CN106978630B - Selenium copper silicon barium and selenium copper silicon barium mid and far infrared nonlinear optical crystal and preparation method and purposes - Google Patents
Selenium copper silicon barium and selenium copper silicon barium mid and far infrared nonlinear optical crystal and preparation method and purposes Download PDFInfo
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Abstract
The present invention relates to a kind of selenium copper silicon barium and selenium copper silicon barium mid and far infrared nonlinear optical crystal and preparation method and purposes, chemical formula BaCu2SiSe4, molecular weight 608.35, which is trigonal system, and space group is non-centrosymmetry space groupP3221, cell parameter isa=b=6.4188 (19),c=16.083 (10),α=β=90 °,γ=120°、Z=3, unit-cell volume V=573.9 (5)3；It is made of solid reaction process, the powder X-ray RD spectrogram and theoretical calculation of selenium copper silicon barium of the invention and selenium copper silicon barium mid and far infrared nonlinear optical crystal；Under the laser irradiation of 2090 nm, granularity 55-88μThe BaCu of m2SiSe4Frequency-doubled effect is S-Ga-Ag (AgGaS under same granularity2) 1.6 times.
Description
Technical field
The invention belongs to infrared nonlinear optical crystal material fields, and in particular in a kind of selenium copper silicon barium and selenium copper silicon barium
Far infrared nonlinear optical crystal and preparation method and purposes
Background technique
Non-linear optical crystal material can be classified as three categories through range of wave band according to it: one, it is infrared and in it is remote
FTIR radiation transmittance；Two, visible light and near infrared band nonlinear optical material；Three, ultraviolet and deep ultraviolet band is non-
Linear optical material.Work of the invention belongs to visible light and mid and far infrared nonlinear optical material.The nonlinear optical of the wave band
It learns crystalline material tool to have been widely used, such as in preparation laser guidance, infrared remote sensor, environmental monitor and coherent infrared radar
Application in equal devices
Core devices of the infrared nonlinear optical crystal as laser frequency switch technology are the technology realities that matched using position
A kind of monocrystal material of tunable mid and far infrared laser is now exported to laser frequency conversion.Due to two important atmospheric electricities
Mouth (3-5 μm and 8-14 μm) is in this wavelength band, therefore exploration at present and development infrared nonlinear optical crystal one
As require to guarantee in the two wavelength bands have high transmission ability.
FTIR radiation transmittance practical now is ABC mostly2The chalcopyrite class of type, such as AgGaS2And ZnGeP2Deng
Commercialized crystal.But the crystalloid is there are some serious deficiencies, wherein lower laser damage threshold, swashing to near-infrared
The two-photon absorption problem of light (such as Nd:YAG 1064nm), serious anisotropic thermal expansion cause to be difficult to obtain large scale height
Quality single crystalline etc. all seriously limits their practical application.
At present in the world, although some oxide nonlinear optical crystals of discovery very good solution near-infrared
Frequency conversion problem, but for the laser of 3-5 μ m, lattice vibration frequency and the wave band of many oxide crystals
Laser frequency is suitable, so as to cause the strong competition of radiationless relaxation and Laser emission, can cause the high passive loss of laser, very
The mid and far infrared laser of 4 μm of hardly possible output or more.Therefore effective mid and far infrared nonlinear optical crystal is explored at present mainly to concentrate
In the halide, sulfide or phosphide etc. of non-oxygen system.
The first purpose of this invention, provides a kind of compound selenium copper silicon barium, and the chemical formula of the compound is
BaCu2SiSe4, molecular weight 608.35, be non-centrosymmetric structure monocrystalline, belong to trigonal system, space group P3221, structure cell
Parameter is α=β=90 °, γ=120 °, Z=3, unit-cell volume Polycrystal powder is made using solid reaction process；
Second purpose of the present invention provides selenium copper silicon barium mid and far infrared nonlinear optical crystal and preparation method, the crystallization
Formula is BaCu2SiSe4, molecular weight 608.35, be non-centrosymmetric structure monocrystalline, belong to trigonal system, space group is
P3221, cell parameter isα=β=90 °, γ=120 °, Z=3,
Unit-cell volumeIt is made of solid reaction process.
