CN105350081A - Preparation method and use of potassium lithium sulfate nonlinear optical crystal - Google Patents

Preparation method and use of potassium lithium sulfate nonlinear optical crystal Download PDF

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Publication number
CN105350081A
CN105350081A CN201510781647.7A CN201510781647A CN105350081A CN 105350081 A CN105350081 A CN 105350081A CN 201510781647 A CN201510781647 A CN 201510781647A CN 105350081 A CN105350081 A CN 105350081A
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crystal
lithium
solution
potassium
nonlinear optical
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潘世烈
韩国鹏
王颖
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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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

Abstract

The invention relates to a preparation method and use of a potassium lithium sulfate nonlinear optical crystal. The potassium lithium sulfate nonlinear optical crystal is prepared by a room temperature solution method, has a molecular formula of LiKSO4 and molecular weight of 142.1, belongs to a hexagonal system, and has a space group P63 and cell parameters of a=b=5.1453(2)A, c=8.6342(7)A and V=197.65A<3>. The crystal has nonlinear optical effects about 1 time that of KDP(KH2PO4), optical band gap width of 6.53eV, UV cutoff edge of 190nm and high visible light near infrared wave band transmittance. The preparation method has simple processes, a low cost and less pollution, utilizes low toxicity raw materials and has a short production period. The large-size potassium lithium sulfate nonlinear optical crystal does not air-slake in air, has stable physicochemical performances, can be cut and polished easily, can produce large-size and high-quality transparent potassium lithium sulfate nonlinear optical crystal and is suitable for preparation of a nonlinear optical device.

