CN105624774A - Inorganic material single crystal growth method based on optical float-zone method quasi-continuous components - Google Patents
Inorganic material single crystal growth method based on optical float-zone method quasi-continuous components Download PDFInfo
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- CN105624774A CN105624774A CN201610136787.3A CN201610136787A CN105624774A CN 105624774 A CN105624774 A CN 105624774A CN 201610136787 A CN201610136787 A CN 201610136787A CN 105624774 A CN105624774 A CN 105624774A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/16—Heating of the molten zone
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/28—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/24—Complex oxides with formula AMeO3, wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. ortho ferrites
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Abstract
The invention discloses an inorganic material single crystal growth method based on optical float-zone method quasi-continuous components and belongs to the field of crystal growth. The preparation method includes the steps that high-purity raw materials are processed and react according to the molar ratio to prepare a polycrystal non-continuous component raw material series. The raw materials obtained according to an expected component change range are sequentially distributed and pressed into bars according to finite non-continuous component changes, sintered and placed in a float-zone furnace to grow. The method is characterized in that components are the same during butt joint of upper bars and lower bars, the components are gradually changed in sequence in the growth process, sequential growth of crystal in the minimum mismatch direction is facilitated, adjustment of parameters in the growth process is paid attention to, and a continuous change of the components in a melting zone is achieved through gradually-changed continuous mixing of the upper bar components and the lower bar components on component change portions and the stirring function of relative rotation. Through inspection, prepared crystal is good in performance, the components are easy to control, and prepared single crystal with continuous components provides possibility for high-flux material characterization analysis and preferential selection.
Description
Technical field
The present invention relates to the preparation method of a kind of monocrystalline crystalline material, particularly relate to the preparation method of the inorganic monocrystalline material of a kind of compositional variation, be applied to technical field of crystal growth and high-throughput technical field of material.
Background technology
In traditional material development process, investigator often through discrete in a large number and repeat crystal preparation experiment obtain enough monocrystal materials for various physical property characterize and test; And in this course, often need the growth conditions of long period to explore and direction detection to obtain the single crystal samples of specific components and direction; The more important thing is, in traditional material preparation method, what often obtain is the character of crystal in order to simulation sign consecutive variations of the fixing component of minority. Along with the development of material genome project, particularly high-throughput material design, preparation and the progress of high-throughput material characterization technology, the single crystal growth of continuous component becomes one of emphasis of studying from now on.
By the material preparation technology of continuous component, material planner only needs the character according to material to make fuzzy screening at first, then a large amount of continuous component samples is prepared by high-throughout material, then by characterizing the material that triage techniques just can obtain objective function continuously. The preparation of continuous component material can also in material character is explored quick position optimal component thus greatly shorten detective period, and can significantly reduce investigation of materials cost of development.
Floating zone method is the molten growing method in a kind of vertically district. Crystal interface in growth relies on optical focus heated sample melting, and maintains a stable melting zone by gravity and surface tension balance. Melting zone is moved from top to bottom or from bottom to top, after polycrystalline thawing in the process of a slow cooling, completes crystallisation process in the given direction of optimal direction or seed crystal. In crystal growth with floating zone method process, the balance that melting zone stable is abutment surface tension force and gravity keeps, and therefore, the material grown to be had bigger surface tension and less molten density of states(DOS) near fusing point. The major advantage of float-zone method does not need crucible, namely can not introduce impurity by crucible, also namely heats and does not limit by crucible fusing point, it is possible to the material that growth fusing point is extremely high; The crystal grown quality except having less component ununiformity vertically is good, and easily observes in process of growth and adjust growth conditions in real time. Can also be realized movement and the purification impurities removal of flux by control condition, this is the off-eutectic material of growth or the prerequisite with uneven component Solid solution material. The single crystal performance of continuous component prepared by existing floating zone method is desirable not enough, and the regulation and control of its composition are still technical barriers, limit high-throughout material characterization analysis and choose.
