CN107217302B - Selenium antimony gallium barium compound, selenium antimony gallium barium infrared nonlinear optical crystal and its preparation method and application - Google Patents
Selenium antimony gallium barium compound, selenium antimony gallium barium infrared nonlinear optical crystal and its preparation method and application Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention discloses a kind of selenium antimony gallium barium compounds, and chemical formula is Ba23Ga8Sb2Se38.The invention also discloses the preparation methods of selenium antimony gallium barium compound.In addition, the invention also discloses a kind of selenium antimony gallium crystal of barium and its preparation method and application.The advantages that growing crystals of selenium antimony gallium barium infrared nonlinear optical crystal of the invention are easily grown up and transparent no package, have the speed of growth very fast, at low cost, are easy to get larger size crystal；Selenium antimony gallium barium infrared nonlinear optical crystal obtained has many advantages, such as than wider infrared light transmission wave band, good mechanical property, easy to process and preservation；The selenium antimony gallium crystal of barium can be used for making infrared laser frequency conversion device.
Description
Technical field
The present invention relates to inorganic compound field of material technology, and in particular to selenium antimony gallium barium compound and preparation method thereof,
Selenium antimony gallium barium infrared nonlinear optical crystal and its preparation method and application.
Background technique
Second-order non-linear optical crystal be it is a kind of combine closely with laser technology, important photoelectric functional material, such
Crystal can realize the tune to commodity laser frequency by nonlinear effects such as frequency multiplication, difference frequency and frequency and optical parametric oscillators
Section generates laser with new wavelength source, and then greatly expands the application range of laser.Such as it using suitable frequency-doubling crystal, can incite somebody to action
Nd:YAG (output wavelength 1064nm) laser freuqency doubling, generation wavelength are the laser of 532nm；2.1 μm of laser is after frequency multiplication
It can produce the laser that wavelength is 1.05 μm.
Currently, a series of outstanding nonlinear optical crystals have been found to and realize quotient in Uv and visible light wave band
With, including KBBF (KBe2BO3F2)、BBO(β-BaB2O4)、LBO(LiB3O5)、CBO(CsB3O5)、KDP(KH2PO4) and KTP
(KTiOPO4) etc., they have been obtained in terms of generating new Uv and visible light wave band of laser is widely applied and can
Meet various requirements.However, the research to infrared band nonlinear optical crystal is still relatively deficient, can be practical
Crystal only has ZGP (ZnGeP2)、AGS(AgGaS2) and AGSe (AgGaSe2) etc. it is few in number several.Meanwhile these crystal are also
Have the shortcomings that serious, for example AGS and AGSe, there are big anisotropic thermal expansion, high quality large size crystal growth is tired
It is difficult；In addition thermal conductivity is low, stronger thermal gradient and thermal lensing effect can be generated in high power pump leads to laser damage threshold
It is extremely low, it is impossible to be used in the output of high power infrared laser；ZGP crystal is the current optimal material for generating 3~5 μm of infrared lasers, so
And its crystal growth is extremely difficult, and there are inevitable, serious residual absorptions, and it must be used near infrared region
Laser of the wavelength greater than 2 μm is pumped.Disadvantage mentioned above seriously limits the practical application of above-mentioned infrared crystal；It finds in the recent period
Novel infrared non-linear crystal BGS (BaGa4S7) and BGSe (BaGa4Se7) it is still within the development in laboratory stage, it is specific practical
Use value needs further to be studied with application band；In addition, still lacking the non-thread of function admirable in 8~12 μm of infrared bands
Property crystalline material.
Therefore, it explores excellent with being easy to grow, being machined good property, high laser damage threshold, infrared non-linear
Novel crystal seem especially urgent, and the research hotspot and one of difficult point in current nonlinear optical material field.
Summary of the invention
Present invention aim to address above-mentioned prior art problem, a kind of selenium antimony gallium barium compound and its preparation side are provided
Method, selenium antimony gallium barium infrared nonlinear optical crystal and its preparation method and application.
In order to reach above-mentioned technical effect, the present invention takes following technical scheme:
The chemical formula of a kind of selenium antimony gallium barium compound, the selenium antimony gallium barium compound is Ba23Ga8Sb2Se38。
Ba provided by the invention23Ga8Sb2Se38The preparation method of compound, its step are as follows:
Ba substance, substance containing Ga, substance containing Sb and simple substance Se ingredient and after mixing will be contained, be heated to 800~850 DEG C
High temperature solid state reaction is carried out, selenium antimony gallium barium compound is obtained；
All Ba:Ga:Sb:Se elemental mole ratios are in the substance containing Ba, substance containing Ga, substance containing Sb and simple substance Se
23:8:2:38；
The substance containing Ba is barium simple substance or barium selenide；The substance containing Ga is two gallium of gallium simple substance or three selenizings；It is described to contain
Sb substance is antimony simple substance or antimony triselenide.
