CN105586639A - Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} - Google Patents

Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} Download PDF

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CN105586639A
CN105586639A CN201610112650.4A CN201610112650A CN105586639A CN 105586639 A CN105586639 A CN 105586639A CN 201610112650 A CN201610112650 A CN 201610112650A CN 105586639 A CN105586639 A CN 105586639A
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CN105586639B (en
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张金方
刘宇航
张弛
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Ganzhou Zhongneng Industrial Co ltd
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Jiangnan 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nonlinear Science (AREA)
  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
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  • Inorganic Chemistry (AREA)
  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)

Abstract

The invention discloses a preparation method of a second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} which has secondary harmonic generation and approximates potassium dihydrogen phosphate crystals. The preparation method comprises the following steps: introducing hydrogen sulfide into tungstic acid aqua ammonia to react, carrying out suction filtration, and drying to obtain an ammonium tetrathiotungstate; adding silver iodide and the ammonium tetrathiotungstate into a N-methyl-2-pyrrolidone solvent to obtain a solution; adding terbium nitrate hexahydrate into the prepared solution, stirring to obtain a solution containing the second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]}, filtering, adding a precipitant, crystallizing, filtering, washing and drying to obtain the second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]}. The method can be used for obtaining a crystal material {[Tb(NMP)7][WS4Ag3I4]} with excellent second-order nonlinear optical properties.

