CN109160526A - Li8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal and its preparation method and purposes - Google Patents
Li8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal and its preparation method and purposes Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D17/00—Rubidium, caesium or francium compounds
- C01D17/003—Compounds of alkali metals
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- 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
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- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
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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
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Abstract
The present invention relates to a kind of Li8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal, Li8NaRb3(SO4)6·2H2The preparation method and Li of O crystal8NaRb3(SO4)6·2H2O crystal is used to make the purposes of device for non-linear optical.The method have the advantages that: have many advantages, such as it is easy to operate, at low cost, pollution less, raw materials used toxicity is low, growth cycle is short；Crystal obtained has many advantages, such as shorter UV absorption cut-off side, biggish nonlinear optical effect, physical and chemical performance stabilization, good mechanical property；The crystal can be used for making device for non-linear optical；The device for non-linear optical of nonlinear optical crystal production of the present invention can be used in several military and civilian high-tech areas, such as blinding laser weapons, video disc recording, laser projection tv, optical oomputing and optical-fibre communications etc..
Description
Technical field
The present invention relates to a kind of Li8NaRb3(SO4)6·2H2O compound, Li8NaRb3(SO4)6·2H2O nonlinear optics
Crystal, Li8NaRb3(SO4)6·2H2The preparation method and Li of O crystal8NaRb3(SO4)6·2H2O crystal is non-linear for making
The purposes of optical device.
Technical background
The nonlinear optical effect of crystal refers to such a effect: when a branch of laser with certain polarization direction is by one
When determining direction by one block of nonlinear optical crystal, the frequency of the light beam will change.Crystalline substance with nonlinear optical effect
Body is known as nonlinear optical crystal.Using the nonlinear optical effect of crystal, second harmonic generator and upper and lower frequency can be made
The device for non-linear optical such as rate converter and optical parametric oscillator.The complete solid of frequency transformation is carried out using nonlinear optical crystal
State laser is a developing direction of the following laser, and its key is to obtain outstanding nonlinear optical crystal.
Currently, being applied to ultraviolet and deep ultraviolet band nonlinear optical crystal is all borate, mainly there is β-BaB2O4
(BBO)、LiB3O5(LBO)、RbLiB6O10(CLBO) and K2Be2BO3F2(KBBF) etc., but all there is respective deficiency in them
Place.For example, the birefringence of LBO and CBO is all smaller, the quadruple output of 1064nm wavelength laser can not achieve；BBO's
Birefringence is bigger than normal, there are photorefractive effect when the quadruple for 1064nm wavelength laser exports, limits its output power
And beam quality；And CLBO is easily deliquesced, it is difficult to realize commercial applications；KBBF is then since its serious layer growth habit is led
It is caused to be difficult to obtain the c crystal big to thickness.Therefore, the new ultra-violet nonlinear optical crystal of excellent combination property is explored still
It is urgent and necessary.
In recent years, phosphate deep ultraviolet NLO crystal system just receives more and more attention, and has a series of new phosphorus in succession
Hydrochlorate deep ultraviolet NLO crystal is reported, such as Ba3P3O10Cl、Ba3P3O10Br、Rb2Ba(PO3)5、Ba5P6O10、CsLi2PO4Deng.
Sulfate radical and phosphate radical belong to tetrahedral configuration, and theoretically there is sulfate radical the microcosmic second nonlinear bigger than phosphate radical to polarize
Rate conducive to big macroscopical NLO effect is generated, and has and the comparable band gap of phosphate radical, is conducive to crystal in deep ultraviolet spectral regions
Through.For example, Li2SO4·H2The frequency-doubled effect of O crystal is suitable with standard K DP, has reached 200nm depth below through range
Ultra-violet (UV) band.Therefore, sulfate deep ultraviolet nonlinear optical crystal has very big potentiality really.
Summary of the invention
It is Li the purpose of the present invention is to provide a kind of chemical formula8NaRb3(SO4)6·2H2The compound of O, one kind
Li8NaRb3(SO4)6·2H2The preparation method of O compound, a kind of Li8NaRb3(SO4)6·2H2O7Nonlinear optical crystal,
Li8NaRb3(SO4)6·2H2The preparation method and Li of O crystal8NaRb3(SO4)6·2H2The use of O nonlinear optical crystal
On the way.
