CN111041558A - Rare earth sesquioxide laser crystal growth method - Google Patents
Rare earth sesquioxide laser crystal growth method Download PDFInfo
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- CN111041558A CN111041558A CN201910638970.7A CN201910638970A CN111041558A CN 111041558 A CN111041558 A CN 111041558A CN 201910638970 A CN201910638970 A CN 201910638970A CN 111041558 A CN111041558 A CN 111041558A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/24—Complex oxides with formula AMeO3, wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. ortho ferrites
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Abstract
The invention provides a growth method of a rare earth sesquioxide laser crystal, wherein the crystal growth adopts a cold crucible method, the growth process comprises six steps of charging, igniting, melting, heat balancing, growing and cooling, a layer of unmelted shell is formed outside a raw material by using a water-cooled copper pipe to play a role of a crucible, and the rare earth sesquioxide laser crystal with the required size is grown. The invention can avoid the pollution of the crucible to the melt, can grow the high-quality rare earth sesquioxide laser crystal in a short time, can repeatedly utilize the crystallization excess material in the growth process, and reduce the growth cost.
Description
Technical Field
The invention belongs to the technical field of crystal growth, and particularly relates to a growth method of a rare earth sesquioxide laser crystal.
Background
Rare earth sesquioxide laser crystal (Ln)xRe1-x)2O3(Ln/Re ═ Y/Sc/Lu/Gd, x is more than or equal to 0 and less than or equal to 1) has high thermal conductivity, low phonon energy and excellent optical and spectral characteristics, and is a laser host crystal material with excellent performance. The rare earth sesquioxide crystal can be formed into a laser crystal (chemical formula is b% at. Y: (Ln) by doping an appropriate rare earth active ion (Yb/Nd/Dy/Ho/Er/Tm/Pr)xRe1-x)2O3) The laser can generate visible light to mid-infrared multiband laser output, and has wide application prospect in the fields of industrial processing, communication, medical treatment, military affairs, scientific research and the like.
The melting point of the rare earth sesquioxide laser crystal is very high and is generally over 2400 ℃, and only a crucible made of a high-melting-point material, such as a rhenium crucible or a tungsten crucible, can be selected when the crystal grows. Under high temperature conditions, the crucible materials are easy to corrode to generate compound components which float on the surface of a melt, impurity inclusions are generated in crystals, optical quality of the crystals is affected, and great difficulty is brought to growth of the crystals. The cold crucible method is an effective high-temperature crystal growth method, and is characterized by that the raw material powder body is placed in a water-cooled crucible system formed from copper tube, and its interior is melted by high-frequency heating, and its exterior is equipped with cooling tube to form a layer of non-melted shell, then slowly cooled and crystallized and grown. The rare earth sesquioxide laser crystal grown by the cold crucible method can avoid crucible pollution and grow high-quality crystal, but has a plurality of difficulties in the aspects of coil frequency selection, crystal growth temperature control and the like, has great technical challenges, and has no report of related technologies at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for growing high-quality rare earth sesquioxide laser crystal by using a cold crucible method, which comprises the following steps:
① charging, namely, preparing raw material powder according to a molecular formula proportion, uniformly mixing the raw material powder, adding the mixture into a cold crucible with the inner diameter phi of 50-500mm and the height of 50-800mm, wherein the charging volume is 70-90% of the volume of the crucible, adding (50-300) g of ignition agent at one half of the volume of the raw material, the specific mass of the ignition agent is determined by calculation according to the size of the cold crucible and the volume of the raw material, and adjusting the position of the crucible to ensure that the position of the ignition agent is positioned in the middle of the induction coil;
② igniting, starting a high-frequency power supply with frequency range of 50kHz-1MHz, igniting the igniting agent to generate high temperature to melt the raw material powder in the nearby area, adjusting the power of the power supply to 10-30kW and keeping for 0.5-1h to keep the melt level in the middle of the induction coil;
③ melting, namely slowly increasing the power of a power supply to (40-100) kW, gradually enlarging a melting area, gradually increasing the melting liquid level to be higher than the upper part of the induction coil, and forming a layer of unmelted shell on the raw material powder on the outer wall due to water cooling;
④ heat balance, stopping raising power and keeping the melt in this state for (1-5) h to reach the heat balance between the melt and the cold crucible after the melt level is 2-40 cm away from the crucible top;
⑤ growing, wherein after the melt and the cold crucible reach thermal equilibrium, the crystal can be grown by adopting a temperature gradient method, a crucible moving method, an induction coil moving method, a kyropoulos method, a czochralski method and other crystal means;
⑥ cooling, after the crystal growth is finished, the power of the power supply is gradually reduced, the temperature is slowly reduced to room temperature, and then the crystal is taken out.
