CN109797428A - A kind of heat-exchanging method grows rare earth ion doped crystal of fluoride porous graphite crucible and its growing method - Google Patents
A kind of heat-exchanging method grows rare earth ion doped crystal of fluoride porous graphite crucible and its growing method Download PDFInfo
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Abstract
The porous graphite crucible of rare earth ion doped crystal of fluoride, including crucible body are grown the present invention provides a kind of heat-exchanging method, porous graphite crucible is cylindrical body, and cylinder bottom is convex shape structure；The shaft centre line position of the cylindrical body is provided with a perforative cylindrical body heat release hole, the heat release hole top end opening, bottom closing；3-24 cavity is distributed with around heat release hole, the cavity surface is covered with crucible cover, is provided with venthole on crucible cover.The porous graphite crucible has structure simple, it is easy to process, crystal of fluoride that can be rare earth ion doped with more variety classes of single growth and various concentration, and each crucible is furnished with independent crucible cover, melt volatilization is utmostly reduced, the cross contamination between different crystal is prevented.The growing method of above-mentioned crystal is additionally provided, it can be achieved that entire crystal growing process is full-automatic, saving manpower reduces production cost.
Description
Technical field
The invention belongs to field of crystal growth, are related to a kind of growing method of rare earth ion doped crystal of fluoride, tool
Body is related to a kind of growing rare earth ion doped crystal of fluoride porous graphite crucible and its growing method with heat-exchanging method.
Background technique
Crystal of fluoride is as a kind of more traditional material, compared with oxide crystal, has many superior properties:
It, can be infrared in from far ultraviolet including very wide transparency range；Constant and low mean refractive index and local indexes of refraction,
The nonlinear effect under high intensity laser beam pumping effect can be limited；Low phonon energy reduces the non-spoke between adjacent energy levels
Relaxation is penetrated, and makes active ions luminous quantum efficiency with higher in fluoride matrix crystal.In addition, fluoride is brilliant
The features such as body also has sufficiently stable physicochemical characteristics, and relative dispersion is big, and damage threshold is high.Therefore, crystal of fluoride is suitable
The window material in vacuum ultraviolet to infrared band is shared, is also widely used in industry and scientific research.
Czochralski method is one of the method for growing crystal of fluoride.Using Czochralski grown crystal of fluoride, can be very good
Realizing observation of growth state of crystal improves crystal quality by techniques such as control necking downs.But czochralski method itself has some defects,
For example a crystal can only be grown every time, high production cost is unfavorable for the industrialized production of crystal of fluoride；Fluoride growth course
More, the equipment seriously corroded of middle volatilization；And the hardness of fluoride is low compared with oxide hardness, and the load-bearing of seed crystal is restricted, no
Conducive to the growth of crystal of fluoride large scale.Currently, temperature gradient method and Bridgman-Stockbarger method are the main sides of fluoride combination crystal growth
Method.Traditional temperature gradient method and Bridgman-Stockbarger method equally exists the drawbacks of can only once growing a kind of crystal, and utilization rate of crystal is low,
It is unfavorable for industrialized production, and Bridgman-Stockbarge method single crystal growth furnace is antivacuum furnace, the crystal of fluoride of growth is oxidized easily.
Chinese patent (CN201610808276) discloses growth apparatus and its life that a kind of multi-crucible lowering method prepares magnesium fluoride crystal
Long method, the method can grow more magnesium fluoride crystals simultaneously, but crucible used is assembling crucible, cumbersome；Because of crucible
Lid is not corresponded with crucible hole, can only grow a kind of crystal every time, otherwise can be because of vacuumizing or during the growth process
Cross contamination occurs.
Summary of the invention
The purpose of the invention is to overcome the problems, such as that existing conventional method growth efficiency is low and asgrow variety is single, it is
Reach above-mentioned purpose, the present invention provides one kind can disposably grow more variety classes and various concentration rare earth with heat-exchanging method
The crystal of fluoride of ion doping porous graphite crucible and growing method.Specific technical solution are as follows:
A kind of heat-exchanging method grows rare earth ion doped crystal of fluoride porous graphite crucible, including crucible body, institute
Stating porous graphite crucible is cylindrical body, and cylinder bottom is convex shape structure；It is arranged along the shaft centre line position of the cylindrical body
There are a perforative cylindrical body heat release hole, the heat release hole top end opening, bottom closing；It is distributed with around heat release hole on 3-24
The cavity of end opening, lower end closed, the cavity are followed successively by seed crystal area, crystal growth area from the bottom to top, and the cavity surface is covered
It is stamped crucible cover, each crucible cover center is provided with a venthole, and wherein it is straight to be less than crystal growth area for seed crystal area diameter
Diameter.
