CN110791812B - BaHgSnSe4Nonlinear optical crystal and preparation method and application thereof - Google Patents
BaHgSnSe4Nonlinear optical crystal and preparation method and application thereof Download PDFInfo
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- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000002269 spontaneous effect Effects 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 32
- 150000001875 compounds Chemical class 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
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- 238000002156 mixing Methods 0.000 claims description 6
- 230000005670 electromagnetic radiation Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 238000003746 solid phase reaction Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
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- 229910013321 LiB3O5 Inorganic materials 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
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- 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
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- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- 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
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Abstract
The invention discloses BaHgSnSe4Nonlinear optical crystal and its preparation method and application; BaHgSnSe4The nonlinear optical crystal grows by adopting a high-temperature melt spontaneous crystallization method or a Bridgman method; in the BaHgSnSe4In the growth of the nonlinear optical crystal, the crystal has the advantages of high growth speed, low cost, easy obtainment of crystals with larger size and the like; the obtained BaHgSnSe4The nonlinear optical crystal has large nonlinear optical effect (AgGaS under the same condition)26.3 times of the total reflection band), wide light-transmitting wave band (1-22 mu m), high hardness, good mechanical property, easy processing and the like; the BaHgSnSe4The nonlinear optical crystal can be used for manufacturing nonlinear optical devices.
Description
Technical Field
The invention relates to BaHgSnSe4Non-linear optical crystal of (BaHgSnSe)4Single crystal) and the BaHgSnSe4Method for producing single crystal and BaHgSnSe4Use of a single crystal for the manufacture of a non-linear optical device.
Background
Crystals with nonlinear optical effects are referred to as nonlinear optical crystals. The nonlinear optical effect refers to the effects of frequency doubling, sum frequency, difference frequency, parametric amplification and the like. Only crystals that do not have a center of symmetry may have nonlinear optical effects. By using the nonlinear optical effect of crystal, the nonlinear optical devices such as second harmonic generator, upper and lower frequency converter, optical parametric oscillator, etc. can be made. The laser generated by the laser can be subjected to frequency conversion through the nonlinear optical device, so that more useful wavelengths of laser can be obtained, and the laser can be widely applied. The optical materials can be divided into three categories of nonlinear optical materials in ultraviolet region, visible and near infrared region and middle infrared region according to different application wave bands of the materials. The nonlinear optical crystal materials in the visible light region and the ultraviolet light region can meet the requirements of practical application; e.g. at double frequency (53)2nm) crystal is mainly KTP (KTiOPO)4)、BBO(β-BaB2O4)、 LBO(LiB3O5) A crystal; among the frequency tripling (355nm) crystals that are practical are BBO, LBO, CBO (CsB)3O5) And (4) selecting. The development of the nonlinear crystal of the infrared band is slower; most of materials for infrared region are ABC2Type chalcopyrite-structured semiconductor materials, e.g. AgGaQ2The optical damage threshold of the (Q ═ S, Se) infrared nonlinear crystal is too low and the crystal growth is difficult, which directly affects the practical use. The mid-infrared band nonlinear optical crystal has important application in the field of photoelectron, for example, it can extend the laser (such as 1.064 μm) of near-infrared band to the mid-infrared region by means of optical parametric oscillation or optical parametric amplification; it can also be used for important laser (such as CO)2Laser, 10.6 μm) is frequency doubled, which is of great significance for obtaining laser with continuously adjustable wavelength. Therefore, the search for new infrared nonlinear optical crystal materials with excellent performance has become one of the difficulties and leading directions in the current nonlinear optical material research field.
Disclosure of Invention
The invention aims to provide BaHgSnSe4A nonlinear optical crystal. The obtained BaHgSnSe4The nonlinear optical crystal has the advantages of large nonlinear optical effect, wide light-transmitting wave band, high hardness, good mechanical property, easy processing and the like; the BaHgSnSe4The nonlinear optical crystal can be used for manufacturing nonlinear optical devices.
Another object of the present invention is to provide BaHgSnSe4A preparation method of nonlinear optical crystal.
It is still another object of the present invention to provide BaHgSnSe4The application of the nonlinear optical crystal in the preparation of nonlinear optical devices.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
BaHgSnSe4A nonlinear optical crystal of BaHgSnSe4The nonlinear optical crystal has no symmetry center, belongs to an orthorhombic system, has a space group of Fdd2, and has the following unit cell parameters:
α＝β＝γ＝90°，Z＝32。
the BaHgSnSe provided by the invention4The preparation method of the nonlinear optical crystal comprises the following steps: BaHgSnSe growth by high-temperature melt spontaneous crystallization method or crucible descent method4A nonlinear optical crystal.