Summary of the invention
In order to solve prior art problem, it is an object of the invention to overcome the deficiency of prior art existence, a kind of inorganic materials method for monocrystal growth based on the quasi-continuous composition of floating zone method is provided, floating zone method is adopted to carry out the inorganic materials single crystal growth of continuous component, introducing brand-new fuel rod preparation means makes follow-up continuous component growth be easy to operation, the inventive method has fast, efficiently, pollution-free, low cost, the advantage that crystal mass is high, crystal prepared by the inventive method is functional through checking, composition is easy to regulation and control, obtained continuous component monocrystalline for high-throughout material characterization analysis and will preferentially choose a kind of possibility of offer.
Create object for reaching foregoing invention, adopt following technical proposals:
Based on an inorganic materials method for monocrystal growth for the quasi-continuous composition of floating zone method, comprise the steps:
1) preparation of quasi-continuous composition polycrystalline rod:
A. initial feed adopts the high-purity raw material of a series of more than 3N, the raw-material component of series, with corresponding element mass content difference in the starting material of 0.1 ~ 10wt%, form serial raw-material combination, the element chemistry metering ratio of required raw material is calculated according to the element series proportioning of target polycrystalline material system, again according to the element chemistry metering of required raw material than calculating the raw-material constituent mass proportioning of required whole series, according to the raw-material constituent mass proportioning of required whole series, accurate weighing respectively, grinding, fully it is mixed to get raw mixture series, phase condition is become again according to target polycrystalline crystal, series raw material mixture is complied with in High Temperature Furnaces Heating Apparatus at 400��1500 DEG C of temperature the presintering that phase condition carries out setting-up time, then room temperature naturally it is down to stove, complete the pre-sintering process of the polycrystal raw material to series,
B. the serial polycrystal raw material agate mortar of presintering in described step a is ground, increase or reduce the stoichiometric ratio order as series polycrystal raw material using corresponding element mass content in series polycrystal raw material again, series polycrystal raw material is put into mould according to stoichiometric ratio order, isostatic pressing under 50-200MPa pressure, prepare diameter 3 ~ 15mm respectively, the fuel rod biscuit of the discontinuous limited variable composition of length 50 ~ 150mm and diameter 3 ~ 15mm, the seed crystal rod biscuit that the component of length 30mm is consistent with fuel rod polycrystalline composition bottom, described fuel rod biscuit forms the integrated precast body with series components section of connection segment, by series polycrystal raw material according to stoichiometric ratio order put into mould make fuel rod biscuit time, according to expect variable constituents scope, it is preferable that least significant end becomes segmentation to account for 30mm, it is preferable that the polycrystal raw material of other every segment components accounts for die length 10mm,
C. the high temperature sintering 12h under setting furnace temperature by the fuel rod biscuit of preparation in described step b and seed crystal rod biscuit, leads to into protectiveness gas during sintering, with stove Temperature fall after having sintered, obtains fuel rod and seed crystal rod; When fuel rod and seed crystal rod are sintered, it is preferred to use protectiveness gas be the mixed gas of any one gas or any several gas in rare gas element, oxygen and air, it is preferable that Control protection air flow rate is between 2-6L/min; Fuel rod biscuit and seed crystal rod biscuit preferably carry out high temperature sintering at 500��1500 DEG C of temperature;
