CN104894637B - The grower and growing method of a kind of crystal - Google Patents
The grower and growing method of a kind of crystal Download PDFInfo
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- CN104894637B CN104894637B CN201510383437.2A CN201510383437A CN104894637B CN 104894637 B CN104894637 B CN 104894637B CN 201510383437 A CN201510383437 A CN 201510383437A CN 104894637 B CN104894637 B CN 104894637B
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Abstract
This application provides a kind of grower of crystal, including：Light condensation screen；The infrared light supply and transparent crucible being arranged in light condensation screen, the infrared light supply are arranged on around the crucible；Support bar for supporting the crucible；The support bar is connected with crucible by crucible tray.The grower that the present invention is provided is using place of the transparent crucible as crystal growth, the grower for the crystal that the present invention is provided can be not only grown outside the crystal that normal optical float-zone method can grow, the relatively low crystal of growing surface tension force, the crystal that easily aoxidizes and there can also be the crystal of volatile components, test result indicates that, the crystal structure that the grower that the present invention is provided is obtained is functional, the defects such as bubble-free, monocrystalline repetitive rate is higher, and monocrystalline mass discrepancy is small between different batches.Crystal forming rate is between 90~100%.Present invention also offers a kind of growing method of crystal.
Description
Technical field
The invention belongs to the grower and growing method of technical field of crystal growth, more particularly to a kind of crystal.
Background technology
Traditional crystal growth method by melt technology includes czochralski method, descent method, float-zone method, kyropoulos, temperature gradient method, heat
Exchange process, cold crucible method, EFG technique, flame method etc..
These crystal techniques being developed at present, still with certain limitation.Czochralski method and EFG technique growth
Can be with Real Time Observation during crystal, but it is difficult to growth incongruent melting or the crystal with compared with lower thermal conductivity；Descent method, temperature ladder
Degree method and heat-exchanging method can grow with compared with lower thermal conductivity crystal, but can not Real Time Observation crystal growth condition, can not yet
Grow the crystal of incongruent melting；Kyropoulos and cold crucible method are beneficial to the crystal for preparing large-size, but can not produce inconsistent
The crystal of melting；Flame method can grow the crystal of incongruent melting, the crystal relatively low compared with lower thermal conductivity or surface tension,
Can be with home position observation crystal growth condition, but the crystal stress of flame method growth is larger, and defect is more, still suffers from more limitation
Property.
Float-zone method by Keck et al. nineteen fifty-three invent, after gradually develop floating zone method, this method is in prior art
Middle application is relatively broad.What Science Press published《Crystal growth science and technology》Floating zone method is described in detail in one book
Principle features.Floating zone method can grow the crystal of incongruent melting, can also realize the Real Time Observation of crystal growth, because
This, floating zone method has obtained very big development in recent years.
Floating zone method growth crystal is carried out in the stove of optics floating region, and such as A of Publication No. CN 104389013 China is specially
Profit discloses the device that a kind of floating zone method grows crystal, and the device mainly by seed crystal rod turntable, charge bar turntable and adds
Hot systems are constituted, but this device can not grow the crystal with compared with low surface tension, and are difficult to grow what is easily aoxidized
Crystal.
The content of the invention
It is an object of the invention to provide a kind of grower of crystal and growing method, the crystal provided using the present invention
Grower, can not only grow outside the crystal that normal optical float-zone method can grow, additionally it is possible to which growth has relatively low surface
The crystal of tension force, the crystal easily aoxidized and the crystal for having volatile components.
A kind of grower of crystal, including：Light condensation screen；
The infrared light supply and transparent crucible being arranged in light condensation screen, the infrared light supply are arranged on the week of the crucible
Enclose；
Support bar for supporting the crucible；
The support bar is connected with crucible by crucible tray.
It is preferred that, the crucible is crystalline ceramics crucible, glass pot or transparent crystal crucible.
It is preferred that, the crucible includes sidewall of crucible and crucible bottom, and the sidewall of crucible has inclination angle, and the crucible bottom is provided with
Seed slot.