In particular, the high-temperature melt spontaneous crystallization method is used for growing BaHgSnSe4A nonlinear optical crystal comprising the steps of: will have a composition equivalent to BaHgSnSe4Mixture of (A) or powdered BaHgSnSe4Heating the compound to melt to obtain high-temperature melt, keeping the high-temperature melt for 24-96 hours, and then cooling to room temperature at the cooling rate of 1-10 ℃/hour to obtain red BaHgSnSe4A nonlinear optical crystal.
The BaHgSnSe provided by the invention4Another preparation method of the nonlinear optical crystal is the Bridgman-Stockbarge method for growing BaHgSnSe4A nonlinear optical crystal comprising the steps of:
will have a composition equivalent to BaHgSnSe4Mixture of (A) or powdered BaHgSnSe4Placing the compound in a crystal growth device, slowly heating until the raw materials are molten, after the raw materials are completely molten, vertically descending the crystal growth device at a speed of 0.1-10mm/h, and carrying out BaHgSnSe in the descending process of the crystal growth device4The nonlinear optical crystal grows in a growth period of 5-20 days.
In the invention, the composition is equal to BaHgSnSe4The mixture of (a) is prepared by mixing a Ba source material, a Hg source material, a Sn source material and a Se simple substance according to a molar ratio of Ba: Hg: Sn: Se ═ 1: 1: 1: 4, and mixing the components in a ratio of 4. The Ba source material is Ba or BaSe; the Hg source material is Hg or HgSe; the Sn source material is Sn or SnSe2。
In the invention, the powdered BaHgSnSe4The compounds were prepared as follows:
ba source material, Hg source material, Sn source material and simple substance Se are mixed according to a molar ratio BHg, Sn, Se, 1: 1: 1: 4, heating to 600-1150 ℃ for solid phase reaction (in principle, BaHgSnSe can be prepared by general chemical synthesis method4A compound; the solid phase reaction method is preferred in the invention), the chemical formula of BaHgSnSe is obtained4Crushing and grinding the compound to obtain powder BaHgSnSe4A compound of (1);
the Ba source material is Ba or BaSe;
the Hg source material is Hg or HgSe;
the Sn source material is Sn or SnSe2。
The BaHgSnSe4The compound can be prepared according to the following chemical reaction formula:
(1)Ba+Hg+Sn+4Se＝BaHgSnSe4；
(2)Ba+Hg+SnSe+3Se＝BaHgSnSe4；
(3)Ba+Hg+SnSe2+2Se＝BaHgSnSe4；
(4)Ba+HgSe+Sn+3Se＝BaHgSnSe4；
(5)Ba+HgSe+SnSe+2Se＝BaHgSnSe4；
(6)Ba+HgSe+SnSe2+Se＝BaHgSnSe4；
(7)BaSe+Hg+Sn+3Se＝BaHgSnSe4；
(8)BaSe+Hg+SnSe+2Se＝BaHgSnSe4；
(9)BaSe+Hg+SnSe2+Se＝BaHgSnSe4；
(10)BaSe+HgSe+Sn+2Se＝BaHgSnSe4；
(11)BaSe+HgSe+SnSe+Se＝BaHgSnSe4；
(12)BaSe+HgSe+SnSe2＝BaHgSnSe4。
the BaHgSnSe with centimeter-level size can be obtained by adopting the two methods4A nonlinear optical crystal; by using large-size crucible and prolonging growth period, BaHgSnSe with correspondingly large size can be obtained4A nonlinear optical crystal.
According to the crystallographic data of the crystal, the crystal blank is oriented according to the required angle and thicknessCutting crystal according to the size and the cross section, and polishing the light passing surface of the crystal to obtain the BaHgSnSe crystal serving as a nonlinear optical device4The nonlinear optical crystal has the advantages of large nonlinear optical effect, wide light transmission range, stable physical and chemical properties, higher hardness, good mechanical properties, difficult cracking, difficult deliquescence, easy processing and storage and the like; therefore, the invention further provides BaHgSnSe4The application of the nonlinear optical crystal in the preparation of nonlinear optical devices is to use the BaHgSnSe4Nonlinear optical crystal for preparing nonlinear optical device, the nonlinear optical device comprises at least one beam of incident electromagnetic radiation passing through at least one piece of BaHgSnSe4Means for generating at least one output radiation having a frequency different from that of the incident electromagnetic radiation after the nonlinear optical crystal.
The invention has the following technical effects:
in the BaHgSnSe4The crystal is easy to grow in the growth of the nonlinear optical crystal, is transparent and has no package, and has the advantages of high growth speed, low cost, easy obtainment of crystals with larger size and the like; the BaHgSnSe obtained4The nonlinear optical crystal has the advantages of large nonlinear optical effect, wide light-transmitting wave band, high hardness, good mechanical property, difficult cracking and deliquescence, easy processing and storage and the like; the BaHgSnSe4The nonlinear optical crystal can be used for manufacturing nonlinear optical devices.
