CN106835262B - A method of growth aluminium tetraborate salt crystal - Google Patents

A method of growth aluminium tetraborate salt crystal Download PDF

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CN106835262B
CN106835262B CN201710071990.1A CN201710071990A CN106835262B CN 106835262 B CN106835262 B CN 106835262B CN 201710071990 A CN201710071990 A CN 201710071990A CN 106835262 B CN106835262 B CN 106835262B
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CN106835262A (en
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林炎富
陈雨金
黄艺东
黄建华
龚兴红
罗遵度
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Fujian Institute of Research on the Structure of Matter of CAS
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B9/00Single-crystal growth from melt solutions using molten solvents
    • C30B9/04Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12Salt solvents, e.g. flux growth
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides

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Abstract

The present invention relates to the growing methods of aluminium tetraborate salt crystal.This method uses new NaF-AlF3‑B2O3Chemical combination objects system can weaken the volatilization of the certain ingredients of solution in crystal growing process as fluxing agent growth aluminium tetraborate salt crystal, to effectively avoid the crystal growth due to caused by the volatilization of the certain ingredients of solution unstable and crystal defect.The aluminium tetraborate single-crystal of salt for obtaining large scale and high optical quality can be grown using technical solution of the present invention, be conducive to improve the performance of the laser and device for non-linear optical using monocrystalline production.

Description

A method of growth aluminium tetraborate salt crystal
Technical field
The present invention relates to a kind of growing method of monocrystalline, the flux growth metrhod for particularly relating to aluminium tetraborate salt crystal is raw It is long.
Background technique
Aluminium tetraborate salt crystal RAl3(BO3)4With good physical and chemical performance and higher thermal conductivity and lesser Thermal expansion anisotropy, strong alkali-acid resistance do not deliquesce.The crystalloid has biggish nonlinear optical coefficients, and moderate is two-fold Rate and wide transmission region are penetrated, is a kind of outstanding non-linear optical crystal material.Part R in the crystalloid3+Ion lattice If position is by certain rare earth ion (such as Nd3+, Yb3+And Er3+Deng) occupied, fundamental wave can be achieved under semiconductor laser pumping and swash Light, therefore be also a kind of outstanding laser crystal material;It, can also be further real if the crystal is cut along certain phase matching angle Existing self frequency-changing's laser output, thus referred to as self frequency-changing's laser crystal material.Since the crystalloid is off-congruent fusing, so It must be grown using flux growth metrhod.What is generallyd use at present is the fluxing agent system based on molybdenum trioxide, is being grown Molybdenum trioxide is readily volatilized in the process, not only causes crystal growth unstable, but also Mo3+Can enter crystal in become impurity from Son, to reduce the optical quality of grown crystal.
Summary of the invention
The purpose of the present invention is to provide a kind of new fluxing agent systems for growing aluminium tetraborate single-crystal of salt.The fluxing agent System can be effectively reduced volatilization of the pyrosol ingredient in crystal growing process, improve the stability of crystal growth, thus Obtain the aluminium tetraborate single-crystal of salt of centimeter-scale and high optical quality.
The present invention includes following technical solution:
1. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: use NaF-AlF3-B2O3Chemical combination objects system It is fluxing agent growth aluminium tetraborate salt crystal RAl3(BO3)4, wherein R is certain in Y, Gd, Lu, Er, Yb, Nd, Dy, Tb, Sm element The combination of one element or several elements;By aluminium tetraborate salt compound and NaF-AlF3-B2O3Chemical combination objects system mixes by a certain percentage Conjunction is uniformly placed in platinum crucible, is heated to 1050-1150 DEG C of fusing and constant temperature certain time, then be down to solution saturation temperature point Solution temperature after obtaining accurate saturation temperature point, is increased to saturation temperature by the test for nearby carrying out accurate saturation temperature point 5-15 DEG C of degree or more, then the seed crystal being fixed on seed rod is put into solution, with 0.5-3 DEG C/day after constant temperature 10-30 hours Rate cooling, while with 5-30 revs/min of rate rotate crystal.After crystal growth is to required size, stop operating crystal And lift-off liquid level, then room temperature is down to 5-40 DEG C/h of rate, it can be obtained aluminium tetraborate salt crystal.