It is preferred that, infrared band transmitance >=80% of the crucible.
It is preferred that, the fusing point of crystal of the fusing point than being grown of the crucible is high 400~2000 DEG C.
It is preferred that, the infrared light supply is that the number of the infrared light light source is 2~4 without shadow Halogen lamp LED.
It is preferred that, the center plumb line of the infrared light supply using the crucible is distributed in the week of the crucible as axisymmetrical
Enclose.
It is preferred that, the support bar is the support bar of liftable and rotation.
The present invention provides a kind of growing method of crystal, comprises the following steps：
Polycrystalline is melted and solidified successively, the polycrystalline pre-processed；
Using above-mentioned grower, the polycrystalline of pretreatment is heated in crucible, the growth of crystal is carried out, obtains list
It is brilliant.
It is preferred that, the process of the heating is specifically included：
Polycrystalline is heated with the first temperature, second temperature is cooled to first rate after 20~60min of heating, to many
Crystalline substance is heated, and carries out the growth of crystal, and crystal growth is cooled to the 3rd temperature with the second speed after terminating, obtains crystal；
First temperature is is grown more than crystalline melting point 50~100 DEG C；
Second temperature is is grown more than crystalline melting point 0~25 DEG C；
3rd temperature is 20~35 DEG C；
First rate is 1~10 DEG C/h；
Second speed is 20~50 DEG C/h.
Float-zone method growth crystal efficiency is high, and materials are few, have obvious advantage in material science research field.Scientific publication
What society published《Crystal growth science and technology》The principle features of floating zone method are described in detail in one book.Float-zone method melting zone
Maintain, by the effect of smelt surface tension, and have the surface tension γ and melt of height L that melt can maintain and melt
The relational expression of density p is as follows：
Formula 1
Wherein, g is acceleration of gravity.It can be seen that, if the surface tension of melt is too small, and density is excessive, is difficult to shape
Into stable melting zone.Such as Bi4Ge3O12Crystal, the density of crystal is 7.13g/cm3, surface tension is 233mN/m (Journal
of Crystal Growth,1994；137:509-515.), g is 9.8m/s2, according to calculating, L is 5mm, and melting zone is shorter, is used
The stove growth of existing optics floating region is more difficult, and present invention research is found, containing the oxide without surface-active for example
Al2O3, CaO, MgO, SiO2Deng the surface tension increase of, melt, crystal growth is relatively easy；B containing surface-active2O3,
V2O5, P2O5, PbO, K2O, bismuth germanium oxide etc., the surface tension reduction of melt, crystal growth relative difficult.In addition, existing optics
Stove open growth pattern in floating region is extremely not suitable in material and oxidizable material of the growth with volatile components, for example
The crystal such as calcirm-fluoride, cadmium-zinc-teiluride.
The invention provides a kind of grower of crystal, including：Light condensation screen；Be arranged on infrared light supply in light condensation screen and
Transparent crucible, the infrared light supply is arranged on around the crucible；Support bar for supporting the crucible；The support
Bar is connected with crucible by crucible tray.The grower that the present invention is provided is using field of the transparent crucible as crystal growth
Institute, when carrying out crystal growth, the grower for the crystal that the present invention is provided can give birth to except that can grow normal optical float-zone method
Outside long crystal, additionally it is possible to the relatively low crystal of growing surface tension force, the crystal easily aoxidized and the crystal for having volatile components,
Test result indicates that, the crystal structure that the grower that the present invention is provided is obtained is functional, the defect such as bubble-free, and monocrystalline is repeated
Rate is higher, and monocrystalline mass discrepancy is small between different batches.Crystal forming rate is between 90~100%.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
The structural representation for the crystal growing apparatus that Fig. 1 provides for the present invention.