Description

Second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] preparation method
One technical field
The present invention relates to the preparation of second-order non-linear optical crystal material, be specifically related to a kind of frequency-doubled effect (SHG) and be similar toHybrid inorganic-organic the second-order non-linear optical crystal material { [Tb (NMP) of potassium dihydrogen phosphate crystal7][WS4Ag3I4]}Preparation method.
Two background technologies
1860s people start to come with high intensity monochromatic light source-laser the optically nonlinearity of excitation materialCan, then photoelectric effect, optical rectification effect, optical parameter amplification and vibration, Self-focusing, two-photon absorption, timesThe nonlinear optical phenomenas such as frequency effect stimulated Raman scattering, stimulated Brillouin scattering are found thereupon, utilize these effects to grindThe device for non-linear optical of making has been widely used in optic communication, photometry calculation, optical information processing, optical storage and holographyArt, Laser Processing, laser medicine, laser printing, laser telecine, laser device, laser guidance, range finding and orientationMany aspects such as energy weapon. The development of nonlinear optical material is always with strong nonlinear response, high nonlinear opticsCoefficient, good environmental stability and the material property of high-quality are target, and at Inorganic Nonlinear Optical Materials, organicExtensive and deep research has been launched in little molecular nonlinear optical materials field.
Inorganic Nonlinear Optical Materials is conventionally more stable, and intensity is higher, and they have than organic material purity moreHigh crystal form is the nonlinear optical material of extensive use. For example document J.Am.Chem.Soc., 2011,133,12422 and J.Am.Chem.Soc., 2012,134,14818 have all reported to have outstanding second-order nonlinear optical propertyInorganic material. Organic small molecule material has larger nonlinear optical coefficients, is easy to the advantages such as machine-shaping. For exampleDocument Cryst.GrowthDes., 2015,15,946 and Cryst.GrowthDes., 2015,15,5560 have all reported and have hadThe organic small molecule material of outstanding second-order nonlinear optical property. But Inorganic Nonlinear Optical Materials and organic non-linear lightLearn material and still have some very important drawbacks, for example Inorganic Nonlinear Optical Materials is difficult to synthetic processing; Organic non-Linear optical material fusing point is low, heat endurance and the transparency are all poor etc. Therefore, under this background, prepare organic-Inorganic hybridization nonlinear optical material, gives full play to the advantage of bi-material, becomes the hot subject of research.
Three summary of the invention
The object of the present invention is to provide the hybrid inorganic-organic second order of the approximate potassium dihydrogen phosphate crystal of a kind of frequency-doubled effectNon-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] preparation method.
Described crystalline material, is characterized in that, chemical formula is { [Tb (NMP)7][WS4Ag3I4], belong to rhombic system,Space group is Pca21, cell parameter isα=β=γ=90 °, Z=4. Described crystalline material structure as shown in Figure 1, belongs to anion and cation zero-dimension structural. SunIon [Tb (NMP)7]3+By seven NMP (METHYLPYRROLIDONE) and Tb3+Coordination forms, anion[WS4Ag3I4]3-For the assorted bimetallic W/S/Cu bunch of cubane shape.
Realization the present invention includes following steps:
1.1 are passed into hydrogen sulfide gas in wolframic acid ammonia spirit and react, through suction filtration, the dry tetrathio ammonium tungstate that makes;
The tetrathio ammonium tungstate making in silver iodide and 1.1 is joined organic solvent stirred for several minute by 1.2 makes solution;
1.3 join six nitric hydrate terbiums in the solution making in step 1.2 and are stirred to whole dissolvings, make and containSecond-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filter;
1.4 is heavy to adding in the assorted bimetallic W/S/Cu cluster compound crystalline material solution of the cubane shape making in step 1.3Shallow lake agent, passes through crystallization, filtration, washs, is drying to obtain second-order non-linear optical crystal material{[Tb(NMP)7][WS4Ag3I4]}。
The present invention has the second-order non-linear optical crystal material of the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect{[Tb(NMP)7][WS4Ag3I4] preparation method in, the rubbing of tetrathio ammonium tungstate, silver iodide and six nitric hydrate terbiumsYou are than being 1:1～2:0.5～1.
Compared with prior art, its remarkable advantage is in the present invention: (1) synthetic route is simple, process conditions are gentle, easyControl; (2) synthetic raw material is easy to get; (3) products collection efficiency obtaining is higher; (4) second nonlinear optic of materialCan be better; (5) chemistry of material, optical stability are good.
Four brief description of the drawings
Fig. 1: second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] zwitterion structure chart.
Fig. 2: second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] with the biphosphate of approx. dimensionThe second harmonic response signal contrast figure of potassium crystal.
The second-order non-linear optical crystal material of the prepared 20-26 μ m size class of the present invention{[Tb(NMP)7][WS4Ag3I4] and potassium dihydrogen phosphate crystal, under 400mV voltage, there is close secondary humorousWave response signal.
Fig. 3: prepared second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] powder X-rayDiffraction spectrogram.
The second-order non-linear optical crystal material { [Tb (NMP) that the present invention is prepared7][WS4Ag3I4] powder X-ray-penetrateLine diffraction diffraction pattern is substantially consistent with the theoretical X-ray diffraction pattern calculating, illustrate the present invention prepared twoRank non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] there is very high purity.
Five detailed description of the invention
Embodiment 1: second-order non-linear optical crystal material of the present invention { [Tb (NMP)7][WS4Ag3I4] preparation method,Comprise the following steps:
The first step, joins wolframic acid in ammonia spirit and stirs, and makes the ammonia spirit of wolframic acid;
Second step, is passed into hydrogen sulfide in the wolframic acid ammonia spirit making in the first step and reacts, through suction filtration, dry systemObtain compound tetrathio ammonium tungstate;
The 3rd step, 0.2mmol silver iodide and 0.1mmol tetrathio ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEsSolvent, stirs 20 minutes, makes orange settled solution;
The 4th step, takes 0.1mmol six nitric hydrate terbiums and joins in the solution making in the 3rd step and stir 30 minutes,Make orange the second-order non-linear optical crystal material { [Tb (NMP) that contains7][WS4Ag3I4] solution and filter;
The 5th step adds ethanol in the filtrate making in the 4th step, obtains orange bulk crystals through crystallization, filter,Wash, be drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property test: the second-order non-linear optical crystal material of preparation{[Tb(NMP)7][WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out 20-26 μ mThe sample of size is measured respectively the power of their second harmonic response signal under 400mV.
Embodiment 2: second-order non-linear optical crystal material of the present invention { [Tb (NMP)7][WS4Ag3I4] preparation method,Comprise the following steps:
The first step, joins wolframic acid in ammonia spirit and stirs, and makes the ammonia spirit of wolframic acid;
Second step, is passed into hydrogen sulfide in the wolframic acid ammonia spirit making in the first step and reacts, through suction filtration, dry systemObtain compound tetrathio ammonium tungstate;
The 3rd step, 0.1mmol silver iodide and 0.1mmol tetrathio ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEsIn solvent, stir 20 minutes, make orange-yellow settled solution;
The 4th step, takes 0.1mmol six nitric hydrate terbiums and joins in the solution making in the 3rd step and stir 30 minutes,Make orange-yellow the second-order non-linear optical crystal material { [Tb (NMP) that contains7][WS4Ag3I4] solution and filter;
The 5th step adds ethanol in the filtrate making in the 4th step, obtains orange bulk crystals through crystallization, filter,Wash, be drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property test: the second-order non-linear optical crystal material of preparation{[Tb(NMP)7][WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out 20-26 μ mThe sample of size is measured respectively the power of their second harmonic response signal under 400mV.
Embodiment 3: second-order non-linear optical crystal material of the present invention { [Tb (NMP)7][WS4Ag3I4] preparation method,Comprise the following steps:
The first step, joins wolframic acid in ammonia spirit and stirs, and makes the ammonia spirit of wolframic acid;
Second step, is passed into hydrogen sulfide in the wolframic acid ammonia spirit making in the first step and reacts, through suction filtration, dry systemObtain compound tetrathio ammonium tungstate;
The 3rd step, 0.2mmol silver iodide and 0.1mmol tetrathio ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEsIn solution, stir 20 minutes, make orange settled solution;
The 4th step, takes 0.05mmol six nitric hydrate terbiums and joins in the solution making in the 3rd step and stir 30 minutes,Make orange the second-order non-linear optical crystal material { [Tb (NMP) that contains7][WS4Ag3I4] solution and filter;
The 5th step adds ethanol in the filtrate making in the 4th step, obtains orange bulk crystals through crystallization, filter,Wash, be drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property test: the second-order non-linear optical crystal material of preparation{[Tb(NMP)7][WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out 20-26 μ mThe sample of size is measured respectively the power of their second harmonic response signal under 400mV.
Embodiment 4: second-order non-linear optical crystal material of the present invention { [Tb (NMP)7][WS4Ag3I4] preparation method,Comprise the following steps:
The first step, joins wolframic acid in ammonia spirit and stirs, and makes the ammonia spirit of wolframic acid;
Second step, is passed into hydrogen sulfide in the wolframic acid ammonia spirit making in the first step and reacts, through suction filtration, dry systemObtain compound tetrathio ammonium tungstate;
The 3rd step, 0.1mmol silver iodide and 0.1mmol tetrathio ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEsIn solution, stir 20 minutes, make orange-yellow settled solution;
The 4th step, takes 0.05mmol six nitric hydrate terbiums and joins in the solution making in the 3rd step and stir 30 minutes,Make orange-yellow the second-order non-linear optical crystal material { [Tb (NMP) that contains7][WS4Ag3I4] solution and filter;
The 5th step adds ethanol in the filtrate making in the 4th step, obtains orange bulk crystals through crystallization, filter,Wash, be drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property test: the second-order non-linear optical crystal material of preparation{[Tb(NMP)7][WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out 20-26 μ mThe sample of size is measured respectively the power of their second harmonic response signal under 400mV.

