CN109811409A - A kind of middle infrared nonlinear optical crystal material of high laser damage threshold and its preparation method and application - Google Patents
A kind of middle infrared nonlinear optical crystal material of high laser damage threshold and its preparation method and application Download PDFInfo
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- CN109811409A CN109811409A CN201910166180.3A CN201910166180A CN109811409A CN 109811409 A CN109811409 A CN 109811409A CN 201910166180 A CN201910166180 A CN 201910166180A CN 109811409 A CN109811409 A CN 109811409A
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- 230000003287 optical effect Effects 0.000 title claims abstract description 84
- 239000000463 material Substances 0.000 title claims abstract description 73
- 239000013078 crystal Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 7
- 230000004580 weight loss Effects 0.000 claims abstract description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000011780 sodium chloride Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 241001074085 Scophthalmus aquosus Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229910007475 ZnGeP2 Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
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- Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
Abstract
The invention discloses middle infrared nonlinear optical crystal material of a kind of high laser damage threshold and its preparation method and application, chemical formula Pb7F12Cl2, it is 0.27-20 μm through range that powder SHG effect, which is 2 times of potassium dihydrogen phosphate,;Optical band gap value is 4.5eV, and the laser damage threshold of powder is 80MW/cm2, thermal weight loss temperature is 570 °C;When preparation, the Pb7F12Cl2It is prepared using hydro-thermal reaction method or solution deposit;Middle infrared nonlinear optical crystal material provided by the invention have it is stronger can phase matched second order nonlinear optical effect, there is wider optical transmission window in visible region and mid-infrared light area, with very high laser damage threshold and thermal stability, synthetic method is easy to operate, product purity is high, can be widely used in optical field.
Description
Technical field
The present invention relates to inolrganic chemicals technical field, the middle infrared non-linear of specifically a kind of high laser damage threshold
Optical crystal material and its preparation method and application.
Background technique
Nonlinear optical effect originates from the interaction of laser and medium.When laser is with non-zero second order susceptibility
When Propagation, the nonlinear optical effects such as frequency multiplication and frequency, difference frequency, optically erasing can be generated.It is non-using the second order of crystal
The nonlinear opticses device such as second harmonic generator, frequency converter, optical parametric oscillator can be made in linear optics effect
Part suffers from important application value such as laser technology, atmospheric monitoring, defense military etc. in many fields.It is inorganic non-
Linear optical material occupies leading position in the practical research of second-order non-linear optical materials.According to transmission region and applicable model
It encloses, inorganic nonlinear optical crystal material can be divided into ultraviolet region nonlinear optical material, visible region nonlinear optical material
With infrared light district nonlinear optical material.
Middle infrared band non-linear optical crystal material has in terms of laser spectrum, optical communication and high intensity laser beam
Highly important application is a kind of important new and high technology material.When the medium interaction of laser and non-centrosymmetric structure
When, nonlinear optical effect, such as frequency multiplication, optical parametric oscillation and the Preset grating of laser will be generated.Utilize the non-thread of crystal
Property optical effect, may be implemented the conversion of laser frequency, obtains the laser of more different wave lengths, so that it is continuous to open up new wavelength
Adjustable laser light source, manufactured device can be widely applied for the fields such as optical information storage, laser communications, laser countermeasure (s).
Current commercialized middle infrared band non-linear optical crystal material is mainly with the chalcopyrite compound of chalcogen class
Based on, such as AgGaS2、AgGaSe2、ZnGeP2Deng, they the advantages of be that all there are biggish nonlinear optical coefficients and preferable
It is infrared to penetrate range.However this kind of materials lead to their laser damage threshold often due to its characteristic of semiconductor, band gap is narrow
It is low, so that serious limit their application range.Therefore, the novel middle infrared band for studying high laser damage threshold is non-thread
Property optical crystal material is one of forward position and the significant challenge in current nonlinear optical material field.
