CN109112626A - Non-linear optical crystal material β-BaB2O4Growing method - Google Patents

Non-linear optical crystal material β-BaB2O4Growing method Download PDF

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Publication number
CN109112626A
CN109112626A CN201811252389.3A CN201811252389A CN109112626A CN 109112626 A CN109112626 A CN 109112626A CN 201811252389 A CN201811252389 A CN 201811252389A CN 109112626 A CN109112626 A CN 109112626A
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China
Prior art keywords
crucible
crystal
linear optical
barium
boric acid
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CN201811252389.3A
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Chinese (zh)
Inventor
孙立辉
李国平
陈文�
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Laiwu Vocational and Technical College
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Laiwu Vocational and Technical College
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Priority to CN201811252389.3A priority Critical patent/CN109112626A/en
Publication of CN109112626A publication Critical patent/CN109112626A/en
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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
    • 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
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention relates to non-linear optical crystal material β-BaB2O4Growing method, comprising the following steps: (1) weigh the barium hydroxide that molar ratio is 2: 3 and be stirred and mix with boric acid, fluxing agent is added in mixed process；(2) it is dried under conditions of 200-250 DEG C after the reaction was completed, is placed on after being sintered 4-5 hours at 500 DEG C -600 DEG C and obtains low-temperature phase defection barium borate crystal.The invention has the advantages that the method that the present invention uses solid-state reaction at low temperature, using barium hydroxide and boric acid as raw material, without other cumbersome steps, simple process；Convection current is reinforced below crystal, reduces the convection current blind area of lower section, reduces ratio of defects.

