CN209741305U - mould for growing rare earth ion doped crystal by heterogeneous high-melting point arc seed crystal - Google Patents
mould for growing rare earth ion doped crystal by heterogeneous high-melting point arc seed crystal Download PDFInfo
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- CN209741305U CN209741305U CN201920190694.8U CN201920190694U CN209741305U CN 209741305 U CN209741305 U CN 209741305U CN 201920190694 U CN201920190694 U CN 201920190694U CN 209741305 U CN209741305 U CN 209741305U
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Abstract
The utility model provides a mold for growing rare earth ion doped crystals by heterogeneous high melting point arc seed crystals, which comprises a crucible consisting of a cone cavity and a cylinder cavity, wherein the cone cavity is an arc seed crystal area, and the middle part in the cylinder cavity is provided with a cylindrical mold with heat dissipation holes; a plurality of strip-shaped conical holes are formed in the cylindrical die, a crucible cover is arranged at the top of each conical hole, and a vent hole is formed in the middle of each crucible cover; the crucible, the cylindrical die and the heat dissipation holes are symmetrical in a central axis. Meanwhile, the crystal growth method comprises the following steps: batching, charge, evacuation and let in protective gas, intensification and change material, crystal growth, annealing and get the crystal, compare with prior art, the utility model discloses a mould has simple structure, easily processing, and growth process flow is simple, can many different types of and the not crystal of different concentration rare earth ion doping of single growth.
Description
Technical Field
The utility model belongs to the technical field of crystal growth, a rare earth ion doped crystal's growth method is related to, concretely relates to mould and growth method of rare earth ion doped crystal with heterogeneous high melting point arc seed crystal growth.
background
the particles (atoms, molecules, ions or atomic groups) in the crystal are arranged in a periodic order, and the glass and the ceramic are in an amorphous structure with short-range order and long-range disorder; the emission spectrum of the glass matrix is the most smooth due to the completely disordered amorphous lattice structure, but the efficiency and the application range of the glass matrix are severely limited due to the small emission section, the short radiation life and the low thermal conductivity. The crystal generally has higher thermal conductivity and larger mechanical property, the doping concentration in the crystal is influenced by an ordered crystal field, the absorption cross section of the crystal is larger, the emission spectral line is uniformly widened, the line width is narrower, and the gain is higher, so the crystal is widely applied to scientific research and industry. Glass, optical fiber and ceramic may replace crystals in some application fields, but cannot fundamentally replace the positions of the crystals.
The Czochralski method is one of the methods for growing crystals. The parameters in the crystal growth process can be conveniently controlled by using the Czochralski method to grow the crystal; the crystal grows on the surface of the melt without contacting the crucible wall, so that the stress of the crystal is obviously reduced, and parasitic nucleation is effectively prevented; the crystal quality is improved by controlling the processes of necking, shouldering and the like. However, the Czochralski method has some defects, such as only one crystal can be grown at a time, the production cost is high, and the industrial production of the crystal is not facilitated; if the crystal is volatilized more in the growth process, the equipment is corroded seriously. The traditional growth method has the defect that only one crystal can be grown at one time, and the crystal utilization rate is low, so that the method is not beneficial to industrial production. Chinese patent (CN201610808276) discloses growth equipment and a growth method for preparing magnesium fluoride crystals by a multi-crucible descent method, wherein a plurality of magnesium fluoride crystals can be grown simultaneously by the method, but the crucible is an assembly crucible and is complex to operate; because the crucible covers do not correspond to the crucible holes one by one, only one crystal can be grown at a time, otherwise, the crystal can be subjected to vacuum pumping or cross contamination in the growth process. Chinese patent (CN201310045422.6) discloses a preparation process for growing multiple crystals by a guided mode method, which can only grow one crystal at a time.
disclosure of Invention
the utility model aims at overcoming the problems existing in the prior art, providing a mold and a growth method which can use heterogeneous high melting point arc seed crystal to grow rare earth ion doped crystal, and overcoming the problems of easy melting of seed crystal, low growth efficiency and single growth type in the traditional method.
the utility model provides a mould for growing rare earth ion doped crystals by heterogeneous high melting point arc seed crystals, which comprises a crucible consisting of a cone cavity and a cylinder cavity, wherein the cone cavity is an arc seed crystal area, and the middle part in the cylinder cavity is provided with a cylinder mould with heat dissipation holes; a plurality of strip-shaped conical holes are formed in the cylindrical die, a crucible cover is arranged at the top of each conical hole, and a vent hole is formed in the middle of each crucible cover; the crucible, the cylindrical die and the heat dissipation holes are symmetrical in a central axis.