The crystal growth device adopted by the invention consists of a cold crucible system, a cold crucible system and a crystal growth device, wherein the cold crucible system consists of an induction coil, a water-cooling copper lobe, a water-cooling chassis, a crucible lifting system and an induction coil lifting system; the induction coil surrounds the outside of the water-cooled copper petal, the water-cooled copper petal and the water-cooled chassis form a cold crucible, the inner diameter phi of the cold crucible is 50-500mm, and the height is 50-800 mm; the position of the cold crucible is controlled by a crucible lifting system, and the position of the induction coil is controlled by an induction coil lifting system.
The chemical formula of the crystal is b% at.Y:(LnxRe1-x)2O3wherein x is more than or equal to 0 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 10, Y is Yb/Nd/Dy/Ho/Er/Tm/Pr, Re is Y/Sc/Lu/Gd, and Ln is Y/Sc/Lu/Gd;
the preferred inner diameter of the cold crucible in step ① is phi 100-300mm, and the preferred height is 200-500 mm;
the preferred material of the initiator in step ① is a rare earth metal corresponding to the composition of the rare earth sesquioxide being grown, and the less preferred material is graphite;
in step ④, after the melt volume reaches the desired value, the heat balance of the system is achieved by keeping the melt in this state for 1-5 h;
the crystal growth method described in step ⑥ includes, but is not limited to, a temperature gradient method, a crucible moving method, an induction coil moving method, a kyropoulos method, and a czochralski method.
Compared with the prior art, the invention has the technical advantages that:
① the traditional rare earth sesquioxide laser crystal growth method needs high melting point rare metal crucibles (such as rhenium crucibles, tungsten crucibles, etc.), the cost is high and pollution of different degrees exists.
② can grow crystal with melting point above 3000 deg.C;
③ may be grown in a variety of atmospheres including air, oxygen, and the like;
④ the crystallized residual material in the growth process can be re-melted and used, thus reducing the cost.
Drawings
FIG. 1 is a schematic view of a crystal apparatus.
Fig. 2 is a cross-sectional view of a crystal device.
In the figure: 1 is an induction coil; 2, water-cooling copper petals; 3 is a crucible lifting system; 4 is an induction coil lifting system; and 5, a water-cooling chassis.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear, the present invention is specifically described below with reference to the accompanying drawings and embodiments. The examples herein are provided only for the purpose of explaining the present invention and are not intended to limit the present invention.
Example one
(growth 1% at. Nd)3+：Gd2O3Crystal (II)
Weighing the raw material powder, adding Nd2O3、Gd2O3The raw materials are mixed according to the required proportion in the chemical formula and then are stirred uniformly, and the purity of the raw materials is not lower than 5N. Putting the prepared raw materials into a cold crucible with the diameter of 200mm and the height of 300mm, filling 80 percent of the volume of the raw materials, inserting 100g of high-purity graphite ring into 1/2 parts of the internal volume of the raw materials, and adjusting the position of the crucible to ensure that the graphite ring is positioned in the middle of the induction coil; starting a high-frequency power supply and adjusting the frequency to 1MHz to perform induction heating on the high-purity graphite ring in the raw material; the high-purity graphite ring is rapidly heated, the raw materials near the graphite ring begin to melt at 2300 ℃ to form a small melting zone, the power of a power supply is adjusted to 15kW and is kept for 40min, and the melting liquid level is kept in the middle of the induction coil in the process. The power of the induction coil is slowly increased to 50kW, the melting zone is gradually enlarged, and the outer layer raw material forms a layer of unmelted shell due to water cooling. When the distance between the melting liquid level and the top of the crucible is 8cm, keeping the cold crucible system for 3 hours in the state; after the heat balance between the melt and the cold crucible is achieved, the cold crucible is controlled to descend at the speed of 5mm/h, the temperature of the melt descends, and the crystal grows. And after the melt in the cold crucible is completely crystallized, stopping the cold crucible from descending, reducing the power of the power supply to 0.5kW at the rate of 2kW/h, and turning off the power supply. Multiple large size 1% at.nd can be obtained from cold crucible3 +：Gd2O3And (3) single crystal.
