CN102912438B - Method for crucible-free rapid growth of centimeter magnitude Ti:Ta2O5 crystals - Google Patents

Method for crucible-free rapid growth of centimeter magnitude Ti:Ta2O5 crystals Download PDF

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CN102912438B
CN102912438B CN201210353144.6A CN201210353144A CN102912438B CN 102912438 B CN102912438 B CN 102912438B CN 201210353144 A CN201210353144 A CN 201210353144A CN 102912438 B CN102912438 B CN 102912438B
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CN102912438A (en
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蒋毅坚
徐宏
马云峰
王越
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Beijing University of Technology
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Abstract

A method for crucible-free rapid growth of centimeter magnitude Ti:Ta2O5 crystals belongs to the field of Ti:Ta2O5 crystal growth. Mixing, ball-milling and burning are carried out on TiO2 and Ta2O5 powder to press rob-shaped polycrystalline rods; the polycrystalline rods respectively serve as charge rods and seed crystals to be installed in a single crystal furnace, a heating rate is set, crystal growth is carried out, cooling time is set, the crystals after growing are cooled to a room temperature. The method is a crucible-free growth technique which can rapidly grow centimeter magnitudes, is free of macroscopic defect and has high-quality Ti:Ta2O5 crystals.

Description

One grows centimetres Ti:Ta fast without crucible 2o 5the method of crystal
Technical field
The invention belongs to Ti:Ta 2o 5field of crystal growth, relates to one and grows centimetres Ti:Ta fast without crucible 2o 5the method of crystal.
Technical background
Crystalline material plays a very important role in scientific technological advance, is the important foundation stone of information age, is also the basic substance of Development of Hi-Tech.Main crystal preparing technology mainly contains: melt growth, solution growth, vapor phase growth, solid state growth.Non-crucible growing method is novel without crucible crystal growth method as one, have without the need to crucible, pollute few, the advantages such as fast growth, the crystal growing (comprising the crystal that crystal pulling method can not grow), easily pollution is difficult to for some, demonstrates very large superiority.Float-zone method has one section of melting zone between the crystal and polycrystalline rod of growth, and this melting zone supported by surface tension.Melting zone from top to bottom, or is moved from bottom to top, to complete crystallisation process.Float-zone method, without the need to crucible, pollution-free, fast growth, is applicable to the dystectic crystal of growth.High quality, undersized crystal can be provided, be convenient to control component.Wide application, can be used for the multiclass materials such as oxide compound, semi-conductor, intermetallic compound, the crystal that especially fusant reaction is strong.The major advantage of the method does not need crucible, and the crystal purity of growth is very high, and uniform doping.Also because heating is not by the restriction of crucible fusing point, in growth materials with high melting point, unique advantage is had.Compared with crystal pulling method, the field of research material is just broad many.Float-zone method is research many body system, the Crystal study of high-melting-point, synthesis difficulty provides a kind of new research method and approach.Due to the miniaturization, integrated of device, require more and more less to crystalline size.Float-zone method obtains a lot of application in crystal growth.
Ta 2o 5(Tantalum Pent-oxide) is important dielectric materials and optical waveguide material, simultaneously because it is easily mutually compatible with semiconductor integrated circuit technique, has become the hot-candidate material of dynamic RAM of new generation (DRAM).Grow Ta after the doping of high-k 2o 5base crystal also studies the relation of its physical properties with crystal orientation, for exploitation high-performance Ta 2o 5base device and high κ material will provide the technical foundation having independent intellectual property right significant.But, Ta 2o 5fusing point close to 1900 DEG C, adopt traditional growing technology to be difficult to obtain Ti:Ta 2o 5crystal, makes Ti:Ta 2o 5physical property Quality Research encounters difficulty.At present, to Ti:Ta 2o 5research mainly concentrate on preparation Ti:Ta 2o 5on film, about Ti:Ta 2o 5the document of crystal growth is little.Up to now, employing float-zone method growing large-size Ti:Ta is not also seen 2o 5the report of crystal.
Use crucible method growing crystal, because its condition is limited to, growth cycle is long, and cost is high, and requirement for experiment condition is harsh, and plant and instrument is complicated, complicated operation, is subject to certain restrictions in growth high-melting-point crystal.Without crucible method growing crystal without the need to crucible, pollution-free, fast growth, high quality, undersized crystal can be provided, be convenient to control component.Compared with crystal pulling method, the field of research material is just broad many.Non-crucible growing method has not only enriched the means of crystal growth, has shortened the cycle of crystal growth, also for the Crystal study of research many body system, high-melting-point, synthesis difficulty provides a kind of new research method and approach.
Artificial without the quick growing large-size Ti:Ta of crucible 2o 5crystal and the technology improving its specific inductivity is still a challenge is also a study hotspot.As for this, the present invention has attempted use floating zone method and has grown centimetres, non-nuclear density gauge, high quality Ti:Ta fast 2o 5crystal without crucible growing technology.
Summary of the invention
The object of the invention is to overcome existing large size centimetres Ti:Ta 2o 5the blank existed in crystal technique, grows the Ti:Ta of large size (diameter is centimetre-sized), non-nuclear density gauge with floating zone method 2o 5crystal is not only important problem in science, for exploitation high-performance Ta 2o 5base device and high dielectric material (also known as high κ material) aspect will provide the technical foundation having independent intellectual property right.The invention provides the quick growing large-size of a kind of float-zone method (centimetre-sized) Ti:Ta 2o 5the method of crystal.
