CN107190318A - A kind of second-order non-linear optical crystal material and its preparation and application - Google Patents
A kind of second-order non-linear optical crystal material and its preparation and application Download PDFInfo
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- CN107190318A CN107190318A CN201710320951.0A CN201710320951A CN107190318A CN 107190318 A CN107190318 A CN 107190318A CN 201710320951 A CN201710320951 A CN 201710320951A CN 107190318 A CN107190318 A CN 107190318A
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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
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The present invention relates to a kind of novel crystal material and preparation method and application, the chemical formula of the crystalline material is NaSr3(OH)(B9O16)[B(OH)4], belong to trigonal system, space group is P31c, and cell parameter is α=β=90 °, γ=120 °, Z=2.Compared with prior art, crystalline material of the present invention has larger frequency-doubled effect, about KH2PO4(KDP) 3.20 times of crystal, 0.45 times of bbo crystal.In addition, the crystalline material has wider transmission scope, its UV-permeable cut-off side is less than 190nm, is with a wide range of applications in fields such as nonlinear optics, Electro-optical Modulation, Preset grating information processings.
Description
Technical field
The present invention relates to optical crystal material technical field, and in particular to a kind of second-order non-linear optical crystal material and its
Preparation and application.
Background technology
Second-order non-linear optical crystal is typically characterised by with frequency-doubled effect (SHG), is a kind of important photoelectric functional
Material, the extensive use in terms of frequency doubling device, Electro-optical Modulation, holographic memory element.Largely there is the metal boron of non-core structure
Hydrochlorate has excellent second-order nonlinear optical property, has attracted the broad interest of domestic and international research worker.Current Yi cities
Wide variety of nonlinear optical crystal includes LiB on field3O5(being abbreviated as LBO), β-BaB2O4(being abbreviated as BBO) and in depth
Ultra-violet (UV) band can realize the KBe of frequency-doubled effect2BO3F2The most short output wavelength of (being abbreviated as KBBF) etc., wherein KBBF crystalline materials can
Reach 179.4nm.
But the preparation method of these materials is mostly high temperature process heat at present, and the pure phase of compound is difficult to make
Standby, nonlinear optical coefficients also await further raising.
The content of the invention
The purpose of the present invention is exactly in order to overcome defect present on above-mentioned existing synthetic method, so that providing one kind has
Simple second-order non-linear optical crystal material of larger frequency-doubled effect, preparation method and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：A kind of second-order non-linear optical crystal material, institute
The chemical formula for stating crystalline material is NaSr3(OH)(B9O16)[B(OH)4], the crystalline material is trigonal system, and its space group is
P31c, the cell parameter of the crystalline material is α=
β=90 °, γ=120 °, Z=2.The crystalline material has larger frequency-doubled effect, about the 3.20 of KDP crystal times, bbo crystal
0.45 times.In addition, the crystalline material has wider transmission scope, its UV-permeable cut-off side is less than 190nm, non-linear
The fields such as optics, Electro-optical Modulation, Preset grating information processing have wide practical use.
Preferably, the cell parameter of the crystalline material is Z=2, unit cell volume is
The inorganic compound NaSr3(OH)(B9O16)[B(OH)4] crystal structure it is as follows：Each B atoms and 3 O originals
Son or 4 O atoms connect the BO to be formed3Planar delta or BO4Tetrahedral structure, 3 BO3Triangle and 6 BO4Tetrahedron leads to
Cross side altogether and the mode on summit forms B altogether9O16Cluster, each B9O16Cluster and six adjacent identical B9O16Cluster is connected, flat in (001)
Face forms three-dimensional zeolites shape structure, and Na ions and Sr ions are filled in zeolite structured duct.The BO of planar delta3And distortion
BO4Tetrahedral cooperative effect causes the big second order nonlinear effect of compound.
According to the another aspect of the application there is provided the preparation method of the crystalline material, prepared using hydro-thermal method, strontium
Source, sodium source, boron source, mineralizer and water are mixed to form initial gel mixture, and water is as reaction medium, barium source, sodium source under normal temperature
Solubility is relatively low in water with boron source, and the gel compound for being conducive to above-mentioned three to be formed under HTHP dissolves and reacted,
Material is obtained in crystallization at 180~240 DEG C, mineralizer is not involved in the reaction, but the formation to crystal has facilitation.