D. the lower end of fuel rod of preparation in described step c and the upper end of seed crystal rod being thrown respectively and wear into circular cone shape, cone angle controls within the scope of 45-60 ��, respectively as upper and lower rod, completes the preparation of quasi-continuous composition polycrystalline rod;
2) growth of quasi-continuous composition monocrystalline:
1. adopting optics floating region stove, optics floating region stove mainly contains three parts and forms: heating system, Machinery Control System, atmosphere control system, and the Heating temperature of control heating system is 2000��3000 DEG C; Heating system preferably adopts halogen iodine tungsten lamp or xenon lamp, and corresponding Heating temperature is preferably 2000-2200 DEG C or 2800-3000 DEG C respectively;
2. below the seed crystal rod of preparation in the steps d in described step 1) being fixed on the seat platform of seed rod as under excellent, the fuel rod of preparation in the steps d in described step 1) is suspended on the hook of upper fabric bar as on excellent, adjust the position relation of rod up and down again, maintain upper and lower rod and coaxially and vertically arrange;
3. start described step 1. in the rotational system of optics floating region stove that adopts, control rotating speed 10 ~ 30rpm, make described step 2. in set up and down rod reverse rotation, according to monocrystalline crystal growth condition controlled atmosphere and air flow rate, automatic volume power to close to but do not reach the melting temperature of target material, prepare to carry out the docking of rod up and down;
4. volume power is controlled just molten to rod up and down, start rod docking up and down, and observe melting zone situation, dock after successfully at rod up and down, control is applicable to the growth velocity of aimed single crystal crystalline material system, single crystal is upwards grown, in single crystal growth process, along with the change of the material component of rod on quasi-continuous composition, corresponding fine setting heating power makes melting zone keep stable, finally grow with the velocity-stabilization set, growth is slowly down to room temperature after terminating again, the inorganic materials monocrystalline series of the crystal that growth obtains and quasi-continuous composition, finally obtain quasi-continuous composition monocrystalline bar. in single crystal growth process, it is preferable that upwards grow with the velocity-stabilization of 0.05��10.00mm/h.
As the preferred technical scheme of the present invention, based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method, it is preferable that for the preparation of SmxDy1-xFeO3The quasi-continuous change monocrystalline of composition, wherein x=0.4 ~ 0.6.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. the raw material that the present invention obtains according to desired change of component scope arranges compacting material rod in turn according to limited discontinuous change of component and sinters, it is placed in floating region stove growth again, when the feature of the inventive method is rod docking up and down, component is identical, gradual change in turn in process of growth, crystal is conducive to grow successively along the direction that mismatch is minimum, the adjustment of attention parameters in process of growth, at composition transfer place, gradual change based on up and down rod component mixes and stirring action owing to relatively rotating makes melting zone composition consecutive variations continuously;
2. the crystal that prepared by the inventive method is functional through checking, and composition is easy to regulation and control, and obtained continuous component monocrystalline for high-throughout material characterization analysis and will preferentially choose a kind of possibility of offer.
Accompanying drawing explanation
Fig. 1 is the floating zone method growing principle figure of preferred embodiment of the present invention continuous component inorganic materials single crystal.
Fig. 2 is that the preferred embodiment of the present invention prepares SmxDy1-xFeO3The schematic diagram of the material rod of the dispersion composition of the quasi-continuous change monocrystalline of composition.