Third purpose of the present invention provides the purposes of selenium copper silicon barium mid and far infrared nonlinear optical crystal.
A kind of compound selenium copper silicon barium of the present invention, the chemical formula of the compound are BaCu2SiSe4, molecular weight is
608.35, belong to trigonal system, space group P3221, cell parameter is
α=β=90 °, γ=120 °, Z=3, unit-cell volumeFor polycrystal powder.
The preparation method of the compound selenium copper silicon barium, using solid reaction process, concrete operations follow these steps to carry out:
It a, is the glove box filled with inert nitrogen gas in the gas-tight container that water content and oxygen content are 0.01-0.1ppm
It is interior to be put into clean graphite crucible after mixing by by Ba:Cu:Si:Se molar ratio 1:2:1:4, it is packed into a length of 20cm, straight
Diameter be 10mm quartz glass tube in, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3After being vacuumized under conditions of Pa
Sealing；
B, the quartz ampoule sealed in step a is risen to 500-600 DEG C from room temperature with the heating rate of 35-40 DEG C/h of temperature,
Heat preservation 40-50 hours, then it is warming up to 800-1000 DEG C with 35-40 DEG C/h of temperature, keep the temperature 80-100 hours；
C, room temperature is cooled down to the rate of 3-5 DEG C/h of temperature, taking-up sample, which is put into mortar, to be smashed to pieces, is ground to get arriving
Compound BaCu2SiSe4Obtained compound selenium copper silicon barium polycrystal powder is carried out X-ray analysis, gained X-ray by polycrystal powder
Diffraction spectrogram and the BaCu parsed with mono-crystalline structures2SiSe4Theoretical X-ray spectrogram is consistent.
A kind of selenium copper silicon barium mid and far infrared nonlinear optical crystal, the crystal-chemical formula are BaCu2SiSe4, molecular weight is
608.35, it is non-centrosymmetric structure monocrystalline, belongs to trigonal system, space group P3221, cell parameter is α=β=90 °, γ=120 °, Z=3, unit-cell volume
The preparation method of the selenium copper silicon barium mid and far infrared non-linear optical crystal, follows these steps to carry out:
It a, is the glove box filled with inert nitrogen gas in the gas-tight container that water content and oxygen content are 0.01-0.1ppm
It is interior to be put into clean graphite crucible after mixing by by Ba:Cu:Si:Se molar ratio 1:2:1:4, it is packed into a length of 20cm, straight
Diameter be 10mm quartz glass tube in, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3After being vacuumized under conditions of Pa
Sealing；
B, the quartz ampoule sealed in step a is risen to 500-600 DEG C from room temperature with the heating rate of 35-40 DEG C/h of temperature,
Heat preservation 40-50 hours, then it is warming up to 800-1000 DEG C with 35-40 DEG C/h of temperature, keep the temperature 80-100 hours；
C, room temperature is cooled down to the rate of 3-5 DEG C/h of temperature, obtains selenium copper silicon barium BaCu2SiSe4Mid and far infrared is non-linear
Optical crystal.
The selenium copper silicon barium mid and far infrared nonlinear optical crystal is preparing infrared band laser frequency-doubling crystal, infrared communication
Purposes in device and infrared laser guidance device.
The powder xrd pattern and theory of selenium copper silicon barium and selenium copper silicon barium mid and far infrared nonlinear optical crystal of the present invention
Value is coincide；Under the laser irradiation of 2090nm, granularity is 55-88 μm of BaCu2SiSe4Frequency-doubled effect is under same granularity
S-Ga-Ag (AgGaS2) 1.6 times.
