CN107201547A - The Preparation method and use of lithium ammonium sulfate nonlinear optical crystal - Google Patents
The Preparation method and use of lithium ammonium sulfate nonlinear optical crystal Download PDFInfo
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- CN107201547A CN107201547A CN201610157180.3A CN201610157180A CN107201547A CN 107201547 A CN107201547 A CN 107201547A CN 201610157180 A CN201610157180 A CN 201610157180A CN 107201547 A CN107201547 A CN 107201547A
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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
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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
- 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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- G—PHYSICS
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- 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
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Abstract
The present invention relates to a kind of preparation method and purposes of lithium ammonium sulfate nonlinear optical crystal, lithium ammonium sulfate nonlinear optical crystal is prepared using solution at room temperature method, the molecular formula of the crystal is Li (NH4)SO4, molecular weight is 121.035, belongs to rhombic system, and space group isPna21, cell parameter is：a=8.753 (3),b=9.102(3)Å,c=5.2647 (16),V=419.4(2)Å3.The nonlinear optical effect of the crystal is about 0.6 times of KDP (KH2PO4), optical band gap width is 7.52eV, and ultraviolet cut-on side is 165nm, has higher transmitance to visible ray and near infrared band, and this method is easy to operate, cost is low, pollute less, raw materials used toxicity is low, growth cycle is short；The large scale lithium ammonium sulfate nonlinear optical crystal obtained by method of the present invention, deliquescence, physical and chemical performance be not stable in atmosphere, is easy to cutting and polishing, and large scale, high-quality transparent lithium ammonium sulfate nonlinear optical crystal can be grown, it is adapted to make device for non-linear optical.
Description
Technical field
The present invention relates to a kind of preparation method and purposes of large scale lithium ammonium sulfate nonlinear optical crystal, this method is using water-soluble
Liquid method prepares crystal, and device for non-linear optical is made using lithium ammonium sulfate nonlinear optical crystal.
Background technology
Nonlinear optics is to specialize in strong relevant light-matter interaction mechanism, phenomenon and the optical branching of application.Qiang Xiang
The physical essence of the interaction of dry light and material and the interaction of traditional dim light and material is the same, be can be understood as
Light wave electric field causes the polarization process of medium, simply the difference of degree of polarization, and dim light can only make medium linear polarization, and swash by force
Light can then cause the nonlinear polarization of medium.A series of this phenomenons as caused by nonlinear polarization are referred to as " nonlinear optical
Learn effect ".When laser is in the Propagation with non-zero second order susceptibility, frequency multiplication and frequency, difference frequency, light can be produced
The nonlinear optical effects such as parameter amplification.
The main task of information photonics is to carry out the transmission and processing of signal, the ground zero stage, due to transmission information content
It is limited, thus the transmission belonged between small-signal transmission, carrier wave also all meets the independent propagation principle of light wave, uses linear light
Just can be very good to explain.But therewith society, science and technology continue to develop, system transmission information content be continuously increased, pass
Defeated energy density is very high, and the independent propagation principle of light is not used, and then nonlinear optics attracts attention.
Laser as a kind of intensity is big, brightness is high, good directionality coherent monochromatic source, be widely used in scientific research, traffic,
The association area such as national defence and health care.However, due to the limitation of material, technology etc., current all kinds of lasers are directly defeated
The laser wavelength that goes out is limited to have remained laser blank wave band.It is that each wavelength is sought due to the particularity of laser genesis mechanism
Find a kind of practical laser medium relatively difficult.So carrying out frequency conversion to obtain broad tuning using nonlinear optical crystal
LASER Light Source one of advanced subject as Development of Laser Technology.
Non-linear optical crystal material has been deep into the every field of laser technology, as laser frequency, Electro-optical Modulation and
The essential crystalline material of technology such as photorefractive crystal memory and storage.Begin from the seventies and eighties in 20th century, China is inorganic
The leading level in the world is in the research of crystal, many great scientific achievements are achieved in terms of crystal technique.At present should
Have with relatively broad nonlinear optical material：KDP(KH2PO4)、BBO(β-BaB2O4)、LBO(LiB3O5) etc..Although these
The growing technology of crystal has reached its maturity, but there is such as easy deliquescence of crystal, and growth cycle is long, and raw materials used toxicity is big, stratiform
Habit seriously waits not enough and defect.Therefore find that to be more suitable for the new nonlinear optical crystal of industrialization be still before one
Along the work of emphasis.