Drawings
FIG. 1 shows BaHgSnSe according to the present invention4Working principle diagram of a typical nonlinear optical device made of nonlinear optical crystal;
wherein 1 is a laser, 2 is an incident laser beam, and 3 is BaHgSnSe after crystal post-treatment and optical processing4A nonlinear optical crystal, 4 is the generated outgoing laser beam, and 5 is a filter.
FIG. 2 is BaHgSnSe4The structure of the nonlinear optical crystal is shown schematically.
Detailed Description
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The description is only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
The invention is described in further detail below with reference to the figures and the detailed description.
Example 1 preparation of BaHgSnSe by high temperature melt spontaneous crystallization4Crystal:
10.82 g BaSe, 13.98 g HgSe and 13.84 g SnSe were weighed2(i.e., BaSe: HgSe: SnSe)20.05 mol: 0.05 mol: 0.05mol), uniformly mixing, putting into a quartz glass tube with the diameter of 12mm multiplied by 200mm, and vacuumizing to 10 DEG-3Packaging with oxyhydrogen flame, placing in a tubular growth furnace, slowly heating to 900 ℃, keeping the temperature for 72 hours, slowly cooling to room temperature at the speed of 1 ℃/h, and closing the tubular growth furnace; cutting the quartz tube after cooling to obtain red BaHgSnSe with the color of 12mm phi and 60mm phi4And (4) crystals.
Example 2 preparation of BaHgSnSe by Bridgman method4Crystal:
43.26 g BaSe, 55.92 g HgSe and 55.34 g SnSe were weighed2(Ba: Hg: Sn: Se 0.2 mol: 0.2 mol: 0.2 mol: 0.8mol), uniformly mixed, put into a quartz glass tube of phi 25 mm. times.200 mm, and evacuated to 10mm-3Packaging with oxyhydrogen flame, placing in a crystal growth furnace, slowly heating to 950 ℃ to melt the raw materials, and vertically descending the growth device at a speed of 10mm/h after the raw materials are completely melted; 5 days of crystal growth, after the growth is finished, the growth device is cooled to room temperature for 50 hours to obtain red BaHgSnSe with the diameter of 25mm multiplied by 90mm4A nonlinear optical crystal.
Example 3 preparation of BaHgSnSe by high temperature melt spontaneous crystallization4Crystal:
weighing powdery BaHgSnSe4The compound (2) is put into a quartz glass tube with the diameter of phi 10mm multiplied by 100mm and vacuumized to 10-3Packaging with oxyhydrogen flame, placing in a tubular growth furnace, slowly heating to 1000 ℃, keeping the temperature for 24 hours, slowly cooling to room temperature at the speed of 10 ℃/h, and closing the tubular growth furnace; cutting the quartz tube after the quartz tube is cooled,the red BaHgSnSe with the diameter of 10mm multiplied by 60mm can be obtained4A nonlinear optical crystal.
Example 4 preparation of BaHgSnSe by Bridgman method4Crystal:
weighing powdery BaHgSnSe4The compound (2) is put into a quartz glass tube with the diameter of phi 20mm multiplied by 200mm and vacuumized to 10-3Packaging with oxyhydrogen flame, placing in a crystal growth furnace, slowly heating to 1000 deg.C to melt the raw materials, and vertically lowering the growth device at a speed of 0.1 mm/hr after the raw materials are completely melted; growing the crystal for 20 days, and after the growth is finished, cooling the growth device to room temperature for 40 hours to obtain red BaHgSnSe with the color of phi 20 multiplied by 90mm4A nonlinear optical crystal.
Tested, BaHgSnSe prepared in examples 1-4 above4The nonlinear optical crystal belongs to an orthorhombic system, the space group is Fdd2, and the unit cell parameters are:
α＝β＝γ＝90°，Z＝32，
has frequency doubling effect, and the light transmission range is 1-22 μm; FIG. 2 shows the BaHgSnSe4The structure of the nonlinear optical crystal is shown schematically.
Example 5:
BaHgSnSe obtained in examples 1 to 44The crystal is not easy to be broken and deliquesced, and is easy to be cut, polished and stored. BaHgSnSe obtained in examples 1 to 44A crystal placed at the position 3 of the device shown in figure 1, using Q-switched Ho: Tm: Cr: YAG laser as light source at room temperature, and inputting infrared light with wavelength of 2090nm and outputting frequency-doubled light with wavelength of 1045nm, wherein the laser intensity is AgGaS under the same condition26.3 times of the total weight of the powder.