Summary of the invention
It is an object of the invention to provide a kind of high laser damage threshold, preparation method is simple and stability it is good in it is infrared
Non-linear optical crystal material Pb7F12Cl2And its preparation method and application.
The present invention is achieved through the following technical solutions:
A kind of middle infrared nonlinear optical crystal material of high laser damage threshold of the invention, chemical formula Pb7F12Cl2。
Preferably, heretofore described middle infrared nonlinear optical crystal material Pb7F12Cl2Powder SHG effect be phosphorus
2 times of acid dihydride potassium are 0.27-20 μm through range.
Preferably, heretofore described middle infrared nonlinear optical crystal material Pb7F12Cl2Optical band gap value be
4.5eV, the laser damage threshold of powder are 80MW/cm2, about commercialization materials A gGaS2(5.2MW/cm2) 16 times, heat lose
Degree of reviewing is 570 °C.
The present invention also provides a kind of preparation method of the middle infrared nonlinear optical crystal material of high laser damage threshold,
The Pb7F12Cl2It is prepared using hydro-thermal reaction method or solution deposit.
Heretofore described hydro-thermal reaction method is by PbF2It is dissolved in aqueous solution with NaCl, carries out hydro-thermal reaction.
Preferably, heretofore described hydro-thermal reaction method is the PbF for being 7:2 by molar ratio2It is anti-that hydro-thermal is added to NaCl
Answer in kettle, be added water, be put into Muffle furnace after reaction kettle is sealed, 230 DEG C, then isothermal reaction 7 days be heated in 3h, with 1 DEG C/
The speed of h is cooled to 30 DEG C, after cooling, is washed with distilled water product, dries after suction filtration, obtains colorless and transparent small crystals,
As middle infrared nonlinear optical crystal material.
Further, heretofore described reaction kettle, liner are polytetrafluoroethylene (PTFE).
Heretofore described solution deposit is by PbF2It is added with NaCl into distilled water, heating stirring can be obtained
White precipitate, after filter, washing and drying.
Further, heretofore described solution deposit is the PbF for being 7:2 by molar ratio2It is added with NaCl to temperature
For in 70-80 DEG C of distilled water, heating stirring to temperature is 90-100 DEG C, white precipitate can be obtained, white precipitate is filtered,
After distilling water washing 2-3 times, being dry.
The present invention also provides a kind of middle infrared nonlinear optical crystal materials of high laser damage threshold in optical field
In application.
Since often there is biggish band gap containing fluorine halide, it is beneficial to improve the laser damage threshold of material.Therefore,
The middle infrared nonlinear optical crystal material that novel high laser damage threshold is found from containing fluorine halide is a kind of new spy
Rope approach.The present invention is with PbF2With NaCl be initial reactant, with hydro-thermal reaction method or solution deposit prepared in it is infrared
Non-linear optical crystal material Pb7F12Cl2.As the strong heavy metal atom Pb of metallicity and F bonding, it will there is bigger band
Therefore gap value, explores high laser grandson damage threshold so as to cause higher laser damage threshold from containing halide of the Pb containing F
The middle infrared nonlinear optical crystal material of value is also a kind of preferable approach.Experiment shows infrared non-thread in the present invention
Property optical crystal material powder frequency-doubled effect be 2 times of KDP;Phase matched can be achieved;It is 0.27-20 μm that full impregnated, which crosses range,;
The laser damage threshold of powder is 80MW/cm2;Thermal weight loss temperature is 570 °C.
Inorganic middle FTIR radiation transmittance Pb disclosed in this invention7F12Cl2With [Pb3F9Cl]4-As anion base
Group has the distortion not exclusively offset, can generate dipole moment, which arranges in crystal unanimously, to show macroscopically
Nonlinear optical effect.And the compound be free of the crystallization water, middle infrared transparency range up to 20 μm;UV absorption
Ending side is 0.27 μm.With very high laser damage threshold (80MW/cm2), it is about commercialization material under same test condition
Expect AgGaS2(5.2MW/cm2) 16 times, nonlinear optical effect is 2 times of KDP.Therefore, it has excellent comprehensive performance,
It can be used as middle infrared nonlinear optical crystal material to be applied.