Embodiment
The preferred embodiments of the present invention describe in detail as follows:
In the present embodiment, see Fig. 1 and Fig. 2, a kind of inorganic materials method for monocrystal growth based on the quasi-continuous composition of floating zone method, preparation SmxDy1-xFeO3The quasi-continuous change monocrystalline of (x=0.4 ~ 0.6) composition, comprises the steps:
1) preparation of quasi-continuous composition polycrystalline rod:
A. initial feed adopts the high-purity raw material R of a series of more than 3N2O3(R=Sm, Dy) and Fe2O3, by Sm2O3��Dy2O3With Fe2O36:4:10,5:5:10,4:6:10 accurate weighing, grinding in molar ratio respectively, fully mix, then it is placed in High Temperature Furnaces Heating Apparatus at 1300 DEG C of temperature air presintering 12h, be then naturally down to room temperature with stove, preparation Sm0.6Dy0.4FeO3��Sm0.5Dy0.5FeO3��Sm0.4Dy0.6FeO3As starting material;
B. the serial polycrystal raw material agate mortar of presintering in described step a is ground, then by grinding raw material and load 35mmSm from top to bottom respectively0.4Dy0.6FeO3��25mmSm0.5Dy0.5FeO3And 40mmSm0.6Dy0.4FeO3To in mould, under 100MPa pressure, the fuel rod biscuit of the long discontinuous limited variable composition for 100mm and diameter being 5mm made by isostatic pressing, and according to the composition of the lower end of fuel rod and Sm0.6Dy0.4FeO3Compacting long for 30mm's and diameter be the seed crystal rod biscuit of 5mm; Described fuel rod biscuit forms the integrated precast body with series components section of connection segment;
C. by the fuel rod biscuit of preparation in described step b and seed crystal rod biscuit high temperature sintering 12h under 1300 DEG C of furnace temperature, lead to into protectiveness gas during sintering, with stove Temperature fall after having sintered, obtain fuel rod and seed crystal rod;
D. the lower end of fuel rod of preparation in described step c and the upper end of seed crystal rod being thrown respectively and wear into circular cone shape, cone angle controls within the scope of 45-60 ��, respectively as upper and lower rod, completes the preparation of quasi-continuous composition polycrystalline rod;
2) growth of quasi-continuous composition monocrystalline:
1. optics floating region stove is adopted, the Heating temperature of control heating system is 2000��3000 DEG C, optics floating region stove mainly contains three parts and forms: heating system, Machinery Control System, atmosphere control system, heating system selects halogen iodine tungsten lamp or xenon lamp according to differing materials fusing point, and its limit Heating temperature reaches 2200 DEG C and 2800 DEG C respectively; Fig. 1 is SmxDy1-xFeO3(x=0.4 ~ 0.6) monocrystalline optics float zone growth schematic diagram;
2. by the Sm of the 30mm of preparation in the steps d in described step 1)0.4Dy0.6FeO3Seed crystal rod is fixed on as lower rod on the seat platform of seed rod below, by the steps d in described step 1) preparation by 35mmSm0.4Dy0.6FeO3��25mmSm0.5Dy0.5FeO3And 40mmSm0.6Dy0.4FeO3The material rod fuel rod loaded and sinter is suspended on as upper rod on the hook of upper fabric bar, then adjusts the position relation of rod up and down, maintains upper and lower rod and coaxially and vertically arranges;
3. start described step 1. in the rotational system of optics floating region stove that adopts, control rotating speed 10 ~ 30rpm, make described step 2. in set up and down rod reverse rotation, air atmosphere is controlled according to monocrystalline crystal growth condition, control air draught flow is between 2-6L/min, and automatic volume power to 60%, continues manual regulation power to 66%, to close to but do not reach the melting temperature of target material, prepare to carry out the docking of rod up and down;
4. volume power is controlled just molten to rod up and down, start rod docking up and down, and observe melting zone situation, dock after successfully at rod up and down, control is applicable to the growth velocity of aimed single crystal crystalline material system, single crystal is upwards grown, in single crystal growth process, along with the change of the material component of rod on quasi-continuous composition, corresponding fine setting heating power makes melting zone keep stable, finally grows with the velocity-stabilization of 2mm/h, notes the change of growth conditions at composition transfer point, growth is slowly down to room temperature after terminating again, the Sm of the crystal that growth obtains and quasi-continuous compositionxDy1-xFeO3The inorganic materials monocrystalline series of the quasi-continuous change of (x=0.4 ~ 0.6) component, finally obtains SmxDy1-xFeO3The quasi-continuous change monocrystalline bar of (x=0.4 ~ 0.6) composition.
