CN115467009A - Silicon-containing mixed anion nonlinear optical crystal and preparation method and application thereof - Google Patents
Silicon-containing mixed anion nonlinear optical crystal and preparation method and application thereof Download PDFInfo
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- CN115467009A CN115467009A CN202211248737.6A CN202211248737A CN115467009A CN 115467009 A CN115467009 A CN 115467009A CN 202211248737 A CN202211248737 A CN 202211248737A CN 115467009 A CN115467009 A CN 115467009A
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- 230000003287 optical effect Effects 0.000 title claims abstract description 69
- 239000013078 crystal Substances 0.000 title claims abstract description 63
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 24
- 239000010703 silicon Substances 0.000 title claims abstract description 24
- 150000001450 anions Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000523 sample Substances 0.000 claims abstract description 11
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 9
- 230000010365 information processing Effects 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012612 commercial material Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 18
- 239000010453 quartz Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000002447 crystallographic data Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3551—Crystals
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Abstract
The application provides a silicon-containing mixed anion nonlinear optical crystal, which has a chemical formula as follows: ba 5 Ga 2 SiO 4 S 6 Has excellent second-order nonlinear optical property, namely phase matching in infrared band, and wide optical band gap (such as E) g =4.03 eV), the powder frequency doubling strength can reach the commercial material AgGaS 2 0.65 times of the laser damage threshold value of the crystal and the laser damage threshold value of the crystal is AgGaS 2 The crystal is 17.5 times, the balance of large second-order frequency multiplication coefficient and wide optical band gap is well realized, the preparation method is simple, and the crystal has important application value in high-tech fields such as laser frequency conversion, near-infrared probes, photorefractive information processing and the like, and is particularly used for infrared detectors and infrared lasers.
Description
Technical Field
The application relates to a silicon-containing mixed anion nonlinear optical crystal and a preparation method and application thereof, belonging to the technical field of inorganic nonlinear optical materials.
Background
The second order nonlinear optical (NLO) crystal is a very important functional material and has wide application in the aspects of laser communication, optical information processing, integrated circuits, military technology and the like. In general, an ideal second order NLO crystal must satisfy the following conditions: (1) large second order frequency multiplication coefficient; (2) high laser damage threshold; (3) appropriate birefringence; (4) wide optical transmission range; and (5) good physical and chemical properties, mechanical properties and the like. The second-order nonlinear optical materials can be classified into inorganic nonlinear optical materials, organic nonlinear optical materials, polymer nonlinear optical materials and organic metal complex nonlinear optical materials according to the physicochemical properties of the second-order nonlinear optical materials. Most of the second-order NLO crystals currently marketed are inorganic nonlinear optical materials, and can be classified into three categories, i.e., ultraviolet light band, visible light band and infrared light band, according to their application bands. The second-order NLO crystal material with ultraviolet and visible light wave bands can meet the requirements of practical application.
The infrared second order NLO crystals currently commercialized are mainly chalcopyrite type materials, such as AgGaS 2 、AgGaSe 2 And ZnGeP 2 However, a series of performance defects brought by the low optical band gap of the materials affect the practical application range of the materials. Excellent infrared second order NLO crystal material requires large second order frequency multiplication coefficient>0.5×AgGaS 2 ) And a wide optical band gap (E) g >3.5 eV). However, the second order multiplication coefficient of a material has an inverse relationship with the optical bandgap. Therefore, how to realize the performance balance of the second-order frequency multiplication coefficient and the wide optical band gap of the material becomes the difficulty and the hot spot for exploring a novel infrared second-order NLO crystal material with excellent performance.
Disclosure of Invention
According to one aspect of the application, the silicon-containing mixed anion nonlinear optical crystal is provided, the optical crystal material has excellent second-order nonlinear optical properties, can realize phase matching in an infrared band, has a wide optical band gap and is higher than a commercial material AgGaS 2 The second-order frequency multiplication intensity and the laser damage threshold value of the laser can well realize the balance of large second-order frequency multiplication coefficient and wide optical band gap.
The technical scheme adopted by the application is as follows:
silicon-containing mixed anion nonlinearityAn optical crystal having the formula: ba 5 Ga 2 SiO 4 S 6 。
Optionally, the structure of the optical crystal belongs to a monoclinic system, the space group is Cc, and the unit cell parameter is Cc
α＝90°，β＝110～120°，γ＝90°。
Optionally, the optical crystal has a unit cell parameter of
α＝90°，β＝115.847±1°，γ＝90°。
Optionally, the optical crystal has a zero-dimensional isolated cluster structure.
Optionally, the zero-dimensional isolated cluster structure is composed of tetra-coordinated [ SiO ] 4 ]And heteroleptic [ GaOS 3 ]As basic asymmetric units, are formed by connecting common vertices to each other.
Optionally, the alkaline earth metal element Ba in the optical crystal is dispersedly filled in discrete clusters as a charge balance.
Optionally, the optical crystal realizes phase matching in an infrared band, has an optical band gap of 4.01-4.05 eV, and has an optical transmission range of 0.26-11.1 μm.