Embodiment
The present invention provides a kind of crystal growing apparatus, including：Light condensation screen；
The infrared light supply and transparent crucible being arranged in light condensation screen, the infrared light supply are arranged on the week of the crucible
Enclose；
Support bar for supporting the crucible；
The support bar is connected with crucible by crucible tray.
The grower that the present invention is provided being capable of the relatively low crystal of growing surface tension force.
Referring to Fig. 1, the structural representation of crystal growing apparatus that Fig. 1 provides for the present invention, in Fig. 1,1 is light condensation screen, and 2 are
Infrared light supply, 3 be crucible, and 4 be crucible tray, and 5 be support bar, and 6 be sidewall of crucible, and 7 be crucible bottom, and 8 be seed slot.
The grower that the present invention is provided includes light condensation screen 1, and the effect of the light condensation screen mainly sends infrared light supply
Infrared light converge to certain, concentration is heated to certain.In the present invention, the light condensation screen is preferably shaped to two
Individual hemispherical Shell shape, the light condensation screen is preferably stainless steel light condensation screen, and the present invention does not have special to the size of the light condensation screen
Limitation, with the space of the crucible and infrared light supply can be accommodated.
The grower that the present invention is provided includes infrared light supply 2, and the infrared light supply is arranged on the inside of the light condensation screen,
The infrared light supply is preferably that the number of the infrared light supply is preferably 2~4, more preferably 3, described without shadow Halogen lamp LED
Infrared light supply is arranged on around the crucible, is preferably distributed in the earthenware using the center plumb line of the crucible as axisymmetrical
Around crucible, the infrared light supply is preferably on same horizontal plane, to strengthen the convergence effect of infrared light.
The grower that the present invention is provided includes crucible 3, and the crucible is the place of crystal growth, is transparent crucible, with
Just infrared light can be passed through, and the polycrystalline and seed crystal in crucible are heated.The infrared band transmitance of the crucible is preferred
>=80%, more preferably >=85%, most preferably >=90%；The crucible requires that heat endurance is good, can be resistant to larger temperature ladder
Degree, is preferably able to be resistant to 20 DEG C/more than mm thermograde；The fusing point of the crucible is preferably above the crystalline substance grown inside crucible
Body, the fusing point of the preferably crystal than being grown is high 400~2000 DEG C, more preferably high 500~1500 DEG C, most preferably high by 600~
1200℃.Also, the crucible in the present invention does not react with any one of the melt of grown crystal composition, also will not
The melt attack of the crystal grown.In the present invention, the crucible is preferably crystalline ceramics crucible, glass pot or transparent
Crystal crucible, specifically, the transparent crystal crucible is preferably alpha-alumina crystals crucible.
In the present invention, the crucible includes sidewall of crucible 6 and crucible bottom 7, the crucible be preferably able to it is closed, can be for
The volatile or oxidizable crystal of growth, the sidewall of crucible 6 has certain inclination angle, so as to the taking-up of crystal, the inclination angle
It it is preferably 0 °~3 °, more preferably 1 °~2 ° for the angle at the inclination angle；The crucible bottom 7 is preferably inverted conical shape, described
Crucible bottom 7 is provided with seed slot 8, for placing seed crystal, for can be with the crystal of spontaneous nucleation, can be without seed crystal.The present invention
There is no special limitation to the size of the crucible.
The grower that the present invention is provided includes crucible tray 4, and the crucible tray is used to connect crucible and support bar, plays support
The effect of crucible.In the present invention, the crucible tray is preferably firmly connected with the crucible, and the crucible tray shown in Fig. 1 is
One example, the present invention has no special limitation to the shape of the crucible tray, can play a part of the support crucible i.e.
Can.
The grower that the present invention is provided includes support bar 5, and the support bar is used to support the crucible, in the present invention
In, the support bar is preferably able to rotate and lifted, and the support bar can ensure that crucible adds with certain rotating speed rotation
Hot uniform, the support bar, which can be lifted, can ensure that infrared light is carried out to the diverse location of the polycrystalline in the crucible and seed crystal
Heating, the present invention does not have special limitation to the material and size of the support bar.