The present embodiment has successfully prepared the not congruent discontinuous material rod coexisted, and in order to successfully grown the monocrystalline of the quasi-continuous change of composition; The present embodiment has prepared rare earth orthoferrites SmxDy1-xFeO3(the quasi-continuous change of x=0.4 ~ 0.6 component) single crystal, no matter the single-crystal surface smooth finish of gained, density, homogeneity are all very desirable; The present embodiment is for SmxDy1-xFeO3The feature of the quasi-continuous change monocrystal material of (x=0.4 ~ 0.6) component itself, orthoferrites lattice mismatch like phase-splitting be less than 2%, control the processing parameter such as rational melting zone, the relative flow rotating (namely stirring) speed and atmosphere and obtain stable growing across component, thus realize growth SmxDy1-xFeO3The novel method of (the quasi-continuous change of x=0.4 ~ 0.6 component) monocrystalline. The Sm that the present embodiment is grown by the methodxDy1-xFeO3(the quasi-continuous change of x=0.4 ~ 0.6 component) monocrystalline has and is separated into subregion and consecutive variations Composition Region, can obtain the single crystal samples of the component of any one between x=0.4 ~ 0.6 by becoming component selections thus realize the growth of high-throughout floating zone method inorganic materials crystal.
The inorganic materials method for monocrystal growth of the quasi-continuous composition of the present embodiment: with high-purity raw material in molar ratio processing reaction prepare polycrystalline discontinuous component raw material series. The raw material obtained according to desired change of component scope arranges compacting material rod in turn according to limited discontinuous change of component and sinters, then is placed in floating region stove growth. When the feature of the present embodiment method is rod docking up and down, component is identical, gradual change in turn in process of growth, crystal is conducive to grow successively along the direction that mismatch is minimum, the adjustment of attention parameters in process of growth, at composition transfer place, gradual change based on up and down rod component mixes and stirring action owing to relatively rotating makes melting zone composition consecutive variations continuously. Crystal prepared by the present embodiment method is functional through checking, and composition is easy to regulation and control. Obtained continuous component monocrystalline for high-throughout material characterization analysis and will preferentially choose a kind of possibility of offer.
Above in conjunction with accompanying drawing, the embodiment of the present invention is illustrated; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of the innovation and creation of the present invention; change, modification, replacement, combination or the simplification made under all spirit according to technical solution of the present invention and principle; all should be the substitute mode of equivalence; if goal of the invention according to the invention; as long as not deviating from the present invention based on the know-why of the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method and invention design, all belong to protection scope of the present invention.
Claims (7)
1. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method, it is characterised in that, comprise the steps:
1) preparation of quasi-continuous composition polycrystalline rod:
A. initial feed adopts the high-purity raw material of a series of more than 3N, the raw-material component of series, with corresponding element mass content difference in the starting material of 0.1 ~ 10wt%, form serial raw-material combination, the element chemistry metering ratio of required raw material is calculated according to the element series proportioning of target polycrystalline material system, again according to the element chemistry metering of required raw material than calculating the raw-material constituent mass proportioning of required whole series, according to the raw-material constituent mass proportioning of required whole series, accurate weighing respectively, grinding, fully it is mixed to get raw mixture series, phase condition is become again according to target polycrystalline crystal, series raw material mixture is complied with in High Temperature Furnaces Heating Apparatus at 400��1500 DEG C of temperature the presintering that phase condition carries out setting-up time, then room temperature naturally it is down to stove, complete the pre-sintering process of the polycrystal raw material to series,
B. the serial polycrystal raw material agate mortar of presintering in described step a is ground, increase or reduce the stoichiometric ratio order as series polycrystal raw material using corresponding element mass content in series polycrystal raw material again, series polycrystal raw material is put into mould according to stoichiometric ratio order, isostatic pressing under 50-200MPa pressure, prepare diameter 3 ~ 15mm respectively, the fuel rod biscuit of the discontinuous limited variable composition of length 50 ~ 150mm and diameter 3 ~ 15mm, the seed crystal rod biscuit that the component of length 30mm is consistent with fuel rod polycrystalline composition bottom, described fuel rod biscuit forms the integrated precast body with series components section of connection segment,