As a modification, the outer diameter of the cylindrical mold is 1-2mm smaller than the inner diameter of the cylindrical cavity of the crucible.
As an improvement, the number of the tapered holes is 3-24, the whole body is long-strip-shaped, and the bottom end is of a tapered structure.
As an improvement, the diameter of the vent hole is 0.5-1.5 mm.
meanwhile, a crystal growth method adopting any one of the moulds is also provided, and the method comprises the following steps: s01, loading heterogeneous high-melting-point arc seed crystals in an arc seed crystal area of the crucible, placing a cylindrical mold in a cylindrical cavity, weighing all raw materials in proportion, respectively loading the raw materials into the conical holes after fully and uniformly mixing, and screwing a crucible cover;
s02, vacuumizing, and introducing helium as a protective atmosphere;
s03, heating to 150-350 ℃, and keeping the temperature for 4-7h to remove the water in the raw materials;
S04, continuously heating until the raw materials are completely melted, and carrying out constant-temperature heat treatment for 3-8 h;
S05, slowly cooling at the speed of 0.25-1.8 ℃/h to crystallize the melt in the crucible from bottom to top;
S06, after the crystal growth is finished, cooling to a certain temperature at 1.2-3.9 ℃/h to finish the annealing process;
And S07, cooling to room temperature according to the cooling rate of 7-40 ℃/h, slowly taking out the cylindrical mold and taking out the crystal in the conical hole.
as an improvement, the seed crystal in S01 is a single crystal, the melting point of the single crystal is higher than that of the grown crystal by more than 100 ℃, the shape of the single crystal is arc-shaped, and the external dimension of the single crystal is 0.2-0.5mm smaller than that of the seed crystal.
In an improvement, the rare earth ion of S01 is any one of Pr ion, Dy ion, Er ion, Ho ion and the like, and the matrix is any one of PbF2, CaF2, SrF2, YAG-Y3Al5O12, CNGG-Ca3Nb1.6875Ga3.1875O12.
As an improvement, the purity of the raw material of S01 is 4N or more.
has the advantages that: compared with the prior art, the utility model has the advantages of it is following: (1) the heterogeneous high-melting-point arc-shaped seed crystal is used for growing the crystal, the melting of the seed crystal with overhigh temperature is avoided, and the requirement on temperature control in the growing process is reduced. (2) The porous mold has the advantages of simple structure and easy processing, can grow a plurality of rare earth ion doped crystals of different types and different concentrations in a single time, and each hole is provided with the independent crucible cover, thereby reducing the volatilization of a melt to the maximum extent and preventing the cross contamination among different crystals. (3) The heat exchange method is utilized to grow the crystal, the crucible, the crystal and the heat exchanger are not moved in the growth process, no mechanical disturbance exists, the crystal growth interface is stable, the internal defects of the crystal are reduced, and the optical quality of the crystal is effectively improved. (4) The crystal is still kept in a hot area after growing, the temperature change and the furnace environment are controlled by controlling the heating power and the protective gas flow, the in-situ annealing of the crystal is realized, and the defects of internal stress, dislocation and the like of the crystal are reduced. (5) The whole crystal growth process can realize full automation, labor is saved, and production cost is reduced.
The above description is only an overview of the technical solution of the present invention, and in order to make the technical means of the present invention clearer and can be implemented according to the content of the description, the following detailed description is made with reference to the preferred embodiments of the present invention and accompanying drawings.