For the ease of observing the growth course of crystal, the grower that the present invention is provided preferably also includes observation device (figure
In be not drawn into), it is described observation device can be infrared camera either optical filter.
Present invention also offers a kind of growing method of crystal, comprise the following steps：
Polycrystalline is melted and solidified successively, the polycrystalline pre-processed；
Using above-mentioned grower, the polycrystalline of pretreatment is heated in crucible, the growth of crystal is carried out, obtains list
It is brilliant.
In order to ensure the continuity of crystal growth, the present invention needs that polycrystalline is first melted and solidified successively, obtains pre-
The polycrystalline of processing, the polycrystalline fusing can be carried out directly in the crucible of crystal growth, then directly in crystal life
Solidified in long crucible；It can also enter in other sizes with the crucible of the crystal growth, shape identical crucible
OK, polycrystalline is taken out after after many crystal solidifications, in the crucible for being further filled with the crystal growth；Or by the polycrystalline in other crucibles
After interior fusing, obtained polycrystalline melt is poured into the crucible of the crystal growth, solidified.In the present invention, regrowth
During the crystal easily aoxidized, the fusing and solidification are carried out preferably under protective gas atmosphere, to avoid polycrystalline from aoxidizing, described to protect
It is preferably inert gas or nitrogen to protect gas；More preferably argon gas, the purity of the inert gas is preferably 4N (99.99%).
The fusing and solidification polycrystalline method in the present invention are the method that those skilled in the art commonly use.
In the present invention, during the polycrystalline is preferably germanium polycrystalline, calcirm-fluoride polycrystalline, cadmium-zinc-teiluride polycrystalline, bismuth germanium oxide polycrystalline
It is one or more of.
After the polycrystalline pre-processed, the present invention uses above-mentioned grower, by the polycrystalline of pretreatment in the crucible
Heated, carry out the growth of crystal, obtain crystal.In the present invention, if polycrystalline can spontaneous nucleation, can not make
With seed crystal, if polycrystalline is unable to spontaneous nucleation, it is necessary to be put into seed crystal to carry out the growth of crystal, i.e. the present invention by seed crystal and
The polycrystalline of pretreatment is heated in crucible, is carried out the growth of crystal, is obtained crystal.
The present invention is preferably heated with the first temperature to polycrystalline or seed crystal, is dropped after 20~60min of heating with first rate
Temperature is heated to second temperature to polycrystalline, carries out the growth of crystal, and crystal growth is cooled to the 3rd after terminating with the second speed
Temperature, obtains crystal.
The present invention is preferably with the first temperature to heating at the 1/3 of seed crystal upper end, and first temperature is preferably to give birth to
More than long crystal fusing point 50~100 DEG C, more preferably 60~90 DEG C are grown more than crystalline melting point；Heated with first temperature
Time be preferably 20~60min, more preferably 30~50min, most preferably 40min；Treat that the melting zone of seed crystal finally keeps steady
After fixed, the present invention is preferably cooled to second temperature with first rate, and polycrystalline is heated, and carries out crystal growth, described first
Speed is preferably 1~10 DEG C/h, more preferably 2~8 DEG C/h, most preferably 3~7 DEG C/h；The second temperature is excellent
Elect more than grown crystalline melting point 0~25 DEG C as, more preferably grow more than crystalline melting point 5~20 DEG C；With the described second temperature
The time of degree heating is preferably 20~60min, more preferably 30~50min, most preferably 40min；In the crystal growth
During, the present invention suitably finely tunes the second temperature so that melt concaves towards growth preferably according to the propulsion situation of solid liquid interface
Germanium crystal；Complete after crystal growing process, the present invention, to the 3rd temperature, obtains crystal preferably with the second speed information.It is described
Second speed is preferably 20~50 DEG C/h, more preferably 25~45 DEG C/h, most preferably 30~40 DEG C/h；It is described
3rd temperature is preferably 20~35 DEG C, more preferably 25~30 DEG C.In the present invention, the growth of the crystal is preferably in vacuum bar
Carried out under part, the vacuum is preferably 10-2Below Pa, more preferably 10-3Below Pa.