2. method as described in item 1, it is characterised in that: aluminium tetraborate salt compound and NaF-AlF3-B2O3Chemical combination objects system Between mass percent be (20-30): 100.
3. method as described in item 1, it is characterised in that: NaF-AlF3-B2O3NaF, AlF in chemical combination objects system3And B2O3Change Closing the mass percent between object is 1:(1-2): (1.5-2.5).
Aluminium tetraborate salt crystal is grown using the fluxing agent system that technical solution of the present invention proposes, crystal growth can be weakened The volatilization of the certain ingredients of solution in the process, therefore it is possible to prevente effectively from the crystal due to caused by the volatilization of the certain ingredients of solution is raw Long unstable and crystal defect.The tetraboric acid aluminium salt for obtaining large scale and high optical quality can be grown using technical solution of the present invention Monocrystalline is conducive to improve the performance of the laser and device for non-linear optical using monocrystalline production.
Specific embodiment
Example 1: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth YAl3(BO3)4Crystal
The Y of 43g is weighed respectively2O3, 514.3g H3BO3, 58.2g Al2O3, 333.4g AlF3·3H2O and 142.9g NaF be placed in agate mortar together and grind and be uniformly mixed.Uniformly mixed raw material by high temperature melt furnace at 1100 DEG C 70 × 70mm of φ is poured into after melting several times3Platinum crucible in, and be placed in crystal growing furnace, growth furnace be warming up to 1150 DEG C 1050 DEG C are down to after constant temperature 20 hours.The saturation temperature point that solution is determined with continuous seeding down crystal method, then heats up solution More than to saturation temperature point after 10 DEG C, the seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, constant temperature half Saturation temperature point is down to after hour.Constant temperature is cooled down after growing 24 hours with the rate of 1 DEG C/day, and with the rotation of 15 revs/min of rate Crystal.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.It is annealed again with 40 DEG C/h of rate To room temperature, obtains size and be greater than 15 × 20 × 30mm3High-quality transparent YAl3(BO3)4Crystal.
Example 2: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth GdAl3(BO3)4Crystal
The Gd of 64g is weighed respectively2O3, 514.3g H3BO3, 58.2g Al2O3, 333.4g AlF3·3H2O and 104.5g NaF be placed in agate mortar together and grind and be uniformly mixed.Uniformly mixed raw material by high temperature melt furnace at 1100 DEG C 70 × 70mm of φ is poured into after melting several times3Platinum crucible in, and be placed in crystal growing furnace, growth furnace be warming up to 1150 DEG C 1080 DEG C are down to after constant temperature 15 hours.The saturation temperature point that solution is determined with continuous seeding down crystal method, then heats up solution More than to saturation temperature point after 7 DEG C, the seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, constant temperature half is small When after be down to saturation temperature point.Constant temperature is cooled down after growing 20 hours with the rate of 0.5 DEG C/day, and with the rotation of 20 revs/min of rate Crystal.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.It is annealed again with 30 DEG C/h of rate To room temperature, obtains size and be greater than 10 × 25 × 25mm3High-quality transparent GdAl3(BO3)4Crystal.
