CN106192011A - A kind of preparation method of second-order non-linear optical crystal material - Google Patents

A kind of preparation method of second-order non-linear optical crystal material Download PDF

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CN106192011A
CN106192011A CN201610807281.0A CN201610807281A CN106192011A CN 106192011 A CN106192011 A CN 106192011A CN 201610807281 A CN201610807281 A CN 201610807281A CN 106192011 A CN106192011 A CN 106192011A
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organic framework
metal organic
linear optical
preparation
framework compound
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CN106192011B (en
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关磊
王莹
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Liaoning Shihua University
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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
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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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)
  • General Chemical & Material Sciences (AREA)
  • Pyridine Compounds (AREA)

Abstract

The present invention relates to the preparation method of a kind of second-order non-linear optical crystal material, it comprises the steps: NiSO4·6H2O, 4,4 ' bipyridyls, M-phthalic acid 5 sodium sulfonate are soluble in water；Stirring 2 h, then, be encapsulated in the reactor of 25 mL, 120 ° of C heat 36 h；Being cooled to room temperature has blue colored crystal to generate.Metal organic framework compound in the present invention is different from other second nonlinear optic metal organic framework compound, and it utilizes the part of symmetrical structure to synthesize, with metal ion, a kind of metal organic framework compound with non-core structure obtained.Its Nonlinear Second order Optical Properties is 0.8 times of carbamide, also has phase matched.The most also there is fluorescent emission character and magnetic property.Its fluorescence emission peak is at 416 nm, compared with part, there occurs red shift.When 28 K, lone pair electrons are transformed into antiferromagnetic coupling.