Technical scheme is as follows:
(1) a kind of Li8NaRb3(SO4)6·2H2The compound of O, the Li8NaRb3(SO4)6·2H2O compound
Chemical formula is Li8NaRb3(SO4)6·2H2O。
(2) a kind of Li8NaRb3(SO4)6·2H2O nonlinear optical crystal, the Li8NaRb3(SO4)6·2H2O is non-
Linear optical crystal is free of symmetrical centre, belongs to monoclinic system space group, cell parameter isZ=2.
(3) a kind of to prepare Li8NaRb3(SO4)6·2H2The method of O compound and nonlinear optical crystal, using aqueous solution
The method growth Li8NaRb3(SO4)6·2H2O nonlinear optical crystal.
(4) aqua-solution method described in includes the following steps:
A, claim to contain Li+Compound contains Na+Compound contains Rb+Compound and contain (SO4)2-Compound is put into clean container
In, appropriate amount of deionized water and ultrasonication 10-60 minutes are then added, mix them thoroughly dissolution, wherein the n (Li+): n (Na+): n (Rb+): n ((SO4)2-)=8:1:3: 6；
B, by after the completion of step a container pan paper or preservative film seal, and it is multiple by being pricked on pan paper or preservative film
Aperture stands 15-30 days for (30 DEG C -70 DEG C) at a certain temperature；
C, crystal grain is grown in container bottom to the solution in step b, until the no longer significant change of crystal grain size,
Obtain crystal；
(5) contain Li described in step a+Compound is lithium sulfate (Li2SO4), sulfuric acid monohydrate lithium (Li2SO4·H2O) or
Lithium carbonate (Li2CO3), it is described to contain Na+Compound is sodium sulphate (Na2SO4), sal glauberi (Na2SO4·10H2) or sodium carbonate O
(Na2CO3), it is described to contain Rb+Compound is rubidium sulfate (Rb2SO4) or rubidium carbonate (Rb2CO3), described contains (SO4)2-Compound
For Li2SO4、Li2SO4·H2O、Na2SO4、 Na2SO4·10H2O or Rb2SO4。
(6) container in step b be placed on without shake, it is pollution-free, without in cross-ventilated static environment.
(7) Li of the invention8NaRb3(SO4)6·2H2The purposes of O nonlinear optical crystal, including as nonlinear optics
Device uses.
Preferably, prepared device for non-linear optical includes that at least a branch of incidence electromagnetic radiation is passed through at least one piece
Li8NaRb3(SO4)6·2H2After O nonlinear optical crystal, the output spoke that at least a branch of frequency is different from incidence electromagnetic radiation is generated
The device penetrated.
Li of the invention8NaRb3(SO4)6·2H2O compound, nonlinear optical crystal of the compound and preparation method thereof
It is had the advantages that with purposes:
(1) reagent and raw material used in the method for the invention are small to human toxicity, and growth cycle is short, at low cost；
(2) Li obtained8NaRb3(SO4)6·2H2O nonlinear optical crystal have shorter UV absorption cut-off side,
Biggish nonlinear optical effect, physical and chemical performance are stable, be not easy to deliquesce, good mechanical property, it is easy to process the advantages that；
(3) Li8NaRb3(SO4)6·2H2O nonlinear optical crystal can be used for making device for non-linear optical；
(4) device for non-linear optical of nonlinear optical crystal production of the present invention can be used for several military and civilian high-tech
In field, such as blinding laser weapons, video disc recording, laser projection tv, optical oomputing and optical-fibre communications etc..
Detailed description of the invention
Fig. 1 is to use Li8NaRb3(SO4)6·2H2A kind of working principle of typical device for non-linear optical made of O crystal
Figure, wherein 1 is laser, 2 be incoming laser beam, and 3 be the Li through crystal post-processing and optical manufacturing8NaRb3(SO4)6·2H2O
Crystal, 4 be generated laser beam, and 5 be optical filter.
Fig. 2 is Li of the invention8NaRb3(SO4)6·2H2O polycrystal powder X ray diffracting spectrum be based on Li8NaRb3
(SO4)6·2H2The X ray diffracting spectrum of O crystal structure simulation.
Fig. 3 is Li of the invention8NaRb3(SO4)6·2H2O crystal structure figure.