The mol ratio of sodium element, strontium element, boron element, mineralizer and water in described initial gel mixture is Na:
Sr:B:Mineralizer:Water=(2~40)：(0.5~10)：(4~40)：(0.1~5)：(200~1000), it is furthermore preferred that Na:
Sr:B:Mineralizer:Water=(4~12)：(1~3)：(4~12)：(1~3)：(200~400).
It is preferred that, described sodium source is selected from sodium chloride, sodium hydroxide, sodium carbonate, sodium nitrate, sodium acetate, sodium tetraborate, partially
At least one of Boratex, four eight Boratexes of hydration.
It is preferred that, described barium source is in strontium nitrate, strontium hydroxide, strontium carbonate, strontium fluoride, strontium chloride, strontium metaborate
At least one.
It is preferred that, described boron source be selected from boric acid, boric anhydride, lithium metaborate, kodalk, sodium tetraborate, potassium metaborate,
At least one of magnesium metaborate, calcium metaborate, barium metaborate, lead borate, four eight Boratexes of hydration.
Preferably, the sodium source and boron source are hydrated eight Boratexes from same compound four, i.e., four eight Boratexes of hydration were both
It is that sodium source is also boron source.The barium source and boron source are both barium source and boron from same compound strontium metaborate, i.e. strontium metaborate
Source.
It is preferred that, described mineralizer is selected from least one of hydrofluoric acid, potassium fluoride, sodium fluoride.
It is preferred that, described crystallization temperature is 200~240 DEG C, and crystallization time is no less than 24 hours, it is furthermore preferred that crystallization
Time is 24~240 hours.
According to the another aspect of the application there is provided a kind of laser frequency converter, containing any of the above-described crystalline material or
As the crystalline material prepared by any of the above-described method.
According to the another aspect of the application there is provided the application process of the laser frequency converter, for being by wavelength
1.064 μm of laser beam with two frequencys multiplication or frequency tripling harmonic wave, simultaneously can be used for wavelength be 532nm laser beam with
Two multiplied frequency harmonics are exported.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects：
(1) this application provides a kind of novel crystal material, crystalline material has larger frequency-doubled effect, and about KDP is brilliant
3.20 times of body, 0.45 times of bbo crystal.In addition, the crystalline material has wider transmission scope, its UV-permeable cut-off side
Less than 190nm, have wide practical use in fields such as nonlinear optics, Electro-optical Modulation, Preset grating information processings.
(2) this application provides the preparation method of above-mentioned crystalline material, the not high using reaction condition gentle hydro-thermal method
Warm solid phase method, in a low temperature of 180~240 DEG C, by hydrothermal crystallizing, can high productivity obtain high-purity sample.Method is simple,
Mild condition, is advantageously implemented large-scale industrial production.
(3) this application provides application above-mentioned material laser frequency converter, available for by wavelength for 1.064 μm swash
Light light beam simultaneously can be used for laser beam that wavelength is 532nm with two multiplied frequency harmonics with two frequencys multiplication or frequency tripling harmonic wave
Output.
Brief description of the drawings
Fig. 1 is NaSr3(OH)(B9O16)[B(OH)4] crystal structure schematic diagram；
Fig. 2 is sample 1# X ray diffracting spectrum；Wherein (a) is the crystal parsed according to single crystal X-ray diffraction data
Structure, is fitted obtained X ray diffracting spectrum；(b) it is that sample 1# pulverizes the collection of illustrative plates that the test of last X-ray diffraction obtains；
The diffusing reflection absorption that Fig. 3 is sample 1# passes through spectrum；
Fig. 4 is second harmonic phase matched figures of the sample 1# under 1.064 mu m wavebands；
Fig. 5 is second harmonic phase matched figures of the sample 1# under 532nm wave bands；
Fig. 6 be sample 1# and standard specimen KDP size in 105-150 μ ms second harmonic signal figure；
Fig. 7 be sample 1# and standard specimen BBO size in 105-150 μ ms second harmonic signal figure.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
The preferred NaSr of inorganic compound is prepared as one3(OH)(B9O16)[B(OH)4] preferred embodiment, Dian Xingfang
Method is as follows：By raw material Sr (OH)2·8H2O and Na2B8O13·4H2O and watertight, which are encapsulated in hydrothermal reaction kettle, carries out hydro-thermal reaction, instead
It is 180~240 DEG C to answer temperature, and the reaction time is 1~10 day, and then slow cooling is to 30 DEG C, cooling rate is 0.5~30 DEG C/
My god, filtering cleaning, you can obtain the NaSr of colourless needles3(OH)(B9O16)[B(OH)4] crystal.