Compared with prior art, inorganic middle infrared nonlinear optical crystal material of the invention has the advantage that
1. having can show that its powder SHG effect is phosphorus with the frequency-doubled effect (SHG) of phase matched, powder frequency doubling test result
2 times of acid dihydride potassium (KDP);
2. the laser damage threshold of compound powder is 80MW/cm2, it is current commercial middle infrared nonlinear optical crystal
Material AgGaS2It (is 5.2 MW/cm under same test condition2) 16 times of laser damage threshold.
3. the powder of the compound has wider through range in visible region and mid-infrared light area, it is through wave band
0.27〜20μm;
4. being free of the crystallization water, to air-stable, and better heat stability, thermal weight loss temperature have reached 570 DEG C;
5. material can be prepared using simple hydro-thermal reaction method or solution deposit.
6. middle infrared nonlinear optical crystal material provided by the invention have it is stronger can phase matched second nonlinear
Optical effect has wider optical transmission window in visible region and mid-infrared light area, has very high laser damage threshold and heat steady
Qualitative, synthetic method is easy to operate, product purity is high, can be widely used in optical field.
Detailed description of the invention
Fig. 1 is Pb of the present invention7F12Cl2[Pb3F9Cl]4- Group configuration picture;
Fig. 2 is Pb of the present invention7F12Cl2In [Pb3F9Cl]4-Group arrangement figure;
Fig. 3 is Pb of the present invention7F12Cl2The UV-visible-near infrared absorption of powder;
Fig. 4 is Pb of the present invention7F12Cl2The Fourier transform decaying infrared absorption spectrum of powder;
Fig. 5 is Pb of the present invention7F12Cl2The hot property map of powder;
Fig. 6 is Pb of the present invention7F12Cl2The frequency-doubled effect phase matched map of powder.
Specific embodiment
Embodiment 1
A kind of middle infrared nonlinear optical crystal material of high laser damage threshold of the present embodiment, chemical formula are
Pb7F12Cl2。
Middle infrared nonlinear optical crystal material Pb described in the present embodiment7F12Cl2Powder SHG effect be di(2-ethylhexyl)phosphate
2 times of hydrogen potassium are 0.27-20 μm through range.
Middle infrared nonlinear optical crystal material Pb described in the present embodiment7F12Cl2Optical band gap value be 4.5eV, powder
The laser damage threshold at end is 80MW/cm2, about commercialization materials A gGaS2(5.2MW/cm2) 16 times, thermal weight loss temperature is
570°C。
The present embodiment additionally provides a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold
Method, the Pb7F12Cl2It is prepared using hydro-thermal reaction method.
Hydro-thermal reaction method described in the present embodiment is by PbF2Be dissolved in aqueous solution with NaCl, carry out hydro-thermal reaction to get
To middle infrared nonlinear optical crystal material.
Preferably, hydro-thermal reaction method described in the present embodiment is the PbF for being 7:2 by molar ratio2Hydro-thermal is added to NaCl
In reaction kettle, water is added, is put into Muffle furnace after reaction kettle is sealed, 230 DEG C, then isothermal reaction 7 days is heated in 3h, with 1
DEG C/speed of h is cooled to 30 DEG C, after cooling, it is washed with distilled water product, is dried after suction filtration, colorless and transparent small crystalline substance is obtained
Body.
Further, heretofore described reaction kettle, liner are polytetrafluoroethylene (PTFE).