Present invention preferably employs the device shown in Fig. 1, the growth of crystal is carried out in the method for above-mentioned crystal growth, in 4N argons
Under gas atmosphere, polycrystal raw material is melted in crucible 3, and the cooled and solidified in argon gas atmosphere, polycrystal raw material is taken out afterwards,
Seed crystal is loaded on seed slot 8, then polycrystal raw material is fitted into crucible 3, inner air and sealed crucible 3 is evacuated, crucible 3 is put
On crucible tray 4；After fixation, lift supporting rod 5 so that the convergence center of light condensation screen 1 is located at seed crystal bottom.Open support
The rotating speed of bar 5, makes rotating speed be maintained between 0~20rpm；Open Halogen lamp LED 2；Power is gradually risen, until seed crystal starts fusing；
20~30min of constant temperature, begins to decline crucible 3, the fall off rate of crucible is 5~15mm/h；According to the propulsion situation of solid liquid interface,
Adjust heating power so that the melt in crucible 3 concaves towards the crystal of growth, and growth interface is stable；Until unfused polycrystalline
It is completely melt, crystal growth is completed.Crystal growth starts cooling after terminating, rate of temperature fall is 30~50 DEG C/h；Treat that crystal is cold
When but arriving room temperature, crucible 3 is taken out, crystal is taken out, obtains crystal.
The invention provides a kind of grower of crystal, including：Light condensation screen；Be arranged on infrared light supply in light condensation screen and
Transparent crucible, the infrared light supply is arranged on around the crucible；Support bar for supporting the crucible；The support
Bar is connected with crucible by crucible tray.The grower that the present invention is provided is using field of the transparent crucible as crystal growth
Institute, the grower for the crystal that the present invention is provided can be not only grown outside the crystal that normal optical float-zone method can grow, also
The relatively low crystal of growing surface tension force, the crystal that easily aoxidizes and there can be the crystal of volatile components, test result indicates that, this
The crystal structure that the grower that invention is provided is obtained is functional, and the defect such as bubble-free, monocrystalline repetitive rate is higher, different batches
Between monocrystalline mass discrepancy it is small.Crystal forming rate is between 90~100%.
In order to further illustrate the present invention, the grower of a kind of crystal that provides with reference to embodiments the present invention and
Growing method is described in detail, but can not be understood as limiting the scope of the present invention.
Embodiment 1
Using grower as shown in Figure 1, no shadow Halogen lamp LED has two, symmetrical, Halogen lamp LED power 500W, voltage
240V；The infrared light sent without shadow Halogen lamp LED is gathered in crystal growth chamber center by the stainless steel light condensation screen of surface gold-plating；Earthenware
Crucible is suprasil crucible, and crucible internal diameter 6mm, length 80mm, wall thickness 2mm, crucible surface is bright and clean；Crucible is placed on positioned at crystal
On the stainless steel crucible tray of growth chamber center plumb line, crucible tray is fixedly secured with crucible；Crucible tray, which is placed on, to be lifted
On the support bar 5 of rotation.There are seed slot, seed slot diameter 4mm, length 10mm in crucible lower end.The inclination angle of crucible internal walls is 1 °.
