CN107792842A - CsCdPO4Compound, CsCdPO4Nonlinear optical crystal and its preparation method and purposes - Google Patents

CsCdPO4Compound, CsCdPO4Nonlinear optical crystal and its preparation method and purposes Download PDF

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Publication number
CN107792842A
CN107792842A CN201710889137.0A CN201710889137A CN107792842A CN 107792842 A CN107792842 A CN 107792842A CN 201710889137 A CN201710889137 A CN 201710889137A CN 107792842 A CN107792842 A CN 107792842A
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cscdpo
crystal
compound
nonlinear optical
optical crystal
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CN107792842B (en
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罗军华
沈耀国
赵三根
赵炳卿
李先锋
丁清然
李雁强
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • 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
    • 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
    • C30B9/00—Single-crystal growth from melt solutions using molten solvents
    • C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12—Salt solvents, e.g. flux growth
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of CsCdPO4Compound, CsCdPO4Nonlinear optical crystal and its preparation method and purposes.The transparent no inclusion enclave of crystal of the present invention, has that the speed of growth is very fast, low cost and other advantages；The crystal obtained has the advantages that shorter UV absorption cut-off side, larger nonlinear optical effect, physical and chemical performance stabilization, good mechanical property, easy to process；The crystal can be used for making device for non-linear optical；The device for non-linear optical that nonlinear optical crystal of the present invention makes can be used in some 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

CsCdPO4Compound, CsCdPO4Nonlinear optical crystal and its preparation method and purposes
Technical field
The present invention relates to a kind of CsCdPO4Compound, CsCdPO4Nonlinear optical crystal, CsCdPO4The preparation side of crystal Method, CsCdPO4Crystal is used to make the purposes of device for non-linear optical and comprising CsCdPO4The optics device of nonlinear optical crystal Part.
Background technology
The nonlinear optical effect of crystal refers to such a effect：When a branch of laser with certain polarization direction presses 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 referred to 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 following laser, and its key is to obtain outstanding nonlinear optical crystal.
At present, the nonlinear optical crystal applied to ultraviolet band mainly has β-BaB2O4(BBO)、LiB3O5(LBO)、 CsLiB6O10And K (CLBO)2Be2BO3F2(KBBF) etc., but respective weak point all be present in them.For example, LBO birefringence Rate is all smaller, it is impossible to realizes the quadruple output of 1064nm wavelength lasers；BBO birefringence is bigger than normal, for 1064nm ripples Photorefractive effect be present during the quadruple output of long laser, limit its power output and beam quality；And CLBO easily deliquescence, It is difficult to commercial applications；KBBF then due to its serious layer growth habit, causes it to be difficult to obtain c to the big crystalline substance of thickness Body.Therefore, it is still urgent and necessary to explore the new ultra-violet nonlinear optical crystal of excellent combination property.
The content of the invention
First purpose of the present invention is that it is CsCdPO to provide a kind of chemical formula4Compound.
Second object of the present invention is to provide a kind of CsCdPO4The preparation method of compound.
Third object of the present invention is to provide a kind of CsCdPO4Nonlinear optical crystal.
Fourth object of the present invention is to provide CsCdPO4The preparation method of crystal.
The 5th purpose of the present invention is to provide CsCdPO4The purposes of nonlinear optical crystal.
The 6th purpose of the present invention is to provide a kind of device for non-linear optical.
Technical scheme is as follows：
CsCdPO4Compound, described CsCdPO4The chemical formula of compound is CsCdPO4。
CsCdPO4The preparation method of compound, described CsCdPO is prepared using solid reaction process4Compound, including it is as follows Step：
After Cs compounds, compound containing Cd will be contained and uniformly mixed with stoichiometric proportion containing P-compound, with 10~200 DEG C/ The speed of hour is warming up to 400~500 DEG C, then heat preservation sintering more than 12 hours, and grinding is taken out uniformly after being down to room temperature, then with 10~200 DEG C/h of speed is warming up to 500~1100 DEG C and sintered more than 24 hours, produces the CsCdPO of pure phase4Compound.