Example two
[ growth 2% at.Ho ]3+:(Sc0.4Y0.6)2O3Crystal (II)
Weighing the raw material powder and adding Sc2O3、Ho2O3、Y2O3The raw materials are mixed according to the required proportion in the chemical formula and then are stirred uniformly, and the purity of the raw materials is not lower than 5N. Pouring the prepared raw material part into a cold crucible with the diameter of 50mm and the height of 50mm, filling 90 percent of the raw material volume of the crucible in the raw material1/2 g of high-purity yttrium sheet is inserted, and the position of the crucible is adjusted to ensure that the position of the yttrium sheet is positioned in the middle of the induction coil; starting a high-frequency induction power supply and adjusting the power supply frequency to about 100kHZ to perform induction heating on the yttrium sheets in the raw materials; the yttrium sheet is rapidly heated, when the temperature reaches 2430 ℃, raw materials near the yttrium sheet begin to melt to form a small melting zone, the power of a power supply is adjusted to 10kW and is kept for 30min, and the melting liquid level is kept in the middle of the induction coil. The coil power is slowly increased to 40kW, the melting zone is gradually enlarged, and the outer layer raw material forms a layer of melting shell due to water cooling. After the melt level was 2cm from the crucible top, the cold crucible system was kept in this state for 1h to achieve thermal equilibrium between the melt and the cold crucible, and then the induction coil was raised at a rate of 5mm/h, the melt temperature dropped and crystal growth occurred. And after the melt in the cold crucible is completely crystallized, stopping the rising of the induction coil, reducing the power of the power supply to 0.5kW at the rate of 1.5kW/h, and turning off the power supply. Multiple large size 2% at.Ho can be obtained from cold crucible3+:(Sc0.4Y0.6)2O3Single crystal
EXAMPLE III
[ growth (Lu)0.2Sc0.8)2O3Crystal (II)
Weighing the raw material powder and adding Sc2O3、Lu2O3The raw materials are mixed according to the required proportion in the chemical formula and then are stirred uniformly, and the purity of the raw materials is not lower than 5N. Pouring the prepared raw material part into a cold crucible with the diameter of 500mm and the height of 800mm, filling 80 percent of the volume of the raw material, inserting 1/2 g of high-purity lutetium sheet into the raw material, and adjusting the position of the crucible to ensure that the lutetium sheet is positioned in the middle of the induction coil; starting a high-frequency power supply and adjusting the frequency to about 200kHz to perform induction heating on the lutetium sheets in the raw materials; the lutetium sheet is heated rapidly, when the temperature reaches 2500 ℃, raw materials near the lutetium sheet begin to melt to form a small melting zone, the power of a power supply is adjusted to 30kW and kept for 1 hour, and the melting liquid level is kept in the middle of the induction coil. The power of the induction coil is gradually increased to 100kW, the melting zone is gradually enlarged, and the outer layer raw material forms a layer of melting shell due to water cooling. After the melt level was 40cm from the crucible top, the cold crucible system was held in this state for 5h to achieve a hot plateau between the melt and the cold crucibleAnd (5) balancing, then reducing the power of the power supply at the speed of 500W/h, reducing the temperature of the melt, growing crystals, and turning off the power supply after the power is reduced to 0.5 kW. Obtaining a plurality of large-size Sc2O3、Lu2O3And (3) single crystal.
Example four
[ growth 10% at.Ho ]3+：Lu2O3Crystal (II)
Weighing raw material powder, and mixing Lu2O3、Ho2O3The raw materials are mixed according to the required proportion in the chemical formula and then are stirred uniformly, and the purity of the raw materials is not lower than 5N. The prepared raw materials are poured into a cold crucible with the diameter of 300mm and the height of 500mm, the volume of the filled raw materials is 80 percent of the volume of the crucible, 150g of high-purity graphite flakes are inserted into 1/2 parts inside the raw materials, and the position of the crucible is adjusted to ensure that the graphite flakes are positioned in the middle of the induction coil. Starting a high-frequency power supply and adjusting the frequency to about 300kHZ to perform induction heating on the graphite blocks in the raw materials; the graphite block is rapidly heated, when the temperature reaches 2500 ℃, raw materials near the graphite block begin to melt to form a small melting zone, the power of a power supply is adjusted to 20kW and is kept for 45min, and the melting liquid level is kept in the middle of the induction coil. The coil power is slowly increased to 60kW, the melting zone is gradually enlarged, and the outer layer raw material forms a layer of melting shell due to water cooling. When the melt level is 20cm away from the top of the crucible, the cold crucible system is kept for 3h in the state to achieve the heat balance between the melt and the cold crucible, then the lifting rod lifting system is started, and the lifting head fixes Lu in the direction of one (111)2O3And (3) slowly descending the seed crystal to enable the seed crystal to be in contact with the surface of the melt, stopping for 1h, then starting to carry out pulling growth, wherein the pulling speed is 4mm/h, and after 5h, entering a pulling method for isodiametric growth. And stopping growing after obtaining the single crystal rod with the diameter of 25mm and the length of 150mm, and slowly cooling to room temperature.
