CN107792842B - 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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CN107792842B
CN107792842B CN201710889137.0A CN201710889137A CN107792842B CN 107792842 B CN107792842 B CN 107792842B CN 201710889137 A CN201710889137 A CN 201710889137A CN 107792842 B CN107792842 B CN 107792842B
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cscdpo
crystal
nonlinear optical
optical crystal
compound
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CN107792842A (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 invention, has many advantages, such as that the speed of growth is very fast, at low cost；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, easy to process；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

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 for making the purposes of device for non-linear optical and comprising CsCdPO4The optics device of nonlinear optical crystal Part.
Background technique
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 the nonlinear optical crystal of ultraviolet band mainly has β-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 1064nm wavelength laser；The birefringence of BBO is bigger than normal, is used for 1064nm wave There are photorefractive effect when the quadruple output of long laser, its output power and beam quality are limited；And CLBO is easily deliquesced, It is difficult to realize commercial applications；KBBF causes it to be difficult to obtain the c crystalline substance big to thickness then due to its serious layer growth habit Body.Therefore, it is still urgent and necessary for exploring the new ultra-violet nonlinear optical crystal of excellent combination property.
Summary of the invention
It is CsCdPO that the first purpose of this invention, which is to provide a kind of chemical formula,4Compound.
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.
Of the invention the 5th is designed to provide CsCdPO4The purposes of nonlinear optical crystal.
Of the invention the 6th is designed to provide a kind of device for non-linear optical.
Technical scheme is as follows:
CsCdPO4Compound, the CsCdPO4The chemical formula of compound is CsCdPO4。
CsCdPO4The preparation method of compound, using the solid reaction process preparation CsCdPO4Compound, including it is as follows Step:
To contain Cs compound, compound containing Cd and containing P-compound with stoichiometric ratio after evenly mixing, with 10~200 DEG C/h rate be warming up to 400~500 DEG C, then heat preservation sintering 12 hours or more, be cooled to room temperature taking-up grinding uniformly, 500~1100 DEG C of sintering 24 hours or more the CsCdPO to get pure phase are warming up to 10~200 DEG C/h of rate again4Change Close object.
Preferably, midway is needed to take out during 500~700 DEG C of sintering grinding 1 time or more,
Preferably, the compound containing Cs is Cs2CO3Or CsNO3；The compound containing Cd is CdCO3Or Cd (NO3)2； The P-compound that contains is NH4H2PO4Or (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, the CsCdPO4Nonlinear optical crystal is free of Symmetrical centre belongs 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 Vertex connection altogether forms three-dimensional hole configurations, 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 includes the following steps:
Firstly, will contain Cs compound, compound containing Cd and containing P-compound with stoichiometric ratio after evenly mixing, with 10~ 200 DEG C/h of rate is warming up to 400~500 DEG C, and then heat preservation sintering 12 hours or more, it is equal to be cooled to room temperature taking-up grinding It is even, then be warming up to 500~1100 DEG C of sintering 24 hours or more with 10~200 DEG C/h of rate, obtain CsCdPO4Raw material；
Then, by fluxing agent and the CsCdPO4Raw material mixing be placed in crystal growing furnace, be warming up to 700 DEG C with On be fused into melt, the saturation temperature (when test, platinum wire test saturation temperature) of the melt is then tested, then by melt 5 DEG C of saturation temperature or more are cooled to, then slow cooling is cooled to room temperature rapidly then near 600 DEG C to get CsCdPO4 Nonlinear optical crystal；
The fluxing agent is by Cs2O and P2O5It is mixed according to molar ratio for 0.5-2:0-2；
The fluxing agent and the CsCdPO4The molar ratio of raw material is 1:0.1-5.5.
The CsCdPO4Nonlinear optical crystal is with physical and chemical performance is stable, hardness is moderate, 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.
The present invention also provides 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 further 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 CsCdPO4After nonlinear optical crystal, the output radiation that at least a branch of frequency is different from incidence electromagnetic radiation is generated.
CsCdPO of the invention4Compound, the compound nonlinear optical crystal and its preparation method and application just like It is lower the utility model has the advantages that
(1) CsCdPO obtained4Nonlinear optical crystal has shorter UV absorption cut-off side, biggish 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 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 CsCdPO4A kind of working principle 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 generated laser Beam, 5 be optical filter.
Fig. 2 is CsCdPO of the invention4Polycrystal powder X ray diffracting spectrum be based on CsCdPO4The X of crystal structure simulation X ray diffraction map.
Fig. 3 is CsCdPO of the invention4Crystal structure figure.
Fig. 4 is the CsCdPO prepared using the method for embodiment 44The picture of nonlinear optical crystal.
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.
Examples 1 and 2 are about powdered CsCdPO4The preparation of compound.
Embodiment 1
Using solid reaction process, reaction equation is as follows:
0.5Cs2CO3+CdCO3+NH4H2PO4=CsCdPO4+1.5CO2↑+1.5H2O↑+NH3↑
Above-mentioned four kinds of reagent inventorys are respectively as follows: Cs2CO3 1.629g(0.005mol),CdCO3 1.724g (0.010mol),NH4H2PO4 1.150g(0.010mol)。
Concrete operation step is: weighing reagent respectively by above-mentioned dosage, places them into mortar, mixes and grind It is even, it is then charged into corundum ceramic crucible, is compacted into, be put into Muffle furnace, be warming up to 500 DEG C with 10 DEG C/h of rate, Then heat preservation sintering 12 hours or more, it is cooled to room temperature taking-up grinding uniformly, then be warming up to 600 DEG C with 10 DEG C/h of rate Sintering 24 hours or more, grinding 1 time or more the CsCdPO to get pure phase was taken out in midway4Compound.