Example 3: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth LuAl3(BO3)4Crystal
The Lu of 71.8g is weighed respectively2O3, 509.3g H3BO3, 55.1g Al2O3, 333.4g AlF3·3H2O and The NaF of 126.3g is placed in agate mortar together and grinds and be uniformly mixed.Uniformly mixed raw material is existed by high temperature melt furnace 70 × 70mm of φ is poured into after 1150 DEG C of fusings several times3Platinum crucible in, and be placed in crystal growing furnace, growth furnace heated up 1060 DEG C are down to after constant temperature 30 hours to 1150 DEG C.The saturation temperature point that solution is determined with continuous seeding down crystal method, then will be molten After liquid is warming up to 15 DEG C of saturation temperature point or more, the seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, Saturation temperature point is down to after constant temperature half an hour.Constant temperature is cooled down after growing 30 hours with the rate of 2 DEG C/day, and with 25 revs/min of speed Rate rotates crystal.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.Again with 20 DEG C/h of speed Rate is annealed to room temperature, obtains size and is greater than 20 × 30 × 25mm3High-quality transparent LuAl3(BO3)4Crystal.
Example 4: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth Nd0.04Y0.96Al3(BO3)4Crystal
The Nd of 2.56g is weighed respectively2O3, 41.28g Y2O3, 514.3g H3BO3, 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 142.9g is placed in agate mortar together and grinds and be uniformly mixed.Uniformly mixed raw material is passed through height Warm melt furnace pours into 70 × 70mm of φ after melting several times at 1100 DEG C3Platinum crucible in, and be placed in crystal growing furnace, will Growth furnace is warming up to 1150 DEG C of constant temperature and is down to 1050 DEG C after 20 hours.The saturation temperature of solution is determined with continuous seeding down crystal method Point slowly drops to the seed crystal being fixed on seed rod in advance after solution is then warming up to 8 DEG C of saturation temperature point or more Liquid level is hereinafter, be down to saturation temperature point after constant temperature half an hour.Constant temperature is cooled down after growing 30 hours with the rate of 1.5 DEG C/day, and with 20 revs/min of rate rotates crystal.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.Again with 35 DEG C/h rate be annealed to room temperature, obtain size and be greater than 20 × 20 × 30mm3High-quality transparent single crystal Nd0.04Y0.96Al3 (BO3)4Crystal.
Example 5: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth Yb0.1Gd0.9Al3(BO3)4Crystal
The Yb of 7.5g is weighed respectively2O3, 57.7g Gd2O3, 514.3g H3BO3, 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 142.9g is placed in agate mortar together and grinds and be uniformly mixed.Uniformly mixed raw material is passed through height Warm melt furnace pours into 70 × 70mm of φ after melting several times at 1100 DEG C3Platinum crucible in, and be placed in crystal growing furnace, will Growth furnace is warming up to 1150 DEG C of constant temperature and is down to 1060 DEG C after 20 hours.The saturation temperature of solution is determined with continuous seeding down crystal method Point slowly declines the seed crystal being fixed on seed rod in advance after solution is then warming up to 10 DEG C of saturation temperature point or more To liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour.Constant temperature is cooled down after growing 24 hours with the rate of 2 DEG C/day, and with 20 revs/min of rate rotates crystal.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.Again with 40 DEG C/h rate be annealed to room temperature, obtain size and be greater than 15 × 15 × 30mm3High-quality transparent Yb0.1Gd0.9Al3(BO3)4It is brilliant Body.
Example 6: NaF-AlF is used3-B2O3Chemical combination objects system is fluxing agent growth Er0.015Yb0.15Lu0.835Al3(BO3)4It is brilliant Body
The Er of 1.03g is weighed respectively2O3, 10.67g Yb2O3, 60g Lu2O3, 509.3g H3BO3, 55.1g Al2O3, 333.4g AlF3·3H2The NaF of O and 126.3g is placed in agate mortar together and grinds and be uniformly mixed.Mixing Uniform raw material pours into 70 × 70mm of φ after melting several times by high temperature melt furnace at 1100 DEG C3Platinum crucible in, and place In crystal growing furnace, 1060 DEG C are down to after growth furnace is warming up to 1150 DEG C of constant temperature 20 hours.It is true with continuous seeding down crystal method The saturation temperature point for determining solution after solution is then warming up to 12 DEG C of saturation temperature point or more, will be fixed on seed rod in advance Seed crystal slowly drop to liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour.With 1.5 after constant temperature growth 30 hours The rate of DEG C/day cools down, and rotates crystal with 30 revs/min of rate.When cooling amount is up to 80 DEG C, stop operating crystal and lift-off Liquid level terminates growth.Room temperature is annealed to 40 DEG C/h of rate again, size is obtained and is greater than 15 × 20 × 25mm3It is high-quality Bright Er0.015Yb0.15Lu0.835Al3(BO3)4Crystal.