Preferably, midway is needed to take out grinding more than 1 time during being sintered at 500~700 DEG C,
Preferably, the compound containing Cs is Cs2CO3Or CsNO3；The compound containing Cd is CdCO3Or Cd (NO3)2；Institute It is NH to state containing P-compound4H2PO4Or (NH4)2HPO4。
It is further preferred that CsCdPO of the present invention4Compound can be obtained by following typical reaction：
1)0.5Cs2CO3+CdCO3+NH4H2PO4=CsCdPO4+1.5CO2↑+1.5H2O↑+NH3↑
2)1CsNO3+Cd(NO3)2+(NH4)2HPO4=CsCdPO4+1.5H2O↑+O2↑+2NH3↑+2NO2↑
The present invention also provides a kind of CsCdPO4Nonlinear optical crystal, described CsCdPO4Nonlinear optical crystal is free of Symmetrical centre, belong to monoclinic system P21Space group.
The cell parameter of the crystal is β=90.244 (4),Z=4；The structure of the crystal is CdO4Tetrahedron and PO4Tetrahedron is total to Summit connects, and forms three-dimensional pore space structure, and Cs+Ion is filled out in hole.
The present invention also provides a kind of CsCdPO4The preparation method of nonlinear optical crystal：Using described in melt method for growing CsCdPO4Nonlinear optical crystal, comprise the following steps：
First, after Cs compounds, compound containing Cd will be contained and uniformly mixed with stoichiometric proportion containing P-compound, with 10~ 200 DEG C/h of speed is warming up to 400~500 DEG C, then heat preservation sintering more than 12 hours, and grinding is taken out after being down to room temperature It is even, then be warming up to 500~1100 DEG C with 10~200 DEG C/h of speed and sinter more than 24 hours, obtain CsCdPO4Raw material；
Then, by fluxing agent and described CsCdPO4Raw material mixing after be placed in crystal growing furnace, be warming up to 700 DEG C with On be fused into melt, the saturation temperature (during test, platinum filament test saturation temperature) of the melt is then tested, then by melt More than 5 DEG C of saturation temperature is cooled to, then slow cooling is then cooled to rapidly room temperature, produces CsCdPO near 600 DEG C4 Nonlinear optical crystal；
The fluxing agent is by Cs2O and P2O5It is 0.5-2 according to mol ratio:0-2 is mixed；
Described fluxing agent and described CsCdPO4The mol ratio of raw material is 1:0.1-5.5.
The CsCdPO4Nonlinear optical crystal has moderate physical and chemical performance stabilization, hardness, good mechanical property, is not easy Fragmentation, it is easy to process the advantages that；So the invention furthermore provides CsCdPO4The purposes of nonlinear optical crystal.
Present invention also offers a kind of device for non-linear optical, wherein the device includes CsCdPO of the present invention4 Nonlinear optical crystal.
According to the present invention, the device for non-linear optical is also including laser etc..
Preferably, the operation principle of the device for non-linear optical is：At least a branch of incidence electromagnetic radiation is passed through at least One piece of CsCdPO4After nonlinear optical crystal, the output radiation that at least a branch of frequency is different from incidence electromagnetic radiation is produced.
The CsCdPO of the present invention4Compound, the compound nonlinear optical crystal and its production and use just like Lower beneficial effect：
(1) CsCdPO obtained4Nonlinear optical crystal has shorter UV absorption cut-off side, larger non-linear Optical effect, physical and chemical performance stabilization, good mechanical property, it is easy to process the advantages that；
(2) CsCdPO4Nonlinear optical crystal can be used for making device for non-linear optical；
(3) device for non-linear optical that nonlinear optical crystal of the present invention makes can be used for some 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..
Brief description of the drawings
Fig. 1 is to use CsCdPO4A kind of fundamental diagram of typical device for non-linear optical made of crystal, wherein 1 is Laser, 2 be incoming laser beam, and 3 be the CsCdPO through crystal post processing and optical manufacturing4Crystal, 4 be caused laser Beam, 5 be optical filter.
Fig. 2 is the CsCdPO of the present invention4Polycrystal powder X ray diffracting spectrum is with being based on CsCdPO4The X of crystal structure simulation X ray diffraction collection of illustrative plates.
Fig. 3 is the CsCdPO of the present invention4Crystal structure figure.
Fig. 4 is the CsCdPO prepared using the method for embodiment 44The picture of nonlinear optical crystal.
Embodiment
The present invention is further described with reference to embodiment and accompanying drawing.Those skilled in the art know that following embodiments are not It is limiting the scope of the invention, any improvement made on the basis of the present invention and change are all in the protection model of the present invention Within enclosing.
Examples 1 and 2 are on powdered CsCdPO4The preparation of compound.