Further technical solution according to the present invention, it is described to be heated to 800~850 DEG C of progress high temperature solid state reactions and be
Refer to:
Uniformly mixed material is fitted into plating carbon quartz ampoule, 10 then are evacuated to quartz ampoule-3Pa is simultaneously melted
Sealed knot；The quartz ampoule of sealed knot is put into Muffle furnace, 800~850 DEG C is warming up to the rate of 30~50 DEG C/h, keeps the temperature 96h, to
Sample is taken out after cooling；It is again placed in after being ground to the sample of taking-up in plating carbon quartz ampoule and is evacuated to 10-3Pa is simultaneously carried out
Sealed knot is melted, is put into Muffle furnace later and is warming up to 800 DEG C of sintering 72h；Sample is taken out, and grind obtain it is powdered
Ba23Ga8Sb2Se38Compound.
A kind of selenium antimony gallium crystal of barium, it is characterised in that the chemical formula of the crystal is Ba23Ga8Sb2Se38, the crystal is red
Outer nonlinear optical crystal has non-centrosymmetric structure, belongs to rhombic system, space group Cmc21, cell parameter are as follows: α=β=γ=90 °,Z
=2.
The preparation method of above-mentioned selenium antimony gallium crystal of barium, it is the following steps are included: be placed in temperature for selenium antimony gallium barium compound
Gradient is that selenium antimony gallium barium is prepared using horizontal gradient condensation method or Bridgman-Stockbarger method in the crystal growing furnace of 5~10 DEG C/cm
Crystal.
Further technical solution according to the present invention, the horizontal gradient condensation method refer to powdered selenium antimony gallium barium
It closes after object encloses silica crucible, is put into horizontal crystal growth furnace, after being heated to compound melts and keeping 24~72h, with 5~
The mobile thermal field of the speed of 10mm/d, to crystal growth after, room temperature is down to 10~30 DEG C/h rate of temperature fall, it is saturating to obtain brown
Bright selenium antimony gallium crystal of barium.
Further technical solution according to the present invention, the Bridgman-Stockbarger method refer to powdered selenium antimony gallium barium compound
After enclosed silica crucible, it is put into crystal growing furnace, is to slowly warm up to compound melts, be completely melt and keep 24 to powder~
After 72h, silica crucible is vertically declined with the speed of 0.3~2.0mm/h, carries out selenium antimony gallium crystal of barium during crucible decline
Growth, to crystal growth after room temperature is down to 10~30 DEG C/h rate of temperature fall, growth cycle is 10~30d.
Above-mentioned selenium antimony gallium crystal of barium is used to prepare infrared laser frequency conversion device.
It will be described in detail the present invention below.
In the present invention, chemical formula Ba23Ga8Sb2Se38Selenium antimony gallium barium compound, preparation related chemistry reaction equation
Include:
(1)23BaSe+8Ga+Sb2Se3+ 12Se=Ba23Ga8Sb2Se38；
(2) 23BaSe+8Ga+2Sb+15Se=Ba23Ga8Sb2Se38；
(3) 23Ba+8Ga+2Sb+38Se=Ba23Ga8Sb2Se38；
(4)23Ba+8Ga+Sb2Se3+ 35Se=Ba23Ga8Sb2Se38；
(5)23BaSe+4Ga2Se3+Sb2Se3=Ba23Ga8Sb2Se38；
(6)23BaSe+4Ga2Se3+ 2Sb+3Se=Ba23Ga8Sb2Se38；
(7)23Ba+4Ga2Se3+ 2Sb+26Se=Ba23Ga8Sb2Se38；
(8)23Ba+4Ga2Se3+Sb2Se3+ 23Se=Ba23Ga8Sb2Se38；
The crystal structure of the selenium antimony gallium barium compound is as shown in Figure 1, be a kind of non-centrosymmetrical zero-dimension structural: Ga with
Four Se are connected to form GaSe4Tetrahedron, it is top, Se as the SbSe of pedestal that Sb and three Se, which is connected to form using Sb,3Pyramid, this
A little GaSe4Tetrahedron and SbSe3Pyramid is mutually completely separated by Ba ion, forms zero-dimension structural.
The present invention prepares selenium antimony gallium crystal of barium using horizontal gradient condensation method or Bridgman-Stockbarger method and can get having a size of cm
The Ba of grade23Ga8Sb2Se38Infrared nonlinear optical crystal；Using larger-sized crucible, while extending growth cycle, then can obtain
Obtain corresponding larger size Ba23Ga8Sb2Se38Infrared nonlinear optical crystal.
