CN109137073A - A kind of lithium phosphate caesium yttrium nonlinear optical crystal and the preparation method and application thereof - Google Patents
A kind of lithium phosphate caesium yttrium nonlinear optical crystal and the preparation method and application thereof Download PDFInfo
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- CN109137073A CN109137073A CN201811102265.7A CN201811102265A CN109137073A CN 109137073 A CN109137073 A CN 109137073A CN 201811102265 A CN201811102265 A CN 201811102265A CN 109137073 A CN109137073 A CN 109137073A
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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
- C30B29/14—Phosphates
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- 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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Abstract
The invention discloses a kind of LiCs2Y2(PO4)3Nonlinear optical crystal and the preparation method and application thereof.It is using compound containing Li, compound containing Cs, compound containing Y and to contain P-compound as raw material, is sintered and LiCs is made2Y2(PO4)3Powder, then by gained LiCs2Y2(PO4)3Powder and fluxing agent mixed melting, are made the LiCs2Y2(PO4)3Nonlinear optical crystal.The transparent no inclusion enclave of crystal prepared by the present invention, have many advantages, such as that the speed of growth is very fast, at low cost, and it has many advantages, such as shorter UV absorption cut-off side, biggish nonlinear optical effect, physical and chemical performance stabilization, good mechanical property, easy to process, to can be used for making the device for non-linear optical such as blinding laser weapons, video disc recording, laser projection tv, optical oomputing and optical-fibre communications.
Description
Technical field
The present invention relates to a kind of LiCs2Y2(PO4)3Nonlinear optical crystal and preparation method thereof and its prepare it is non-linear
Application in optical device.
Background technique
The nonlinear optical effect of crystal refers to: when a branch of laser with certain polarization direction passes through one in certain direction
When block nonlinear optical crystal, the frequency of the light beam will change.Crystal with nonlinear optical effect is referred to as non-linear
Optical crystal.Using the nonlinear optical effect of crystal, can be made second harmonic generator and upper and lower frequency converter and
The device for non-linear optical such as optical parametric oscillator, and all solid state laser of frequency transformation is carried out using nonlinear optical crystal
It is a developing direction of the following laser, but its key is to obtain outstanding nonlinear optical crystal.
Currently, being applied to the nonlinear optical crystal of ultraviolet band mainly hasβ-BaB2O4(BBO), LiB3O5(LBO),
CsLiB6O10(CLBO) and K2Be2BO3F2(KBBF) etc., but all there is respective shortcoming in them.For example, LBO's is birefringent
Rate is all smaller, can not achieve the quadruple output of 1064 nm wavelength lasers；The birefringence of BBO is bigger than normal, is used for 1064 nm
There are photorefractive effect when the quadruple output of wavelength laser, its output power and beam quality are limited；And CLBO is easily damp
Solution, it is difficult to realize commercial applications；KBBF then due to its serious layer growth habit, causes it to be difficult to obtaincIt is big to thickness
Crystal.Therefore, it is still urgent and necessary for exploring the new ultra-violet nonlinear optical crystal of excellent combination property.
Summary of the invention
The purpose of the present invention is to provide a kind of LiCs2Y2(PO4)3Nonlinear optical crystal and the preparation method and application thereof.
To achieve the above object, the present invention adopts the following technical scheme:
The present invention first to be protected is a kind of LiCs2Y2(PO4)3Nonlinear optical crystal, the LiCs2Y2(PO4)3It is non-linear
Optical crystal is free of symmetrical centre, belongs to cubic systemP213 space groups, structure YO6Octahedra and PO4Tetrahedron is total to vertex
Connection forms three-dimensional frame structure, and Li+Ion and Cs+Ion is filled out in frame hole；Its cell parameter isa=b=c=
10.5945(5),α=β=γ=90.00,V=1189.16(10) ,Z=4。
The present invention second to be protected is the LiCs2Y2(PO4)3The preparation method of nonlinear optical crystal is first
LiCs is prepared using solid reaction process2Y2(PO4)3Powder, then the LiCs is made using melt method for growing2Y2(PO4)3It is non-linear
Optical crystal；Itself specifically includes the following steps:
1) by compound containing Li, compound containing Cs, compound containing Y and containing P-compound by Li, Cs, Y, P stoichiometric ratio be 1:
2:2:3 is warming up to 400 ~ 500 DEG C after evenly mixing, with 10 ~ 200 DEG C/h of rate, and heat preservation sintering 12 ~ 72 hours, then
It is down to room temperature, is taken out, grinding uniformly, then with 10 ~ 200 DEG C/h of rate is warming up to 500 ~ 1100 DEG C, and sintering 24 ~ 72 is small
When to get pure phase LiCs2Y2(PO4)3Powder；
2) by fluxing agent and LiCs2Y2(PO4)3Powder mixing is placed in crystal growing furnace, and being warming up to 700 ~ 1200 DEG C makes it
It is fused into melt, then measures the saturation temperature of the melt, then melt is cooled to lower than 5 ~ 15 DEG C of saturation temperature, then
With the speed slow cooling of 0.5 ~ 10 DEG C/day to 600 DEG C, it is rapidly decreased to room temperature then to get LiCs2Y2(PO4)3It is non-linear
Optical crystal.