Description

The Preparation method and use of lithium potassium sulfate non-linear optic crystal
Technical field
The present invention relates to a kind of preparation method and purposes of large size lithium potassium sulfate non-linear optic crystal, the method adopts aqua-solution method to prepare crystal, utilizes lithium potassium sulfate non-linear optic crystal to make device for non-linear optical.
Background technology
Nonlinear optics specializes in the optical branching of strong relevant light-matter interaction mechanism, phenomenon and application.Strong coherent light is the same with the interaction of material and the interactional physical essence of traditional low light level and material, can be interpreted as that light wave electric field causes the polarization process of medium, the just difference of degree of polarization, the low light level can only make medium linear polarization, and light laser then can cause the nonlinear polarization of medium.This series of phenomenons caused by nonlinear polarization are called " non-linear optical effect ".When laser is when having the Propagation of non-zero second order susceptibility, the non-linear optical effect such as frequency multiplication and frequency, difference frequency, optically erasing can be produced.
The main task of information photonics carries out transmission and the process of signal, in the ground zero stage, because transmission information amount is limited, thus all belong to small-signal transmission, transmission between carrier wave also all meets the independent propagation principle of light wave, just can well explain by linear optics.But thereupon social, scientific and technological development, the quantity of information of system transfers constantly increases, and the energy density of transmission is very high, and the independent propagation principle of light does not re-use, so nonlinear optics receives publicity.
Laser is large as a kind of intensity, brightness is high, the coherent monochromatic source of good directionality, is widely used in the association areas such as scientific research, traffic, national defence and health care.But due to the restriction of material, technology etc., the laser wavelength that current all kinds of laser apparatus directly export is limited has remained the blank wave band of laser.Due to the singularity of laser genesis mechanism, the laser medium searching out a kind of practicality for each wavelength is more difficult.So utilize non-linear optic crystal to carry out frequency inverted to obtain LASER Light Source one of advanced subject becoming Development of Laser Technology of broad tuning.
Non-linear optical crystal material has been deep into the every field of laser technology, has now become the requisite crystalline materials of technology such as the memory of laser frequency, Electro-optical Modulation and photorefractive crystal and storage.Begin from the seventies and eighties in 20th century, China is in the leading level in the world in the research of mineral crystal, achieves a lot of great scientific payoffs in crystal technique.Current widely used nonlinear optical material has: KDP (KH 2pO 4), BBO (β-BaB 2o 4), LBO (LiB 3o 5) etc.Although the growing technology of these crystal reaches its maturity, there is deliquescence as easy in crystal, growth cycle is long, and raw materials used toxicity is large, and layer growth habit seriously waits not enough and defect.Therefore the work that the novel non-linear optic crystal being more suitable for industrialization is still a forward position emphasis is found.
Although LiKSO 4compound had been reported (G.PasupathiandP.Philomnathan in 2012, " Growth, structural, opticalandhardnessstudiesoflithiumpotassiumsulphatesingl ecrystals – aninorganicNLOmaterial, " JournalofMineralsandMaterialsCharacterizationandEngineer ing, vol.11, pp.904-907, 2012.), but not yet prepare large size, high quality, the lithium potassium sulfate non-linear optic crystal of regular appearance, more cannot commercially buy this non-linear optic crystal, in addition, also not about LiKSO 4monocrystalline is used for the report of device for non-linear optical.
Summary of the invention
The object of the invention is the preparation method and the purposes that provide a kind of lithium potassium sulfate non-linear optic crystal, and adopt solution at room temperature legal system for lithium potassium sulfate non-linear optic crystal, the molecular formula of this crystal is LiKSO 4, molecular weight is 142.1, belongs to hexagonal system, and spacer is P6 3, unit cell parameters is: the non-linear optical effect of this crystal is about 1 times of KDP (KH 2pO 4), optical band gap width is 6.53eV, and ultraviolet is 190nm by limit, has higher transmitance, the method is easy and simple to handle, cost is low, pollutes less, raw materials used toxicity is low, growth cycle is short to visible ray and near-infrared band; The large size lithium potassium sulfate non-linear optic crystal obtained by method of the present invention, deliquescence, physical and chemical performance are not stablized, are easy to cutting and polishing in atmosphere, and large size, high-quality transparent lithium potassium sulfate non-linear optic crystal can be grown, be applicable to making device for non-linear optical.
The preparation method of a kind of lithium potassium sulfate non-linear optic crystal of the present invention, the molecular formula of this crystal is LiKSO 4, molecular weight is 142.1, belongs to hexagonal system, and spacer is P6 3, unit cell parameters is: adopt solution at room temperature method growing crystal, concrete operations follow these steps to carry out:
A, will be Lithium Sulphate or sulfuric acid monohydrate lithium containing lithium sulfide, containing potassium sulfide be lithium in potassium sulfate or sulfuric acid monohydrate potassium, potassium, sulphur in molar ratio 1:1:1 take and put into the container of wash clean, add the deionized water of 20-40ml, ultrasonication is about 10-60 minute, makes its abundant mixed dissolution;
B, by the container pan paper in step a or preservative film sealing, and with the some apertures of pinprick, at room temperature standing 15-30 days;
C, the solution treated in step b grow crystal grain at container bottom, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: will be Lithium Sulphate or sulfuric acid monohydrate lithium containing lithium sulfide, containing potassium sulfide be lithium in potassium sulfate or sulfuric acid monohydrate potassium, potassium, sulphur in molar ratio 1:1:1 take and be mixed with saturated aqueous solution, 10-60 minute is about by ultrasonication, to ensure that it fully dissolves, then with qualitative filter paper by the contaminant filter in solution, to ensure an only having nucleation centre in solution;
The good seed crystal of quality obtained in e, selection step c, hangs in the solution of steps d configuration by seed crystal, growth 30-60 days, can obtain the transparent LiKSO of centimetre-sized 4non-linear optic crystal.
Container in step b is placed on without rocking, pollution-free, without in cross-ventilated static environment, by the some apertures of sealing bundle in order to regulate evaporation of water speed in the aqueous solution.
The purposes of the lithium potassium sulfate non-linear optic crystal that described method obtains in preparation times frequency generator, upper frequency transmodulator, lower frequency transmodulator or optical parametric oscillator.
The lithium potassium sulfate non-linear optic crystal obtained by the method for the invention, put into mortar grinding and carry out X-ray analysis to it, gained X-ray spectrogram is consistent with theoretical value.The lithium potassium sulfate non-linear optic crystal quality grown by the method is good, size large, regular appearance.
Prepare the chemical equation of lithium potassium sulfate:
(1)Li 2SO 4·H 2O+K 2SO 4→LiKSO 4+H 2O
(2)Li 2SO 4·H 2O+K 2SO 4·H 2O→LiKSO 4+H 2O
(3)Li 2SO 4+K 2SO 4·H 2O→LiKSO 4+H 2O
(4)Li 2SO 4+K 2SO 4→LiKSO 4
Large size lithium potassium sulfate non-linear optic crystal prepared by the present invention can be used as prepares device for non-linear optical crystalline material, comprises and makes times frequency generator, upper or lower frequency transmodulator and optical parametric oscillator.Described comprising with the device for non-linear optical that lithium potassium sulfate non-linear optic crystal makes produces through at least a branch of incident fundamental frequency light the coherent light that at least a branch of frequency is different from incident light.