The seed crystal for cleaning (111) direction is placed in seed slot, seed crystal length is 10mm, diameter 4mm.By 5N 8g germanium
After polycrystal raw material melts in other silica crucibles, pour into silica crucible, and make melt slow solidification, ensure in the process
Seed crystal not exclusively melts；Whole fusing and toppling process are carried out in the glove box full of 4N argon gas atmospheres, it is to avoid germanium high temperature melting
Body is aoxidized.Germanium melt solidifies and after silica crucible cooling, silica crucible taken out, sealed after being vacuumized silica crucible.Afterwards will
Silica crucible is placed on crucible tray；After fixation, lift supporting rod so that the convergence center of light condensation screen is located at seed crystal upper end 1/
At 3, and ensure to have in the range of this not molten seed crystal.The rotating speed of support bar is adjusted in 20rpm；Open without shadow Halogen lamp LED；Gradually rise
Halogen lamp LED power, until seed crystal starts to melt；After constant temperature 60min, melting zone gradually expands and finally keeps stable；Under starting afterwards
Silica crucible drops, and the fall off rate of crucible is 10mm/h；According to the propulsion situation of solid liquid interface, heating power is adjusted so that molten
Body concaves towards the germanium crystal of growth, and maintains growth interface stable；Until the polycrystalline not melted melts completely, crystal growth is completed.
Crystal growth starts cooling after terminating, rate of temperature fall is 50 DEG C/h；When crystal is cooled to room temperature, silica crucible is taken out, is taken
Go out crystal, obtain germanium single crystal.
The germanium single crystal crystalline condition that the present embodiment is obtained is good, and crystal forming rate is between 90~100%；Without cracking, polycrystalline, gas
The defects such as bubble；Monocrystalline repetitive rate is higher, and monocrystalline mass discrepancy is small between different batches.
Detected according to GB/T5252, the germanium single crystal dislocation density that the present embodiment is obtained is in 10000/cm2Left and right, with document report
Dislocation density substantially similar (the electronics industry special equipment, 2012 of the germanium single crystal of the floating zone method growth in road:210；36-
39)。
Embodiment 2
Using the grower shown in Fig. 1, no shadow Halogen lamp LED has two, symmetrical, Halogen lamp LED power 1000W, voltage
240V；The infrared light sent without shadow Halogen lamp LED is gathered in crystal growth chamber center by the stainless steel light condensation screen of surface gold-plating；Earthenware
Crucible is suprasil crucible, and crucible internal diameter 5mm, length 80mm, wall thickness 2mm, crucible surface is bright and clean；Crucible is placed on positioned at crystal
On the crucible tray of growth chamber center plumb line, crucible tray and the crucible of stainless steel are fixedly secured；Crucible tray is placed on can be with
On the support bar of lifting and rotation.There are seed slot, seed slot a diameter of 4mm, length 5mm in crucible lower end.Crucible internal walls inclination angle is
3°。
Under 4N argon gas atmospheres, by 4g 5N CaF2Powder stock melts in suprasil crucible, and in argon gas atmosphere
Cooling.Polycrystal material is taken out afterwards, seed crystal, seed crystal diameter 4mm, length 5mm are loaded on seed slot；Polycrystal material is loaded afterwards
In crucible, evacuate inner air and seal silica crucible；Silica crucible is placed on crucible tray；After fixation, lifting support
Bar so that the convergence center of light condensation screen is located at seed crystal bottom.The rotating speed of support bar is opened, rotating speed is maintained at 5rpm；Open halogen
Plain lamp；Power is gradually risen, until seed crystal starts to melt；Constant temperature 20min, begins to decline silica crucible, the fall off rate of crucible
For 5mm/h；According to the propulsion situation of solid liquid interface, heating power is adjusted so that melt concaves towards the CaF of growth2Monocrystal, and it is raw
Long interface stability；Until the polycrystalline not melted melts completely, crystal growth is completed.Crystal growth starts cooling, drop after terminating
Warm speed is 30 DEG C/h；When crystal is cooled to room temperature, crucible is taken out, crystal is taken out, obtains CaF2Monocrystalline.
The CaF that the present embodiment is obtained2Crystal structure is functional, the defect such as bubble-free；Monocrystalline repetitive rate is higher, difference batch
Monocrystalline mass discrepancy is small between secondary.