After obtaining high quality large size crystal, the crystal of growth can be carried out according to the crystallographic characteristics of the crystal
Orientation.It later, can be by required angle, thickness and sectional dimension sliced crystal；Finally simultaneously by the light pass surface polishing of quartz crystal device
Plated film completes the preparation of the crystal infrared laser frequency conversion device.Ba23Ga8Sb2Se38Crystal have physical and chemical performance it is stable,
Good mechanical property is not easy the advantages that deliquescing, easy to process and preservation；The present invention furthermore provides Ba23Ga8Sb2Se38It is infrared non-
The purposes of linear optical crystal, the Ba23Ga8Sb2Se38Crystal is used to prepare infrared laser frequency conversion device, which includes near
Few a branch of incident laser passes through at least one piece of Ba23Ga8Sb2Se38At least a branch of frequency is generated after crystal different from incident laser
The device of radiant output.
Compared with prior art, the present invention have it is below the utility model has the advantages that
Effect of the invention is that providing a kind of chemical formula is Ba23Ga8Sb2Se38Novel infrared nonlinear optical crystal
And its preparation method and application.It easily grows up and transparent no packet in the growing crystals of the selenium antimony gallium barium infrared nonlinear optical crystal
It wraps up in, has the speed of growth very fast, at low cost, the advantages that being easy to get larger size crystal；Selenium antimony gallium barium obtained is infrared non-
Linear optical crystal has many advantages, such as than wider infrared light transmission wave band, good mechanical property, easy to process and preservation；The selenium antimony gallium
Crystal of barium can be used for making infrared laser frequency conversion device.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of selenium antimony gallium barium infrared nonlinear optical crystal prepared by the present invention.
Fig. 2 is the Ba23Ga8Sb2Se38Infrared nonlinear optical crystal tests (Experimental) and fitting
(Simulated) x-ray diffractogram of powder spectrum control.
Fig. 3 is former using a kind of work of typical infrared nonlinear optical device made of selenium antimony gallium crystal of barium of the present invention
Reason figure.
Specific embodiment
Below with reference to the embodiment of the present invention, the invention will be further elaborated.
Embodiment 1
Using 23BaSe+4Ga2Se3+Sb2Se3=Ba23Ga8Sb2Se38Reaction equation prepares selenium antimony with high-temperature solid phase reaction method
Gallium barium compound；
The BaSe is 19.899 grams, the Ga2Se3It is 6.021 grams, the Sb2Se3It is 1.922 grams；That is BaSe:
Ga2Se3:Sb2Se3=0.092mol:0.016mol:0.004mol；
Concrete operation step is to weigh reagent respectively by above-mentioned dosage in glove box, place them into mortar, mixing
And grind, it is then charged into the plating carbon quartz ampoule of Φ 19mm × 25mm, is evacuated to 10-3Quartz ampoule is melted with oxyhydrogen flame after Pa
Encapsulation, is put into Muffle furnace, rises to 800 DEG C with the heating rate of 50 DEG C/h, keeps the temperature 96h, sample is taken out after cooling, to taking-up
Sample be ground after be again placed in plating carbon quartz ampoule in be evacuated to 10-3Pa simultaneously carries out fusing sealed knot, is put into Muffle later
800 DEG C of sintering 72h are warming up in furnace；Sample is taken out, and grinds and obtains powdered Ba23Ga8Sb2Se38Compound.
Embodiment 2
Using 23Ba+4Ga2Se3+Sb2Se3+ 23Se=Ba23Ga8Sb2Se38Reaction equation prepares selenium with high-temperature solid phase reaction method
Antimony gallium barium compound；
The Ba is 12.634 grams, the Ga2Se3It is 6.021 grams, the Sb2Se3It is 1.922 grams, the Se is 7.264
Gram；That is Ba:Ga2Se3:Sb2Se3: Se=0.092mol:0.016mol:0.004mol:0.092mol；
Concrete operation step is to weigh reagent respectively by above-mentioned dosage in glove box, they are mixed, be then charged into Φ
In the plating carbon quartz ampoule of 19mm × 25mm, it is evacuated to 10-3Quartz ampoule is melted with oxyhydrogen flame after Pa and is encapsulated, Muffle furnace is put into
In, 800 DEG C are risen to the heating rate of 40 DEG C/h, 96h is kept the temperature, takes out sample after cooling, the sample of taking-up is ground
After be again placed in plating carbon quartz ampoule in be evacuated to 10-3Pa simultaneously carries out fusing sealed knot, is put into Muffle furnace later and is warming up to 800 DEG C
It is sintered 72h；Sample is taken out, and grinds and obtains powdered Ba23Ga8Sb2Se38Compound.