Reagent used in the present invention and raw material little to human toxicity, growth cycle is short, easily obtains the advantage such as high quality, large-size crystals.
Lithium potassium sulfate non-linear optic crystal provided by the present invention to working accuracy without particular requirement.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of lithium potassium sulfate crystal of the present invention;
Fig. 2 is crystallogram figure of the present invention;
Fig. 3 is the fundamental diagram of the device for non-linear optical that the present invention makes, be laser apparatus comprising (1), (2) be convex lens, (3) be lithium potassium sulfate non-linear optic crystal, (4) be beam splitting prism, (5) be filter plate, ω is 2 times that the frequency of refracted light equals incident light frequency or incident light frequency.
Embodiment
Embodiment 1:
By chemical equation: Li 2sO 4h 2o+K 2sO 4=LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal;
A, by Li 2sO 4h 2o, K 2sO 4in element lithium, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 20ml, then ultrasonication about 10 minutes, makes its abundant mixed dissolution;
B, the Erlenmeyer flask pan paper that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked several apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 15 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4h 2o, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 10 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, and hung in the solution of steps d configuration, at room temperature constant temperature grows high quality, the transparent LiKSO of large size that within 30 days, can obtain centimetre-sized 4non-linear optic crystal.
Embodiment 2:
By chemical equation: Li 2sO 4h 2o+K 2sO 4=LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal;
A, by Li 2sO 4h 2o, K 2sO 4in element lithium, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 25ml, then ultrasonication 20 minutes, make its abundant mixed dissolution;
B, the Erlenmeyer flask pan paper that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked several apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 20 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, obtain seed crystal;
D, reconfigure solution: by Li 2sO 4h 2o, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 20 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, and hung in the solution of steps d configuration, at room temperature constant temperature 40 days, can obtain the high quality of centimetre-sized, the transparent LiKSO of large size 4non-linear optic crystal.
Embodiment 3:
By chemical equation: Li 2sO 4h 2o+K 2sO 4=LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal;
A, by Li 2sO 4h 2o, K 2sO 4in element lithium, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 30ml, then ultrasonication 30 minutes, make its abundant mixed dissolution;
B, the Erlenmeyer flask preservative film that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked some apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 30 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4h 2o, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 30 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
Select the good crystal of quality as seed crystal in e, selection step c, seed crystal is hung in the solution of steps d configuration, grow 50 days, the transparent LiKSO of centimetre-sized can be obtained 4non-linear optic crystal.
Embodiment 4:
By chemical equation: Li 2sO 4h 2o+K 2sO 4=LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal;
A, by Li 2sO 4h 2o, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 40ml, then ultrasonication 60 minutes, make its abundant mixed dissolution;
B, the Erlenmeyer flask preservative film that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked some apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 15 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4h 2o, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 60 minutes, to ensure that it fully dissolves.Then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, is hung on by seed crystal in the solution of steps d configuration, grows 60 days, can obtain the transparent LiKSO of centimetre-sized 4non-linear optic crystal.
Embodiment 5:
By reaction formula Li 2sO 4h 2o+K 2sO 4h 2o → LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal:
A, by Li 2sO 4h 2o, K 2sO 4h 2lithium in O, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 35ml, then ultrasonication about 40 minutes, makes its abundant mixed dissolution;
B, the Erlenmeyer flask preservative film that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked some apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 20 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4h 2o, K 2sO 4h 2lithium in O, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 40 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, is hung on by seed crystal in the solution of steps d configuration, grows 60 days, can obtain the transparent LiKSO of centimetre-sized 4non-linear optic crystal.
Embodiment 6:
By reaction formula: Li 2sO 4+ K 2sO 4h 2o → LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal:
A, by Li 2sO 4, K 2sO 4h 2lithium in O, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 40ml, then ultrasonication about 50 minutes, makes its abundant mixed dissolution;
B, the Erlenmeyer flask preservative film that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked some apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 30 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4, K 2sO 4h 2lithium in O, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication about 40 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, is hung on by seed crystal in the solution of steps d configuration, grows 60 days, can obtain the high quality of centimetre-sized, the transparent LiKSO of large size 4non-linear optic crystal.
Embodiment 7:
By reaction formula: Li 2sO 4+ K 2sO 4→ LiKSO 4+ H 2o synthesizes large size lithium potassium sulfate non-linear optic crystal:
A, by Li 2sO 4, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and put into wash clean Erlenmeyer flask (Erlenmeyer flask must first with acid Erlenmeyer flask is cleaned up, use deionized water rinse again), add the deionized water of 35ml, then ultrasonication 30 minutes, make its abundant mixed dissolution;
B, the Erlenmeyer flask preservative film that solution is housed in step a to be sealed, is placed on without rocking, pollution-free, without in cross-ventilated static environment, sealing is pricked some apertures in order to regulate evaporation of water speed in the aqueous solution, at room temperature standing 40 days;
C, the solution treated in step b grow crystal grain bottom Erlenmeyer flask, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: by Li 2sO 4, K 2sO 4in lithium, potassium, sulphur in molar ratio 1:1:1 take and prepare saturated aqueous solution, by ultrasonication 55 minutes, to ensure that it fully dissolves, then with qualitative filter paper by other contaminant filters in crystal grain and solution, to ensure an only having nucleation centre in solution;
In e, selection step c, the good crystal of quality is as seed crystal, is hung on by seed crystal in the solution of steps d configuration, grows 55 days, can obtain the high quality of centimetre-sized, the transparent LiKSO of large size 4non-linear optic crystal.
Embodiment 8:
By the LiKSO4 crystal of gained in embodiment 1-7, be placed on the position of 3 by shown in accompanying drawing 3, at room temperature, export with adjusting the 1064nm of QNd:YAG laser apparatus and make light source, observe obvious 532nm frequency doubling green light to export, output intensity is about 1 times of equal conditions KDP.
Figure 3 shows that, sending wavelength by adjusting QNd:YAG laser apparatus 1 is that the infrared beam of 1064nm injects lithium potassium sulfate non-linear optic crystal through convex lens 2, produce the green frequency doubled light that wavelength is 532nm, outgoing beam 4 is the infrared light of 1064nm and the green glow of 532nm containing wavelength, after filter plate 5 elimination, obtain the frequency doubled light that wavelength is 532nm.