Specific embodiment
The present invention is further described below with reference to examples and drawings.As known to those skilled in the art, following embodiments are not
It is limiting the scope of the invention, any improvements and changes made on the basis of the present invention are all in protection model of the invention
Within enclosing.
Embodiment 1-11 is about Li8NaRb3(SO4)6·2H2The preparation of O compound and crystal.
Embodiment 1
Using aqua-solution method, reaction equation is as follows:
8Li2SO4·H2O+Na2SO4+3Rb2SO4=2Li8NaRb3(SO4)6·2H2O+4H2O
Concrete operation step is:
A, by Li2SO4·H2O、Na2SO4、Rb28 (10.234g): 1 (1.420g): 3 (8.010g) claim SO4 in molar ratio
Take and be put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), be added 60ml go from
Sub- water, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, (30 DEG C -70 at a certain temperature
DEG C) stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 2
Using aqua-solution method, reaction equation is as follows:
8Li2SO4·H2O+Na2SO4·10H2O+3Rb2SO4=2Li8NaRb3(SO4)6·2H2O+14H2O
Concrete operation step is:
A, by Li2SO4·H2O、Na2SO4·10H2O、Rb2SO4 in molar ratio 8 (10.234g): 1 (3.222g): 3
(8.010g) weighs and is put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), is added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, (30 DEG C -70 at a certain temperature
DEG C) stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 3
Using aqua-solution method, reaction equation is as follows:
8Li2SO4+Na2SO4+3Rb2SO4+4H2O=2Li8NaRb3(SO4)6·2H2O
Concrete operation step is:
A, by Li2SO4、Na2SO4、Rb28 (8.795g): 1 (1.420g): 3 (8.010g) are weighed and are put SO4 in molar ratio
Enter in clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), the deionized water of 60ml is added, so
Ultrasonication 10 minutes afterwards mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, (30 DEG C -70 at a certain temperature
DEG C) stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 4
Using aqua-solution method, reaction equation is as follows:
8Li2SO4+Na2SO4·10H2O+3Rb2SO4=2Li8NaRb3(SO4)6·2H2O+6H2O
Concrete operation step is:
A, by Li2SO4、Na2SO4·10H2O、Rb28 (8.795g): 1 (3.222g): 3 (8.010g) claim SO4 in molar ratio
Take and be put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), be added 60ml go from
Sub- water, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, (30 DEG C -70 at a certain temperature
DEG C) stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 5
Using aqua-solution method, reaction equation is as follows:
8Li2CO3+8H2SO4+Na2SO4+3Rb2SO4=2Li8NaRb3(SO4)6·2H2O+4H2O+8CO2
Concrete operation step is:
A, by Li2CO3、H2SO4、Na2SO4、Rb2SO4 in molar ratio 8 (5.904g): 8 (4.345ml): 1 (1.420g): 3
(8.010g) weighs and is put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), is added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 6
Using aqua-solution method, reaction equation is as follows:
8Li2CO3+8H2SO4+Na2SO4·10H2O+3Rb2SO4=
2Li8NaRb3(SO4)6·2H2O+14H2O+8CO2
Concrete operation step is:
A, by Li2CO3、H2SO4、Na2SO4·10H2O、Rb2SO4 in molar ratio 8 (5.904g): 8 (4.345ml): 1
(3.222g): 3 (8.010g) are weighed and are put into clean beaker and (must first clean up beaker with acid, then use deionized water
Rinse), the deionized water of 60ml is added, then ultrasonication 10 minutes, mixes them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 7
Using aqua-solution method, reaction equation is as follows:
8Li2SO4+H2SO4+Na2CO3+3Rb2SO4+3H2O=2Li8NaRb3(SO4)6·2H2O+CO2
Concrete operation step is:
A, by Li2SO4、H2SO4、Na2CO3、Rb2SO4 8 (8.795g): 1 (0.543ml): 1 (1.060g) in molar ratio:
3 (8.010g) weigh and are put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), are added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 8
Using aqua-solution method, reaction equation is as follows:
8Li2SO4·H2O+H2SO4+Na2CO3+3Rb2SO4=2Li8NaRb3(SO4)6·2H2O+CO2+5H2O
Concrete operation step is:
A, by Li2SO4·H2O、H2SO4、Na2CO3、Rb2SO4 in molar ratio 8 (10.234g): 1 (0.543ml): 1
(1.060g): 3 (8.010g) are weighed and are put into clean beaker and (must first clean up beaker with acid, then use deionized water
Rinse), the deionized water of 60ml is added, then ultrasonication 10 minutes, mixes them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 8
Using aqua-solution method, reaction equation is as follows:
8Li2SO4·H2O+Na2SO4+3Rb2CO3+3H2SO4=2Li8NaRb3(SO4)6·2H2O+3CO2+7H2O
Concrete operation step is:
A, by Li2SO4、Na2SO4、Rb2CO3、H2SO4 in molar ratio 8 (8.795g): 1 (1.420g): 3 (6.928g): 3
(1.630ml) weighs and is put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), is added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 9
Using aqua-solution method, reaction equation is as follows:
8Li2SO4+Na2SO4+3Rb2CO3+3H2SO4+H2O=2Li8NaRb3(SO4)6·2H2O+3CO2
Concrete operation step is:
A, by Li2SO4、Na2SO4、Rb2CO3、H2SO4 in molar ratio 8 (8.795g): 1 (1.420g): 3 (6.928g): 3
(1.630ml) weighs and is put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), is added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 10
Using aqua-solution method, reaction equation is as follows:
8Li2SO4·H2O+Na2SO4·10H2O+3Rb2CO3+3H2SO4=2Li8NaRb3(SO4)6·2H2O+3CO2+7H2O
Concrete operation step is:
A, by Li2SO4、Na2SO4·10H2O、Rb2CO3、H2SO4 in molar ratio 8 (8.795g): 1 (3.222g): 3
(6.928g): 3 (1.630ml) are weighed and are put into clean beaker and (must first clean up beaker with acid, then use deionized water
Rinse), the deionized water of 60ml is added, then ultrasonication 10 minutes, mixes them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
Embodiment 11
Using aqua-solution method, reaction equation is as follows:
8Li2SO4+Na2SO4·10H2O+3Rb2CO3+3H2SO4=2Li8NaRb3(SO4)6·2H2O+3CO2+9H2O
Concrete operation step is:
A, by Li2SO4、Na2SO4、Rb2CO3、H2SO4 in molar ratio 8 (8.795g): 1 (1.420g): 3 (6.928g): 3
(1.630ml) weighs and is put into clean beaker (must first be cleaned up beaker with acid, then with deionized water rinse), is added
The deionized water of 60ml, then ultrasonication 10 minutes, mix them thoroughly dissolution；
B, by step a be equipped with solution beaker preservative film sealing be placed on without shake, it is pollution-free, without cross-ventilated quiet
In state environment, evaporation rate of several apertures to adjust water in aqueous solution is pricked into sealing, at a certain temperature (30-70 DEG C)
Stand 15-30 days；
C, crystal grain is grown in beaker bottom to the solution in step b, until the no longer significant change of crystal grain size,
Growth terminates, and obtains crystal；
Resulting map one is fitted with according to its mono-crystalline structures as shown in Fig. 2, testing resulting x-ray diffractogram of powder spectrum
It causes.
By the resulting Li of embodiment 18NaRb3(SO4)6·2H2O nonlinear optical crystal makees diffuse reflectance spectroscopy, the crystalline substance
The UV absorption cut-off side of body is lower than 200nm, and the crystal is not easily broken, nonhygroscopic；By the resulting Li of embodiment 18NaRb3
(SO4)6·2H2O nonlinear optical crystal is placed at position of 1 shown device of attached drawing marked as 1, at room temperature, with adjust Q Nd:
YAG laser makees fundamental frequency light source, and incident wavelength is the near infrared light of 1064nm, and output wavelength is the green laser of 532nm, laser
Intensity is approximately equivalent to KDP (KH2PO4) 0.5 times.
Attached drawing 1 is to use Li to the present invention8NaRb3(SO4)6·2H2The device for non-linear optical of O crystal production is briefly
It is bright.Light beam 2 is issued by laser 1 and injects RbNaMgP2O7Crystal 3, generated outgoing beam 4 is by filter plate 5, to obtain
Laser beam required for obtaining.The nonlinear optics laser can be times frequency generator or upper and lower frequency converter or optical parameter
Oscillator etc..
