CN105586639B - Second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] preparation method - Google Patents

Second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] preparation method Download PDF

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CN105586639B
CN105586639B CN201610112650.4A CN201610112650A CN105586639B CN 105586639 B CN105586639 B CN 105586639B CN 201610112650 A CN201610112650 A CN 201610112650A CN 105586639 B CN105586639 B CN 105586639B
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nmp
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CN105586639A (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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  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)

Abstract

The invention discloses a kind of second-order non-linear optical crystal material { [Tb (NMP) with frequency-doubled effect approximation potassium dihydrogen phosphate crystal7][WS4Ag3I4] preparation method.Hydrogen sulfide is passed into the ammonia spirit of wolframic acid and reacted, through filtering, dry obtained tetrathio ammonium tungstate；Silver iodide and tetrathio ammonium tungstate add the pyrrolidinone solvent obtained solution of N methyl 2；It will be stirred in solution made from the addition of six nitric hydrate terbiums, the { [Tb (NMP) containing second-order non-linear optical crystal material be made7][WS4Ag3I4] solution, after filtering, precipitating reagent is added, by crystallizing, filtering, washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}.Advantages of the present invention is：Obtain a kind of crystalline material { [Tb (NMP) for possessing excellent second-order nonlinear optical property7][WS4Ag3I4]}。