As shown in Fig. 2, the x-ray diffractogram of powder spectrum of compound manufactured in the present embodiment is fitted with according to its mono-crystalline structures Resulting map (shown in Fig. 2) is consistent.
Embodiment 2
Prepare powdered CsCdPO4Compound
Using solid reaction process, reaction equation is as follows:
1CsNO3+Cd(NO3)2+(NH4)2HPO4=CsCdPO4+1.5H2O↑+O2↑+2NH3↑+2NO2
Above-mentioned four kinds of reagent inventorys are respectively as follows: CsNO3 1.949g(0.010mol),CdCO3 1.724g (0.010mol),NH4H2PO4 1.150g(0.010mol)。
Concrete operation step is: weighing reagent respectively by above-mentioned dosage, places them into mortar, mixes and grind It is even, it is then charged into corundum ceramic crucible, is compacted into, be put into Muffle furnace, be warming up to 500 with 200 DEG C/h of rate DEG C, then heat preservation sintering 12 hours or more, it is cooled to room temperature taking-up grinding uniformly, then be warming up to 200 DEG C/h of rate Grinding 1 time or more the CsCdPO to get pure phase is taken out in 600 DEG C of sintering 24 hours or more, midway4Compound.
The x-ray diffractogram of powder spectrum and the x-ray diffractogram of powder of embodiment 1 of compound manufactured in the present embodiment compose phase Together.
Embodiment 3~4 is to prepare CsCdPO4Crystal
Embodiment 3
Using CsCdPO described in melt method for growing4Nonlinear optical crystal includes the following steps:
CsCdPO prepared by embodiment 1 or 24Compound and fluxing agent are placed in crystal growing furnace, 700 DEG C with Upper heat preservation 2 hours or more, then cools down, obtain the crystal.
The rate of temperature fall is 0.5 DEG C/day.
The fluxing agent is by Cs2O and P2O5It is mixed according to molar ratio for 0.5-2:0-2；
The fluxing agent and the CsCdPO4The molar ratio of compound is 1:0.1-5.5.
Embodiment 4
Using CsCdPO described in melt method for growing4Nonlinear optical crystal includes the following steps:
CsCdPO prepared by embodiment 1 or 24Compound and cosolvent are placed in crystal growing furnace, 700 DEG C with Upper heat preservation 2 hours or more, then cools down, obtain the crystal.
The rate of temperature fall is 1.5 DEG C/day.
The fluxing agent is by Cs2O and P2O5It is mixed according to molar ratio for 0.5-2:0-2；
The fluxing agent and the CsCdPO4The molar ratio of compound is 1:0-5.5.
After tested, 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 is total to vertex Connection forms three-dimensional hole configurations, and Cs+Ion is filled out in hole.Crystal of the present invention has frequency-doubled effect.Wherein Fig. 4 is to adopt The crystal grown with the method for embodiment 4, is prepared millimetre-sized transparent crystal using this method.
By the resulting CsCdPO of embodiment 44Nonlinear optical crystal makees diffuse reflectance spectroscopy, the UV absorption of the crystal Cut-off is lower than 243nm；The crystal is not easily broken, nonhygroscopic；By the resulting CsCdPO of embodiment 44Nonlinear optical crystal is placed on At position of 1 shown device of attached drawing marked as 3, at room temperature, with adjusting Q Nd:YAG laser to make fundamental frequency light source, incident wavelength is The near infrared light of 1064nm, output wavelength are the green laser of 532nm, and laser intensity is approximately equivalent to KH2PO4(KDP) 0.6 Times.
Attached drawing 1 is to use CsCdPO to the present invention4The simple declaration of the device for non-linear optical of crystal production.By laser 1, which issues light beam 2, injects CsCdPO4Crystal 3, generated outgoing beam 4 is by filter plate 5, thus laser required for obtaining Beam.The nonlinear optics laser can be times frequency generator or upper and lower frequency converter or optical parametric 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 (5)

1.CsCdPO4Nonlinear optical crystal, it is characterised in that: the CsCdPO4Nonlinear optical crystal is free of in symmetrical The heart belongs to monoclinic system P21Space group.
2. CsCdPO according to claim 14Nonlinear optical crystal, it is characterised in that: the cell parameter of the crystal is A=9.0589 (4), b=5.6406 (2), c=9.4634 (4), β=90.244 (4), V=483.55 (3) Å3, Z=4.
3. CsCdPO according to claim 1 or 24The preparation method of nonlinear optical crystal:
Firstly, will contain Cs compound, compound containing Cd and containing P-compound with stoichiometric ratio after evenly mixing, with 10~200 DEG C/h rate be warming up to 400~500 DEG C, then heat preservation sintering 12 hours or more, be cooled to room temperature taking-up grinding uniformly, It is warming up to 500~1100 DEG C of sintering 24 hours or more with 10~200 DEG C/h of rate again, obtains CsCdPO4Raw material；
Then, by fluxing agent and the CsCdPO4Raw material mixing is placed in crystal growing furnace, is warming up to 700 DEG C or more and is melted It is melted into melt, the saturation temperature of the melt is then tested, melt is then cooled to 5 DEG C of saturation temperature or more, then slowly 600 DEG C are cooled to, is cooled to room temperature rapidly then to get CsCdPO4Nonlinear optical crystal；
The fluxing agent is by Cs2O and P2O5It is mixed according to molar ratio for 0.5-2: 0-2；
The fluxing agent and the CsCdPO4The molar ratio of raw material is 1: 0.1-5.5.
4. CsCdPO according to claim 1 or 24The purposes of nonlinear optical crystal, it is characterised in that: described CsCdPO4Nonlinear optical crystal is used as device for non-linear optical.
5. a kind of device for non-linear optical, it is characterised in that: including CsCdPO according to claim 1 or 24Nonlinear 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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