CN102383196B - Nonlinear optical crystal sulfuration gallium germanium barium and growing method and purposes - Google Patents
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Abstract
The invention provides a kind of novel nonlinear optical crystal sulfuration gallium germanium barium and growing method and purposes, its chemical formula is BaGa2GeS6(being called for short BGGS). Its chemical formula is BaGa2GeS6, for center of asymmetry structure, belonging to trigonal system, space group is R3, does is cell parameter: a=9.5967 (5)?, b=9.5967 (5)?, c=8.6712 (7)?, α=β=90 °, γ=120 °, Z=1, V=691.62?3. Its Clock Multiplier Factor is AgGaS20.8 times. Adopt at high temperature sintering acquisition of solid phase synthesis process BGGS compound. Use Bridgman-Stockbarger method can successfully grow BGGS monocrystal. BaGa2GeS6Have nonlinear optical effect, be insoluble to diluted acid, chemical stability is good, can in various non-linear optical fields, be used widely, and by the nonlinear optics application of developing middle-infrared band.
Description
Technical field
The present invention relates to a kind of photoelectron functional material and growing method and purposes, particularly relate to a kind of non-linearOptical crystal material and its production and use, vulcanizes gallium germanium barium, and its chemical formula is BaGa2GeS6, be called for short BGGS.
Background technology
The nonlinear optical effect of crystal refers to so a kind of effect: when a branch of laser with certain polarization direction is by oneWhile determining incident direction by a nonlinear optical crystal (as BGGS), the frequency of this light beam changes.
The crystal with non-linearity optical effect is called nonlinear optical crystal. Here non-linearity optical effect refers to doublyFrequently and the effect such as frequency, difference frequency, optical parametric oscillation and optical parameter amplification. Only have the crystal without symmetrical centre just may have non-Linear optics effect. Utilize the nonlinear optical effect of crystal, can make second harmonic generator, upper and lower frequency converter,The device for non-linear optical such as optical parametric oscillator. The laser that laser instrument produces can carry out frequency by device for non-linear optical and turnChange, thereby the laser of the how useful wavelength of acquisition is more widely used laser instrument. According to transmission region and applicable modelEnclose, inorganic nonlinear optical crystal material can be divided into ultraviolet nonlinear optical material, visible region nonlinear optical material, infraredNonlinear optical material. Drop into practicality for existing several of Inorganic Nonlinear Optical Materials of ultraviolet and visible region at present, asKDP(potassium dihydrogen phosphate), KTP(potassium titanium oxide phosphate), BBO(beta-barium metaborate), LBO(lithium borate) etc. But for infrared non-lineProperty optical material, also has gap from practicality. Reason is existing infrared non-linear optical material, as AgGaS2、ZnGeP2Deng, although there is very large nonlinear second-order optical susceptibility, also there are the very wide scope that sees through, its laser deflection at infrared regionBe worth on the low sidely, can not meet the real requirement of non-linear optical crystal material. And the frequency inverted that realizes infrared laser is its peopleThere is important value in the field such as economy, national defence, as obtains the tunable laser beyond 3 μ m and realize mid and far infrared wave bandLaser output etc. Thereby the research of infrared inorganic nonlinear optical material has become current nonlinear optical material research fieldAn important topic.
For the research of infrared inorganic nonlinear optical material, how to overcome non-linear and lance laser damage thresholdShield, takes into account larger optical nonlinearity and higher laser damage threshold, is one of novel infrared non-linear optical material designIndividual key. For the mechanism of damage from laser, it has been generally acknowledged that band gap size is the key factor that determines laser damage threshold. SemiconductorMaterial bandwidth is little, although nonlinear optical coefficients are larger, also easily causes damage from laser. Novel infrared non-linear optics in the recent periodThe focus material of Crystal study is LiGaS2Series (LiXY2, X=Ga, In; Y=S, S, Te), their band gap is obviously greater than HuangThe semiconducting compound of copper mine configuration, reaches 3.1 to 3.7eV, has higher photo-damage resistance.
Sulfuration gallium germanium crystal of barium is to belong to trigonal system, and space group is R3. The properties table that sulfuration gallium germanium barium is testedBright this crystal likely becomes middle infrared nonlinear optical crystal that can practical application. In sulfuration gallium germanium crystal of barium structure,Ge occupies identical case with Ga, forms Ga(Ge) S tetrahedron, structure is similar to sulfurized gallium and barium (BaGa4S7,Pmn21), therefore,Sulfuration gallium germanium barium may have higher laser damage threshold and larger nonlinear optical coefficients, is expected in laser infraredWave band obtains practical application.