Description

Non-linear optical crystal material β-BaB2O4Growing method
Technical field
The present invention relates to a kind of non-linear optical crystal material β-BaB2O4Growing method.
Background technique
Usually there are two types of crystal forms, i.e. high-temperature-phase (α-BaB2O4) and low-temperature phase (β β-BaB2O4) for BBO Crystal.Its Middle low-temperature phase barium metaborate (β-BaB2O4) crystal is a kind of excellent nonlinear optical crystal, is obtained in ultraviolet frequency double field It is widely applied.In addition β-BaB2O4 itself has frequency-doubled effect, and nonlinear optical property is expected to open in nonlinear optics It is applied in the fields such as pass, function ceramics.The phase transition temperature of high and low temperature phase barium metaborate two-phase is 920 ± 10 DEG C.Two kinds The fusing point of different crystal forms barium metaborate is all at 1095 ± 5 DEG C.It is brilliant in order to grow the low-temperature phase barium metaborate with high value Body, the molten-salt growth method for being all made of addition fluxing agent both at home and abroad at present grow the crystal in its transformation temperature following temperature.
Solution convection intensity is fairly small in straight tube shape crucible at present, and solute transport is the slowest, and the crystal grown is often The defect of column distribution can be formed below germ nucleus.
Summary of the invention
To overcome the shortcomings of existing technologies, the present invention provides a kind of denomination of invention, the technical scheme is that
Non-linear optical crystal material β-BaB2O4Growing method, comprising the following steps:
(1) it weighs the barium hydroxide that molar ratio is 2: 3 to be stirred and mix with boric acid, be added in mixed process fluxing Agent；
(2) it is dried, is placed on after being sintered 4-5 hours at 500 DEG C -600 DEG C under conditions of 200-250 DEG C after the reaction was completed Obtain low-temperature phase defection barium borate crystal；
(3) low-temperature phase defection barium borate crystal obtained in step (2) is placed in crucible, the diameter of crucible opening is greater than crucible The diameter at bottom is arranged in peviform, and the bottom in the crucible is additionally provided with a cone, the opening shape of the cone and crucible At spacing；
(4) after crucible being warming up to 1200-1500 DEG C, constant temperature 5-12 hours, and carry out being cooled to 600-800 DEG C, seed crystal is added It is grown, starts cooling processing after three days, with the cooling of 8 DEG C/day, Crystal Rotation rate is 3-6 revs/min, cooling 3-4 months Afterwards, the large single crystal of low-temperature phase defection barium borate crystal is obtained.
The cosolvent is sodium oxide molybdena.
The content of the sodium oxide molybdena is the 1/3-1/5 of barium hydroxide and boric acid total content.
The invention has the advantages that the method that the present invention uses solid-state reaction at low temperature, using barium hydroxide and boric acid as raw material, nothing Other cumbersome steps, simple process；Convection current is reinforced below crystal, reduces the convection current blind area of lower section, reduces ratio of defects.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and It is apparent.But examples are merely exemplary for these, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art Member it should be understood that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form into Row modifications or substitutions, but these modifications and replacement are fallen within the protection scope of the present invention.
Embodiment 1: non-linear optical crystal material β-BaB2O4Growing method, comprising the following steps:
(1) it weighs the barium hydroxide that molar ratio is 2: 3 to be stirred and mix with boric acid, be added in mixed process fluxing Agent；
(2) it is dried under conditions of 200 DEG C after the reaction was completed, is placed on after being sintered 4 hours at 500 DEG C and obtains low temperature skew Barium borate crystal；
(3) low-temperature phase defection barium borate crystal obtained in step (2) is placed in crucible, the diameter of crucible opening is greater than crucible The diameter at bottom is arranged in peviform, and the bottom in the crucible is additionally provided with a cone, the opening shape of the cone and crucible At spacing；
(4) after crucible being warming up to 1200 DEG C, constant temperature 5 hours, and carry out being cooled to 600 DEG C, seed crystal is added and is grown, three days After start cooling processing, with 8 DEG C/day cooling, Crystal Rotation rate be 3 revs/min, 3 months after, obtain low-temperature phase barium metaborate The large single crystal (120 × 60mm of Ф) of crystal.
The cosolvent is sodium oxide molybdena.
The content of the sodium oxide molybdena is the 1/3 of barium hydroxide and boric acid total content.
Embodiment 2: non-linear optical crystal material β-BaB2O4Growing method, comprising the following steps:
(1) it weighs the barium hydroxide that molar ratio is 2: 3 to be stirred and mix with boric acid, be added in mixed process fluxing Agent；
(2) it is dried under conditions of 250 DEG C after the reaction was completed, is placed on after being sintered 5 hours at 600 DEG C and obtains low temperature skew Barium borate crystal；
(3) low-temperature phase defection barium borate crystal obtained in step (2) is placed in crucible, the diameter of crucible opening is greater than crucible The diameter at bottom is arranged in peviform, and the bottom in the crucible is additionally provided with a cone, the opening shape of the cone and crucible At spacing；
(4) after crucible being warming up to 1500 DEG C, constant temperature 12 hours, and carry out being cooled to 800 DEG C, seed crystal is added and is grown, three Start cooling processing after it, with the cooling of 8 DEG C/day, after Crystal Rotation rate is 6 revs/min, 4 months, obtains low-temperature phase metaboric acid The large single crystal (130 × 80mm of Ф) of crystal of barium.
The cosolvent is sodium oxide molybdena.
The content of the sodium oxide molybdena is the 1/5 of barium hydroxide and boric acid total content.

Claims (3)

1. non-linear optical crystal material β-BaB2O4Growing method, which comprises the following steps:
(1) it weighs the barium hydroxide that molar ratio is 2: 3 to be stirred and mix with boric acid, be added in mixed process fluxing Agent；
(2) it is dried, is placed on after being sintered 4-5 hours at 500 DEG C -600 DEG C under conditions of 200-250 DEG C after the reaction was completed Obtain low-temperature phase defection barium borate crystal；
(3) low-temperature phase defection barium borate crystal obtained in step (2) is placed in crucible, the diameter of crucible opening is greater than crucible The diameter at bottom is arranged in peviform, and the bottom in the crucible is additionally provided with a cone, the opening shape of the cone and crucible At spacing；
(4) after crucible being warming up to 1200-1500 DEG C, constant temperature 5-12 hours, and carry out being cooled to 600-800 DEG C, seed crystal is added It is grown, starts cooling processing after three days, with the cooling of 8 DEG C/day, Crystal Rotation rate is 3-6 revs/min, cooling 3-4 months Afterwards, the large single crystal of low-temperature phase defection barium borate crystal is obtained.
2. non-linear optical crystal material β-BaB according to claim 12O4Growing method, which is characterized in that it is described Cosolvent be sodium oxide molybdena.
3. non-linear optical crystal material β-BaB according to claim 12O4Growing method, which is characterized in that it is described Sodium oxide molybdena content be barium hydroxide and boric acid total content 1/3-1/5.
CN201811252389.3A 2018-10-25 2018-10-25 Non-linear optical crystal material β-BaB2O4Growing method Pending CN109112626A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845936A (en) * 2019-11-18 2020-02-28 成都新柯力化工科技有限公司 Corrosion-resistant coating for buried plastic pipe and preparation method thereof