By middle infrared nonlinear optical crystal material Pb manufactured in the present embodiment7F12Cl2Carry out coherent detection, test result
It is as follows:
(1) powder SHG effect is tested:
The frequency doubling property of middle infrared nonlinear optical crystal material is obtained by Kurtz-Perry powder frequency doubling test method.Tool
Steps are as follows for gymnastics work:
Middle infrared nonlinear optical crystal material prepared by embodiment 1 is ground into the powder that partial size is about 150~200 μm, so
Have in the sample cell of windowpane mounted in two sides afterwards, sample cell is placed on laser optical path later, uses Nd:YAG pulse laser
For light source generation wavelength be 1064nm fundamental frequency light inject sample cell, using about 150~200 μm of partial size of KDP monocrystal as
Standard specimen, signal are shown on oscillograph through photomultiplier tube.Kurtz-Perry powder frequency doubling test result shows that embodiment 1 is made
The powder SHG effect of standby middle infrared nonlinear optical crystal material is 2 times of KDP.The test of the laser damage threshold of powder
Method are as follows: sample to be tested powder is placed between two sheet glass, using (1064nm, 5ns, 1Hz) in laser irradiation to sample, no
Disconnected to improve laser energy, until sample powder surface state changes, the laser damage threshold of the powder measured is 80MW/
cm2。
(2) Pb7F12Cl2Frequency-doubled effect can phase matched test:
Middle infrared nonlinear optical crystal material prepared by embodiment 1 grinds respectively and is sieved into the powder of different grain size range
(20 ~ 40 μm, 40 ~ 60 μm, 60 ~ 80 μm, 80 ~ 100 μm, 100 ~ 125 μm, 125 ~ 150 μm and 150 ~ 200 μ
M), being then attached separately to two sides has in the sample cell of windowpane, and sample cell is placed on laser optical path later, uses Nd:YAG arteries and veins
Rushing laser is that the fundamental frequency light that light source generation wavelength is 1064nm injects sample cell, and signal is shown in oscillograph through photomultiplier tube
On, the frequency-doubled signal intensity size of different-grain diameter is tested, mapping post analysis judges that can the frequency-doubled effect of compound phase matched.
Fig. 1, Fig. 2 are Pb respectively7F12Cl2[the Pb of crystal3F9Cl]4- The arrangement figure of group configuration picture and it.It can from figure
To find out, Pb7F12Cl2Structure it is more complicated, each Pb atom and 3 F, 1 Cl are connected, and form [a PbF3Cl] four sides
Body, wherein have a longer Pb-Cl key (3.168 (1)), three shorter Pb-F keys (2.418 (5) -2.446 (2)),
[PbF is allowed in this way3Cl] tetrahedron has a biggish distortion, a microcosmic dipole moment can be generated, and can be with from figure
Find out three [PbF3Cl] the tetrahedral dipole moment [Pb that is not completely counterbalanced by, therefore is formed3F9Cl]4- Group also has one
Microcosmic dipole moment, although as can be seen from Figure 2 this four anionic groups are connected with each other, the arrangement in crystal space
Direction is substantially coincident, just because of such arrangement mode, just results in the dipole moment of crystal macroscopically, so that
Pb7F12Cl2Show a degree of nonlinear optical effect.
Fig. 3 is middle infrared nonlinear optical crystal material Pb7F12Cl2Dusty material UV-visible absorption spectrum,
It can be seen from the figure that its UV absorption cut-off side is 0.27 μm, the band gap size of calculating is 4.5eV.
Fig. 4 is middle infrared nonlinear optical crystal material Pb prepared by embodiment 17F12Cl2Fourier transform decaying it is red
Outer abosrption spectrogram, from infrared spectrogram as can be seen that the material 4000 wave numbers between 500 wave numbers without any absorption
Peak, this illustrate the material 4000 wave numbers between 500 wave numbers all without absorption.Integrated UV-visible absorption spectra and infrared spectroscopy
As a result, can deduce the material have wider transparency range, transparency range be 0.27-20 μm.The heat of the material point
The test result of analysis and powder frequency doubling phase matched is shown in Fig. 5 and Fig. 6, from fig. 5, it can be seen that the material is in 570 DEG C or more
Start thermal weight loss, there is good thermal stability;From fig. 6, it can be seen that the material has the frequency multiplication that phase matched may be implemented
Effect is 2 times of KDP.