Above-mentioned specific embodiment is only explained in detail technical solution of the present invention, the present invention not only only office
Be limited to above-described embodiment, it will be understood by those skilled in the art that it is all according to above-mentioned principle and spirit on the basis of the present invention
It improves, substitution, it all should be within protection scope of the present invention.
Claims (8)
1.Li8NaRb3(SO4)6·2H2The compound of O, it is characterised in that: the Li8NaRb3(SO4)6·2H2The compound of O
Chemical formula be Li8NaRb3(SO4)6·2H2O。
2.Li8NaRb3(SO4)6·2H2O nonlinear optical crystal, it is characterised in that: the Li8NaRb3(SO4)6·2H2O is non-
Linear optical crystal is free of symmetrical centre, belongs to monoclinic system, C2 space group.
3. Li according to claim 28NaRb3(SO4)6·2H2O nonlinear optical crystal, it is characterised in that: cell parameter
For Z=2.
4. Li according to claim 2 or 38NaRb3(SO4)6·2H2The preparation method of O nonlinear optical crystal, feature
It is: includes the following steps:
A, claim to contain Li+Compound contains Na+Compound contains Rb+Compound and contain (SO4)2-Compound is put into clean container, so
Appropriate amount of deionized water and ultrasonication 10-60 minutes are added afterwards, make containing Li+Compound contains Na+Compound contains Rb+Compound
With contain (SO4)2-Compound is sufficiently mixed dissolution, wherein the n (Li+): n (Na+): n (Rb+): n ((SO4)2-)=8:1:3:
6；
B, by after the completion of step a container pan paper or preservative film seal, and multiple apertures will be pricked on pan paper or preservative film,
15-30 days are stood at being 30 DEG C -70 DEG C in temperature；
C, crystal grain is grown in container bottom to the solution in step b, until the no longer significant change of crystal grain size, obtains
Crystal.
5. Li according to claim 48NaRb3(SO4)6·2H2The preparation method of O nonlinear optical crystal, feature exist
In: contain Li described in step a+Compound is Li2SO4、Li2SO4·H2O or Li2CO3, described to contain Na+Compound is Na2SO4、
Na2SO4·10H2O or Na2CO3, described to contain Rb+Compound is Rb2SO4Or Rb2CO3, described contains (SO4)2-Compound is
Li2SO4、Li2SO4·H2O、Na2SO4、Na2SO4·10H2O or Rb2SO4。
6. Li according to claim 48NaRb3(SO4)6·2H2The preparation method of O nonlinear optical crystal, feature exist
In: the condition of standing described in step b be without shake, it is pollution-free and without cross-ventilated static environment.
7. Li according to claim 2 or 38NaRb3(SO4)6·2H2The purposes of O nonlinear optical crystal, feature exist
In: the Li8NaRb3(SO4)6·2H2O nonlinear optical crystal is used as device for non-linear optical.
8. a kind of device for non-linear optical, it is characterised in that: including Li according to claim 2 or 38NaRb3(SO4)6·
2H2O nonlinear optical crystal.
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| CN113912091A (en) * | 2021-10-19 | 2022-01-11 | 中国科学院福建物质结构研究所 | Cs3C6N9·H2O compound, Cs3C6N9·H2O-nonlinear optical crystal and its preparation method and use |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2018
- 2018-09-04 CN CN201811026132.6A patent/CN109160526B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| R. L. MOREIRA ET AL.: ""Raman and birefringence studies of the low-temperature phase transitions in LiK1-xRbxSO4 crystals"", 《PHYSICAL REVIEW B》 * |
| 姬亚芹: "《地学基础》", 30 September 2008, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912091A (en) * | 2021-10-19 | 2022-01-11 | 中国科学院福建物质结构研究所 | Cs3C6N9·H2O compound, Cs3C6N9·H2O-nonlinear optical crystal and its preparation method and use |
| CN113912091B (en) * | 2021-10-19 | 2022-10-14 | 中国科学院福建物质结构研究所 | Cs 3 C 6 N 9 ·H 2 O compound, cs 3 C 6 N 9 ·H 2 O-nonlinear optical crystal and its preparation method and use |
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