Embodiment 1
(1) preparation of 1#~9# samples
Barium source, sodium source, boron source, mineralizer and water are uniformly mixed to get initial gel mixture according to a certain percentage, will be just
Beginning gel mixture is sealed in the hydrothermal reaction kettle of 25mL polytetrafluoroethyllining lining, is put into chamber type electric resistance furnace, in crystallization
At a temperature of crystallization for a period of time after, through filtering, cleaning, dry, obtain colourless needles NaSr3(OH)(B9O16)[B(OH)4] crystal
Sample.The species and proportioning of raw material in initial gel mixture, crystallization temperature, the relation such as table 1 of crystallization time and sample number into spectrum
It is shown.
The relation of the sample synthesis condition of table 1. and sample number into spectrum
(2) crystallographic structural analysis of sample
Using single crystal X-ray diffraction and powder x-ray diffraction method, structure elucidation is carried out to sample 1#~9#.
Wherein single crystal X-ray diffraction is on German Bruker companies D8VENTURE CMOS X-type X-ray single crystal diffractometers
Carry out.Crystalline size is 0.20 × 0.12 × 0.1mm3；Data Collection temperature is 293K, and diffraction light sources are graphite monochromatised
Mo-K alpha raysScan mode is ω -2 θ；Data are carried out at absorption correction using Multi-Scan methods
Reason.Structure elucidation is completed using SHELXTL-97 program bags；The position of heavy atom is determined with direct method, is synthesized with difference Fourier
Method obtains remaining atomic coordinates；With based on F2All atoms of complete matrix least square method refine coordinate and anisotropy physochlaina infudibularis
Number.
Powder x-ray diffraction is carried out on the x-ray powder diffraction instrument of German Bruker companies Bruker D8 types, test
Condition is fixed target monochromatic source Cu-K α, wavelengthVoltage x current is 40kV/20A, slit DivSlit/
RecSlit/SctSlit is respectively 2.00deg/0.3mm/2.00deg, 5-70 ° of scanning range, 0.02 ° of scanning step.
Wherein, single crystal X-ray diffraction result is shown, sample 1#~10# has identical chemical structural formula and crystal structure,
Chemical formula is NaSr3(OH)(B9O16)[B(OH)4], belong to trigonal system, space group is P31c, and cell parameter isα=β=90 °, γ=120 °, Z=2, unit cell volume
For
Using sample 1# as Typical Representative, its crystal structural data is α=β=90 °, γ=120 °, Z=2, unit cell volume is As shown in table 2, its crystal structure is as shown in Figure 1 for each atomic coordinates of sample 1#.
Each atomic coordinates, equivalent thermal parameter and occupation rate in the sample 1# of table 2.
Wherein, powder x-ray diffraction result is shown, sample 1#~9# is on XRD spectra, and peak is essentially identical, respectively
Sample peak intensity slightly has difference.
Using sample 1# as Typical Representative, as shown in Figure 2.The crystal parsed in Fig. 2 (a) according to its single crystal X-ray diffraction
Structure, is fitted obtained X ray diffracting spectrum with testing what is obtained through X-ray diffraction after sample 1# grind into powders in Fig. 2 (b)
Collection of illustrative plates, peak is consistent with peak intensity.Illustrate that gained sample has very high-purity.
(3) absorption spectrum is tested
Sample 1# diffusing reflection absorption spectrum is tested in Shimadzu Corporation's UV-3600Plus types ultraviolet-visible-near-infrared light splitting
Carried out on photometer.As a result as shown in figure 3, the compound does not absorb significantly 190 to 2000nm as seen from Figure 3.
The compound has wider transmission scope, and its ultraviolet cut-on side is less than 190nm.