As an improvement, the ventilation bore dia is 0.5-1.5mm.
Meanwhile the growing method that a kind of heat-exchanging method grows rare earth ion doped crystal of fluoride is additionally provided, including
Following steps:
Seed crystal is packed into the seed crystal area of above-mentioned crystal of fluoride porous graphite crucible by S01, weigh in proportion raw material and
The oxygen scavenger of material quality 0.5-1.8% is packed into above-mentioned crystal of fluoride porous graphite crucible after being sufficiently mixed uniformly
In crystal growth area；
S02 is vacuumized, and is passed through inert gas as protective atmosphere；
S03 is warming up to (200 ± 10) DEG C, and keeps the temperature 3-7h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 4-8h, and by control power and is passed through indifferent gas
The rate control seed crystal of body not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 750-980 DEG C of temperature with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
As an improvement, seed crystal described in S01 is fluoride single crystal, shape is cylinder, hole of the seed crystal diameter than seed crystal area
The small 0.2-0.5mm of diameter, seed crystal length are identical as the depth of seed crystal area inner hole.
As an improvement, rare earth ion described in S01 are as follows: Pr ion, Dy ion, Er ion, any in Ho ion, fluorination
Object is LaF3、PbF2、CaF2、SrF2In it is any.
As an improvement, material purity described in S01 is 4N or more, wherein oxygen content is in 200ppm or less.
As an improvement, inert gas described in S02 is high-purity helium.
As an improvement, heating power 15-45KW, it is 50-80L/min that inert gas, which is passed through rate, in S04.
The utility model has the advantages that compared with prior art, the invention has the following advantages that (1) the porous graphite crucible has structure
Simply, easy to process, crystal of fluoride that can be rare earth ion doped with more variety classes of single growth and various concentration, and it is every
A crucible is furnished with independent crucible cover, utmostly reduces melt volatilization, prevents the cross contamination between different crystal.(2) sharp
Crystal of fluoride is grown with heat-exchanging method, crucible, crystal and heat exchanger neither move in growth course, no mechanical disturbance, brilliant
Body growth interface is stablized, and reduces matter crystal internal defect, effectively improves crystal optics quality.(3) heat is remained at after crystal growth
Area controls temperature change and furnace inner environment by control heating power and shield gas flow rate, realizes crystal in-situ annealing, reduces
The defects of crystals stress and dislocation.(4) entire crystal growing process can realize full-automation, save manpower, reduce production
Cost.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is porous graphite crucible outline drawing of the present invention.
Fig. 2 is porous graphite crucible sectional view of the present invention.
1 is crucible cover in figure, and 2 be crucible body, and 3 be venthole, and 4 be cavity, and 5 be seed crystal hole, and 6 be heat release hole.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
A kind of heat-exchanging method grows rare earth ion doped crystal of fluoride porous graphite crucible, including crucible body 2, institute
Stating porous graphite crucible is cylindrical body, and cylinder bottom is convex shape structure.Wherein diameter is 10-20mm, length 180-
300mm, preferably 210mm.
The shaft centre line position of the cylindrical body is provided with a perforative cylindrical body heat release hole 6,6 top of heat release hole
Opening, bottom closing；The cavity 4 of 3-24 upper end opening, lower end closed is distributed with around heat release hole 6, the diameter of cavity 4 can
It can also be different with identical, the position apart from heat release hole 6 be set and is also not fixed.
Cavity 4 is followed successively by seed crystal area, crystal growth area from the bottom to top, and 4 surface of cavity is covered with crucible cover 1, each
1 center of crucible cover is provided with a venthole 3, and wherein seed crystal area diameter is less than crystal growth area diameter；The seed crystal area
Inside it is provided with seed crystal hole 5.3 diameter of venthole is 0.5-1.5mm.Seed crystal diameter is 4-10mm, length 15-30mm.It may be selected
Each cavity 4 in seed crystal type can be the same or different.
