CN113502536A - Ionothermal synthesis of nonlinear optical polycrystalline powder lead boron oxygen bromine - Google Patents

Ionothermal synthesis of nonlinear optical polycrystalline powder lead boron oxygen bromine Download PDF

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CN113502536A
CN113502536A CN202110561959.2A CN202110561959A CN113502536A CN 113502536 A CN113502536 A CN 113502536A CN 202110561959 A CN202110561959 A CN 202110561959A CN 113502536 A CN113502536 A CN 113502536A
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nonlinear optical
bromine
boron
lead
oxygen
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谭德明
李秀军
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Chengdu Jiuying Information Technology Co ltd
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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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/35—Non-linear optics
    • G02F1/355—Non-linear optics characterised by the materials used
    • G02F1/3551—Crystals
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams

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  • Crystallography & Structural Chemistry (AREA)
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  • Optics & Photonics (AREA)
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Abstract

And (3) performing ionothermal synthesis on the nonlinear optical polycrystalline powder lead boron oxygen bromine. Lead boron oxygen bromine (molecular formula: Pb)2B5O9Br) with molecular weight of 692.34, belonging to orthorhombic system, space group Pnn2, unit cell parameter of
Figure DSA0000242728020000011
α＝β＝γ＝90°，
Figure DSA0000242728020000012
And Z is 4. The preparation method adopts a low-temperature ionothermal reaction method. The preparation method can synthesize lead-boron-oxygen-bromine at 170 ℃ (the traditional method needs high temperature of more than 700 ℃), and the method greatly reduces resource consumption. Nonlinear optical experiments show that the synthesized lead-boron-oxygen-bromine nonlinear optical polycrystalline powderHas excellent nonlinear optical performance.

Description

Ionothermal synthesis of nonlinear optical polycrystalline powder lead boron oxygen bromine
Technical Field
The present invention belongs to the preparation of non-linear optical material
Background
The nonlinear optical material is widely used in the aspects of optical information processing, optical fiber communication, laser devices, laser frequency doubling, remote sensing, laser guidance, laser radar and the like. These nonlinear optical materials have played a critical role in chemistry, information, biology, and the like.
Lead boron oxygen bromine (Pb)2B5O9Br) is a non-linear optical material in the ultraviolet band. Having high nonlinear optical coefficients thereon, stableChemical property and wide industrial application prospect. The traditional synthesis method of the lead-boron-oxygen-bromine adopts a high-temperature solid phase method, requires a high temperature of more than 700 ℃, and has large resource consumption. The invention adopts an ionothermal method to prepare the lead-boron-oxygen-bromine polycrystalline powder, and the method only needs a synthesis temperature of 170 ℃. In addition, the method is also suitable for large-scale preparation, and provides a good idea for industrial expanded production.
Disclosure of Invention
The invention aims to prepare lead-boron-oxygen-bromine polycrystalline powder.
The molecular formula of the lead-boron-oxygen-bromine polycrystalline powder prepared by the invention is Pb2B5O9Br, molecular weight of 692.34, belonging to orthorhombic system, space group Pnn2, unit cell parameter of
Figure BSA0000242728040000011
Figure BSA0000242728040000012
α＝β＝γ＝90°，
Figure BSA0000242728040000013
Figure BSA0000242728040000014
Z＝4。
Nonlinear optical test experiment shows that lead boron oxygen bromine (Pb)2B5O9Br) have high nonlinear optical effects.
The lead-boron-oxygen-bromine is expected to have important application value in the field of nonlinear optics as a nonlinear optical material.
Description of the drawings:
FIG. 1 is a pure phase powder diagram of lead boron oxygen bromine; the experimental values and the theoretical values are well matched, and the obtained powder sample is a pure phase.
FIG. 2 is a performance diagram of Pb-B-O-Br under a second harmonic microscope, which shows that the Pb-B-O-Br has high nonlinear optical performance.
Detailed Description
And (3) preparing lead boron oxygen bromine polycrystalline powder.
With Pb (OAc)2·3H2O and H3BO3As raw material, in a glove box according to Pb (OAc)2·3H2O∶H3BO3The mixture is placed in a single-neck glass flask with the mol ratio of 2: 5, and then the ionic liquid [ P ] is added66614]Br is added. The final ratio of reactants to ionic liquid is Pb (OAc)2·3H2O∶H3BO3∶[P66614]Br is 4: 10: 15. The flask was closed with a glass stopper and then placed in an oil bath to heat to 170 ℃ with stirring. After 10h of reaction, the flask was taken out of the oil bath and cooled to room temperature. The solid product was separated using a centrifuge, and the solid powder was washed 3 times with ethanol and then 2 times with distilled water. Finally, the solid powder obtained was dried overnight under dynamic vacuum at room temperature. The powder is single-phase lead-boron-oxygen-bromine as shown by powder X-ray diffraction analysis.

Claims (1)

1. The compound of formula (I) is Pb2B5O9Br) polycrystalline powder, comprising the following steps: with Pb (OAc)2·3H2O and H3BO3As raw material, in a glove box according to Pb (OAc)2·3H2O∶H3BO3The mixture is placed in a single-neck glass flask with the mol ratio of 2: 5, and then the ionic liquid [ P ] is added66614]Br, final ratio of reactants and ionic liquid Pb (OAc)2·3H2O∶H3BO3∶[P66614]Br 4: 10: 15, the flask was capped with a glass stopper and then placed in an oil bath to heat to 170 ℃ with stirring, after 10h of reaction, the flask was taken out of the oil bath, cooled to room temperature, the solid product was isolated using a centrifuge, the solid powder was washed 3 times with ethanol and then 2 times with distilled water, and finally the solid powder obtained was dried overnight under dynamic vacuum at room temperature.
CN202110561959.2A 2021-05-21 2021-05-21 Ionothermal synthesis of nonlinear optical polycrystalline powder lead boron oxygen bromine Withdrawn CN113502536A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101435108A (en) * 2008-11-28 2009-05-20 中国科学院新疆理化技术研究所 Large size nonlinear optical crystal lead bromoborate, and preparation and use thereof
CN101498040A (en) * 2009-01-08 2009-08-05 中国科学院新疆理化技术研究所 K3B6O10 Br nonlinear optical crystal, preparation and use
CN111621848A (en) * 2020-06-02 2020-09-04 中国科学院新疆理化技术研究所 Compound tin boron oxygen bromine, tin boron oxygen bromine nonlinear optical crystal, preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101435108A (en) * 2008-11-28 2009-05-20 中国科学院新疆理化技术研究所 Large size nonlinear optical crystal lead bromoborate, and preparation and use thereof
CN101498040A (en) * 2009-01-08 2009-08-05 中国科学院新疆理化技术研究所 K3B6O10 Br nonlinear optical crystal, preparation and use
CN111621848A (en) * 2020-06-02 2020-09-04 中国科学院新疆理化技术研究所 Compound tin boron oxygen bromine, tin boron oxygen bromine nonlinear optical crystal, preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DEMING TAN ET AL.: "Resource-Efficient Low-Temperature Synthesis of Microcrystalline Pb2B5O9X (X = Cl, Br) for Surfaces Studies by Optical Second Harmonic Generation", SMALL *

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