Drawings
Fig. 1 is a cross-sectional view of the mold of the present invention.
in the drawings: 1. a crucible cover; 2. a crucible; 3. a cylindrical mold; 4. a vent hole; 5. a tapered hole; 6. an arc-shaped seed crystal region; 7. and (4) heat dissipation holes.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings and examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
A mould for growing rare earth ion doped crystals by heterogeneous high-melting point arc seed crystals comprises a crucible 2 consisting of a conical cavity and a cylindrical cavity, wherein the conical cavity is an arc seed crystal area 6, and the cylindrical mould 3 is provided with a heat dissipation hole 7 in the middle in the cylindrical cavity; a plurality of strip-shaped conical holes 5 are formed in the cylindrical die 3, a crucible cover 1 is arranged at the top of each conical hole 5, and a vent hole 4 is formed in the middle of each crucible cover 1; the crucible 2, the cylindrical mold 3 and the heat dissipation holes 7 are in central axis symmetry.
The diameter of the cylindrical die 3 is 1-2mm smaller than the inner diameter of the crucible 2. 3-24 conical holes 5 are arranged, the selectable diameters are the same or different, the whole body is in a strip shape, and the bottom end is in a conical structure; the diameter of the taper hole 5 is 10-20mm and the length is 200-240 mm.
the crystal growth method adopting the die comprises the following steps: s01, loading heterogeneous high-melting-point arc seed crystals in the arc seed crystal area 6 of the crucible 2, placing the cylindrical die 3 in a cylindrical cavity, weighing all raw materials in proportion, respectively loading the raw materials into the tapered holes 5 after fully and uniformly mixing, and screwing the crucible cover 1;
S02, vacuumizing, and introducing helium as a protective atmosphere;
S03, heating to 150-350 ℃, and keeping the temperature for 4-7h to remove the water in the raw materials;
s04, continuously heating until the raw materials are completely melted, and carrying out constant-temperature heat treatment for 3-8 h;
S05, slowly cooling at the speed of 0.25-1.8 ℃/h to crystallize the melt in the crucible 2 from bottom to top;
S06, after the crystal growth is finished, cooling to a certain temperature at 1.2-3.9 ℃/h to finish the annealing process;
S07, cooling to room temperature according to the cooling rate of 7-40 ℃/h, slowly taking out the cylindrical mold column 3 and taking out the crystal in the tapered hole 5.
wherein the seed crystal in the S01 is a single crystal with any orientation, the melting point of the seed crystal is higher than that of the grown crystal by more than 100 ℃, the seed crystal is arc-shaped, and the overall dimension of the seed crystal is 0.2-0.5mm smaller than that of the seed crystal.
the rare earth ions of S01 are Pr ions, Dy ions, Er ions or Ho ions, and the matrix is any one of PbF2, CaF2, SrF2, YAG-Y3Al5O12 and CNGG-Ca3Nb1.6875Ga3.1875O12. The raw material purity of S01 is 4N or more. Wherein the temperature is reduced to 600-1000 ℃ in the setting S06.
Example 1
the moulds used were 12 cylindrical moulds with a diameter of 10mm and a length of 210 mm.
S01, arc-shaped pure calcium fluoride crystal seeds are firstly loaded in the arc-shaped seed crystal area 6 of the crucible 2. Weighing all high-purity raw materials and an oxygen scavenger accounting for 1% of the total mass of the raw materials according to a chemical formula DyxPb (1-x) F2+ x (x is 0.01,0.02 and 0.03 …), fully and uniformly mixing, then respectively filling into a cylindrical die, and screwing a crucible cover;
S02, vacuumizing, and introducing helium as a protective atmosphere;
s03, heating to 150 ℃, and keeping the temperature for 5 hours to remove the moisture in the raw materials;
S04, continuously heating until the raw materials are completely melted, and carrying out constant-temperature heat treatment for 5 hours;
S05, slowly cooling at the speed of 0.5-1.0 ℃/h to crystallize the melt in the crucible from bottom to top;
S06, after the crystal growth is finished, reducing the temperature to 600 ℃ at a speed of 1.5-3.0 ℃/h, and finishing the annealing process;
S07, cooling to room temperature according to the cooling rate of 10-30 ℃/h, taking out the cylindrical die 3 and taking out the crystal.
Example 2
The dies used were 24 cylindrical dies with a diameter of 20mm and a length of 210 mm.
