| CN112080790A (en) * | 2020-08-20 | 2020-12-15 | 上海交通大学 | Die for preparing three-crystal and preparation method of three-crystal |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2853913B1 (en) * | 2003-04-17 | 2006-09-29 | Apollon Solar | CUTTER FOR A DEVICE FOR MANUFACTURING A BLOCK OF CRYSTALLINE MATERIAL AND METHOD OF MANUFACTURE |
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1992
- 1992-06-19 CN CN 92104638 patent/CN1025633C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334260C (en) * | 2001-08-13 | 2007-08-29 | 西门子公司 | Method for producing monocrystalline component, having complex moulded structure |
| CN102084037A (en) * | 2008-06-16 | 2011-06-01 | Gt太阳能公司 | Systems and methods for growing monocrystalline silicon ingots by directional solidification |
| CN102002752A (en) * | 2010-11-22 | 2011-04-06 | 福建福晶科技股份有限公司 | Process method for growing bismuth boronate crystals |
| CN104164699A (en) * | 2013-05-17 | 2014-11-26 | 中国科学院合肥物质科学研究院 | Crucible for growing metal bicrystal |
| CN105369361A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and apparatus for preparing sapphire single crystals by moving thermal field |
| CN105369361B (en) * | 2015-12-03 | 2018-04-10 | 河南西格马晶体科技有限公司 | A kind of thermal field movement prepares the method and device of sapphire monocrystal |
| CN107287657A (en) * | 2017-06-26 | 2017-10-24 | 北京中材人工晶体研究院有限公司 | The growing method and gained crystal of a kind of lanthanum bromide scintillation crystal |
| CN107287657B (en) * | 2017-06-26 | 2019-10-08 | 北京中材人工晶体研究院有限公司 | A kind of growing method and gained crystal of lanthanum bromide scintillation crystal |
| CN108048904A (en) * | 2017-11-30 | 2018-05-18 | 安徽省恒伟铋业有限公司 | A kind of bismuth crystal making apparatus |
| CN108048904B (en) * | 2017-11-30 | 2021-02-26 | 安徽省恒伟铋业有限公司 | Bismuth crystal manufacturing equipment |
| CN112080790A (en) * | 2020-08-20 | 2020-12-15 | 上海交通大学 | Die for preparing three-crystal and preparation method of three-crystal |
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|---|---|
| CN1025633C (en) | 1994-08-10 |
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