(4) frequency multiplication test experiments and result
Sample 1# frequency multiplication test experiments are specific as follows：Using the Nd for adjusting Q:YAG solid state lasers produce wavelength be
1064nm and 532nm laser is as fundamental frequency light, and the tested crystal powder of irradiation detects what is produced respectively using photomultiplier
532nm and 266nm second harmonic, with oscilloscope display harmonic wave intensity.By crystal prototype to be measured and standard sample KDP crystal and
Bbo crystal is ground respectively, screens out the crystal of variable grain degree with standard screen, size range be respectively less than 26,26~50,
50~74,74~105,105~150,150~200 μm.Frequency-doubled signal is observed with the variation tendency of granularity, whether it is judged
Phase matched can be realized.Under same test condition, intensity and the reference crystal KDP of the second harmonic produced by comparative sample
With the second harmonic intensity produced by BBO, so as to obtain the relative size of sample frequency-doubled effect.
Test result shows compound N aSr3(OH)(B9O16)[B(OH)4] crystal has great frequency-doubled effect.Such as Fig. 4
With shown in Fig. 5, respectively KH2PO4(KDP) 3.20 times of crystal, BBO (β-BaB2O4) 0.45 times of crystal.Such as Fig. 6 and Fig. 7 institutes
Show, phase matched can be realized in visible ray and ultraviolet band.
Embodiment 2
Using preparation method similar to Example 1, difference is：
(1) sodium source used is sodium chloride, and the barium source used is strontium nitrate, and the boron source used is boric acid, the mineralising of use
Thing is hydrofluoric acid, wherein, the mol ratio of sodium element, strontium element, boron element, mineralizer and water in initial gel mixture is
Na:Sr:B:Mineralizer:Water=2:0.5:40:5:200；
(2) crystallization temperature used is 180 DEG C, and crystallization time is 24 hours.
After testing, obtained compound N aSr3(OH)(B9O16)[B(OH)4] crystal has great frequency-doubled effect, point
Wei not KH2PO4(KDP) 3.2 times of crystal, BBO (β-BaB2O4) 0.45 times of crystal.
Embodiment 3
Using preparation method similar to Example 1, difference is：
(1) sodium source used for sodium carbonate, the mixture of sodium nitrate, the barium source used for strontium carbonate and strontium chloride mixing
Thing, the boron source used for boric anhydride, the mineralizer used for NaF, wherein, sodium element, strontium element in initial gel mixture,
The mol ratio of boron element, mineralizer and water is Na:Sr:B:Mineralizer:Water=40:10:4:0.1:1000；
(2) crystallization temperature used is 240 DEG C, and crystallization time is 240 hours.
After testing, obtained compound N aSr3(OH)(B9O16)[B(OH)4] crystal has great frequency-doubled effect, point
Wei not KH2PO4(KDP) 3.2 times of crystal, BBO (β-BaB2O4) 0.45 times of crystal.
Embodiment 4
Using preparation method similar to Example 1, difference is：
(1) sodium source used is sodium acetate, and the barium source used is strontium metaborate and the mixture of strontium fluoride, the boron source of use
For potassium metaborate and the mixture of magnesium metaborate, the mineralizer used for NaF, wherein, sodium element in initial gel mixture,
Strontium element, boron element, the mol ratio of mineralizer and water are Na:Sr:B:Mineralizer:Water=4:1:12:3:50；
(2) crystallization temperature used is 200 DEG C, and crystallization time is 72 hours.
After testing, obtained compound N aSr3(OH)(B9O16)[B(OH)4] crystal has great frequency-doubled effect, point
Wei not KH2PO4(KDP) 3.2 times of crystal, BBO (β-BaB2O4) 0.45 times of crystal.
Embodiment 5
Using preparation method similar to Example 1, difference is：
(1) sodium source used is sodium tetraborate and the mixture of kodalk, and the barium source used is strontium carbonate, the boron of use
Source is barium metaborate, the mixture of lead borate, the mineralizer used for NaF, wherein, sodium element in initial gel mixture,
Strontium element, boron element, the mol ratio of mineralizer and water are Na:Sr:B:Mineralizer:Water=12:3:4:1:400；
(2) crystallization temperature used is 195 DEG C, and crystallization time is 100 hours.