In selenium copper silicon crystal of barium structure of the present invention, Ba atom, Cu atom, Si atom, the chemical valence difference of Se atom
It is+2 ,+1 ,+4, -2.Si atom and neighbouring four Se atoms form isolated existing [SiSe4] tetrahedral structure；Cu atom
Four adjacent Se atoms form [CuSe4] tetrahedron, and be connected with each other in a manner of total side or altogether vertex, form four sides
Two kinds of three-dimensional open-frameworks of shape and hexagon.Ba atom is then only embedded in [CuSe4] tetrahedroid at hexagon duct in, shape
At [BaSe8] polygon.All atoms, are interconnected to form tridimensional network.
Selenium copper silicon barium compound of the present invention is selenium copper silicon barium polycrystal powder.
Detailed description of the invention
Fig. 1 is the comparison diagram of polycrystal powder X-ray powder diffraction figure and theoretical value of the present invention, and wherein A is theoretical value, and B is
Experiment value.
Fig. 2 is BaCu of the present invention2SiSe4The structure chart of crystal.
Fig. 3 is selenium copper silicon barium mid and far infrared nonlinear optical crystal of the present invention under 2090nm laser, granularity 55-88
μm when and with granularity S-Ga-Ag frequency multiplication comparison diagram, wherein A is AgGaS2Secondary frequency multiplication effect figure, B are BaCu2SiSe4Secondary times
Frequency effect figure.
Fig. 4 is nonlinear optical crystal frequency-doubled effect schematic diagram of the present invention.
Specific embodiment
The present invention is described in detail by embodiment, but is not limited only to given embodiment.
Embodiment 1
The preparation of compound selenium copper silicon barium polycrystal powder:
It a, is the glove box filled with inert nitrogen gas in the gas-tight container that water content and oxygen content are 0.01-0.1ppm
It is interior to be put into clean graphite crucible after mixing by by Ba:Cu:Si:Se molar ratio 1:2:1:4, it is packed into a length of 20cm, straight
Diameter be 10mm quartz glass tube in, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3After being vacuumized under conditions of Pa
Sealing；
B, the quartz ampoule sealed in step a is risen to 500-600 DEG C from room temperature with the heating rate of 35-40 DEG C/h of temperature,
Heat preservation 40-50 hours, then it is warming up to 800-1000 DEG C with 35-40 DEG C/h of temperature, 80-100 hours are kept the temperature, it is each in feedstock composition
Reaction obtains compound between ingredient；
C, room temperature is cooled down to the rate of 3-5 DEG C/h of temperature, taking-up sample, which is put into mortar, to be smashed to pieces, is ground to get arriving
Kermesinus compound BaCu2SiSe4Obtained compound selenium copper silicon barium polycrystal powder is carried out X-ray analysis, institute by polycrystal powder
The BaCu for obtaining X-ray diffraction spectrogram and being parsed with mono-crystalline structures2SiSe4Theoretical X-ray spectrogram is consistent, as a result referring to Fig. 1, from figure
In find out, experiment value matches with theoretical value, the powder sample illustrated be pure phase.
Embodiment 2
The preparation of selenium copper silicon barium mid and far infrared nonlinear optical crystal:
A, water content and oxygen content be 0.01ppm gas-tight container be the glove box filled with inert nitrogen gas in by
It is put into clean graphite crucible after mixing by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20cm, diameter is
In the quartz glass tube of 10mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3It is sealed after being vacuumized under conditions of Pa
Mouthful；
B, the quartz ampoule sealed in step a is risen to 500 DEG C from room temperature with the heating rate of 35 DEG C/h of temperature, heat preservation 40 is small
When, then 800 DEG C are warming up to 35 DEG C/h of temperature, keep the temperature 80 hours；
C, room temperature is cooled down to the rate of 3 DEG C/h of temperature, takes out graphite crucible, obtains kermesinus bulk selenium copper silicon barium
BaCu2SiSe4Mid and far infrared nonlinear optical crystal shows that the crystal is in selenium copper silicon barium by single-crystal X-ray diffraction analysis
Far infrared nonlinear optical crystal.