Embodiment 3
Using grower as shown in Figure 1, no shadow Halogen lamp LED has two, symmetrical, Halogen lamp LED power 650W, voltage
240V；The infrared light sent without shadow Halogen lamp LED is gathered in crystal growth chamber center by the stainless steel light condensation screen of surface gold-plating；Earthenware
Crucible is suprasil crucible, and crucible internal diameter is 8mm, and length 80mm, wall thickness 2mm, crucible surface is bright and clean；Crucible is placed on positioned at crystalline substance
On the crucible tray of body growth chamber center plumb line, crucible tray and the crucible of stainless steel are fixedly secured；Crucible tray is placed on can
With on the support bar that lifts and rotate.There are seed slot, seed slot a diameter of 4mm, length 10mm in crucible lower end.Crucible internal walls inclination angle
For 2 °.
Under 4N argon gas atmospheres, 5.5g 5N cadmium-zinc-teilurides polycrystal raw material is melted and cooled and solidified in suprasil crucible；
Internal gas is evacuated afterwards and seals silica crucible；Silica crucible is placed on crucible tray afterwards；After fixation, lifting support
Bar so that the convergence center of light condensation screen is located at seed crystal bottom.The rotating speed of support bar is opened, rotating speed is controlled between 8rpm；Open
Halogen lamp LED；Power is gradually risen, until the polycrystalline at seed crystal position starts to melt；Silica crucible, earthenware are begun to decline after constant temperature 60min
Crucible fall off rate is 3mm/h；According to the propulsion situation of solid liquid interface, heating power is adjusted so that melt concaves towards the tellurium zinc of growth
Cd monocrystal body, and growth interface is stable；Until unfused cadmium-zinc-teiluride polycrystalline is completely melt, tellurium-zincium-cadmium crystal growth is completed.Tellurium
Zincium-cadmium crystal growth starts cooling after terminating, rate of temperature fall is 40 DEG C/h；When tellurium-zincium-cadmium crystal is cooled to room temperature, earthenware is taken out
Crucible, takes out tellurium-zincium-cadmium crystal, obtains Te-Zn-Cd monocrystal.
The tellurium-zincium-cadmium crystal crystal property that the present embodiment is obtained is good, after being eliminated by seeded region polycrystalline geometry, by
Monocrystal is gradually developed into, and maintains to terminate to crystal growth.In addition to seeded region, monocrystalline body portion is without cracking, polycrystalline, bubble etc.
Defect.
The present invention is corroded Te-Zn-Cd monocrystal manufactured in the present embodiment section, polishing corrosion after and with EAg- I, is detected
EPD (low corrosion pit density) is 40000/cm2 or so, suitable with the dislocation density for the crystal that THM methods grow (Li Handong,《Tellurium zinc
The growth of Cd monocrystal body and defect》, Sichuan University's Master's thesis, 2004).
Embodiment 4
With grower as shown in Figure 1, no shadow Halogen lamp LED has four, symmetrical, Halogen lamp LED power 500W, voltage
240V；The infrared light sent without shadow Halogen lamp LED is gathered in crystal growth chamber center by the stainless steel light condensation screen of surface gold-plating；Earthenware
Crucible is transparent alumina crystal crucible, and crucible internal diameter is 8mm, length 80mm, wall thickness 3mm, crucible surface polishing；Crucible is placed on
On the crucible tray of crystal growth chamber center plumb line, crucible tray and the crucible of stainless steel are fixedly secured；Crucible is propped up
Put on the support bar that can be lifted and rotate.The crucible lower end a diameter of 8mm of seed slot is identical with crucible diameter.