FIG. 1 shows BaHgSnSe according to the present invention4Working principle diagram of a typical nonlinear optical device made of nonlinear optical crystal, wherein 1 is laser, 2 is incident laser beam, and 3 is BaHgSnSe after crystal post-treatment and optical processing4A nonlinear optical crystal, 4 is producedEmitting laser beams, 5 is a filter plate; an incident laser beam 2 emitted by a laser 1 is incident on BaHgSnSe4The single crystal 3 generates an outgoing laser beam 4 which is passed through a filter 5 to obtain the desired laser beam.
BaHgSnSe using the invention4The device made of the nonlinear optical crystal can be a frequency doubling generator, an upper frequency converter, a lower frequency converter, an optical parametric oscillator, an optical parametric amplifier and the like.
The method can be realized by upper and lower limit values and interval values of intervals of process parameters (such as temperature, time and the like), and embodiments are not listed.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. BaHgSnSe4A nonlinear optical crystal, wherein the BaHgSnSe is4The nonlinear optical crystal has no symmetry center, belongs to an orthorhombic system, has a space group of Fdd2, and has the following unit cell parameters:
α＝β＝γ＝90°，Z＝32；
the BaHgSnSe4The preparation method of the nonlinear optical crystal comprises the following steps: BaHgSnSe growth by high-temperature melt spontaneous crystallization method or crucible descent method4A nonlinear optical crystal;
high-temperature melt spontaneous crystallization method for growing BaHgSnSe4A nonlinear optical crystal comprising the steps of:
will have a composition equivalent to BaHgSnSe4Mixture of (A) or powdered BaHgSnSe4Heating the compound to melt to obtain high-temperature melt, keeping the high-temperature melt for 24-96 hours, and then cooling to room temperature at the cooling rate of 1-10 ℃/hour to obtain BaHgSnSe4A nonlinear optical crystal;
growth of BaHgSnSe by Bridgman method4A nonlinear optical crystal comprising the steps of:
will have a composition equivalent to BaHgSnSe4Mixture of (A) or powdered BaHgSnSe4Placing the compound in a crystal growth device, slowly heating until the raw materials are molten, after the raw materials are completely molten, vertically descending the crystal growth device at a speed of 0.1-10mm/h, and carrying out BaHgSnSe in the descending process of the crystal growth device4Growing the nonlinear optical crystal, wherein the growth period is 5-20 days;
composition is equivalent to BaHgSnSe4The mixture of (a) is prepared by mixing a Ba source material, a Hg source material, a Sn source material and a Se simple substance according to a molar ratio of Ba: Hg: Sn: Se ═ 1: 1: 1: 4, and mixing the components in a ratio of 4.
2. The BaHgSnSe of claim 14The nonlinear optical crystal is characterized in that the Ba source material is Ba or BaSe; the Hg source material is Hg or HgSe; the Sn source material is Sn or SnSe2。
3. The BaHgSnSe of claim 14Nonlinear optical crystal, characterized in that the powdery BaHgSnSe4The preparation of the compound comprises the following steps:
mixing a Ba source material, a Hg source material, a Sn source material and simple substance Se according to a molar ratio of Ba to Hg to Sn to Se of 1: 1: 1: 4, heating to 600-1150 ℃ for solid phase reaction to obtain BaHgSnSe with the chemical formula of4Crushing and grinding the compound to obtain powder BaHgSnSe4A compound of (1);
the Ba source material is Ba or BaSe;
the Hg source material is Hg or HgSe;
the Sn source material is Sn or SnSe orSnSe2。
4. The BaHgSnSe of claim 14The application of the nonlinear optical crystal in the preparation of nonlinear optical devices.
5. Use according to claim 4, wherein the nonlinear optical device produced comprises passing at least one beam of incident electromagnetic radiation through at least one of the BaHgSnSe' s4Means for generating at least one output radiation having a frequency different from that of the incident electromagnetic radiation after the nonlinear optical crystal.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951181A (en) * | 2016-05-18 | 2016-09-21 | 中国科学院福建物质结构研究所 | Crystal material, method for preparing same and application of crystal material used as infrared nonlinear optical material |
| CN106629819A (en) * | 2016-10-14 | 2017-05-10 | 中国工程物理研究院化工材料研究所 | Compound SrCdGeS4 and preparation method thereof, and infrared nonlinear optical crystal as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951181A (en) * | 2016-05-18 | 2016-09-21 | 中国科学院福建物质结构研究所 | Crystal material, method for preparing same and application of crystal material used as infrared nonlinear optical material |
| CN106629819A (en) * | 2016-10-14 | 2017-05-10 | 中国工程物理研究院化工材料研究所 | Compound SrCdGeS4 and preparation method thereof, and infrared nonlinear optical crystal as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| An investigation of new infrared nonlinear optical material: BaCdSnSe4, and three new related centrosymmetric compounds: Ba2SnSe4, Mg2GeSe4, and Ba2Ge2S6;Kui Wu等;《Dalton Trans.》;20151015;第44卷;19856-19864 * |
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