Embodiment 3
The preparation of selenium copper silicon barium mid and far infrared nonlinear optical crystal:
A, water content and oxygen content be 0.05ppm gas-tight container be the glove box filled with inert nitrogen gas in by
It is put into clean graphite crucible after mixing by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20cm, diameter is
In the quartz glass tube of 10mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3It is sealed after being vacuumized under conditions of Pa
Mouthful；
B, the quartz ampoule sealed in step a is risen to 560 DEG C from room temperature with the heating rate of 40 DEG C/h of temperature, heat preservation 45 is small
When, then 1000 DEG C are warming up to 40 DEG C/h of temperature, keep the temperature 100 hours；
C, room temperature is cooled down to the rate of 4 DEG C/h of temperature, takes out graphite crucible, obtains kermesinus bulk selenium copper silicon barium
BaCu2SiSe4Mid and far infrared nonlinear optical crystal.
Embodiment 4
The preparation of selenium copper silicon barium mid and far infrared nonlinear optical crystal:
A, water content and oxygen content be 0.08ppm gas-tight container be the glove box filled with inert nitrogen gas in by
It is put into clean graphite crucible after mixing by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20cm, diameter is
In the quartz glass tube of 10mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3It is sealed after being vacuumized under conditions of Pa
Mouthful；
B, the quartz ampoule sealed in step a is risen to 600 DEG C from room temperature with the heating rate of 38 DEG C/h of temperature, heat preservation 50 is small
When, then 900 DEG C are warming up to 38 DEG C/h of temperature, keep the temperature 90 hours；
C, room temperature is cooled down to the rate of 5 DEG C/h of temperature, takes out graphite crucible, obtains kermesinus bulk selenium copper silicon barium
BaCu2SiSe4Mid and far infrared nonlinear optical crystal.
Embodiment 5
The preparation of selenium copper silicon barium mid and far infrared nonlinear optical crystal:
A, water content and oxygen content be 0.1ppm gas-tight container be the glove box filled with inert nitrogen gas in by
It is put into clean graphite crucible after mixing by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20cm, diameter is
In the quartz glass tube of 10mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3It is sealed after being vacuumized under conditions of Pa
Mouthful；
B, the quartz ampoule sealed in step a is risen to 580 DEG C from room temperature with the heating rate of 37 DEG C/h of temperature, heat preservation 45 is small
When, then 950 DEG C are warming up to 37 DEG C/h of temperature, keep the temperature 95 hours；
C, room temperature is cooled down to the rate of 5 DEG C/h of temperature, takes out graphite crucible, obtains kermesinus bulk selenium copper silicon barium
BaCu2SiSe4Mid and far infrared nonlinear optical crystal.
Embodiment 6
By any one selenium copper silicon barium mid and far infrared nonlinear optical crystal obtained in embodiment 2-5, by shown in attached drawing 4
It is placed on 3 position, at room temperature, with adjusting the 2090nm output of Q Ho:Tm:Cr:YAG laser to make light source, observes bright
Aobvious 1045nm frequency multiplication light output, output intensity and equal conditions AgGaS2Equal (shown in Fig. 3), by Fig. 4 tune QHo:Tm:
Cr:YAG laser 1 issues the infrared beam that wavelength is 2090nm and injects selenium copper silicon barium nonlinear optical crystal through convex lens 2,
Generation wavelength is the frequency doubled light of 1045nm, light of the outgoing beam 4 containing infrared light and 1045nm that wavelength is 2090nm, through filtering
Piece 5 obtains the frequency doubled light that wavelength is 1045nm after filtering off.
Claims (5)
1. a kind of compound selenium copper silicon barium, it is characterised in that the chemical formula of the compound is BaCu2SiSe4, molecular weight is
608.35, belong to trigonal system, space group isP3221, cell parameter isa = b=6.4188 (19),c = 16.083
(10),α = β=90 °,γ=120 °,Z =3, unit-cell volume V=573.9 (5) 3, it is polycrystal powder.