Embodiment 1
It is as follows using solid reaction process, reaction equation：
0.5Cs2CO3+CdCO3+NH4H2PO4=CsCdPO4+1.5CO2↑+1.5H2O↑+NH3↑
Above-mentioned four kinds of reagent inventorys are respectively：Cs2CO3 1.629g(0.005mol),CdCO3 1.724g (0.010mol),NH4H2PO4 1.150g(0.010mol)。
Concrete operation step is：Reagent is weighed respectively by above-mentioned dosage, is placed them into mortar, is mixed and is ground It is even, it is then charged into corundum ceramic crucible, is compacted into, be put into Muffle furnace, 500 DEG C is warming up to 10 DEG C/h of speed, Then heat preservation sintering more than 12 hours, grinding is taken out uniformly after being down to room temperature, then 600 DEG C is warming up to 10 DEG C/h of speed Grinding more than 1 time is taken out in sintering more than 24 hours, midway, produces the CsCdPO of pure phase4Compound.
As shown in Fig. 2 the x-ray diffractogram of powder spectrum of compound manufactured in the present embodiment according to its mono-crystalline structures with being fitted The collection of illustrative plates (shown in Fig. 2) of gained is consistent.
Embodiment 2
Prepare powdered CsCdPO4Compound
It is as follows using solid reaction process, reaction equation：
1CsNO3+Cd(NO3)2+(NH4)2HPO4=CsCdPO4+1.5H2O↑+O2↑+2NH3↑+2NO2
Above-mentioned four kinds of reagent inventorys are respectively：CsNO3 1.949g(0.010mol),CdCO3 1.724g (0.010mol),NH4H2PO4 1.150g(0.010mol)。
Concrete operation step is：Reagent is weighed respectively by above-mentioned dosage, is placed them into mortar, is mixed and is ground It is even, it is then charged into corundum ceramic crucible, is compacted into, be put into Muffle furnace, 500 is warming up to 200 DEG C/h of speed DEG C, then heat preservation sintering more than 12 hours, take out grinding uniformly, then be warming up to 200 DEG C/h of speed after being down to room temperature 600 DEG C sinter more than 24 hours, and grinding more than 1 time is taken out in midway, produce the CsCdPO of pure phase4Compound.
The x-ray diffractogram of powder of the x-ray diffractogram of powder spectrum and embodiment 1 of compound manufactured in the present embodiment composes phase Together.
Embodiment 3~4 is to prepare CsCdPO4Crystal
Embodiment 3
Using the CsCdPO described in melt method for growing4Nonlinear optical crystal, comprise the following steps：
CsCdPO prepared by embodiment 1 or 24Compound is placed in crystal growing furnace with fluxing agent, more than 700 DEG C Insulation more than 2 hours, then cools, obtains the crystal.
Described rate of temperature fall is 0.5 DEG C/day.
The fluxing agent is by Cs2O and P2O5It is 0.5-2 according to mol ratio:0-2 is mixed；
Described fluxing agent and described CsCdPO4The mol ratio of compound is 1:0.1-5.5.
Embodiment 4
Using the CsCdPO described in melt method for growing4Nonlinear optical crystal, comprise the following steps：
CsCdPO prepared by embodiment 1 or 24Compound is placed in crystal growing furnace with cosolvent, more than 700 DEG C Insulation more than 2 hours, then cools, obtains the crystal.
Described rate of temperature fall is 1.5 DEG C/day.
The fluxing agent is by Cs2O and P2O5It is 0.5-2 according to mol ratio:0-2 is mixed；
Described fluxing agent and described CsCdPO4The mol ratio of compound is 1:0-5.5.
After tested, the CsCdPO prepared by embodiment 3~44Nonlinear optical crystal is free of symmetrical centre, described CsCdPO4Nonlinear optical crystal is free of symmetrical centre, belongs to monoclinic system P21Space group；The cell parameter of the crystal isβ=90.244 (4), Z=4.As shown in figure 3, the structure of the crystal is CdO4Tetrahedron and PO4Tetrahedron summit connection altogether, forms three-dimensional hole knot Structure, and Cs+Ion is filled out in hole.Crystal of the present invention has frequency-doubled effect.Wherein Fig. 4 is grown using the method for embodiment 4 Crystal, millimetre-sized transparent crystal is prepared using this method.