Embodiment 2
A kind of middle infrared nonlinear optical crystal material of high laser damage threshold of the present embodiment, chemical formula are
Pb7F12Cl2。
Middle infrared nonlinear optical crystal material Pb described in the present embodiment7F12Cl2Powder SHG effect be di(2-ethylhexyl)phosphate
2 times of hydrogen potassium are 0.27-20 μm through range.
Middle infrared nonlinear optical crystal material Pb described in the present embodiment7F12Cl2Optical band gap value be 4.5eV, powder
The laser damage threshold at end is 80MW/cm2, about commercialization materials A gGaS2(5.2MW/cm2) 16 times, thermal weight loss temperature is
570°C。
The present embodiment additionally provides a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold
Method, the Pb7F12Cl2It is prepared using solution deposit.
Preferably, solution deposit described in the present embodiment is by PbF2It is added with NaCl into distilled water, heating stirring,
White precipitate can be obtained, after filter, washing and drying.
Further, heretofore described solution deposit is the PbF for being 7:2 by molar ratio2It is added with NaCl to temperature
For in 75 DEG C of distilled water, heating stirring to temperature is 92 DEG C, white precipitate can be obtained, by white precipitate through filtering, distilled water
After washing 2 times, drying.
Embodiment 3
The middle infrared nonlinear optical crystal material Pb of the present embodiment7F12Cl2In the application of optical field, due in middle infrared waves
Section has very wide transmission range, therefore application is relatively broad, civilian etc. to apply in defence and military, can mainly use
In fields such as optical information storage, laser communications, laser countermeasure (s)s.
Claims (10)
1. a kind of middle infrared nonlinear optical crystal material of high laser damage threshold, it is characterised in that: its chemical formula is
Pb7F12Cl2。
2. a kind of middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 1, feature
Be: its powder SHG effect is 2 times of potassium dihydrogen phosphate, is 0.27-20 μm through range.
3. a kind of middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 1 or 2, special
Sign is: its optical band gap value is 4.5eV, and the laser damage threshold of powder is 80MW/cm2, thermal weight loss temperature is 570 °C.
4. a kind of middle infrared nonlinear optical crystal material of high laser damage threshold as claimed in any one of claims 1-3
Preparation method, it is characterised in that: the Pb7F12Cl2It is prepared using hydro-thermal reaction method or solution deposit.
5. a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 4
Method, it is characterised in that: the hydro-thermal reaction method is by PbF2It is dissolved in aqueous solution with NaCl, carries out hydro-thermal reaction.
6. a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 5
Method, it is characterised in that: the PbF for being 7:2 by molar ratio2It is added in hydrothermal reaction kettle with NaCl, water is added, reaction kettle is sealed
After be put into Muffle furnace, after 230 DEG C, then isothermal reaction 7 days are heated in 3h, be cooled to 30 DEG C with the speed of 1 DEG C/h, cooling knot
Shu Hou is washed with distilled water product, dries after suction filtration, obtains colorless and transparent small crystals, as middle infrared nonlinear optical crystal
Material.
7. a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 6
Method, it is characterised in that: the reaction kettle, liner are polytetrafluoroethylene (PTFE).
8. a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 4
Method, it is characterised in that: the solution deposit is by PbF2It is added with NaCl into distilled water, heating stirring, can be obtained white
Color precipitating, after filter, washing and drying.
9. a kind of preparation side of the middle infrared nonlinear optical crystal material of high laser damage threshold according to claim 8
Method, it is characterised in that: the PbF for being 7:2 by molar ratio2It is added in the distilled water for being 70-80 DEG C to temperature with NaCl, heating stirring
It is 90-100 DEG C to temperature, white precipitate can be obtained, after white precipitate is filtered, distills water washing 2-3 times, is dry.
10. a kind of middle infrared nonlinear optical crystal of high laser damage threshold according to any one of claim 1-3
Application of the material in optical field.
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