One grows centimetres Ti:Ta fast without crucible 2o 5the method of crystal, comprises the following steps:
(1) batching and charge bar preparation: the TiO high-purity (being not less than 99.99%) being met stoichiometric ratio 2and Ta 2o 5powder is through mixing and ball milling, pre-burning; Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar that polycrystalline rod step (1) suppressed is fixed on single crystal growing furnace, another root polycrystalline rod is put into the bottom of axis as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, and the rotating speed of adjustment charge bar and seed crystal and sense of rotation, inoculate behind solubilized stable district to be formed; By the movement of condensing lens, form constitutional supercooling, realize crystallization;
(4) cooling down: arrange temperature fall time, is cooled to room temperature by the crystal grown.
Preferably TiO in described step (1) in the technology of the present invention 2doping Ta 2o 5stoichiometric ratio scope is: TiO 2account for the Ta of doping 2o 5molar percentage not higher than 10at%, the calcined temperature of powder is 1350 DEG C, and burn-in time is 12 ~ 24 hours.
In the technology of the present invention preferably described step (3) crystal growing process in, the sense of rotation of charge bar and seed crystal is that oppositely speed of rotation is 10 ~ 30rpm, arranges crystalline growth velocity and carries out crystal growth, and crystalline growth velocity is 3-8mm/h.
In the technology of the present invention, preferably the middle temperature fall time of described step (4) is 0.5 ~ 1.5h.
The present invention is without the quick growing large-size Ti:Ta of crucible 2o 5the key problem in technology of (centimetre-sized) crystal is: due to Ti:Ta 2o 5the fusing point that crystal is higher, and high temperature will experience different phase transformations to low temperature, makes the Ti:Ta of growing high-quality 2o 5there is a lot of difficulty in crystal.Theoretical according to Foundation of Crystal Growth, condensate depression is the motivating force of crystallization.When only having the condensate depression Δ T>0 when solid-liquid interface place, could crystallization be realized, thus realize crystal growth.The temperature-fall period of float-zone method in the process of crystal growth is the movement by condensing lens, or movement excellent up and down, makes melting zone away from focus point, melting zone temperature is declined, thus realizes crystallization.Namely growth velocity is the main regulate factors of crystal structure.Float-zone method growing large-size Ti:Ta 2o 5crystal growth technique condition is groped: the determination comprising polycrystalline charge bar sintering temperature, and growth regulation speed, speed of rotation, crystal growth power demand export.Only have suitable crystal growth technique, float-zone method could be utilized to grow the Ti:Ta of large size, high quality, non-nuclear density gauge 2o 5crystal.
Without crucible quick growing large-size high-k Ti:Ta 2o 5groping of crystal processing condition is emphasis of the present invention, and studies the relation of its physical properties with crystal orientation with this.Therefore, Ti:Ta is grown by float-zone method 2o 5crystal
Be not only important problem in science, for exploitation high-performance Ta 2o 5base device and high dielectric material (also known as high κ material) aspect will provide the technical foundation having independent intellectual property right.Float-zone method growth Ti:Ta 2o 5the crystal cycle is short, consumes energy low, and requirement for experiment condition is loose, and plant and instrument is simple, processing ease.
Compared with the prior art, the obvious advantage of present invention process:
1, existing Ti:Ta is overcome 2o 5the blank existed in crystal technique, grows the Ti:Ta of large size (centimetre-sized), non-nuclear density gauge by float-zone method 2o 5crystal.
2, the charge bar that this technology uses does not need to be prepared into pottery, as long as make charge bar after pre-burning; And seed crystal charge bar and crystal all can, greatly reduce energy consumption.
3, this technology does not need crucible, and can grow under air ambient, growing method is simple to operate, repeatable strong, advantage of lower cost.
4, the speed of growth, be that other growing methods are beyond one's reach, growth cycle is short, and preparation efficiency is high, can grow centimetres, non-nuclear density gauge, high quality Ti:Ta fast 2o 5crystal.
5, the Ti:Ta for preparing of this technique 2o 5crystal does not have the macroscopic defectss such as bubble, cloud layer, inclusion.X-ray diffractogram of powder diffraction peak is very sharp-pointed, shows that crystal growth quality is fine.
6, adopt without crucible crystal growth technology, avoid the etching problem of high-temperature fusant to crucible, eliminate the potentially contaminated that crucible brings.
Accompanying drawing explanation
Fig. 1 is comparative example 1 and embodiment of the present invention 1-4 gained Ti:Ta 2o 5the crystal morphology figure of crystal;
Fig. 2 is comparative example 1 and embodiment of the present invention 1-4 gained Ti:Ta 2o 5the XRD powdery diffractometry image of crystal;
Fig. 3 is comparative example 1 and embodiment of the present invention 1-4 gained Ti:Ta 2o 5the Raman micro-image of plane of crystal.
Embodiment
The present invention's one grows centimetres Ti:Ta fast without crucible 2o 5the growing apparatus of the method for crystal---four ellipsoid optics floating region stoves (Crystal Systems Co., 10000H-HR-I-VPO-PC).From the shape appearance figure 1 of crystal, we find out that crystal is transparent, and crystal mass is higher, and diameter is 5-10mm, and length is 60-100mm.The XRD powdery diffractometry image of crystal is shown in Fig. 2, can find out, diffraction peak is very sharp-pointed, and crystal growth quality is fine.As can be seen from the Raman micro-image 3 of crystal, the crystal peak position after doping has considerable change, and after doping is described, crystalline structure changes, and this is also one of microscopic sdIBM-2+2q.p.approach of being improved of specific inductivity.The raw materials used TiO of following examples 2and Ta 2o 5purity be not less than 99.99%.