The seed crystal for cleaning (111) direction is placed in seed slot, seed crystal length is 10mm, diameter 8mm.By 5N 15g germanium
After sour bismuth polycrystal raw material melts in other platinum crucibles, pour into alpha-alumina crystals crucible, and make melt slow solidification, herein
During ensure seed crystal not exclusively melt；Alpha-alumina crystals crucible is placed on crucible tray afterwards；After fixation, lifting support
Bar so that the convergence center of light condensation screen is located at seed crystal bottom.The rotating speed of support bar is opened, rotating speed is controlled between 15rpm；Open
Halogen lamp LED；Power is gradually risen, until the polycrystalline at seed crystal position starts to melt；Alpha-alumina crystals are begun to decline after constant temperature 60min
Crucible, crucible fall off rate is 2mm/h；According to the propulsion situation of solid liquid interface, heating power is adjusted so that melt concaves towards growth
Bismuth germanate single crystal, and growth interface is stable；Until unfused bismuth germanium oxide polycrystalline is completely melt that bismuth-germanium-oxide crystal has grown
Into.Bismuth-germanium-oxide crystal growth starts cooling after terminating, rate of temperature fall is 30 DEG C/h；When bismuth-germanium-oxide crystal is cooled to room temperature,
Crucible is taken out, bismuth-germanium-oxide crystal is taken out, obtains bismuth-germanate single crystal.
The bismuth-germanium-oxide crystal crystal property that the present embodiment is obtained is good, visually observes without defects such as cracking, polycrystalline, bubbles.
Monocrystalline repetitive rate is higher, and monocrystalline mass discrepancy is small between different batches.
Through above example as can be seen that the grower provided using the present invention, can not only grow normal optical and float
Outside the crystal that area's method can grow, additionally it is possible to grow low surface tension crystal, the crystal easily aoxidized and have volatile components
Crystal, and obtained crystal structure is functional, the defect such as bubble-free；Monocrystalline repetitive rate is higher, monocrystalline between different batches
Mass discrepancy is small, and dislocation density is relatively low.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of grower of crystal, including：Light condensation screen；
The infrared light supply and transparent crucible being arranged in light condensation screen, the infrared light supply are arranged on around the crucible；Institute
State infrared band transmitance >=80% of crucible；The fusing point of crystal of the fusing point of the crucible than being grown is high 400~2000 DEG C；
The infrared light supply is that the number of the infrared light light source is 2~4 without shadow Halogen lamp LED；The infrared light supply is with the crucible
Center plumb line be distributed in around the crucible for axisymmetrical；
Support bar for supporting the crucible；The support bar is the support bar of liftable and rotation；
The support bar is connected with crucible by crucible tray.
2. grower according to claim 1, it is characterised in that the crucible is crystalline ceramics crucible, glass pot
Or transparent crystal crucible.
3. grower according to claim 1, it is characterised in that the crucible includes sidewall of crucible and crucible bottom, described
Sidewall of crucible has inclination angle, and the crucible bottom is provided with seed slot.
4. a kind of growing method of crystal, comprises the following steps：
Polycrystalline is melted and solidified successively, the polycrystalline pre-processed；
Using the grower described in claims 1 to 3 any one, the polycrystalline of pretreatment is heated in crucible, entered
The growth of row crystal, obtains monocrystalline.
5. growing method according to claim 4, it is characterised in that the process of the heating is specifically included：
Polycrystalline is heated with the first temperature, second temperature is cooled to first rate after 20~60min of heating, polycrystalline is entered
Row heating, carries out the growth of crystal, and crystal growth is cooled to the 3rd temperature with the second speed after terminating, obtains crystal；
First temperature is is grown more than crystalline melting point 50~100 DEG C；
Second temperature is is grown more than crystalline melting point 0~25 DEG C；
3rd temperature is 20~35 DEG C；
First rate is 1~10 DEG C/h；
Second speed is 20~50 DEG C/h.
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| CN106757353A (en) * | 2017-02-16 | 2017-05-31 | 广东先导稀材股份有限公司 | The growing method of bismuth germanate single crystal |
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| US6451111B1 (en) * | 2001-03-27 | 2002-09-17 | Corning Incorporated | Seed crystal for epitaxial growth of single-crystal calcium fluoride |
| CN1234920C (en) * | 2003-09-01 | 2006-01-04 | 山东大学 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
| CN100526519C (en) * | 2006-12-27 | 2009-08-12 | 钟毅 | Device for cultivating DKDP crystal with high-quality and high deuterium-content using light bath method |
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