Optionally, the frequency doubling intensity of the optical crystal under the incident laser with the wavelength of 2050nm is 190-200 mV.
Optionally, the laser damage threshold intensity of the optical crystal under the incident laser with the wavelength of 1064nm is 47.7-50.3 MW/cm 2
According to another aspect of the present application, there is provided a method for preparing the above silicon mixed anion containing nonlinear optical crystal, comprising the steps of:
raw materials BaS and Ga 2 S 3 、Ga 2 O 3 、SiO 2 Mixing, putting into a closed container, heating and reacting to obtainTo silicon-containing mixed anion nonlinear optical crystals.
Optionally, the Ga 2 S 3 The mol ratio of the BaS to the BaS is 1;
Ga 2 S 3 and Ga 2 O 3 The molar ratio of (A) to (B) is 1;
Ga 2 S 3 with SiO 2 The molar ratio of (A) to (B) is 1.
Alternatively, the Ga 2 S 3 The molar ratio to BaS is selected from any one of 1.
Optionally, the Ga 2 S 3 And Ga 2 O 3 Is selected from any one of 1.
Optionally, the Ga 2 S 3 With SiO 2 Is selected from any one of 1.
Optionally, the reaction conditions are: heating the raw materials to 600-1200 ℃, keeping the temperature for 50-300 h, then cooling to 400-600 ℃ at a cooling rate of 1-10 ℃/h, and then naturally cooling.
Optionally, the heat preservation temperature is 800-1100 ℃.
Optionally, the heat preservation time is 120-200 h.
Optionally, the heat preservation temperature is 1100 ℃, and the heat preservation time is 150h.
Optionally, the holding temperature is 1050 ℃, and the holding time is 100h.
Optionally, the cooling rate is 1-2 ℃/h.
Optionally, the temperature reduction is reduced to 500 ℃.
Alternatively, the reaction is at 10 -4 ～10 -3 The preparation is carried out under a Pa vacuum environment.
Optionally, the method further comprises the steps of washing and drying the silicon-containing mixed anion nonlinear optical crystal obtained by the reaction.
Optionally, the drying is accelerated volatilization drying by spraying ethanol on the surface of the silicon-containing anion-mixed nonlinear optical crystal.
Optionally, the closed vessel comprises a quartz reaction tube.
According to another aspect of the application, the silicon mixed anion nonlinear optical crystal prepared by the preparation method and the application of the silicon mixed anion nonlinear optical crystal in an infrared detector, an infrared laser, photorefractive information processing, laser frequency conversion and a near-infrared probe are provided.
The beneficial effect that this application can produce includes:
1) The silicon-containing mixed anion nonlinear optical crystal provided by the application has excellent second-order nonlinear optical properties, namely, the phase matching can be realized in an infrared band, and the silicon-containing mixed anion nonlinear optical crystal has a wide optical band gap (such as E) g =4.03 eV), the powder frequency doubling strength can reach the commercial material AgGaS 2 0.65 times of the total laser damage threshold value of the glass, and the laser damage threshold value of the glass is AgGaS 2 The crystal is 17.5 times, the balance of large second-order frequency multiplication coefficient and wide optical band gap is well realized, the preparation method is simple, and the crystal has important application value in high-tech fields such as laser frequency conversion, near infrared probe, photorefractive information processing and the like, and is particularly used for infrared detectors and infrared lasers.
Drawings
FIG. 1 shows Ba obtained in example 1 of the present application 5 Ga 2 SiO 4 S 6 A schematic diagram of a crystal structure;
FIG. 2 shows Ba obtained in example 1 of the present application 5 Ga 2 SiO 4 S 6 X-ray diffraction pattern of the crystals.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials in the examples of the present application were all purchased commercially.
Example 1
Mixing BaS and Ga 2 S 3 、Ga 2 O 3 、SiO 2 The raw materials are fully and uniformly mixed according to a molar ratio of 15. Putting the raw materials into a quartz crucible, putting the quartz crucible filled with the raw materials into a quartz reaction tube, and vacuumizing to 10 DEG -3 Pa and fusing and sealing the quartz reaction tube by using oxyhydrogen flame. The quartz reaction tube is placed in a tube furnace with a temperature controller, heated to 1000 ℃ and kept warm for 150 hours. Then cooling to 500 ℃ at the speed of 3 ℃/hour, stopping heating, naturally cooling to room temperature, washing the product by deionized water and drying by ethanol to obtain the infrared nonlinear optical crystal Ba 5 Ga 2 SiO 4 S 6 And is denoted as sample 1.
Example 2
Mixing BaS and Ga 2 S 3 、Ga 2 O 3 、SiO 2 And (2) mixing the raw materials in a molar ratio of 13. Putting the raw materials into a quartz crucible, putting the quartz crucible filled with the raw materials into a quartz reaction tube, and vacuumizing to 10 DEG -3 Pa and fusing and sealing the quartz reaction tube by using oxyhydrogen flame. The quartz reaction tube is placed in a tube furnace with a temperature controller, heated to 1050 ℃, and kept warm for 120 hours. Then cooling to 500 ℃ at the speed of 3 ℃/hour, stopping heating, naturally cooling to room temperature, washing the product by deionized water and drying by ethanol to obtain the infrared nonlinear optical crystal Ba 5 Ga 2 SiO 4 S 6 And is denoted as sample 2.