Compound containing Li described in step 1) is Li2CO3Or LiOHH2O；The compound containing Cs is Cs2CO3Or
CsNO3；The compound containing Y is Y2O3；The P-compound that contains is NH4H2PO4Or (NH4)2HPO4。
Its reaction process are as follows: 0.5Li2CO3+Cs2CO3+Y2O3+3NH4H2PO4=LiCs2Y2(PO4)3+1.5CO2↑+4.5H2O↑
+3NH3↑；Or LiOHH2O+2CsNO3+Y2O3+3(NH4)2HPO4=LiCs2Y2(PO4)3+6H2O↑+0.5O2↑+6NH3↑+2NO2↑。
Preferably, it should be taken out grinding 1 time or more in 500 ~ 700 DEG C of calefactive interzones in second of sintering process.
Fluxing agent and LiCs used in step 22Y2(PO4)3The molar ratio of compound is 1:0.1-5.5；Wherein, described to help
Flux is by Li2O、Cs2O and P2O5According to molar ratio (0.5-2): (0-3): (0-2) is mixed.
Gained LiCs2Y2(PO4)3Nonlinear optical crystal is with physical and chemical performance is stable, hardness is moderate, mechanical performance
The advantages that good, not easily broken, easy to process.
Third of the present invention to be protected is the LiCs2Y2(PO4)3Nonlinear optical crystal is in preparation nonlinear optics
Application in device.The device for non-linear optical includes laser etc..
Preferably, the working principle of the device for non-linear optical are as follows: pass through at least a branch of incidence electromagnetic radiation at least
One piece of LiCs2Y2(PO4)3After nonlinear optical crystal, the output spoke that at least a branch of frequency is different from incidence electromagnetic radiation is generated
It penetrates.
The beneficial effects of the present invention are: present invention gained LiCs2Y2(PO4)3Nonlinear optical crystal has shorter purple
Outer absorption cut-off side, biggish nonlinear optical effect, physical and chemical performance stabilization, good mechanical property, it is easy to process the advantages that,
It can be used for making the nonlinear opticses device such as blinding laser weapons, video disc recording, laser projection tv, optical oomputing and optical-fibre communications
Part.
Detailed description of the invention
Fig. 1 is LiCs prepared by embodiment 12Y2(PO4)3Polycrystal powder be based on LiCs2Y2(PO4)3Crystal structure simulation
X-ray diffraction compares map.
Fig. 2 is LiCs prepared by embodiment 42Y2(PO4)3The sample drawing of nonlinear optical crystal.
Fig. 3 is LiCs prepared by embodiment 42Y2(PO4)3The structural schematic diagram of crystal.