By the CsCdPO of the gained of embodiment 44Nonlinear optical crystal makees diffuse reflectance spectroscopy, the UV absorption of the crystal Cut-off is less than 243nm；The crystal is not easily broken, nonhygroscopic；By the CsCdPO of the gained of embodiment 44Nonlinear optical crystal, it is placed on Opening position of the shown device of accompanying drawing 1 marked as 3, at room temperature, with tune QNd:YAG laser makees fundamental frequency light source, and incident wavelength is 1064nm near infrared light, output wavelength are 532nm green laser, and laser intensity is approximately equivalent to KH2PO4(KDP) 0.6 times.
Accompanying drawing 1 is to use CsCdPO to the present invention4The simple declaration for the device for non-linear optical that crystal makes.By laser 1, which sends light beam 2, injects CsCdPO4Crystal 3, caused outgoing beam 4 is by filter plate 5, so as to obtain required laser Beam.The nonlinear optics laser can be times frequency generator or upper and lower frequency converter or optical parametric oscillator etc..
Simply technical scheme is explained in detail for above-mentioned embodiment, 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 every according to above-mentioned principle and spirit on the basis of the present invention Improve, substitute, all should be within protection scope of the present invention.

Claims (8)

1.CsCdPO4Compound, it is characterised in that：Described CsCdPO4The chemical formula of compound is CsCdPO4。
2. CsCdPO according to claim 14The preparation method of compound, it is characterised in that：Comprise the following steps：
After Cs compounds, compound containing Cd will be contained and uniformly mixed with stoichiometric proportion containing P-compound, with 10~200 DEG C/h Speed be warming up to 400~500 DEG C, then heat preservation sintering more than 12 hours are down to after room temperature that to take out grinding uniform, then with 10~ 200 DEG C/h of speed is warming up to 500~1100 DEG C and sintered more than 24 hours, produces.
3. CsCdPO according to claim 24The preparation method of compound, it is characterised in that：The compound containing Cs is Cs2CO3Or CsNO3；The compound containing Cd is CdCO3Or Cd (NO3)2；Described containing P-compound is NH4H2PO4Or (NH4)2HPO4。
4.CsCdPO4Nonlinear optical crystal, it is characterised in that：Described CsCdPO4During nonlinear optical crystal is free of symmetrically The heart, belong to monoclinic system P21Space group.
5. CsCdPO according to claim 44Nonlinear optical crystal, it is characterised in that：The cell parameter of the crystal isβ=90.244 (4), Z=4.
6. the CsCdPO according to claim 4 or 54The preparation method of nonlinear optical crystal：
First, after Cs compounds, compound containing Cd will be contained and uniformly mixed with stoichiometric proportion containing P-compound, with 10~200 DEG C/h speed be warming up to 400~500 DEG C, then heat preservation sintering more than 12 hours are down to after room temperature that to take out grinding uniform, 500~1100 DEG C are warming up to 10~200 DEG C/h of speed to sinter more than 24 hours, obtain CsCdPO again4Raw material；
Then, by fluxing agent and described CsCdPO4Raw material mixing after be placed in crystal growing furnace, be warming up to 700 DEG C it is melt above Into melt, the saturation temperature of the melt is then tested, melt is then cooled to more than 5 DEG C of saturation temperature, then slowly dropped Near warm to 600 DEG C, room temperature is then cooled to rapidly, produces CsCdPO4Nonlinear optical crystal；
The fluxing agent is by Cs2O and P2O5It is 0.5-2 according to mol ratio:0-2 is mixed；
Described fluxing agent and described CsCdPO4The mol ratio of raw material is 1:0.1-5.5.
7. the CsCdPO according to claim 4 or 54The purposes of nonlinear optical crystal, it is characterised in that：Described CsCdPO4Nonlinear optical crystal uses as device for non-linear optical.
A kind of 8. device for non-linear optical, it is characterised in that：Including the CsCdPO according to claim 4 or 54Nonlinear optical Learn crystal.
CN201710889137.0A 2017-09-27 2017-09-27 CsCdPO4Compound, CsCdPO4Nonlinear optical crystal and its preparation method and purposes Active CN107792842B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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L. ELAMMARI ET AL: ""Study of phase transitions in the system A1B11PO4 with A1 = Li，Rb and B11 = Mg，Ca，Sr，Ba，Zn，Cd，Pb"", 《PHASE TRANSITIONS: A MULTINATIONAL JOURNAL》 *
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Publication number Priority date Publication date Assignee Title
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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