C. the high temperature sintering 12h under setting furnace temperature by the fuel rod biscuit of preparation in described step b and seed crystal rod biscuit, leads to into protectiveness gas during sintering, with stove Temperature fall after having sintered, obtains fuel rod and seed crystal rod;
D. the lower end of fuel rod of preparation in described step c and the upper end of seed crystal rod being thrown respectively and wear into circular cone shape, cone angle controls within the scope of 45-60 ��, respectively as upper and lower rod, completes the preparation of quasi-continuous composition polycrystalline rod;
2) growth of quasi-continuous composition monocrystalline:
1. adopting optics floating region stove, the Heating temperature of control heating system is 2000��3000 DEG C;
2. below the seed crystal rod of preparation in the steps d in described step 1) being fixed on the seat platform of seed rod as under excellent, the fuel rod of preparation in the steps d in described step 1) is suspended on the hook of upper fabric bar as on excellent, adjust the position relation of rod up and down again, maintain upper and lower rod and coaxially and vertically arrange;
3. start described step 1. in the rotational system of optics floating region stove that adopts, control rotating speed 10 ~ 30rpm, make described step 2. in set up and down rod reverse rotation, according to monocrystalline crystal growth condition controlled atmosphere and air flow rate, automatic volume power to close to but do not reach the melting temperature of target material, prepare to carry out the docking of rod up and down;
4. volume power is controlled just molten to rod up and down, start rod docking up and down, and observe melting zone situation, dock after successfully at rod up and down, control is applicable to the growth velocity of aimed single crystal crystalline material system, single crystal is upwards grown, in single crystal growth process, along with the change of the material component of rod on quasi-continuous composition, corresponding fine setting heating power makes melting zone keep stable, finally grow with the velocity-stabilization set, growth is slowly down to room temperature after terminating again, the inorganic materials monocrystalline series of the crystal that growth obtains and quasi-continuous composition, finally obtain quasi-continuous composition monocrystalline bar.
2. according to claim 1 based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method; it is characterized in that: in the step c in described step 1); when fuel rod and seed crystal rod are sintered; the protectiveness gas adopted is the mixed gas of any one gas or any several gas in rare gas element, oxygen and air, and Control protection air flow rate is between 2-6L/min.
3. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method according to claim 1 or 2, it is characterized in that: in the step c in described step 1), fuel rod biscuit and seed crystal rod biscuit carry out high temperature sintering at 500��1500 DEG C of temperature.
4. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method according to claim 1 or 2, it is characterized in that: in the step b in described step 1), by series polycrystal raw material according to stoichiometric ratio order put into mould make fuel rod biscuit time, least significant end becomes segmentation to account for 30mm, and the polycrystal raw material of other every segment components accounts for die length 10mm.
5. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method according to claim 1 or 2, it is characterized in that: in described step 2) in step 1. in, heating system adopts halogen iodine tungsten lamp or xenon lamp, and corresponding Heating temperature is respectively 2000-2200 DEG C or 2800-3000 DEG C.
6. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method according to claim 1 or 2, it is characterized in that: in described step 2) in step 4. in, in single crystal growth process, upwards grow with the velocity-stabilization of 0.05��10.00mm/h.
7. based on the inorganic materials method for monocrystal growth of the quasi-continuous composition of floating zone method according to claim 1 or 2, it is characterised in that: for the preparation of SmxDy1-xFeO3The quasi-continuous change monocrystalline of composition, wherein x=0.4 ~ 0.6.
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| CN105332057A (en) * | 2015-10-14 | 2016-02-17 | 上海大学 | Method for directly growing magnetoelectric material Mn4Nb2O9 single crystal by using one-step method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108707964A (en) * | 2018-04-13 | 2018-10-26 | 中国电子科技集团公司第十研究所 | Melt crucible and material ingot in the area for being used to prepare molecular beam epitaxy beam source material ingot |
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