CN104451887A - Infrared nonlinear optical crystal Ln8Sb2S15 and preparation method thereof - Google Patents
Infrared nonlinear optical crystal Ln8Sb2S15 and preparation method thereof Download PDFInfo
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- CN104451887A CN104451887A CN201410708047.3A CN201410708047A CN104451887A CN 104451887 A CN104451887 A CN 104451887A CN 201410708047 A CN201410708047 A CN 201410708047A CN 104451887 A CN104451887 A CN 104451887A
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- nonlinear optical
- optical crystal
- infrared nonlinear
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- ln8sb2s15
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Abstract
The invention relates to an infrared nonlinear optical crystal Ln8Sb2S15 and a preparation method thereof, and belongs to the field of inorganic materials. The infrared nonlinear optical crystal is synthesized with a high-temperature inorganic solid phase one-step synthesis method. The synthesis condition is that reaction is performed for 4 days at 950 DEG C. The infrared nonlinear optical crystal Ln8Sb2S15 is crystalized in a tetragonal non-centrosymmetric space group 141cd which is mainly structurally characterized by comprising SbS3 anions adopting tripod-like structure, and the SbS3 anions are isolated by rare earth ions and sulfur ions. Single crystal and pure phase of La8Sb2S15 are synthesized successfully. Non-linear optical tests prove that powder SHG (second harmonic generation) effect is observed when La8Sb2S15 is irradiated by laser with the wavelength of 2.05, and the strength is about 1.2 times of that of a commercial infrared nonlinear optical material AgGaS2. The synthesis method for the nonlinear optical crystal material is simple, the yield is high, and a product has single chemical phase and good uniformity as well as potential infrared nonlinear optical application value.
Description
Technical field
The present invention relates to class infrared nonlinear optical crystal and preparation method thereof, belong to field of inorganic materials.
Background technology
Nonlinear optical material refers to that a class is by outside light field, electric field and strain field effect, and frequency, phase place, amplitude etc. change, thus cause the material of the changes such as specific refractory power, photoabsorption, scattering of light.When doing light source with laser, this non-linear phenomena that the interaction of laser and medium produces can cause the frequency multiplication of light, sum of fundamental frequencies, difference frequency, parametric oscillation, parameter amplify and cause harmonic wave.Utilize frequency conversion and the Preset grating function of nonlinear optical material, especially frequency multiplication and frequency tripling ability, can be widely used in the field such as signal converter and optical switch, photomodulator, frequency multiplier, limiter, amplifier, rectifier lens and transverter of wire television and opticfiber communication by such material.By its service band, the nonlinear optical material of widespread use at present is mainly divided three classes.The main representative of ultraviolet band is BBO and LBO; The representative materials can seeing infrared band has: KDP, KTP and LiNbO
3deng.Comparatively speaking, the research of infrared band nonlinear crystalline material is weaker.AgGaQ is mainly contained at present at this wave band best material
2(Q=S, Se) and ZnGeP
2, its nonlinear factor is comparatively large, in (far) infra-red range transmitance high, but energy gap is less, and laser damage threshold is low, and these features limit their application to a certain extent.Therefore, the FTIR radiation transmittance that exploratory development is new is one of the difficult point and focus of current nonlinear optical material.The principal character of antimony chalcogen compound is contained Sb
3+ion has lone-pair electron effect, non-centrosymmetrical pyrometric cone coordination polyhedron can be formed, and then the compound producing non-core structure may be induced, thus produce the compound may with non-linear nature, but the research of this respect is also less at present, and the exploratory development thus carrying out the antimony chalcogenide materials with infrared non-linear optical property is a very meaningful and challenging job.On the other hand, rare earth ion has higher ligancy, and there is distortion at its coordination polyhedron center more.Usually, rare earth chalcogen compound has high thermal stability, can as luminescence, magneto-optic and material of infrared window etc.These two kinds of non-centrosymmetrical metal centers are successfully introduced by the present invention simultaneously, owing to having different radiuses in compound, different coordination mode, the structural motif of different polyhedra packing modes, makes this compound have non-core structure and nonlinear optical property.
Summary of the invention
In order to explore novel infrared non-linear optical material, the present invention, by high temperature solid state reaction, provides the non-core structure of a class containing the antimony chalcogen compound of rare earth, and they have potential infrared non-linear optical application and are worth.
In the present invention, Ln
8sb
2s
15crystallization is non-heart spacer in four directions: I4
1cd, key structural feature contains the SbS of pyrometric cone configuration
3negatively charged ion, they are separated by rare earth ion and sulfonium ion.The present invention successfully synthesizes Ln
8sb
2s
15monocrystalline and pure phase.