Claims (7)

1. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: use NaF-AlF3-B2O3Chemical combination objects system helps Flux growth aluminium tetraborate salt crystal RAl3(BO3)4, wherein R is certain unitary in Y, Gd, Lu, Er, Yb, Nd, Dy, Tb, Sm element The combination of plain or several elements;By aluminium tetraborate salt compound and NaF-AlF3-B2O3Chemical combination objects system is by mass percentage (20-30): 100 are uniformly mixed and are placed in platinum crucible, are heated to 1050-1150 DEG C of fusing and constant temperature certain time, then are down to Solution saturation temperature point nearby carries out the test of accurate saturation temperature point, after obtaining accurate saturation temperature point, by solution temperature Degree is increased to above 5-15 DEG C of saturation temperature point, then the seed crystal being fixed on seed rod is put into solution, constant temperature 10-30 hours Cooled down afterwards with 0.5-3 DEG C/day of rate, while crystal is rotated with 5-30 revs/min of rate;When crystal growth to required size Afterwards, stop operating crystal and lift-off liquid level, then is down to room temperature with 5-40 DEG C/h of rate, and it is brilliant to can be obtained tetraboric acid aluminium salt Body;The NaF-AlF3-B2O3NaF, AlF in chemical combination objects system3And B2O3Mass percent between compound is 1:(1-2): (1.5-2.5)。
2. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Y of 43g respectively2O3, 514.3g H3BO3、 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 142.9g is placed in agate mortar together and grinds and be uniformly mixed; 70 × 70mm of φ is poured into after uniformly mixed raw material is melted by high temperature melt furnace at 1100 DEG C several times3Platinum crucible in, And be placed in crystal growing furnace, 1050 DEG C are down to after growth furnace is warming up to 1150 DEG C of constant temperature 20 hours;With continuous lower seed crystal Method determines that the saturation temperature point of solution will be fixed on seed after solution is then warming up to 10 DEG C of saturation temperature point or more in advance Seed crystal on crystalline style slowly drops to liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour;After constant temperature is grown 24 hours Cooled down with the rate of 1 DEG C/day, and crystal is rotated with 15 revs/min of rate;When cooling amount is up to 80 DEG C, crystal is stopped operating simultaneously Lift-off liquid level terminates growth.
3. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Gd of 64g respectively2O3, 514.3g H3BO3、 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 104.5g is placed in agate mortar together and grinds and be uniformly mixed; 70 × 70mm of φ is poured into after uniformly mixed raw material is melted by high temperature melt furnace at 1100 DEG C several times3Platinum crucible in, And be placed in crystal growing furnace, 1080 DEG C are down to after growth furnace is warming up to 1150 DEG C of constant temperature 15 hours;With continuous lower seed crystal Method determines that the saturation temperature point of solution will be fixed on seed crystal after solution is then warming up to 7 DEG C of saturation temperature point or more in advance Seed crystal on bar slowly drops to liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour;Constant temperature grow 20 hours after with The rate of 0.5 DEG C/day cools down, and rotates crystal with 20 revs/min of rate;When cooling amount is up to 80 DEG C, crystal is stopped operating simultaneously Lift-off liquid level terminates growth.
4. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Lu of 71.8g respectively2O3, 509.3g H3BO3, 55.1g Al2O3, 333.4g AlF3·3H2The NaF of O and 126.3g is placed in agate mortar together and grinds and mix Uniformly;70 × 70mm of φ is poured into after uniformly mixed raw material is melted by high temperature melt furnace at 1150 DEG C several times3Platinum earthenware It in crucible, and is placed in crystal growing furnace, is down to 1060 DEG C after growth furnace is warming up to 1150 DEG C of constant temperature 30 hours;Under constantly Seed crystal method determines that the saturation temperature point of solution will be fixed in advance after solution is then warming up to 15 DEG C of saturation temperature point or more Seed crystal on seed rod slowly drops to liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour;Constant temperature growth 30 is small When after cooled down with the rates of 2 DEG C/day, and crystal is rotated with 25 revs/min of rate;When cooling amount is up to 80 DEG C, stop operating crystalline substance Body and lift-off liquid level terminate growth.
5. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Nd of 2.56g respectively2O3, 41.28g Y2O3, 514.3g H3BO3, 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 142.9g is placed in agate mortar together Middle grinding is simultaneously uniformly mixed;Uniformly mixed raw material by high temperature melt furnace 1100 DEG C several times melt after pour into φ 70 × 70mm3Platinum crucible in, and be placed in crystal growing furnace, be down to 1050 after growth furnace is warming up to 1150 DEG C of constant temperature 20 hours ℃;The saturation temperature point that solution is determined with continuous seeding down crystal method, after solution is then warming up to 8 DEG C of saturation temperature point or more, The seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour;It is permanent Temperature growth is cooled down after 30 hours with the rate of 1.5 DEG C/day, and rotates crystal with 20 revs/min of rate;When cooling amount is up to 80 DEG C When, stop operating crystal and lift-off liquid level, terminates growth.
6. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Yb of 7.5g respectively2O3, 57.7g Gd2O3、 The H of 514.3g3BO3, 58.2g Al2O3, 333.4g AlF3·3H2The NaF of O and 142.9g is placed in agate mortar together to be ground It grinds and is uniformly mixed;Uniformly mixed raw material by high temperature melt furnace 1100 DEG C several times melt after pour into φ 70 × 70mm3Platinum crucible in, and be placed in crystal growing furnace, be down to 1060 after growth furnace is warming up to 1150 DEG C of constant temperature 20 hours ℃;The saturation temperature point that solution is determined with continuous seeding down crystal method, after solution is then warming up to 10 DEG C of saturation temperature point or more, The seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, being down to saturation temperature point after constant temperature half an hour;It is permanent Temperature growth is cooled down after 24 hours with the rate of 2 DEG C/day, and rotates crystal with 20 revs/min of rate;When cooling amount is up to 80 DEG C, Stop operating crystal and lift-off liquid level, terminates growth.
7. a kind of method for growing aluminium tetraborate salt crystal, it is characterised in that: weigh the Er of 1.03g respectively2O3, 10.67g Yb2O3, 60g Lu2O3, 509.3g H3BO3, 55.1g Al2O3, 333.4g AlF3·3H2The NaF of O and 126.3g is together It is placed in agate mortar and grinds and be uniformly mixed;Uniformly mixed raw material is melted by high temperature melt furnace at 1100 DEG C several times After pour into 70 × 70mm of φ3Platinum crucible in, and be placed in crystal growing furnace, it is small that growth furnace is warming up to 1150 DEG C of constant temperature 20 When after be down to 1060 DEG C;The saturation temperature point that solution is determined with continuous seeding down crystal method, is then warming up to saturation temperature for solution Or more after 12 DEG C, the seed crystal being fixed on seed rod in advance is slowly dropped into liquid level hereinafter, being down to after constant temperature half an hour Saturation temperature point;Constant temperature is cooled down after growing 30 hours with the rate of 1.5 DEG C/day, and rotates crystal with 30 revs/min of rate;When When cooling amount is up to 80 DEG C, stop operating crystal and lift-off liquid level, terminates growth.