Claims (3)

1. a preparation method for lithium potassium sulfate non-linear optic crystal, is characterized in that the molecular formula of this crystal is LiKSO 4, molecular weight is 142.1, belongs to hexagonal system, and spacer is p6 3, unit cell parameters is: a= b=5.1453 (2), c=8.6342 (7), v=197.65 3, adopt solution at room temperature method growing crystal, concrete operations follow these steps to carry out:
A, will be Lithium Sulphate or sulfuric acid monohydrate lithium containing lithium sulfide, containing potassium sulfide be lithium in potassium sulfate or sulfuric acid monohydrate potassium, potassium, sulphur in molar ratio 1:1:1 take and put into the container of wash clean, add the deionized water of 20-40ml, ultrasonication is about 10-60 minute, makes its abundant mixed dissolution;
B, by the container pan paper in step a or preservative film sealing, and with the some apertures of pinprick, at room temperature standing 15-30 days;
C, the solution treated in step b grow crystal grain at container bottom, until the no longer considerable change of crystal grain size, growth terminates, and obtains seed crystal;
D, reconfigure solution: will be Lithium Sulphate or sulfuric acid monohydrate lithium containing lithium sulfide, containing potassium sulfide be lithium in potassium sulfate or sulfuric acid monohydrate potassium, potassium, sulphur in molar ratio 1:1:1 take and be mixed with saturated aqueous solution, 10-60 minute is about by ultrasonication, to ensure that it fully dissolves, then with qualitative filter paper by the contaminant filter in solution, to ensure an only having nucleation centre in solution;
The good seed crystal of quality obtained in e, selection step c, hangs in the solution of steps d configuration by seed crystal, growth 30-60 days, can obtain the transparent LiKSO of centimetre-sized 4non-linear optic crystal.
2. the preparation method of lithium potassium sulfate non-linear optic crystal according to claim 1, the container that it is characterized in that in step b is placed on without rocking, pollution-free, without in cross-ventilated static environment, by the some apertures of sealing bundle in order to regulate evaporation of water speed in the aqueous solution.
3. the purposes in times frequency generator, upper frequency transmodulator, lower frequency transmodulator or optical parametric oscillator prepared by the lithium potassium sulfate non-linear optic crystal that method obtains as claimed in claim 1.
CN201510781647.7A 2015-11-14 2015-11-14 Preparation method and use of potassium lithium sulfate nonlinear optical crystal Pending CN105350081A (en)

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CN107761169A (en) * 2016-08-16 2018-03-06 中国科学院新疆理化技术研究所 The method for fast growing and purposes of lithium potassium sulfate nonlinear optical crystal
CN107761171A (en) * 2016-08-16 2018-03-06 中国科学院新疆理化技术研究所 Sulfuric acid monohydrate lithium nonlinear optical crystal and its production and use
CN108910920A (en) * 2018-09-20 2018-11-30 中国科学院福建物质结构研究所 Li9Na3Rb2(SO4)7Compound, nonlinear optical crystal and its preparation method and purposes
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CN109267151A (en) * 2018-11-14 2019-01-25 闽江学院 Three potassium sulfate zinc are preparing the application in device for non-linear optical
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CN107201547A (en) * 2016-03-18 2017-09-26 中国科学院新疆理化技术研究所 The Preparation method and use of lithium ammonium sulfate nonlinear optical crystal
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CN109160526A (en) * 2018-09-04 2019-01-08 中国科学院福建物质结构研究所 Li8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal and its preparation method and purposes
CN109160526B (en) * 2018-09-04 2020-06-26 中国科学院福建物质结构研究所 Li8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal, and preparation method and application thereof
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