Comparative example 1
(1) batching and charge bar preparation: by high pure raw material TiO 2and Ta 2o 5powder mixes according to stoichiometric ratio 0at%, then carries out mechanically mixing; Put into high temperature pre-burning stove, calcined temperature is 1350 DEG C, and burn-in time is 12 hours, obtains polycrystalline powder.Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar polycrystalline rod suppressed being fixed on single crystal growing furnace, and bottom polycrystalline rod being put into axis is as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, and the sense of rotation of adjustment charge bar and seed crystal is that oppositely speed of rotation is respectively 15rpm, inoculates behind solubilized stable district to be formed; Then arranging crystalline growth velocity is that 8mm/h carries out crystal growth;
(4) cooling down: arrange temperature fall time, is 0.5h by the crystal that grown through temperature fall time, is cooled to room temperature;
Under room temperature, 1MHz condition, the Ti:Ta grown 2o 5the specific inductivity of crystal is respectively 81.17 and 25.04 along the direction of growth and (001) direction.
Embodiment 1
(1) batching and charge bar preparation: by high pure raw material TiO 2and Ta 2o 5powder mixes according to stoichiometric ratio 3at%, then carries out mechanically mixing; Put into high temperature pre-burning stove, calcined temperature is 1350 DEG C, and burn-in time is 14 hours, obtains polycrystalline powder.Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar polycrystalline rod suppressed being fixed on single crystal growing furnace, and bottom polycrystalline rod being put into axis is as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, the sense of rotation of adjustment charge bar and seed crystal is that oppositely speed of rotation is respectively 20rpm, inoculates behind solubilized stable district to be formed; Then arranging crystalline growth velocity is that 5mm/h carries out crystal growth;
(4) cooling down: arrange temperature fall time, is 1h by the crystal that grown through temperature fall time, is cooled to room temperature; Under room temperature, 1MHz condition, the Ti:Ta grown 2o 5the specific inductivity of crystal is respectively 296.72 and 36.73 along the direction of growth and (001) direction.
Embodiment 2
(1) batching and charge bar preparation: by high pure raw material TiO 2and Ta 2o 5powder mixes according to stoichiometric ratio 5at%, then carries out mechanically mixing; Put into high temperature pre-burning stove, calcined temperature is 1350 DEG C, and burn-in time is 16 hours, obtains polycrystalline powder.Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar polycrystalline rod suppressed being fixed on single crystal growing furnace, and bottom polycrystalline rod being put into axis is as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, the sense of rotation of adjustment charge bar and seed crystal is that oppositely speed of rotation is respectively 25rpm, inoculates behind solubilized stable district to be formed; Then arranging crystalline growth velocity is that 3mm/h carries out crystal growth;
(4) cooling down: arrange temperature fall time, is 1.5h by the crystal that grown through temperature fall time, is cooled to room temperature;
Under room temperature, 1MHz condition, the Ti:Ta grown 2o 5the specific inductivity of crystal is respectively 711.34 and 35.58 along the direction of growth and (001) direction.
Embodiment 3
(1) batching and charge bar preparation: by high pure raw material TiO 2and Ta 2o 5powder mixes according to stoichiometric ratio 8at%, then carries out mechanically mixing; Put into high temperature pre-burning stove, calcined temperature is 1350 DEG C, and burn-in time is 18 hours, obtains polycrystalline powder.Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar polycrystalline rod suppressed being fixed on single crystal growing furnace, and bottom polycrystalline rod being put into axis is as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, the sense of rotation of adjustment charge bar and seed crystal is that oppositely speed of rotation is respectively 20rpm, inoculates behind solubilized stable district to be formed; Then arranging crystalline growth velocity is that 3mm/h carries out crystal growth;
(4) cooling down: arrange temperature fall time, is 1h by the crystal that grown through temperature fall time, is cooled to room temperature; Under room temperature, 1MHz condition, the Ti:Ta grown 2o 5the specific inductivity of crystal is respectively 576.96 and 38.21 along the direction of growth and (001) direction.
Embodiment 4
(1) batching and charge bar preparation: by high pure raw material TiO 2and Ta 2o 5powder mixes according to stoichiometric ratio 10at%, then carries out mechanically mixing; Put into high temperature pre-burning stove, calcined temperature is 1350 DEG C, and burn-in time is 24 hours, obtains polycrystalline powder.Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar polycrystalline rod suppressed being fixed on single crystal growing furnace, and bottom polycrystalline rod being put into axis is as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, the sense of rotation of adjustment charge bar and seed crystal is that oppositely speed of rotation is respectively 30rpm, inoculates behind solubilized stable district to be formed; Then arranging crystalline growth velocity is that 3mm/h carries out crystal growth;
(4) cooling down: arrange temperature fall time, is 1.5h by the crystal that grown through temperature fall time, is cooled to room temperature;
Under room temperature, 1MHz condition, the Ti:Ta grown 2o 5the specific inductivity of crystal is respectively 417.04 and 40.96 along the direction of growth and (001) direction.