Fig. 4 is to utilize prepared LiCs2Y2(PO4)3The work that a kind of typical device for non-linear optical is made in crystal is former
Reason figure, wherein 1 is laser, 2 be incoming laser beam, and 3 be the LiCs through crystal post-processing and optical manufacturing2Y2(PO4)3Crystal,
4 be generated shoot laser beam, and 5 be optical filter.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
The powdered LiCs of embodiment 12Y2(PO4)3The preparation of compound
It is prepared using solid reaction process, reaction equation is as follows:
0.5Li2CO3+Cs2CO3+Y2O3+3NH4H2PO4=LiCs2Y2(PO4)3+1.5CO2↑+4.5H2O↑+3NH3↑。
Concrete operation step is: weighing Li respectively2CO3 0.222 g (0.003 mol)、Cs2CO3 1.955 g
(0.006 mol)、Y2O3 1.355 g (0.006 mol)、NH4H2PO41.035 g (0.009 mol), place them into and grind
In alms bowl, mixes and grind uniformly, be then charged into corundum ceramic crucible, be compacted into, be put into Muffle furnace, with 10 DEG C/h
Rate be warming up to 500 DEG C, heat preservation sintering 24 hours, be then down to room temperature, take out, grinding uniformly, then with 10 DEG C/h
Rate is warming up to 900 DEG C, is sintered 48 hours, and grinding 1 time or more the LiCs to get pure phase is taken out in midway2Y2(PO4)3Compound.
As shown in Figure 1, prepared compound x-ray diffractogram of powder spectrum with according to its mono-crystalline structures fitting it is resulting
Map is consistent.
The powdered LiCs of embodiment 22Y2(PO4)3The preparation of compound
It is prepared using solid reaction process, reaction equation is as follows:
LiOH·H2O+2CsNO3+Y2O3+3(NH4)2HPO4=LiCs2Y2(PO4)3+6H2O↑+0.5O2↑+6NH3↑+2NO2↑。
Concrete operation step is: weighing LiOHH respectively2O 0.126g (0.003 mol),CsNO3 1.169 g
(0.006 mol),Y2O3 0.677 g (0.003 mol),(NH4)2HPO41.188 g (0.009 mol), place them into
In mortar, mix and grind uniformly, be then charged into corundum ceramic crucible, be compacted into, be put into Muffle furnace, with 50 DEG C/it is small
When rate be warming up to 500 DEG C, heat preservation sintering 24 hours, be then down to room temperature taking-up, grinding uniformly, then with 50 DEG C/h
Rate be warming up to 900 DEG C and be sintered 48 hours, grinding 1 time or more the LiCs to get pure phase is taken out in midway2Y2(PO4)3Chemical combination
Object.
3 LiCs of embodiment2Y2(PO4)3The preparation of crystal
The LiCs is prepared using melt method for growing2Y2(PO4)3Nonlinear optical crystal is to make embodiment 1 or embodiment 2
Standby LiCs2Y2(PO4)3Compound and fluxing agent Li2O 0.1:1 mixing in molar ratio is placed in crystal growing furnace, 700 ~
1100 DEG C or more heat preservations 2 hours or more make it be fused into melt, the saturation temperature of the melt are then measured, then by melt
It is cooled to lower than 5 DEG C of saturation temperature, then room temperature is then rapidly decreased to 600 DEG C with 0.5 DEG C/day slow cooling, obtain institute
State crystal.
4 LiCs of embodiment2Y2(PO4)3The preparation of crystal
The LiCs is prepared using melt method for growing2Y2(PO4)3Nonlinear optical crystal is to make embodiment 1 or embodiment 2
Standby LiCs2Y2(PO4)30.7:1 is mixed and is placed in crystal growing furnace in molar ratio for compound and fluxing agent, 700 ~ 1100
DEG C heat preservation 2 hours or more makes it be fused into melt, then measures the saturation temperature of the melt, is then cooled to melt and is lower than
5 DEG C of saturation temperature, then it is then rapidly decreased to room temperature to 600 DEG C with 1.5 DEG C/day slow coolings, obtain the crystal.
The fluxing agent is by Li2O、Cs2O and P2O5It is mixed according to molar ratio for 1:2:1.67；
Fig. 2 is the grade transparent crystal grown using 4 method of embodiment.
After tested, prepared LiCs2Y2(PO4)3Nonlinear optical crystal is free of symmetrical centre, belongs to cubic systemP213
Space group；Its cell parameter isa=b=c=10.5945(5),α=β=γ=90.00,V=1189.16(10) ,Z=4.Such as Fig. 3
Shown, the structure of the crystal is YO6Octahedra and PO4Tetrahedron is total to vertex connection, forms three-dimensional frame structure, and Li+Ion
And Cs+Ion is filled out in frame hole.
By resulting LiCs2Y2(PO4)3Nonlinear optical crystal makees diffuse reflectance spectroscopy, and the UV absorption of the crystal is cut
Only it is lower than 200 nm；The crystal is not easily broken, nonhygroscopic.