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, and in particular to a kind of frequency-doubled effect (SHG) is approximate Hybrid inorganic-organic the second-order non-linear optical crystal material { [Tb (NMP) of potassium dihydrogen phosphate crystal7][WS4Ag3I4] system Preparation Method.
Two background technologies
1860s people start with high intensity monochromatic light source-laser come the optically nonlinearity of excitation material Can, then photoelectric effect, optical rectification effect, optically erasing and vibration, Self-focusing, two-photon absorption, frequency-doubled effect by Swash the nonlinear optical phenomenas such as Raman scattering, stimulated Brillouin scattering to be found therewith, developed using these effects non-thread Property optics has been widely used in optic communication, optical oomputing, optical information processing, optical storage and holography, Laser Processing, laser Many aspects such as medical treatment, laser printing, laser telecine, laser device, laser guidance, ranging and directed energy weapon.Nonlinear optical The development of material is learned always with strong nonlinear response, high nonlinear optical coefficients, good environmental stability and high-quality Material property is target, and is expanded extensively in Inorganic Nonlinear Optical Materials, organic molecule nonlinear optical material field And in-depth study.
Inorganic Nonlinear Optical Materials are generally more stable, and intensity is higher, and they have than organic material purity more High crystal form, it is most widely used nonlinear optical material.Such as document J.Am.Chem.Soc., 2011,133, 12422 and J.Am.Chem.Soc., 2012,134,14818 all report with the inorganic of outstanding second-order nonlinear optical property Material.Organic small molecule material has the advantages that larger nonlinear optical coefficients, easily processed into type.Such as document Cryst.Growth Des., 2015,15,946 and Cryst.Growth Des., 2015,15,5560 all report with outstanding The organic small molecule material of second-order nonlinear optical property.But Inorganic Nonlinear Optical Materials and organic non linear optical material are still In the presence of some it is very important the drawbacks of, such as Inorganic Nonlinear Optical Materials be difficult to synthesis processing；Organic non linear optical material Fusing point is low, heat endurance and the transparency are all poor etc..Therefore, in this context, organic-inorganic hybridization nonlinear optical is prepared Material is learned, gives full play to the advantage of two kinds of materials, turns into the hot subject of research.
Three content of the invention
It is an object of the invention to provide a kind of hybrid inorganic-organic second order of frequency-doubled effect approximation potassium dihydrogen phosphate crystal Non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] preparation method.
The crystalline material, it is characterised in that chemical formula is { [Tb (NMP)7][WS4Ag3I4], belong to rhombic system, it is empty Between group be Pca21, cell parameter isα=β=γ =90 °, Z=4.The crystalline material structure is as shown in figure 1, belong to anion and cation zero-dimension structural.Cation [Tb (NMP)7]3+ By seven NMP (METHYLPYRROLIDONE) and Tb3+Coordination forms, anion [WS4Ag3I4]3-For the miscellaneous double of cubane shape Metal W/S/Ag clusters.
Realize that the present invention comprises the following steps：
Hydrogen sulfide gas is passed into wolframic acid ammonia spirit and reacted by 1.1, through filtering, dries obtained tetrathio ammonium tungstate；
Obtained tetrathio ammonium tungstate in silver iodide and 1.1 is added to METHYLPYRROLIDONE by 1.2 to be stirred several minutes Obtained solution；
Six nitric hydrate terbiums are added in step 1.2 stirring in obtained solution by 1.3, to whole dissolvings, to be made and contains two Rank non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
1.4 added into step 1.3 in the obtained miscellaneous bimetallic W/S/Ag cluster compounds crystalline material solution of cubane shape it is heavy Shallow lake agent, by crystallizing, filtering, washing, 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 { [Tb of frequency-doubled effect approximation potassium dihydrogen phosphate crystal (NMP)7][WS4Ag3I4] preparation method in, the mol ratio of tetrathio ammonium tungstate, silver iodide and six nitric hydrate terbiums is 1:1 ~2:0.5~1.
Compared with prior art, its remarkable advantage is the present invention：(1) synthetic route is simple, process conditions are gentle, easily control System；(2) raw material of synthesis is easy to get；(3) products collection efficiency obtained is higher；(4) second-order nonlinear optical property of material is preferable； (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 potassium dihydrogen phosphate of approx. dimension The second harmonic response signal contrast figure of crystal.
The second-order non-linear optical crystal material { [Tb (NMP) of 20-26 μ m in size ranks prepared by the present invention7] [WS4Ag3I4] and potassium dihydrogen phosphate crystal, under 400mV voltages, there is similar second harmonic response signal.
Fig. 3：Prepared second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] powder X-ray spread out Penetrate spectrogram.
Second-order non-linear optical crystal material { [Tb (NMP) prepared by the present invention7][WS4Ag3I4] powder X-ray Diffraction Diffraction pattern is substantially consistent with the X-ray diffraction pattern of theoretical calculation, illustrates the second nonlinear prepared by the present invention Optical crystal material { [Tb (NMP)7][WS4Ag3I4] there is very high purity.
Five embodiments
Embodiment 1：Second-order non-linear optical crystal material { [Tb (NMP) of the present invention7][WS4Ag3I4] preparation method, Comprise the following steps：
The first step, wolframic acid is added in ammonia spirit and stirred, the ammonia spirit of wolframic acid is made；
Second step, hydrogen sulfide is passed into the first step in obtained wolframic acid ammonia spirit and reacted, through filtering, dry be made Compound tetrathio ammonium tungstate；
It is molten that 3rd step, 0.2mmol silver iodide and 0.1mmol tetrathios ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEs Agent, stir 20 minutes, orange settled solution is made；
4th step, weigh the nitric hydrate terbiums of 0.1mmol six and be added in the 3rd step in obtained solution and stir 30 minutes, make Orange it must contain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
5th step, ethanol is added in obtained filtrate into the 4th step, orange bulk crystals are obtained by crystallization, filter, Washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property is tested：The second-order non-linear optical crystal material { [Tb (NMP) of preparation7] [WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out the sample of 20-26 μm of size, exist respectively The power of their second harmonic response signal is determined under 400mV.
Embodiment 2：Second-order non-linear optical crystal material { [Tb (NMP) of the present invention7][WS4Ag3I4] preparation method, Comprise the following steps：
The first step, wolframic acid is added in ammonia spirit and stirred, the ammonia spirit of wolframic acid is made；
Second step, hydrogen sulfide is passed into the first step in obtained wolframic acid ammonia spirit and reacted, through filtering, dry be made Compound tetrathio ammonium tungstate；
It is molten that 3rd step, 0.1mmol silver iodide and 0.1mmol tetrathios ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEs In agent, stir 20 minutes, orange-yellow settled solution is made；
4th step, weigh the nitric hydrate terbiums of 0.1mmol six and be added in the 3rd step in obtained solution and stir 30 minutes, make Orange-yellow it must contain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
5th step, ethanol is added in obtained filtrate into the 4th step, orange bulk crystals are obtained by crystallization, filter, Washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property is tested：The second-order non-linear optical crystal material { [Tb (NMP) of preparation7] [WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out the sample of 20-26 μm of size, exist respectively The power of their second harmonic response signal is determined under 400mV.
Embodiment 3：Second-order non-linear optical crystal material { [Tb (NMP) of the present invention7][WS4Ag3I4] preparation method, Comprise the following steps：
The first step, wolframic acid is added in ammonia spirit and stirred, the ammonia spirit of wolframic acid is made；
Second step, hydrogen sulfide is passed into the first step in obtained wolframic acid ammonia spirit and reacted, through filtering, dry be made Compound tetrathio ammonium tungstate；
It is molten that 3rd step, 0.2mmol silver iodide and 0.1mmol tetrathios ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEs In liquid, stir 20 minutes, orange settled solution is made；
4th step, weigh the nitric hydrate terbiums of 0.05mmol six and be added in the 3rd step in obtained solution and stir 30 minutes, It is made orange and contains second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
5th step, ethanol is added in obtained filtrate into the 4th step, orange bulk crystals are obtained by crystallization, filter, Washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property is tested：The second-order non-linear optical crystal material { [Tb (NMP) of preparation7] [WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out the sample of 20-26 μm of size, exist respectively The power of their second harmonic response signal is determined under 400mV.
Embodiment 4：Second-order non-linear optical crystal material { [Tb (NMP) of the present invention7][WS4Ag3I4] preparation method, Comprise the following steps：
The first step, wolframic acid is added in ammonia spirit and stirred, the ammonia spirit of wolframic acid is made；
Second step, hydrogen sulfide is passed into the first step in obtained wolframic acid ammonia spirit and reacted, through filtering, dry be made Compound tetrathio ammonium tungstate；
It is molten that 3rd step, 0.1mmol silver iodide and 0.1mmol tetrathios ammonium tungstate add 3 milliliters of METHYLPYRROLIDONEs In liquid, stir 20 minutes, orange-yellow settled solution is made；
4th step, weigh the nitric hydrate terbiums of 0.05mmol six and be added in the 3rd step in obtained solution and stir 30 minutes, It is made orange-yellow and contains second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
5th step, ethanol is added in obtained filtrate into the 4th step, orange bulk crystals are obtained by crystallization, filter, Washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4]}。
Second-order nonlinear optical property is tested：The second-order non-linear optical crystal material { [Tb (NMP) of preparation7] [WS4Ag3I4] (15 milligrams) and potassium dihydrogen phosphate standard crystal grind and filter out the sample of 20-26 μm of size, exist respectively The power of their second harmonic response signal is determined under 400mV.