2. the preparation method of compound selenium copper silicon barium as described in claim 1, it is characterised in that use solid reaction process, specifically
Operation follows these steps to carry out:
It a, is in the glove box filled with inert nitrogen gas in the gas-tight container that water content and oxygen content are 0.01-0.1 ppm
It is put into clean graphite crucible after mixing by by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20 cm, diameter
In quartz glass tube for 10 mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3After being vacuumized under conditions of Pa
Sealing；
B, the quartz ampoule sealed in step a is risen to 500-600 DEG C from room temperature with the heating rate of 35-40 DEG C/h of temperature, heat preservation
40-50 hours, then it is warming up to 800-1000 DEG C with 35-40 DEG C/h of temperature, keep the temperature 80-100 hours；
C, room temperature is cooled down to the rate of 3-5 DEG C/h of temperature, taking-up sample, which is put into mortar, to be smashed to pieces, is ground to get chemical combination is arrived
Object BaCu2SiSe4Obtained compound selenium copper silicon barium polycrystal powder is carried out X-ray analysis, gained X-ray diffraction by polycrystal powder
Spectrogram and the BaCu parsed with mono-crystalline structures2SiSe4Theoretical X-ray spectrogram is consistent.
3. a kind of selenium copper silicon barium mid and far infrared nonlinear optical crystal, it is characterised in that the crystal-chemical formula is BaCu2SiSe4, point
Son amount is 608.35, is non-centrosymmetric structure monocrystalline, belongs to trigonal system, space group isP3221, cell parameter isa = b =
6.4188 (19),c=16.083 (10),α = β=90 °,γ=120 °,Z =3, unit-cell volume V=573.9
(5) Å3。
4. the preparation method of selenium copper silicon barium mid and far infrared nonlinear optical crystal as claimed in claim 3, it is characterised in that press
The following steps carry out:
It a, is in the glove box filled with inert nitrogen gas in the gas-tight container that water content and oxygen content are 0.01-0.1 ppm
It is put into clean graphite crucible after mixing by by Ba:Cu:Si:Se molar ratio 1:2:1:4, is packed into a length of 20 cm, diameter
In quartz glass tube for 10 mm, by equipped with raw material quartz ampoule vacuum degree be 10-5-10-3After being vacuumized under conditions of Pa
Sealing；
B, the quartz ampoule sealed in step a is risen to 500-600 DEG C from room temperature with the heating rate of 35-40 DEG C/h of temperature, heat preservation
40-50 hours, then it is warming up to 800-1000 DEG C with 35-40 DEG C/h of temperature, keep the temperature 80-100 hours；
C, room temperature is cooled down to the rate of 3-5 DEG C/h of temperature, obtains selenium copper silicon barium BaCu2SiSe4Mid and far infrared nonlinear optics
Crystal.
5. selenium copper silicon barium mid and far infrared nonlinear optical crystal as claimed in claim 3 is preparing infrared band laser frequency multiplication crystalline substance
Purposes in body, infrared communication device and infrared laser guidance device.
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| CN110735184B (en) * | 2018-07-19 | 2021-06-08 | 中国科学院理化技术研究所 | BaHgGeSe4Nonlinear optical crystal and preparation method and application thereof |
| CN111188092B (en) * | 2020-02-11 | 2021-10-01 | 河北大学 | Cadmium-zinc-silicon-sulfur crystal and preparation method and application thereof |
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| CN102127811A (en) * | 2010-12-27 | 2011-07-20 | 中国科学院新疆理化技术研究所 | Lead fluoroborate nonlinear optical crystal as well as preparation method and application thereof |
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| CN102127811A (en) * | 2010-12-27 | 2011-07-20 | 中国科学院新疆理化技术研究所 | Lead fluoroborate nonlinear optical crystal as well as preparation method and application thereof |
| CN105332045A (en) * | 2015-11-19 | 2016-02-17 | 唐山学院 | Compound Pb0.78Ba8.22B18O36, Pb0.78Ba8.22B18O36 nonlinear optical crystal, preparation methods and application |
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