Description

A kind of preparation method of second-order non-linear optical crystal material
Technical field
The present invention relates to a kind of second-order non-linear optical materials, particularly relate to a kind of second-order non-linear optical crystal material Preparation method.
Background technology
Existing second-order non-linear optical materials focuses mostly at lithium iodate, Lithium metaniobate etc. and semiconductor crystal, such as tellurium and Proustite (Ag3AsS3) etc..Because the good thermal stability of these second nonlinear materials, do not occur when higher temperature point Solve.So rapidly becoming the focus of research, such report is more common.But the metal of existing Nonlinear Second order Optical Properties has Machine frame compound is many with asymmetric part as raw material, constitutes non-core structure, Nonlinear Second order Optical Properties with metal ion Not ideal enough, and not there is photoluminescent property and magnetic property.
Summary of the invention
The present invention is directed to above-mentioned problems of the prior art, it is provided that a kind of second-order non-linear optical crystal material Preparation method, not only increases Nonlinear Second order Optical Properties, also has photoluminescent property and magnetic property.
Technical scheme is as follows:
By the NiSO of 1-1.5mmol4·6H2The 4,4 ' of O, 1-1.5mmol-bipyridyl, 1-1.5mmol M-phthalic acid- 5-sodium sulfonate is soluble in water；Stirring 2 h, then, be encapsulated in the reactor of 25 mL, 120 ° of C heat 36 h；It is cooled to room temperature Having blue colored crystal to generate, productivity is about 75-84%.
Described NiSO4·6H2O with water quality volume ratio is, 0.263-0.395 gNiSO4·6H2O is dissolved in 20 mL water In.
The present invention is compared with other second-order non-linear optical materials, and metal organic framework compound material has following Prominent feature: (1) has good heat stability；(2) structure of part, functional group and conjugated degree all can set in advance Meter；(3) expand the kind of second-order non-linear optical materials, be extended to metal organic framework compound, and utilize symmetry The part of structure synthesizes with metal ion；(4) synthesis second nonlinear material is had and can not only have two with design Rank nonlinear optical property, also has photoluminescent property and magnetic property.
The present invention is to utilize two kinds of part 5-sodium sulfo isophthalates of symmetrical structure and 4,4 '-bipyridyl and mistake Cross the metal organic framework compound that metallic ion coordination is formed.Metal organic framework compound in the present invention is different from other Second nonlinear optic metal organic framework compound, it utilizes the part of symmetrical structure to synthesize, with metal ion, the one obtained There is the metal organic framework compound of non-core structure.Its Nonlinear Second order Optical Properties is 0.8 times of carbamide, also has phase place Coupling.The most also there is fluorescent emission character and magnetic property.Its fluorescence emission peak is at 416 nm, compared with part, occurs Red shift.When 28 K, lone pair electrons are transformed into antiferromagnetic coupling.
Accompanying drawing explanation
Fig. 1 is the schematic arrangement of metal organic framework compound.
Fig. 2 is thermogravimetric curve schematic diagram.
Fig. 3 is fluorescence emission spectrum schematic diagram.
Fig. 4 is Nonlinear Second order Optical Properties schematic diagram.
Fig. 5 a under 1000 Oe magnetic field conditions, χM -1-T schemes.
Fig. 5 b under 1000 Oe magnetic field conditions, χM-T and χMT-T schemes.
Wherein, in Fig. 3, L is 5-sodium sulfo isophthalate, and 1 is metal organic framework compound.
Detailed description of the invention
Embodiment 1
By 0.263 g NiSO4·6H2O (1mmol), 0.156 g 4,4 '-bipyridyl (1mmol), 0.268 g isophthalic two Formic acid-5-sodium sulfonate (1mmol) is dissolved in 20mL water, stirs 2 h, then, is encapsulated in the reactor of 25mL, 120 ° of C heating 36 h, being cooled to room temperature has blue colored crystal to generate, and productivity is about 75%.
Conclusion: learnt by accompanying drawing 1, coordination compound 1 is novel coordination compound；Being learnt by accompanying drawing 2, coordination compound 1 is at 200 DEG C of bars Only dry out under part, and overall structure is not subsided；Being learnt by accompanying drawing 3, the fluorescence emission peak of coordination compound 1 is sent out relative to part Raw red shift；Being learnt by accompanying drawing 4, coordination compound 1 has Nonlinear Second order Optical Properties；Being learnt by accompanying drawing 5, coordination compound 1 has anti-ferrum Magnetic coupling.
Embodiment 2
By the NiSO of 0.395g4·6H2O, 0.234g4,4 '-bipyridyl, 0.402g 5-sodium sulfo isophthalate be dissolved in 20mL In water.Stirring 2 h, then, be encapsulated in the reactor of 25mL, 120 ° of C heat 36 h.Being cooled to room temperature has blue colored crystal raw Becoming, productivity is about 75-84%.
Embodiment 3
By 0.329gNiSO4·6H2The 4,4 ' of O, 0.195g-bipyridyl, 0.335g 5-sodium sulfo isophthalate are dissolved in 20mL In water.Stirring 2 h, then, be encapsulated in the reactor of 25 mL, 120 ° of C heat 36 h.Being cooled to room temperature has blue colored crystal raw Becoming, productivity is about 75-84%.
Embodiment 4
By 0.263gNiSO4·6H2O, 0.234g 4,4 '-bipyridyl, 0.268g 5-sodium sulfo isophthalate are dissolved in 20 mL In water.Stirring 2 h, then, be encapsulated in the reactor of 25mL, 120 ° of C heat 36 h.Being cooled to room temperature has blue colored crystal raw Becoming, productivity is about 75-84%.

Claims (2)

1. the preparation method of a second-order non-linear optical crystal material, it is characterised in that comprise the steps: 1-1.5mmol NiSO4·6H2The 4,4 ' of O, 1-1.5mmol-bipyridyl, 1-1.5mmol 5-sodium sulfo isophthalate soluble in water； Stirring 2 h, then, be encapsulated in the reactor of 25mL, 120 ° of C heat 36 h；Being cooled to room temperature has blue colored crystal to generate.
The preparation method of a kind of second-order non-linear optical crystal material the most according to claim 1, it is characterised in that described NiSO4·6H2O with water quality volume ratio is, 0.263-0.395 gNiSO4·6H2O is dissolved in 20mL water.
CN201610807281.0A 2016-09-07 2016-09-07 A kind of preparation method of second-order non-linear optical crystal material Active CN106192011B (en)

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CN112961532A (en) * 2021-02-08 2021-06-15 米格（浙江）创新科技有限公司 Ultra-wide wave amplitude infrared heat-insulating coating
CN115611801A (en) * 2022-09-16 2023-01-17 中南大学 Second-order nonlinear optical material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112961532A (en) * 2021-02-08 2021-06-15 米格（浙江）创新科技有限公司 Ultra-wide wave amplitude infrared heat-insulating coating
CN112961532B (en) * 2021-02-08 2022-07-05 米格（浙江）创新科技有限公司 Ultra-wide wave amplitude infrared heat-insulating coating
CN115611801A (en) * 2022-09-16 2023-01-17 中南大学 Second-order nonlinear optical material and preparation method thereof

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