Example 3
Mixing BaS and Ga 2 S 3 、Ga 2 O 3 、SiO 2 The raw materials are fully and uniformly mixed according to a molar ratio of 17. Putting the raw materials into a quartz crucible, putting the quartz crucible filled with the raw materials into a quartz reaction tube, and vacuumizing to 10 DEG -3 Pa and fusing and sealing the quartz reaction tube by using oxyhydrogen flame. The quartz reaction tube is placed in a tube furnace with a temperature controller, heated to 1050 ℃, and kept warm for 120 hours. Then cooling to 500 ℃ at the speed of 3 ℃/hour, stopping heating, naturally cooling to room temperature, washing the product by deionized water and drying by ethanol to obtain the infrared nonlinear optical crystal Ba 5 Ga 2 SiO 4 S 6 And is denoted as sample 3.
Test example 1
The samples of examples 1 to 3 were subjected to the X-ray single crystal diffraction test under the following conditions: performed on a Saturn model 724 single crystal diffractometer, mo target, ka radiation source (λ =0.07107 nm), test temperature 293K. The samples were structurally resolved by Shelx-2014. The results of the crystallographic data of the samples are shown in table 1, and the schematic of the crystal structure is shown in fig. 1.
TABLE 1
As shown in FIG. 1, the crystals prepared in examples 1 to 3 were composed of tetra-coordinated [ SiO ] 4 ]And heteroleptic [ GaOS 3 ]As basic asymmetric units, they are formed by connecting common vertexes to each other, and the alkaline earth metal element Ba is dispersedly filled in the discrete clusters and clusters as charge balance.
TABLE 2
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A silicon-containing mixed anion nonlinear optical crystal, wherein the chemical formula of the silicon-containing mixed anion nonlinear optical crystal is as follows: ba 5 Ga 2 SiO 4 S 6 。
2. The silicon-containing mixed anion nonlinear optical crystal of claim 1, wherein the structure of the optical crystal belongs to a monoclinic system, the space group is Cc, and the unit cell parameter is Cc
α＝90°，β＝110～120°，γ＝90°。
3. The silicon-containing mixed anion nonlinear optical crystal of claim 1, wherein the optical crystal has a zero-dimensional isolated cluster structure;
the zero-dimensional isolated cluster structure is composed of four-coordinated SiO 4 ]And heteroleptic [ GaOS 3 ]As basic asymmetric units, formed by connecting common vertexes to each other;
the alkaline earth metal element Ba in the optical crystal is dispersed and filled in the clusters.
4. The silicon-containing mixed anion nonlinear optical crystal according to claim 1, wherein the optical crystal realizes phase matching in an infrared band, has an optical band gap of 4.01 to 4.05eV, and an optical transmission range of 0.26 to 11.1 μm.
5. The silicon-containing mixed anion nonlinear optical crystal of claim 1, wherein the frequency doubling intensity of the optical crystal under an incident laser with a wavelength of 2050nm is 190-200 mV;
preferably, the laser damage threshold intensity of the optical crystal under the incident laser with the wavelength of 1064nm is 47.7-50.3 MW/cm 2 。
6. A method for preparing a silicon-containing mixed anion nonlinear optical crystal according to any one of claims 1 to 5, comprising the steps of:
mixing BaS and Ga 2 S 3 、Ga 2 O 3 、SiO 2 Mixing and putting into a closed container for heating reaction to obtain the silicon-containing mixed anion nonlinear optical crystal.
7. Production method according to claim 6, characterized in that the Ga 2 S 3 The mol ratio of the BaS to the BaS is 1;
Ga 2 S 3 and Ga 2 O 3 The molar ratio of (1);
Ga 2 S 3 with SiO 2 The molar ratio of (A) to (B) is 1.
8. The method of claim 6, wherein the reaction is at 10 -4 ～10 -3 The preparation is carried out under a Pa vacuum environment.
9. The method of claim 6, wherein the reaction conditions are: heating the raw materials to 600-1200 ℃, keeping the temperature for 50-300 h, then cooling to 400-600 ℃ at a cooling rate of 1-10 ℃/h, and then naturally cooling.
10. The use of the silicon-containing mixed anion nonlinear optical crystal according to any one of claims 1 to 5 and the silicon-containing mixed anion nonlinear optical crystal prepared by the preparation method according to any one of claims 6 to 9 in an infrared detector, an infrared laser, photorefractive information processing, laser frequency conversion, and a near-infrared probe.
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| US20210372006A1 (en) * | 2018-07-19 | 2021-12-02 | Technical Institute of Physics and Chemistry of the Chinese Academy of Sciences | Nonlinear optical crystal, method for preparing the same and application thereof |
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| Title |
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