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CN1086552A (en) * 1992-11-04 1994-05-11 中国科学院福建物质结构研究所 Improved growing low temperature phase-deviation barium borate monocrystal by smelting salt crystal method
CN1357494A (en) * 2000-12-07 2002-07-10 中国科学院福建物质结构研究所 Prepn of low temp phase barium metaborate nano powder
CN1443879A (en) * 2002-03-08 2003-09-24 中国科学院福建物质结构研究所 Fused salt pulling method for growing BBO crystal
CN101913619A (en) * 2010-09-29 2010-12-15 河北大学 Preparation method of barium metaborate nano-powder
CN102383182A (en) * 2011-10-23 2012-03-21 福建福晶科技股份有限公司 Molten-salt growth method for reducing central envelope of BBO(Barium Boron Oxide) crystals
CN102965723A (en) * 2012-12-06 2013-03-13 福建福晶科技股份有限公司 Method for inhibiting radial rapid growth of BBO (Barium Boron Oxide) crystal
CN103114327A (en) * 2012-12-24 2013-05-22 福建福晶科技股份有限公司 Molten-salt growth method for eliminating core package of low-temperature phase barium metaborate crystalloid
CN103757708A (en) * 2014-01-17 2014-04-30 中国科学院福建物质结构研究所 High temperature inorganic scintillation crystal growth crucible
CN106048712A (en) * 2016-06-14 2016-10-26 福建福晶科技股份有限公司 Growth process capable of reducing barium boron oxide (BBO) crystal envelope
CN107475771A (en) * 2017-08-30 2017-12-15 福建福晶科技股份有限公司 A kind of method of envelope among reduction bbo crystal

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Publication number Priority date Publication date Assignee Title
CN1086552A (en) * 1992-11-04 1994-05-11 中国科学院福建物质结构研究所 Improved growing low temperature phase-deviation barium borate monocrystal by smelting salt crystal method
CN1357494A (en) * 2000-12-07 2002-07-10 中国科学院福建物质结构研究所 Prepn of low temp phase barium metaborate nano powder
CN1443879A (en) * 2002-03-08 2003-09-24 中国科学院福建物质结构研究所 Fused salt pulling method for growing BBO crystal
CN101913619A (en) * 2010-09-29 2010-12-15 河北大学 Preparation method of barium metaborate nano-powder
CN102383182A (en) * 2011-10-23 2012-03-21 福建福晶科技股份有限公司 Molten-salt growth method for reducing central envelope of BBO(Barium Boron Oxide) crystals
CN102965723A (en) * 2012-12-06 2013-03-13 福建福晶科技股份有限公司 Method for inhibiting radial rapid growth of BBO (Barium Boron Oxide) crystal
CN103114327A (en) * 2012-12-24 2013-05-22 福建福晶科技股份有限公司 Molten-salt growth method for eliminating core package of low-temperature phase barium metaborate crystalloid
CN103757708A (en) * 2014-01-17 2014-04-30 中国科学院福建物质结构研究所 High temperature inorganic scintillation crystal growth crucible
CN106048712A (en) * 2016-06-14 2016-10-26 福建福晶科技股份有限公司 Growth process capable of reducing barium boron oxide (BBO) crystal envelope
CN107475771A (en) * 2017-08-30 2017-12-15 福建福晶科技股份有限公司 A kind of method of envelope among reduction bbo crystal

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蔡巧芬: "纳米复合磷酸锌钙防秀颜料的制备、表征及性能", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845936A (en) * 2019-11-18 2020-02-28 成都新柯力化工科技有限公司 Corrosion-resistant coating for buried plastic pipe and preparation method thereof
CN110845936B (en) * 2019-11-18 2021-12-03 李燕玲 Corrosion-resistant coating for buried plastic pipe and preparation method thereof

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Application publication date: 20190101