After testing, obtained compound N aSr3(OH)(B9O16)[B(OH)4] crystal has great frequency-doubled effect, point
Wei not KH2PO4(KDP) 3.2 times of crystal, BBO (β-BaB2O4) 0.45 times of crystal.
Claims (10)
1. a kind of second-order non-linear optical crystal material, it is characterised in that the chemical formula of the crystalline material is NaSr3(OH)(B9O16)[B
(OH)4], it is trigonal system, its space group is P31c, cell parameter is
α=β=90 °, γ=120 °, Z=2.
2. a kind of preparation method of second-order non-linear optical crystal material as claimed in claim 1, it is characterised in that this method is
Hydro-thermal method, specifically includes following steps：Sodium source, barium source, boron source, mineralizer and water are mixed to form initial gel mixture,
Crystallization produces the crystalline material at 180~240 DEG C.
3. the preparation method of a kind of second-order non-linear optical crystal material according to claim 2, it is characterised in that described
Initial gel mixture in sodium element, strontium element, boron element, the mol ratio of mineralizer and water be Na:Sr:B:Mineralizer:
Water=(2~40)：(0.5~10)：(4~40)：(0.1~5)：(200~1000), it is preferred that Na:Sr:B:Mineralizer:Water=
(4~12)：(1~3)：(4~12)：(1~3)：(200~400).
4. a kind of preparation method of second-order non-linear optical crystal material according to Claims 2 or 3, it is characterised in that
Described sodium source is selected from sodium chloride, sodium hydroxide, sodium carbonate, sodium nitrate, sodium acetate, sodium tetraborate, kodalk, four hydrations eight
At least one of Boratex.
5. a kind of preparation method of second-order non-linear optical crystal material according to Claims 2 or 3, it is characterised in that
Described barium source is selected from least one of strontium nitrate, strontium hydroxide, strontium carbonate, strontium fluoride, strontium chloride, strontium metaborate.
6. a kind of preparation method of second-order non-linear optical crystal material according to Claims 2 or 3, it is characterised in that
Described boron source is selected from boric acid, boric anhydride, lithium metaborate, kodalk, sodium tetraborate, potassium metaborate, magnesium metaborate, metaboric acid
At least one of calcium, barium metaborate, lead borate, four eight Boratexes of hydration.
7. a kind of preparation method of second-order non-linear optical crystal material according to Claims 2 or 3, it is characterised in that
Described mineralizer is selected from least one of hydrofluoric acid, potassium fluoride, sodium fluoride.
8. the preparation method of a kind of second-order non-linear optical crystal material according to claim 2, it is characterised in that described
Crystallization temperature be 200~240 DEG C, crystallization time be no less than 24 hours.
9. a kind of application of second-order non-linear optical crystal material as claimed in claim 1, it is characterised in that the crystalline material is used
In laser frequency converter.
10. the application of a kind of second-order non-linear optical crystal material according to claim 9, it is characterised in that described
It is 1.064 μm of laser beam with two frequencys multiplication or frequency tripling harmonic wave that laser frequency converter, which is used for wavelength, or for ripple
A length of 532nm laser beam is exported with two multiplied frequency harmonics.
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| CN111117612A (en) * | 2018-11-01 | 2020-05-08 | 中国科学院福建物质结构研究所 | White light fluorescent material and preparation method and application thereof |
| CN111217349A (en) * | 2020-01-13 | 2020-06-02 | 合肥学院 | Second-order nonlinear optical material aluminophosphate and preparation method and application thereof |
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| CN111117612A (en) * | 2018-11-01 | 2020-05-08 | 中国科学院福建物质结构研究所 | White light fluorescent material and preparation method and application thereof |
| CN111117612B (en) * | 2018-11-01 | 2021-02-12 | 中国科学院福建物质结构研究所 | White light fluorescent material and preparation method and application thereof |
| CN111217349A (en) * | 2020-01-13 | 2020-06-02 | 合肥学院 | Second-order nonlinear optical material aluminophosphate and preparation method and application thereof |
| CN111217349B (en) * | 2020-01-13 | 2021-10-22 | 合肥学院 | Second-order nonlinear optical material aluminophosphate and preparation method and application thereof |
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