The content of the invention
Present invention aims at there is provided a kind of preparation method and purposes of lithium ammonium sulfate nonlinear optical crystal.Point of the crystal
Minor is Li (NH4)SO4, molecular weight is 121.035, belongs to rhombic system, and space group is Pna21, cell parameter is： The crystal it is non-linear
Optical effect is about 0.6 times of KDP (KH2PO4), optical band gap width is 7.52eV, and ultraviolet cut-on side is 165nm, to visible
Light and near infrared band have higher transmitance.Method of the present invention is easy to operate, cost is low, pollute less, it is used
Material toxicity is low, growth cycle is short；The large scale lithium ammonium sulfate nonlinear optical crystal obtained by this method, in atmosphere
Deliquescence, physical and chemical performance be not stable, is easy to cutting and polishing, and can grow large scale, high-quality transparent lithium sulfate
Ammonium nonlinear optical crystal, is adapted to make device for non-linear optical.
A kind of preparation method of lithium ammonium sulfate nonlinear optical crystal of the present invention, crystal is grown using solution at room temperature method,
Concrete operations follow these steps to carry out：
A, lithium sulfide will be contained for lithium sulfate or sulfuric acid monohydrate lithium, during sulfide containing ammonium is ammonium sulfate or sulfuric acid monohydrate ammonium
Lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into the container of wash clean, adds 20-40ml deionized water, ultrasound
Ripple is handled about 10-60 minutes, it is sufficiently mixed dissolving；
B, the container pan paper in step a or preservative film sealed, and some apertures are pricked on pan paper or preservative film,
Stand 15-30 days at room temperature；
C, treat that the solution in step b grows crystal grain in container bottom, until the no longer significant change of crystal grain size, raw
Length terminates, and obtains seed crystal；
D, reconfigure solution：Lithium sulfide will be contained for lithium sulfate or sulfuric acid monohydrate lithium, sulfide containing ammonium is ammonium sulfate or one
Lithium, ammonium, sulphur in hydrated sulfuric acid ammonium in molar ratio 1:1:1 weighs gross weight 24-96g, adds 100-400ml deionization
Water is configured to the aqueous solution, and with ultrasonication about 10-60 minutes, then fully dissolving stood, treat its bottom at room temperature
When having a small amount of crystal precipitation, solution is filtered with qualitative filter paper, saturated solution is obtained；
It is raw in the preferable seed crystal of quality obtained in e, selection step c, the saturated solution that seed crystal is hung on to step d configurations
It is long 30-60 days, that is, obtain the transparent Li (NH of Centimeter Level4)SO4Nonlinear optical crystal.
Container in step b is placed on without rocking, it is pollution-free, without in cross-ventilated static environment.
Methods described obtain lithium ammonium sulfate nonlinear optical crystal prepare times frequency generator, on frequency converter, lower frequency
Purposes in converter or optical parametric oscillator.
The lithium ammonium sulfate nonlinear optical crystal obtained by the method for the invention, quality is good, size is big, regular appearance.
Prepare the chemical equation of lithium ammonium sulfate：
(1)Li2SO4·H2O+(NH4)2SO4→Li(NH4)SO4+H2O
(2)Li2SO4·H2O+(NH4)2SO4·H2O→Li(NH4)SO4+H2O
(3)Li2SO4+(NH4)2SO4·H2O→Li(NH4)SO4+H2O
(4)Li2SO4+(NH4)2SO4→Li(NH4)SO4
Large scale lithium ammonium sulfate nonlinear optical crystal prepared by the method for the invention can be brilliant as device for non-linear optical is prepared
Body material, including make times frequency generator, up or down frequency converter and optical parametric oscillator.Described use lithium ammonium sulfate is non-
The device for non-linear optical that linear optical crystal makes produces at least a branch of frequency not comprising will transmit through at least a branch of incident fundamental frequency light
It is same as the coherent light of incident light.
The reagent and raw material used in the method for the invention is small to human toxicity, and growth cycle is short, be readily available it is high-quality,
The advantages of large-size crystals.
Lithium ammonium sulfate nonlinear optical crystal provided by the present invention is to machining accuracy without particular/special requirement.
Brief description of the drawings
Fig. 1 is the theoretical X-ray powder diffraction figure of lithium ammonium sulfate crystal of the present invention；
Fig. 2 is the crystallogram figure that the method for the invention grows；
The fundamental diagram for the device for non-linear optical that Fig. 3 makes for the present invention, is laser including (1), (2) are complete
Poly- lens, (3) are lithium ammonium sulfate nonlinear optical crystal, and (4) are Amici prism, and (5) are filter plate, and ω is the frequency of refraction light
Rate is equal to 2 times of incident light frequency or incident light frequency.