Embodiment 3
Using 23Ba+8Ga+Sb2Se3+ 35Se=Ba23Ga8Sb2Se38Reaction equation prepares selenium antimony gallium with high-temperature solid phase reaction method
Barium compound；
The Ba is 12.634 grams, and the Ga is 2.231 grams, the Sb2Se3It is 1.922 grams, the Se is 11.054 grams；
That is Ba:Ga:Sb2Se3: Se=0.092mol:0.032mol:0.004mol:0.140mol；
Its concrete operation step is to weigh reagent respectively by above-mentioned dosage in glove box, be loaded into Φ 19mm ×
In the plating carbon quartz ampoule of 25mm, it is evacuated to 10-3Quartz ampoule is melted with flame after Pa and is encapsulated, is put into Muffle furnace, is slowly risen
To 850 DEG C, heating rate is 30 DEG C/h, keeps the temperature 96h, takes out, set again after cooling after being ground to the sample of taking-up
10 are evacuated in plating carbon quartz ampoule-3Pa simultaneously carries out fusing sealed knot, is put into Muffle furnace later and is warming up to 800 DEG C of sintering 72h；
Sample is taken out, and grinds and obtains powdered Ba23Ga8Sb2Se38Compound.
Embodiment 4
Selenium antimony gallium crystal of barium is prepared using horizontal gradient condensation method:
By Ba obtained in embodiment 1 to 323Ga8Sb2Se38Powder is fitted into Φ 16mm × 20mm silica crucible, is vacuumized
To 10-3After Pa, it is packaged and placed in horizontal growth furnace (temperature gradient is 5~10 DEG C/cm) with oxyhydrogen flame, is slowly increased to 950 DEG C
After being completely melt raw material and keeping 24~72h, with the mobile thermal field of the speed of 5~10mm/d, to crystal growth after, with 10
~30 DEG C/h rate of temperature fall is cooled to room temperature, obtains the Ba of amber transparent23Ga8Sb2Se38Crystal.
Embodiment 5
Selenium antimony gallium crystal of barium is prepared using Bridgman-Stockbarger method:
By Ba obtained in embodiment 1 to 323Ga8Sb2Se38Powder is fitted into Φ 16mm × 20mm silica crucible, is vacuumized
To 10-3It after Pa, is packaged and placed in crystal growing apparatus with oxyhydrogen flame, being slowly increased to 950 DEG C makes raw material be completely melt and keep
After 24~72h, silica crucible is vertically declined with the speed of 0.3~2.0mm/h, is carried out during crucible decline
Ba23Ga8Sb2Se38Infrared nonlinear optical crystal is grown, and after crystal growth, is cooled to room with the rate of 10~30 DEG C/h
Temperature obtains the Ba of amber transparent23Ga8Sb2Se38Crystal.
After tested, Ba prepared by above-described embodiment 4 and 523Ga8Sb2Se38Nonlinear optical crystal has non-centrosymmetry knot
Structure belongs to rhombic system, space group Cmc21, cell parameter are as follows: α=β=γ=90 °,Z=2；The crystal has infrared powder SHG effect；Fig. 1
It is the Ba23Ga8Sb2Se38The structural schematic diagram of infrared nonlinear optical crystal is a kind of non-centrosymmetrical zero-dimension structural: Ga
GaSe is connected to form with four Se4Tetrahedron, it is top, Se as the SbSe of pedestal that Sb and three Se, which is connected to form using Sb,3Pyramid,
These GaSe4Tetrahedron and SbSe3Pyramid is mutually completely separated by Ba ion, forms zero-dimension structural.Fig. 2 is this
Ba23Ga8Sb2Se38Infrared nonlinear optical crystal tests (Simulated) X-ray powder of (Experimental) and fitting
Diffracting spectrum control.
Embodiment 6
By the resulting Ba of embodiment 4 and 523Ga8Sb2Se38Crystal be oriented, cut, polishing and plated film after, be placed on attached drawing
At position of 3 shown devices marked as 4, at room temperature, with the Ho:Tm:Cr:YAG laser light source for adjusting Q, incident wavelength is
The infrared light of 2090nm, output wavelength are the frequency doubled light of 1045nm.