S01, firstly, arc pure YAG crystal seed crystals are loaded in the arc seed crystal area 6 of the crucible 2. Weighing all high-purity raw materials according to Ca3Nb1.6875Ga3.1875O12 and xRe3Ga5O12(Re ═ Pr, Dy, Ho, Tb …, x ═ 0.01,0.02 and 0.03 …) chemical formulas according to a proportion, fully and uniformly mixing, pressing, sintering at high temperature, then respectively filling into a cylindrical mold, and screwing a crucible cover;
S02, vacuumizing, and introducing helium as a protective atmosphere;
s03, heating to 200 ℃, and keeping the temperature for 5 hours to remove the moisture in the raw materials;
S04, continuously heating until the raw materials are completely melted, and carrying out constant-temperature heat treatment for 5 hours;
s05, slowly cooling at the speed of 0.5-1.0 ℃/h to crystallize the melt in the crucible from bottom to top;
s06, when the crystal growth is finished, reducing the temperature to 1000 ℃ at 1.5-3.9 ℃/h, and finishing the annealing process;
s07, cooling to room temperature according to the cooling rate of 10-30 ℃/h, taking out the cylindrical mold 3 and taking out the crystal.
example 3
The moulds used were 22 cylindrical moulds 3 of diameter 15mm and length 240 mm.
S01, firstly, arc pure YAG crystal seed crystals are loaded in the arc seed crystal area 6 of the crucible 2. Weighing all high-purity raw materials according to Ca3Nb1.6875Ga3.1875O12 and xRe3Ga5O12(Re ═ Pr, Dy, Ho, Tb …, x ═ 0.01,0.02 and 0.03 …) chemical formulas according to a proportion, fully and uniformly mixing, pressing, sintering at high temperature, then respectively filling into a cylindrical mold 3, and screwing a crucible cover 1;
s02, vacuumizing, and introducing helium as a protective atmosphere;
s03, heating to 350 ℃, and keeping the temperature for 7h to remove the moisture in the raw materials;
s04, continuously heating until the raw materials are completely melted, and carrying out constant-temperature heat treatment for 3 h;
s05, slowly cooling at the speed of 0.25-1.0 ℃/h to crystallize the melt in the crucible 2 from bottom to top;
S06, after the crystal growth is finished, reducing the temperature to 800 ℃ at 1.2-3.0 ℃/h, and finishing the annealing process;
S07, cooling to room temperature according to the cooling rate of 7-30 ℃/h, taking out the cylindrical mold 3 and taking out the crystal.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (4)
1. A mold for growing rare earth ion doped crystals by heterogeneous high-melting point arc seed crystals is characterized in that: the crucible (2) comprises a conical cavity and a cylindrical cavity, wherein the conical cavity is an arc-shaped seed crystal region (6), and the middle part in the cylindrical cavity is provided with a cylindrical mold (3) with a heat dissipation hole (7); a plurality of strip-shaped conical holes (5) are formed in the cylindrical die (3), a crucible cover (1) is arranged at the top of each conical hole (5), and a vent hole (4) is formed in the middle of each crucible cover (1); the crucible (2), the cylindrical die (3) and the heat dissipation holes (7) are symmetrical about a central axis.
2. The mold for growing a rare earth ion doped crystal by heterogeneous high melting point arc seed crystal according to claim 1, wherein: the outer diameter of the cylindrical die (3) is 1-2mm smaller than the inner diameter of the cylindrical cavity of the crucible (2).
3. The mold for growing a rare earth ion doped crystal by heterogeneous high melting point arc seed crystal according to claim 1, wherein: the number of the tapered holes (5) is 3-24, the whole body is in a strip shape, and the bottom end is in a tapered structure.
4. The mold for growing a rare earth ion doped crystal by heterogeneous high melting point arc seed crystal according to claim 1, wherein: the diameter of the vent hole (4) is 0.5-1.5 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913941A (en) * | 2019-02-12 | 2019-06-21 | 南京同溧晶体材料研究院有限公司 | A kind of mold and growing method of the heterogeneous rare earth ion doped crystal of high-melting-point arc seeded growth |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913941A (en) * | 2019-02-12 | 2019-06-21 | 南京同溧晶体材料研究院有限公司 | A kind of mold and growing method of the heterogeneous rare earth ion doped crystal of high-melting-point arc seeded growth |
| CN109913941B (en) * | 2019-02-12 | 2024-03-26 | 南京同溧晶体材料研究院有限公司 | Die and growth method for growing rare earth ion doped crystal by heterogeneous high-melting-point arc seed crystal |
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