Claims (4)

1. there is the second-order non-linear optical crystal material of the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect (SHG){[Tb(NMP)7][WS4Ag3I4] preparation method, comprise the following steps:
1.1 are passed into hydrogen sulfide gas in wolframic acid ammonia spirit and react, through suction filtration, the dry tetrathio ammonium tungstate that makes;
The tetrathio ammonium tungstate making in silver iodide and 1.1 is joined organic solvent stirred for several minute by 1.2 makes solution;
1.3 join six nitric hydrate terbiums in the solution making in step 1.2 and are stirred to whole dissolvings, make containing second orderNon-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filter;
1.4 add precipitating reagent, warp in the cubane shape sulfo-metal cluster compound functional material solution making in step 1.3Cross crystallization, filtration, the { [Tb (NMP) that washs, is drying to obtain second-order non-linear optical crystal material7][WS4Ag3I4]}。
2. the second nonlinear optic crystalline substance with the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect according to claim 1Body material { [Tb (NMP)7][WS4Ag3I4] preparation method in, it is characterized in that rubbing of tetrathio ammonium tungstate and silver iodideYou are than being 1:1～2.
3. the second nonlinear optic crystalline substance with the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect according to claim 1Body material { [Tb (NMP)7][WS4Ag3I4] preparation method in, it is characterized in that precipitating reagent comprises alcohols solvent, acetonitrile,Acetone and ether.
4. the second nonlinear optic crystalline substance with the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect according to claim 3Body material { [Tb (NMP)7][WS4Ag3I4] preparation method in, it is characterized in that alcohols solvent comprise methyl alcohol, ethanol,Propyl alcohol, butanols, isopropyl alcohol.
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN108796613A (en) * 2018-06-29 2018-11-13 江南大学 A kind of preparation method and crystalline material of W/S/Cu clusters-metallic crystal material with third order non-linear optical property
CN108796614A (en) * 2018-06-29 2018-11-13 江南大学 A kind of preparation method and crystalline material of W/S/Cu clusters-metal framework crystalline material with light limitation capability
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 (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108796613A (en) * 2018-06-29 2018-11-13 江南大学 A kind of preparation method and crystalline material of W/S/Cu clusters-metallic crystal material with third order non-linear optical property
CN108796614A (en) * 2018-06-29 2018-11-13 江南大学 A kind of preparation method and crystalline material of W/S/Cu clusters-metal framework crystalline material with light limitation capability
CN108796613B (en) * 2018-06-29 2020-07-10 江南大学 Preparation method of W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance and crystal material
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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