Embodiment
Embodiment 1：
By chemical equation：Li2SO4·H2O+(NH4)2SO4=Li (NH4)SO4+H2O synthesizes lithium ammonium sulfate non-linear optical crystal
Body；
A, by Li2SO4·H2O and (NH4)2SO4In element lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into wash clean
In conical flask (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 20ml deionization is added
Water, then ultrasonication about 10 minutes, make it be sufficiently mixed dissolving；
B, will be sealed in step a equipped with the conical flask of solution with pan paper, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of several apertures to adjust aqueous solution reclaimed water is pricked into sealing, 15 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4·H2O and (NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs gross weight
24g is measured, the deionized water for adding 100ml is configured to the aqueous solution, with ultrasonication about 10 minutes, to ensure that it is fully molten
Solution, then stands at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturation is obtained
Solution；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution for being hung on step d configurations,
Constant temperature, which grows, at room temperature can obtain size for 30 days for the transparent Li (NH of 5mm × 5mm × 7mm4)SO4Nonlinear optical crystal.
Embodiment 2：
By chemical equation：Li2SO4·H2O+(NH4)2SO4=Li (NH4)SO4+H2O synthesizes lithium ammonium sulfate non-linear optical crystal
Body；
A, by Li2SO4·H2O and (NH4)2SO4In element lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into wash clean
In conical flask (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 25ml deionized water is added,
Then ultrasonication 20 minutes, make it be sufficiently mixed dissolving；
B, will be sealed in step a equipped with the conical flask of solution with pan paper, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of several apertures to adjust aqueous solution reclaimed water is pricked into sealing, 20 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4·H2O and (NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs gross weight
48g is measured, the deionized water for adding 200ml is configured to the aqueous solution, with ultrasonication about 20 minutes, to ensure that it is fully molten
Solution, then stands at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturation is obtained
Solution；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution for being hung on step d configurations,
Constant temperature 40 days at room temperature, you can obtain size for the transparent Li (NH of 7mm × 6mm × 5mm4)2SO4Nonlinear optical crystal.
Embodiment 3：
By chemical equation：Li2SO4·H2O+(NH4)2SO4=Li (NH4)SO4+H2O synthesis large scale lithium ammonium sulfates are non-linear
Optical crystal；
A, by Li2SO4·H2O and (NH4)2SO4In element lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into wash clean
In conical flask (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 30ml deionized water is added,
Then ultrasonication 30 minutes, make it be sufficiently mixed dissolving；
B, will be sealed in step a equipped with the conical flask of solution with preservative film, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of some apertures of bundle to adjust aqueous solution reclaimed water will be sealed, 30 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4·H2O and (NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs gross weight
72g is measured, the deionized water for adding 300ml is configured to the aqueous solution, with ultrasonication about 30 minutes, to ensure that it is fully molten
Solution, then stands at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturation is obtained
Solution；
The selection preferable crystal of quality hangs on seed crystal the saturated solution of step d configurations as seed crystal in e, selection step c
In, grow 50 days, you can obtain the transparent Li (NH that size is 7mm × 7mm × 5mm4)SO4Nonlinear optical crystal.
Embodiment 4：
By chemical equation：Li2SO4·H2O+(NH4)2SO4=Li (NH4)SO4+H2O synthesis large scale lithium ammonium sulfates are non-linear
Optical crystal；
A, by Li2SO4·H2O and (NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into the taper of wash clean
In bottle (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 40ml deionized water is added, so
Ultrasonication 60 minutes, make it be sufficiently mixed dissolving afterwards；
B, will be sealed in step a equipped with the conical flask of solution with preservative film, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of some apertures of bundle to adjust aqueous solution reclaimed water will be sealed, 15 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4·H2O and (NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs gross weight
96g is measured, the deionized water for adding 400ml is configured to the aqueous solution, with ultrasonication about 60 minutes, to ensure that it is fully molten
Solution, then stands at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturation is obtained
Solution；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution that seed crystal is hung on to step d configurations,
Growth 60 days, you can obtain the transparent Li (NH that size is 8mm × 8mm × 6mm4)SO4Nonlinear optical crystal.