EXAMPLE five
[ growth of Y ]2O3Crystal (II)
Weighing Y2O3Raw material powder, the purity of the raw material is not lower than 5N. Pouring the prepared raw materials into a cold crucible with the diameter of 400mm and the height of 600mm, filling 85 percent of the raw material volume of the crucible, inserting 200g of high-purity yttrium sheet into 1/2 parts in the raw materials, and adjustingAnd the position of the crucible is such that the yttrium sheet is positioned in the middle of the induction coil. And (3) switching on a water cooling system, starting a high-frequency power supply, adjusting the frequency to about 500kHZ, carrying out induction heating on yttrium sheets in the raw materials, rapidly heating the yttrium sheets, melting the raw materials near the yttrium sheets to form a small melting zone when the temperature reaches 2450 ℃, adjusting the power of the power supply to 25kW, and keeping the power for 50min to keep the melting liquid level in the middle of the induction coil. The power of the induction coil is gradually increased to 80kW, the melting zone is gradually enlarged, and the outer layer raw material forms a layer of melting shell due to water cooling. After the melt level was 25cm from the crucible top, the cold crucible system was kept in this state for 4 hours to achieve thermal equilibrium between the melt and the cold crucible, and then a Y direction of 100 was fixed at the pulling head2O3And (3) seed crystals, namely slowly descending the seed crystals to enable the seed crystals to contact the surface of the melt, starting kyropoulos growth after staying for 1h, and reducing the power of a power supply at the speed of 500W/h. Along with the reduction of the power, the melt crystallizes along the direction of the seed crystal, the growth is stopped after the crystal size meets the required requirements, and the temperature is slowly reduced to the room temperature.
Claims (3)
1. A rare earth sesquioxide laser crystal growth method is characterized by comprising the following steps:
① preparation work is carried out by mixing the raw powder according to the formula b% at.Y (Ln)xRe1-x)2O3The mixture ratio is carried out, wherein,
x is more than or equal to 0 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 10, Y is Yb/Nd/Dy/Ho/Er/Tm/Pr, Re is Y/Sc/Lu/Gd, and Ln is Y/Sc/Lu/Gd; the used cold crucible system comprises an induction coil (1), a water-cooling copper petal (2) and a water-cooling chassis (5), wherein the water-cooling copper petal (2) and the water-cooling chassis (5) are controlled to lift through a crucible lifting system (3), the induction coil is controlled to lift through an induction coil lifting system (4), the water-cooling copper petal and the water-cooling chassis enclose a cold crucible, and the inner diameter phi (50-500) mm and the height (50-800) mm of the cold crucible are arranged between;
② charging, namely, uniformly mixing the raw material powder, adding the mixture into a cold crucible, wherein the charging volume is 70-90% of the crucible volume, adding 50-300g of ignition agent at one half of the raw material volume, and adjusting the position of the crucible to ensure that the ignition agent is positioned in the middle of the induction coil;
③ igniting, starting a high-frequency power supply with frequency range of 50kHz-1MHz, igniting with an igniting agent to generate high temperature to melt the raw material powder in the nearby area, adjusting power of the power supply to 10-30kW and keeping for 0.5-1h to keep the melt level in the middle of the coil;
④ melting, namely slowly increasing the power of a power supply to 40-100kW, gradually enlarging a melting area, gradually increasing the melting liquid level to be higher than the upper part of the induction coil, and forming a layer of unmelted shell by water cooling the raw material powder on the outer wall;
⑤ heat balance, stopping raising power and keeping the melt in this state for (1-5) h to reach the heat balance between the melt and the cold crucible after the melt level is 2-40 cm away from the crucible top;
⑥ growing, wherein after the melt and the cold crucible reach thermal equilibrium, the cold crucible system lifting device can adopt temperature gradient method, crucible moving method, induction coil moving method, kyropoulos method, pulling method and other crystal methods to grow crystal;
⑦ cooling, after the crystal growth is finished, the power of the power supply is gradually reduced, the temperature is slowly reduced to room temperature, and then the crystal is taken out.
2. The method for growing a rare earth sesquioxide laser crystal as set forth in claim 1, wherein said ignition agent is a rare earth metal (Y/Lu/Sc/Gd) or a graphite material.
3. The method of claim 1, wherein in the step ⑥, the crystal growth method includes, but is not limited to, temperature gradient method, crucible moving method, induction coil moving method, kyropoulos method, and czochralski method.
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| CN111962143A (en) * | 2020-07-27 | 2020-11-20 | 山东大学 | Optical auxiliary induction heating self-crucible single crystal growth device and application |
| WO2022028800A1 (en) * | 2020-08-05 | 2022-02-10 | Forschungsverbund Berlin E.V. | Method and device for growing a rare earth sesquioxide crystal |
| CN115261973A (en) * | 2022-08-15 | 2022-11-01 | 中国科学院上海光学精密机械研究所 | Growth method of large-size gallium oxide crystal |
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