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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070437A (en) * 1992-06-12 1993-03-31 山东大学 A kind of compound function crystal lutetium-doped aluminium-ytterbium-neodymium tetraborate growth technique
CN1148638A (en) * 1996-07-23 1997-04-30 山东大学 Aluminium tetraborate gadolinium crystal blended with rare earth and growth method thereof
JP2003096448A (en) * 2001-09-27 2003-04-03 Sumitomo Chem Co Ltd Fluorescent substance for vacuum ultraviolet-excited light-emitting element
CN1455030A (en) * 2002-05-03 2003-11-12 中国科学院福建物质结构研究所 Self double-frequency blue laser crystal neodymium-doped gadolinium-aluminium borate
CN1780074A (en) * 2004-11-28 2006-05-31 中国科学院福建物质结构研究所 Laser crystal materials doped with thulium borate rolled aluminium, preparation and use thereof
CN1778999A (en) * 2004-11-28 2006-05-31 中国科学院福建物质结构研究所 Aluminium borate with non-linear optical materials
CN1958881A (en) * 2005-11-01 2007-05-09 中国科学院福建物质结构研究所 Boratory laser crystal Li6R(1-x)REx(B03)3 and preparation method, and application
CN101545137A (en) * 2008-03-25 2009-09-30 中国科学院福建物质结构研究所 Erbium ion activated borate laser crystal and method for preparing same and application thereof
CN101831706A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Growth method of low ultraviolet absorption YA13(BO3)4 crystal
CN101831705A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Method for growing YAl3(BO3)4 crystals by tungstate cosolvent system
CN102140690A (en) * 2010-12-31 2011-08-03 陈哲艮 Photoluminescent wafer as well as preparation method and application thereof
CN103290475A (en) * 2012-02-27 2013-09-11 中国科学院理化技术研究所 GdAl3(BO3)4 crystal growth fluxing agent and GdAl3(BO3)4 crystal growth method

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070437A (en) * 1992-06-12 1993-03-31 山东大学 A kind of compound function crystal lutetium-doped aluminium-ytterbium-neodymium tetraborate growth technique
CN1148638A (en) * 1996-07-23 1997-04-30 山东大学 Aluminium tetraborate gadolinium crystal blended with rare earth and growth method thereof
JP2003096448A (en) * 2001-09-27 2003-04-03 Sumitomo Chem Co Ltd Fluorescent substance for vacuum ultraviolet-excited light-emitting element
CN1455030A (en) * 2002-05-03 2003-11-12 中国科学院福建物质结构研究所 Self double-frequency blue laser crystal neodymium-doped gadolinium-aluminium borate
CN1780074A (en) * 2004-11-28 2006-05-31 中国科学院福建物质结构研究所 Laser crystal materials doped with thulium borate rolled aluminium, preparation and use thereof
CN1778999A (en) * 2004-11-28 2006-05-31 中国科学院福建物质结构研究所 Aluminium borate with non-linear optical materials
CN1958881A (en) * 2005-11-01 2007-05-09 中国科学院福建物质结构研究所 Boratory laser crystal Li6R(1-x)REx(B03)3 and preparation method, and application
CN101545137A (en) * 2008-03-25 2009-09-30 中国科学院福建物质结构研究所 Erbium ion activated borate laser crystal and method for preparing same and application thereof
CN101831706A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Growth method of low ultraviolet absorption YA13(BO3)4 crystal
CN101831705A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Method for growing YAl3(BO3)4 crystals by tungstate cosolvent system
CN102140690A (en) * 2010-12-31 2011-08-03 陈哲艮 Photoluminescent wafer as well as preparation method and application thereof
CN103290475A (en) * 2012-02-27 2013-09-11 中国科学院理化技术研究所 GdAl3(BO3)4 crystal growth fluxing agent and GdAl3(BO3)4 crystal growth method

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