Embodiment 5：
By reaction equation Li2SO4·H2O+(NH4)2SO4·H2O→Li(NH4)SO4+H2O synthesis large scale lithium ammonium sulfates are non-linear
Optical crystal:
A, by Li2SO4·H2O and (NH4)2SO4·H2Lithium, ammonium, sulphur in O in molar ratio 1:1:1 weighs and is put into wash clean
In conical flask (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 35ml deionized water is added,
Then ultrasonication about 40 minutes, make it be sufficiently mixed dissolving；
B, will be sealed in step a equipped with the conical flask of solution with preservative film, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of some apertures of bundle to adjust aqueous solution reclaimed water will be sealed, 20 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4·H2O and (NH4)2SO4·H2Lithium, ammonium, sulphur in O in molar ratio 1:1:1 weighs
Gross weight 96g, the deionized water for adding 400ml is configured to the aqueous solution, with ultrasonication about 40 minutes, to ensure that it fills
Divide dissolving, then stand at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, obtained
Saturated solution；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution that seed crystal is hung on to step d configurations,
Growth 60 days, you can obtain the transparent Li (NH that size is 4mm × 7mm × 5mm4)SO4Nonlinear optical crystal.
Embodiment 6：
By reaction equation：Li2SO4+(NH4)2SO4·H2O→Li(NH4)SO4+H2O synthesizes large scale lithium ammonium sulfate nonlinear optical
Learn crystal：
A, by Li2SO4(NH4)2SO4·H2Lithium, ammonium, sulphur in O in molar ratio 1:1:1 weighs and is put into the taper of wash clean
In bottle (conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), 40ml deionized water is added, so
Ultrasonication about 50 minutes, make it be sufficiently mixed dissolving afterwards；
B, will be sealed in step a equipped with the conical flask of solution with preservative film, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of some apertures of bundle to adjust aqueous solution reclaimed water will be sealed, 30 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4(NH4)2SO4·H2Lithium, ammonium, sulphur in O in molar ratio 1:1:1 weighs gross weight
96g is measured, the deionized water for adding 400ml is configured to the aqueous solution, with ultrasonication about 40 minutes, to ensure that it is fully molten
Solution.Then stand at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturation is obtained
Solution；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution that seed crystal is hung on to step d configurations,
Growth 60 days, you can obtain size for the transparent Li (NH of 5mm × 8mm × 7mm4)SO4Nonlinear optical crystal.
Embodiment 7：
By reaction equation：Li2SO4+(NH4)2SO4→Li(NH4)SO4Synthesize large scale lithium ammonium sulfate nonlinear optical crystal：
A, by Li2SO4(NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into the conical flask of wash clean
(conical flask first must be cleaned up conical flask with acid, then use deionized water rinse), adds 35ml deionized water, Ran Houchao
Sonicated 30 minutes, makes it be sufficiently mixed dissolving；
B, will be sealed in step a equipped with the conical flask of solution with preservative film, be placed on without rocking, it is pollution-free, without cross-ventilated
In static environment, evaporation rate of some apertures of bundle to adjust aqueous solution reclaimed water will be sealed, 40 days are stood at room temperature；
C, the solution treated in step b grow crystal grain in conical flask bottom, until the no longer significant change of crystal grain size,
Growth terminates, and obtains seed crystal；
D, reconfigure solution：By Li2SO4(NH4)2SO4In lithium, ammonium, sulphur in molar ratio 1:1:1 weighs gross weight 96g,
The deionized water for adding 400ml is configured to the aqueous solution, with ultrasonication 55 minutes, to ensure that it fully dissolves, Ran Hou
Stand at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturated solution is obtained；
The preferable crystal of quality is as seed crystal in e, selection step c, in the saturated solution that seed crystal is hung on to step d configurations,
Growth 55 days, you can obtain size for the transparent Li (NH of 8mm × 5mm × 6mm4)SO4Nonlinear optical crystal.
Embodiment 8
By the Li (NH of gained in embodiment 1-74)SO4Nonlinear optical crystal, is placed on 3 position as shown in accompanying drawing 3,
At room temperature, with tune Q Nd:Light source is made in the 1064nm outputs of YAG laser, it was observed that obvious 532nm frequency doubling green lights
Output, output intensity is about 0.6 times of equal conditions KDP.
Embodiment 9
By the Li (NH of gained in embodiment 1-74)SO4Nonlinear optical crystal, is placed on 3 position as shown in accompanying drawing 3,
At room temperature, with tune Q Nd:532 frequency doubled lights that YAG laser is exported through KTP (KTiOPO4) crystal double frequency make light source, should
Frequency doubled light passes through the exportable 266nm of lithium ammonium sulfate nonlinear optical crystal ultraviolet light beam again, and output intensity is about equal conditions
0.3 times of BBO；
Fig. 3 is shown, by adjusting Q Nd:It is visible that YAG laser 1 sends infrared beam or 532nm that wavelength is 1064nm
Light beam, lithium ammonium sulfate nonlinear optical crystal is injected through convex lens 2, produces green frequency doubled light or ripple that wavelength is 532nm
A length of 266nm ultraviolet frequency double light, outgoing beam 4 contains fundamental frequency light and frequency doubled light, and filtered 5 elimination fundamental frequency light is obtained
Frequency doubled light.