Claims (4)

1. one kind grows centimetres Ti:Ta fast without crucible 2o 5the method of crystal, comprises the following steps:
(1) batching and charge bar preparation: purity is not less than 99.99%TiO 2and Ta 2o 5powder according to stoichiometric ratio through mixing and ball milling, pre-burning; Polycrystalline powder after pre-burning is loaded in rubber hose, under then putting into isostatic pressed, is pressed into bar-shaped polycrystalline rod;
(2) charge bar and seed crystal are installed: as charge bar on top, the axis charge bar bar that polycrystalline rod step (1) suppressed is fixed on single crystal growing furnace, another root polycrystalline rod is put into the bottom of axis as seed crystal, seed crystal and charge bar in alignment at vertical direction, regulate the position of charge bar and seed crystal, make it contact, point of contact and halogen lamp are on same level line;
(3) crystal growth: arrange temperature rise rate, is warming up to charge bar with 0.5-1h and seed crystal melts, and the rotating speed of adjustment charge bar and seed crystal and sense of rotation, inoculate behind stable melting zone to be formed; By the movement of condensing lens, form constitutional supercooling, realize crystallization;
(4) cooling down: arrange temperature fall time, is cooled to room temperature by the crystal grown.
2. according to the method for claim 1, it is characterized in that, TiO in step (1) 2doping Ta 2o 5stoichiometric ratio scope is: TiO 2account for the Ta of doping 2o 5molar percentage not higher than 10at%, the calcined temperature of powder is 1350 DEG C, and burn-in time is 12 ~ 24 hours.
3. according to the method for claim 1, it is characterized in that, in the crystal growing process of (3), the sense of rotation of charge bar and seed crystal is that oppositely speed of rotation is 10 ~ 30rpm, arranges crystalline growth velocity and carries out crystal growth, and crystalline growth velocity is 3-8mm/h.
4. according to the method for claim 1, it is characterized in that, in step (4), temperature fall time is 0.5 ~ 1.5h.
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CN103436960A (en) * 2013-07-20 2013-12-11 北京工业大学 Technology for growth of rare earth element-doped Ta2O5 crystals through optical floating zone method
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CN102312293A (en) * 2011-09-01 2012-01-11 北京工业大学 Method for growing large size Ta2O5 single crystal by using floating zone method

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CN102312293A (en) * 2011-09-01 2012-01-11 北京工业大学 Method for growing large size Ta2O5 single crystal by using floating zone method

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