Nonlinear optical test shows, La
8sb
2s
15be under the laser radiation of 2.05 at wavelength, observe powder SHG effect, its intensity is approximately commercial infrared nonlinear optical material AgGaS
21.2 times.
Accompanying drawing explanation
Fig. 1 is La
8sb
2s
15structure iron
Fig. 2 is La
8sb
2s
15powder diffraction spectrum
Fig. 3 is La
8sb
2s
15sHG intensity and the graph of a relation of granularity
Embodiment
A class infrared nonlinear optical crystal of the present invention prepare embodiment:
Simple substance raw material is stoichiometrically weighed, loads little silica tube, then little silica tube under vacuo sealing by fusing in large silica tube.Then reactant is in temperature programmed control tube furnace, within 4 days, namely obtains the novel infrared nonlinear optical crystal of the present invention's development at 950 DEG C of long-time sintering reactions.Productive rate reaches 98%.
Preparation method of the present invention, its outstanding advantages is: technology of preparing is simple, and product is single-phase, good uniformity.
Table 1 La
8sb
2s
15and Nd
8sb
2s
15crystallographic data
aR
1＝Σ||F
o|-|F
c||/Σ|F
o|,wR
2＝[Σw(F
o 2-F
c 2)
2/Σw(F
o 2)
2]
1/2。
Claims (2)
1. a class infrared nonlinear optical crystal, is characterized in that molecular formula is: Ln
8sb
2s
15, in formula, Ln is the one in La, Nd rare earth atom, and this compound belongs to tetragonal system, and crystallization is in non-heart spacer: I4
1cd, key structural feature contains the SbS of pyrometric cone configuration
3negatively charged ion, they are separated by rare earth ion and sulfonium ion.
2. the preparation method of a class infrared nonlinear optical crystal of a claim 1, this preparation method is that one-step synthesis comprises the steps: to select simple substance raw material stoichiometrically to weigh, load little silica tube, then little silica tube under vacuo sealing by fusing in large silica tube.Then reactant is in temperature programmed control tube furnace, within 4 days, namely obtains a class novel infrared nonlinear optical crystal at 950 DEG C of sintering reactions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410708047.3A CN104451887B (en) | 2014-11-28 | 2014-11-28 | One class infrared nonlinear optical crystal Ln8Sb2S15And preparation method thereof |
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|---|---|---|---|
| CN201410708047.3A CN104451887B (en) | 2014-11-28 | 2014-11-28 | One class infrared nonlinear optical crystal Ln8Sb2S15And preparation method thereof |
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|---|---|
| CN104451887A true CN104451887A (en) | 2015-03-25 |
| CN104451887B CN104451887B (en) | 2017-10-24 |
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236482A (en) * | 2015-09-02 | 2016-01-13 | 浙江大学 | Quaternary sulfur-antimony compound ACuSb2S4 semiconductor material |
| CN106521630A (en) * | 2016-11-16 | 2017-03-22 | 遵义师范学院 | Second-order nonlinear optical crystal and preparation method thereof |
| CN110195255A (en) * | 2019-07-04 | 2019-09-03 | 遵义师范学院 | A kind of polar crystal La3SbS5Cl2And preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191554A (en) * | 2010-03-02 | 2011-09-21 | 中国科学院福建物质结构研究所 | Infrared non-linear optical crystals Ln4GaSbS9 |
| CN102191553A (en) * | 2010-03-02 | 2011-09-21 | 中国科学院福建物质结构研究所 | Novel infrared nonlinear optical crystal and preparation method thereof |
-
2014
- 2014-11-28 CN CN201410708047.3A patent/CN104451887B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191554A (en) * | 2010-03-02 | 2011-09-21 | 中国科学院福建物质结构研究所 | Infrared non-linear optical crystals Ln4GaSbS9 |
| CN102191553A (en) * | 2010-03-02 | 2011-09-21 | 中国科学院福建物质结构研究所 | Novel infrared nonlinear optical crystal and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236482A (en) * | 2015-09-02 | 2016-01-13 | 浙江大学 | Quaternary sulfur-antimony compound ACuSb2S4 semiconductor material |
| CN106521630A (en) * | 2016-11-16 | 2017-03-22 | 遵义师范学院 | Second-order nonlinear optical crystal and preparation method thereof |
| CN110195255A (en) * | 2019-07-04 | 2019-09-03 | 遵义师范学院 | A kind of polar crystal La3SbS5Cl2And preparation method thereof |
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|---|---|
| CN104451887B (en) | 2017-10-24 |
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