Meanwhile a kind of heat-exchanging method grows the growing method of rare earth ion doped crystal of fluoride, comprising the following steps:
Seed crystal is packed into the seed crystal area of above-mentioned crystal of fluoride porous graphite crucible by S01, weigh in proportion raw material and
The oxygen scavenger of material quality 0.5-1.8% is packed into above-mentioned crystal of fluoride porous graphite crucible after being sufficiently mixed uniformly
In crystal growth area；
S02 is vacuumized, and is passed through inert gas as protective atmosphere；
S03 is warming up to (200 ± 10) DEG C, and keeps the temperature 3-7h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 4-8h, and by control power and is passed through indifferent gas
The rate control seed crystal of body not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 750-980 DEG C of temperature with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
Wherein rare earth ion described in S01 are as follows: in Pr ion, Dy ion, Er ion, Ho ion etc. it is any one or two kinds of with
On any combination, fluoride LaF3、PbF2、CaF2、SrF2In any one or two kinds of any combination.Raw material described in S01
Purity is 4N or more, and wherein oxygen content is in 200ppm or less.Inert gas described in S02 is high-purity helium.In S04, heating
Power is 15-45KW, and it is 50-80L/min that inert gas, which is passed through rate,.
Embodiment 1
Crucible used is 12 hole graphite crucibles, i.e., cavity is 12, diameter 10mm, length 210mm.
S01 is initially introduced into diameter 5mm, the pure lanthanum fluoride crystal seeds of length 20mm.According to DyxLa(1-x)F3(x=
0.01,0.02,0.03 ...) chemical formula weighs the oxygen scavenger of all high pure raw materials and total mass of raw material 1% respectively in proportion
(PbF2Crystalline substance material), it is respectively charged into porous graphite crucible after being sufficiently mixed uniformly；
S02 is vacuumized, and is passed through helium as protective atmosphere；
S03 is warming up to 200 DEG C, and keeps the temperature 5h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 5h, and by control power and is passed through inert gas
Rate control seed crystal not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 900 DEG C with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
Embodiment 2
Crucible used is 12 hole graphite crucibles, i.e., cavity is 12, diameter 20mm, length 210mm.
S01 is initially introduced into diameter 5mm, the pure calcium fluoride crystal seed crystal of length 20mm.According to RexCa(1-x)F2+x(Re=
Pr, Dy, Ho, Tb ..., x=0.01,0.02,0.03 ...) chemical formula, weigh all high pure raw materials and the total matter of raw material respectively in proportion
The oxygen scavenger of amount 1% is respectively charged into porous graphite crucible after being sufficiently mixed uniformly；
S02 is vacuumized, and is passed through helium as protective atmosphere；
S03 is warming up to 200 DEG C, and keeps the temperature 5h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 5h, and by control power and is passed through inert gas
Rate control seed crystal not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 800 DEG C with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
Embodiment 3
Crucible used is 8 hole graphite crucibles, i.e., cavity is 8, diameter 10mm, length 210mm.By 2 institute of embodiment
Process conditions stated, but be added without calcirm-fluoride seed crystal, are grown using no seed crystal, it is also possible to obtain corresponding transparent not of the same race
Class and the rare earth ion doped calcium fluoride crystal of various concentration.
Embodiment 4
Crucible used is 20 hole graphite crucibles, i.e., cavity is 20, diameter 15mm, length 300mm.
S01 is initially introduced into diameter 4mm, the pure calcium fluoride crystal seed crystal of length 30mm.According to RexCa(1-x)F2+x(Re=
Pr, Dy, Ho, Tb ..., x=0.01,0.02,0.03 ...) chemical formula, weigh all high pure raw materials and the total matter of raw material respectively in proportion
The oxygen scavenger of amount 1.8% is respectively charged into porous graphite crucible after being sufficiently mixed uniformly；
S02 is vacuumized, and is passed through helium as protective atmosphere；
S03 is warming up to 210 DEG C, and keeps the temperature 3h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 4h, and passes through control power and the speed for being passed through helium
Rate control seed crystal not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 750 DEG C with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
Embodiment 5
Crucible used is 5 hole graphite crucibles, i.e., cavity is 5, diameter 20mm, length 180mm.