Crystal of the present invention has frequency-doubled effect.Fig. 4 is to use LiCs prepared by the present invention2Y2(PO4)3Crystal makes non-
The structural schematic diagram of linear optics device.At room temperature, it with adjusting Q Nd:YAG laser to make fundamental frequency light source, is issued by laser 1
Incoming laser beam 2(incident wavelength is the near infrared light of 1064 nm) inject LiCs2Y2(PO4)3Crystal 3, generated outgoing swash
Light beam 4(output wavelength is the green laser of 532 nm) by optical filter 5, thus laser beam required for obtaining, laser intensity
It is approximately equivalent to KH2PO40.9 times.The nonlinear optics laser can be times frequency generator or upper and lower frequency converter or light
Parametric oscillator etc..
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of LiCs2Y2(PO4)3The preparation method of nonlinear optical crystal, it is characterised in that: the following steps are included:
1) by compound containing Li, compound containing Cs, compound containing Y and containing P-compound by Li, Cs, Y, P stoichiometric ratio be 1:
2:2:3 is warming up to 400 ~ 500 DEG C after evenly mixing, with 10 ~ 200 DEG C/h of rate, and heat preservation sintering 12 ~ 72 hours, then
It is down to room temperature, is taken out, grinding uniformly, then with 10 ~ 200 DEG C/h of rate is warming up to 500 ~ 1100 DEG C, and sintering 24 ~ 72 is small
When, obtain LiCs2Y2(PO4)3Powder；
2) by fluxing agent and gained LiCs2Y2(PO4)3Powder mixing is placed in crystal growing furnace, and being warming up to 700 ~ 1200 DEG C makes
It is fused into melt, then measures the saturation temperature of the melt, and then melt is cooled to lower than 5 ~ 15 DEG C of saturation temperature,
Again with the speed slow cooling of 0.5 ~ 10 DEG C/day to 600 DEG C, it is rapidly decreased to room temperature then to get LiCs2Y2(PO4)3It is non-thread
Property optical crystal.
2. LiCs according to claim 12Y2(PO4)3The preparation method of nonlinear optical crystal, it is characterised in that: step
1) compound containing Li described in is Li2CO3Or LiOHH2O；The compound containing Cs is Cs2CO3Or CsNO3；The chemical combination containing Y
Object is Y2O3；The P-compound that contains is NH4H2PO4Or (NH4)2HPO4。
3. LiCs according to claim 12Y2(PO4)3The preparation method of nonlinear optical crystal, it is characterised in that: step
2) fluxing agent and LiCs used in2Y2(PO4)3The molar ratio of powder is 1:0.1-5.5；
Wherein, the fluxing agent is by Li2O、Cs2O and P2O5According to molar ratio (0.5-2): (0-3): (0-2) is mixed.
4. LiCs made from a kind of method as described in claim 12Y2(PO4)3Nonlinear optical crystal, it is characterised in that: described
LiCs2Y2(PO4)3Nonlinear optical crystal is free of symmetrical centre, belongs to cubic systemP213 space groups, cell parameter area=b=c=10.5945(5),α=β=γ=90.00,V=1189.16(10) ,Z=4。
5. a kind of LiCs as claimed in claim 42Y2(PO4)3Nonlinear optical crystal is in preparing device for non-linear optical
Using.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079858A (en) * | 2019-05-20 | 2019-08-02 | 闽江学院 | A kind of cesium sulfate magnesium nonlinear optical crystal and its preparation method and purposes |
| CN110079861A (en) * | 2019-06-14 | 2019-08-02 | 山东大学 | Yttrium phosphate strontium crystal and the preparation method and application thereof |
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| CN101831706A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Growth method of low ultraviolet absorption YA13(BO3)4 crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079858A (en) * | 2019-05-20 | 2019-08-02 | 闽江学院 | A kind of cesium sulfate magnesium nonlinear optical crystal and its preparation method and purposes |
| CN110079858B (en) * | 2019-05-20 | 2020-11-27 | 闽江学院 | Cesium magnesium sulfate nonlinear optical crystal and preparation method and application thereof |
| CN110079861A (en) * | 2019-06-14 | 2019-08-02 | 山东大学 | Yttrium phosphate strontium crystal and the preparation method and application thereof |
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