Attached drawing 3 is using Ba of the present invention23Ga8Sb2Se38It is a kind of typical infrared non-made of infrared nonlinear optical crystal
The working principle diagram of linear optics device, wherein 1 is infrared laser；2 represent the laser that will be incident on crystal of 1 generation
Beam；3 be the mirror for having plated film (mirror can be through incident laser 2, signal light and ideler frequency light that total reflection crystal generates)；4
It is the Ba for meeting laser wavelength of incidence phase-matching condition after crystal post-processing and optical manufacturing23Ga8Sb2Se38Crystal；
5 be the mirror for having plated film (mirror can be totally reflected incident laser 2 partially through the signal light and ideler frequency light of crystal generation)；6
It is the required laser beam obtained with 7.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (1)
1. a kind of preparation method of selenium antimony gallium crystal of barium, it is characterised in that:
The chemical formula of the selenium antimony gallium crystal of barium is Ba23Ga8Sb2Se38, the crystal is infrared nonlinear optical crystal, is had
Non-centrosymmetric structure belongs to rhombic system, space group Cmc21, cell parameter are as follows: α=β=γ=90 °,Z=2；The selenium antimony gallium barium is brilliant
Body is a kind of non-centrosymmetrical zero-dimension structural: Ga and four Se is connected to form GaSe4Tetrahedron, Sb are connected to form with three Se
It is top, Se as the SbSe of pedestal using Sb3Pyramid, these GaSe4Tetrahedron and SbSe3Pyramid by Ba ion mutually completely every
It opens, forms zero-dimension structural；
The following steps are included:
Selenium antimony gallium barium compound is placed in the crystal growing furnace that temperature gradient is 5~10 DEG C/cm, utilizes horizontal gradient condensation method
Selenium antimony gallium crystal of barium is prepared；
The horizontal gradient condensation method refers to after the enclosed silica crucible of powdered selenium antimony gallium barium compound, and it is raw to be put into level crystal
In long furnace, after being heated to compound melts and keeping 24~72h, with the mobile thermal field of the speed of 5~10mm/d, to crystal growth knot
Shu Hou is down to room temperature with 10~30 DEG C/h rate of temperature fall, obtains the selenium antimony gallium crystal of barium of amber transparent；The selenium antimony gallium barium chemical combination
The chemical formula of object is Ba23Ga8Sb2Se38；
The selenium antimony gallium barium compound is prepared via a method which:
Ba substance, substance containing Ga, substance containing Sb and simple substance Se ingredient and after mixing will be contained, be heated to 800~850 DEG C of progress
High temperature solid state reaction obtains selenium antimony gallium barium compound；
All Ba:Ga:Sb:Se elemental mole ratios are 23 in the substance containing Ba, substance containing Ga, substance containing Sb and simple substance Se:
8:2:38；
The substance containing Ba is barium simple substance or barium selenide；The substance containing Ga is two gallium of gallium simple substance or three selenizings；The object containing Sb
Matter is antimony simple substance or antimony triselenide；
It is described to be heated to 800~850 DEG C of progress high temperature solid state reactions and refer to:
Uniformly mixed material is fitted into plating carbon quartz ampoule, 10 then are evacuated to quartz ampoule-3Pa simultaneously carries out fusing sealed knot；
The quartz ampoule of sealed knot is put into Muffle furnace, is warming up to 800~850 DEG C with the rate of 30~50 DEG C/h, keeps the temperature 96h, it is to be cooled
After take out sample；It is again placed in after being ground to the sample of taking-up in plating carbon quartz ampoule and is evacuated to 10-3Pa is simultaneously melted
Sealed knot is put into Muffle furnace later and is warming up to 800 DEG C of sintering 72h；Sample is taken out, and grind obtain it is powdered
Ba23Ga8Sb2Se38Compound.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101545141A (en) * | 2008-03-25 | 2009-09-30 | 中国科学院福建物质结构研究所 | Sulfurized gallium and barium monocrystal as well as growing method and infrared nonlinear optical device thereof |
| CN104630891A (en) * | 2015-02-12 | 2015-05-20 | 中国科学院福建物质结构研究所 | Infrared nonlinear optical single crystal sulfur tellurium indium barium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101545141A (en) * | 2008-03-25 | 2009-09-30 | 中国科学院福建物质结构研究所 | Sulfurized gallium and barium monocrystal as well as growing method and infrared nonlinear optical device thereof |
| CN104630891A (en) * | 2015-02-12 | 2015-05-20 | 中国科学院福建物质结构研究所 | Infrared nonlinear optical single crystal sulfur tellurium indium barium |
Non-Patent Citations (1)
| Title |
|---|
| Disconnection Enhances the Second Harmonic Generation Response:Synthesis and Characterization of Ba23Ga8Sb2S38;Mei-Chun Chen;《Journal of the American Chemical Society》;20120328;第134卷;第6058-6060页 |
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