Claims (3)

1. the second-order non-linear optical crystal material { [Tb (NMP) with the approximate potassium dihydrogen phosphate crystal of frequency-doubled effect (SHG)7] [WS4Ag3I4] preparation method, comprise the following steps：
Hydrogen sulfide gas is passed into wolframic acid ammonia spirit and reacted by 1.1, through filtering, dries obtained tetrathio ammonium tungstate；
Obtained tetrathio ammonium tungstate in silver iodide and 1.1 is added to METHYLPYRROLIDONE by 1.2 to be stirred and is made for several minutes Solution；
Six nitric hydrate terbiums are added in step 1.2 stirring in obtained solution by 1.3, to whole dissolvings, to be made and contains second order non-linear Property optical crystal material { [Tb (NMP)7][WS4Ag3I4] solution and filtering；
1.4 add precipitating reagent into step 1.3 in the obtained thio metal cluster compound functional material solution of cubane shape, by knot Brilliant, filtering, washing, drying to obtain second-order non-linear optical crystal material { [Tb (NMP)7][WS4Ag3I4], wherein tetrathio Ammonium tungstate, silver iodide, the mol ratio of six nitric hydrate terbiums are 1:1~2:0.5~2.
2. the second-order non-linear optical crystal material according to claim 1 with frequency-doubled effect approximation potassium dihydrogen phosphate crystal Expect { [Tb (NMP)7][WS4Ag3I4] preparation method in, it is characterised in that precipitating reagent include alcohols solvent, acetonitrile, acetone and Ether.
3. the second-order non-linear optical crystal material according to claim 2 with frequency-doubled effect approximation potassium dihydrogen phosphate crystal Expect { [Tb (NMP)7][WS4Ag3I4] preparation method in, it is characterised in that alcohols solvent include methanol, ethanol, propyl alcohol, fourth Alcohol, isopropanol.
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