S01 is initially introduced into diameter 10mm, the pure calcium fluoride crystal seed crystal of length 15mm.According to RexCa(1-x)F2+x(Re=
Pr, Dy, Ho, Tb ..., x=0.01,0.02,0.03 ...) chemical formula, weigh all high pure raw materials and the total matter of raw material respectively in proportion
The oxygen scavenger of amount 1.8% is respectively charged into porous graphite crucible after being sufficiently mixed uniformly；
S02 is vacuumized, and is passed through helium as protective atmosphere；
S03 is warming up to 190 DEG C, and keeps the temperature 7h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 8h, and passes through control power and the speed for being passed through helium
Rate control seed crystal not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 980 DEG C with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of heat-exchanging method grows rare earth ion doped crystal of fluoride porous graphite crucible, including crucible body (2),
It is characterized in that, the porous graphite crucible is cylindrical body, and cylinder bottom is convex shape structure；Along the axis center of the cylindrical body
Line position is provided with a perforative cylindrical body heat release hole (6), heat release hole (6) top end opening, bottom closing；In heat release hole
(6) cavity (4) of 3-24 upper end opening, lower end closed is distributed with around, the cavity (4) is followed successively by seed crystal from the bottom to top
Area, crystal growth area, cavity (4) surface are covered with crucible cover (1), and each crucible cover (1) center is provided with one
Venthole (3), wherein seed crystal area diameter is less than crystal growth area diameter；Seed crystal hole (5) are provided in the seed crystal area.
2. porous graphite crucible according to claim 1, it is characterised in that: venthole (3) diameter is 0.5-
1.5mm。
3. the growing method that a kind of heat-exchanging method grows rare earth ion doped crystal of fluoride, which is characterized in that including following
Step:
Seed crystal is packed into the seed crystal area of porous graphite crucible of any of claims 1-2 by S01；Original is weighed in proportion
The oxygen scavenger of material and material quality 0.5-1.8% is packed into fluorination of any of claims 1-2 after being sufficiently mixed uniformly
In the crystal growth area of object crystal porous graphite crucible；
S02 is vacuumized, and is passed through inert gas as protective atmosphere；
S03 is warming up to (200 ± 10) DEG C, and keeps the temperature 3-7h, to exclude the moisture in raw material；
S04 is continuously heating to raw material and is completely melt, constant temperature is heat-treated 4-8h, and by control power and is passed through inert gas
Rate control seed crystal does not melt；
S05 crystallizes the melt in crucible from the bottom to top with 0.5-1.0 DEG C/h slow cooling；
S06 is down to 750-980 DEG C of temperature with 1.5-3.0 DEG C/h, completes annealing process to the end of crystal growth；
S07 is down to room temperature according to the cooling rate of 10-30 DEG C/h, takes out crystal.
4. growing method according to claim 3, which is characterized in that in S01, the seed crystal is fluoride single crystal, shape
For cylinder, seed crystal diameter is 0.2-0.5mm smaller than the bore dia in seed crystal area, and seed crystal length is identical as the depth of seed crystal area inner hole.
5. growing method according to claim 3, which is characterized in that in S01, the rare earth ion are as follows: Pr ion, Dy from
Son, Er ion, Ho ion, fluoride LaF3、PbF2、CaF2、SrF2In it is any.
6. the method that a kind of heat-exchanging method according to claim 3 grows rare earth ion doped crystal of fluoride, special
Sign is, in S01, the material purity is 4N or more, and wherein oxygen content is in 200ppm or less.
7. growing method according to claim 3, which is characterized in that in S02, the inert gas is high-purity helium.
8. growing method according to claim 3, which is characterized in that in S04, heating power 15-45KW, inert gas
Being passed through rate is 50-80L/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114635188A (en) * | 2020-12-16 | 2022-06-17 | 中国科学院上海硅酸盐研究所 | Microporous crucible and high-flux fluoride single crystal optical fiber preparation method |
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