Claims (3)
1. a kind of preparation method of lithium ammonium sulfate nonlinear optical crystal, it is characterised in that the molecular formula of the crystal in this method is
Li(NH4)SO4, molecular weight is 121.035, belongs to rhombic system, and space group isPna21, cell parameter is：a =8.753 (3),b = 9.102(3) Å , c=5.2647 (16),V =
419.4(2) Å3, crystal is grown using solution at room temperature method, concrete operations follow these steps to carry out：
A, lithium sulfide will be contained for lithium sulfate or sulfuric acid monohydrate lithium, sulfide containing ammonium is ammonium sulfate or lithium in sulfuric acid monohydrate ammonium, ammonium, sulphur in molar ratio 1:1:1 weighs and is put into the container of wash clean, adds 20-40ml deionized water, and ultrasonication 10-60 minutes makes it be sufficiently mixed dissolving；
B, the container pan paper in step a or preservative film sealed, and some apertures are pricked on pan paper or preservative film, stand 15-30 days at room temperature；
C, treat that the solution in step b grows crystal grain in container bottom, until crystal grain size no longer significant change, growth terminates, obtain seed crystal；
D, reconfigure solution：Lithium sulfide will be contained for lithium sulfate or sulfuric acid monohydrate lithium, sulfide containing ammonium is ammonium sulfate or lithium in sulfuric acid monohydrate ammonium, ammonium, sulphur in molar ratio 1:1:1 weighed gross weight 24-96g, and the deionized water for adding 100-400ml is configured to the aqueous solution, with ultrasonication 10-60 minutes, fully dissolving, then stands at room temperature, when its bottom has a small amount of crystal to separate out, solution is filtered with qualitative filter paper, saturated solution is obtained；
In the preferable seed crystal of quality obtained in e, selection step c, the saturated solution that seed crystal is hung on to step d configurations, grow 30-60 days, that is, obtain the transparent Li (NH of Centimeter Level4)SO4Nonlinear optical crystal.
2. the preparation method of lithium ammonium sulfate nonlinear optical crystal as claimed in claim 1, it is characterised in that the container in step b is placed on without rocking, it is pollution-free, without in cross-ventilated static environment.
3. the lithium ammonium sulfate nonlinear optical crystal that method as claimed in claim 1 is obtained prepare times frequency generator, on purposes in frequency converter, lower frequency converter or optical parametric oscillator.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109295494A (en) * | 2018-12-11 | 2019-02-01 | 闽江学院 | A kind of sulfuric acid difluoro antimony caesium nonlinear optical crystal and its preparation method and application |
| CN113265707A (en) * | 2021-04-12 | 2021-08-17 | 同济大学 | Lanthanum ammonium sulfate nonlinear optical crystal material and preparation and application thereof |
| CN113773231A (en) * | 2021-09-13 | 2021-12-10 | 中国科学院新疆理化技术研究所 | Compound hydroxyl guanidine tetrafluoroborate and hydroxyl guanidine tetrafluoroborate nonlinear optical crystal, preparation method and application |
| CN114059169A (en) * | 2021-10-29 | 2022-02-18 | 中国科学院福建物质结构研究所 | Ferroelectric deep ultraviolet transparent sulfate crystal and optical device |
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| CN105350081A (en) * | 2015-11-14 | 2016-02-24 | 中国科学院新疆理化技术研究所 | Preparation method and use of potassium lithium sulfate nonlinear optical crystal |
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| CN109295494A (en) * | 2018-12-11 | 2019-02-01 | 闽江学院 | A kind of sulfuric acid difluoro antimony caesium nonlinear optical crystal and its preparation method and application |
| CN109295494B (en) * | 2018-12-11 | 2020-03-17 | 闽江学院 | Cesium antimony difluoride sulfate nonlinear optical crystal and preparation method and application thereof |
| CN113265707A (en) * | 2021-04-12 | 2021-08-17 | 同济大学 | Lanthanum ammonium sulfate nonlinear optical crystal material and preparation and application thereof |
| CN113773231A (en) * | 2021-09-13 | 2021-12-10 | 中国科学院新疆理化技术研究所 | Compound hydroxyl guanidine tetrafluoroborate and hydroxyl guanidine tetrafluoroborate nonlinear optical crystal, preparation method and application |
| CN114059169A (en) * | 2021-10-29 | 2022-02-18 | 中国科学院福建物质结构研究所 | Ferroelectric deep ultraviolet transparent sulfate crystal and optical device |
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