Summary of the invention
The object of the present invention is to provide a kind of sulfuration gallium germanium barium compound, its chemical formula is BaGa2GeS6。
The object of the present invention is to provide the large and larger infrared inorganic nonlinear optical of laser damage threshold of a kind of band gapLearn crystalline material sulfuration gallium germanium barium monocrystalline.
Another object of the present invention is to provide a kind of sulfuration gallium germanium barium compound preparation method.
Another object of the present invention is to provide a kind of sulfuration gallium germanium barium infrared inorganic nonlinear optical crystal, its chemical formulaFor BaGa2GeS6。
A further object of the present invention is to provide a kind of growth side of vulcanizing gallium germanium barium infrared inorganic nonlinear optical crystalMethod.
A further object of the invention is to provide the device of sulfuration gallium germanium barium infrared inorganic nonlinear optical crystal.
Technical scheme of the present invention is as follows:
Sulfuration gallium germanium barium compound provided by the invention, its chemical formula is BaGa2GeS6。
The preparation method of sulfuration gallium germanium barium compound provided by the invention, its step is as follows: will be containing Ba, Ga, the former material of GeThe amount of substance of material and simple substance S, than after being the even mixed grinding of ratio of 1:2:1:6, packs in graphite crucible, encloses pressure approximatelyIn quartz ampoule for 0.1Pa, slowly heat up after 200～300 DEG C, heat 1～3 hour; Then at 400～500 DEG C, addHeat 8～10 hours, finally sintering 20～50 hours at 700～900 DEG C, is cooled to room temperature, takes out and grinds, and obtains the present inventionPowdered sulfuration gallium germanium barium compound, it is carried out to XRD detection, and (a), its chemical formula is BaGa to Fig. 22GeS6. Described raw material canTo be Ba, Ga, the simple substance of Ge and S, can be also Ba, the sulfide of Ga and Ge or the sulfide of Ba, Ga, the simple substance of Ge and S.
Sulfuration gallium germanium barium nonlinear optical crystal provided by the invention, its chemical formula is BaGa2GeS6, be center of asymmetryStructure, belongs to trigonal system, and space group is R3, and cell parameter is: a=9.5967 (5), b=9.5967 (5), c=8.6712(7)?，α=β=90°，γ=120°，Z=1，V=691.62?3。
The growing method of sulfuration gallium germanium barium nonlinear optical crystal provided by the invention, its step is as follows: containing Ba, Ga,In the compound melt that the amount of substance ratio of the raw material of Ge and simple substance S is 1:2:1:6, adopt Bridgman technology grown crystal,Under the pressure that is about 0.1Pa, raw material is encapsulated in quartz ampoule, then ampoule is put into grower, slowly heat upTo raw material fusing, after raw material melts completely, growth ampoule vertically declines with the speed of 0 ~ 5 milli m/h, carries out monocrystalline rawLong, and crystal blank is carried out to post processing, crystal growth parameter(s) is 950 DEG C → 650 DEG C of growth temperatures, 0 ~ 5 millimeter of fall off rate/Hour, obtain sulfuration gallium germanium barium nonlinear optical crystal of the present invention, be of a size of 1 ~ 10 millimeter. Described raw material can be Ba, Ga,The simple substance of Ge and S, can be also Ba, the sulfide of Ga and Ge or the sulfide of Ba, Ga, the simple substance of Ge and S. The lenticular obtainingSulfuration gallium germanium barium, then grind into powder, carry out XRD detection to it, and result is as Fig. 2 b.
Described sulfuration gallium germanium barium nonlinear optical crystal, can be used for infrared nonlinear optical device, this nonlinear opticsDevice comprise by least a branch of incidence electromagnetic radiation by least one block of nonlinear optical crystal after at least a branch of frequency be different fromThe device of the output radiation of incidence electromagnetic radiation, is characterized in that nonlinear optical crystal is wherein sulfuration gallium germanium crystal of barium;The wave-length coverage of the electromagnetic radiation of described generation is 1.4 ~ 20 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.0 ~ 1.1 μ m, and the wavelength of the electromagnetic radiation of described generation canTo comprise 3.0 ~ 6.0 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.8 ~ 2.5 μ m, and the wavelength of the electromagnetic radiation of described generation canTo comprise 3.0 ~ 6.0 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.0 ~ 1.1 μ m, and the wavelength of the electromagnetic radiation of described generation canTo comprise 8.0 ~ 12.0 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.8 ~ 2.5 μ m, and the wavelength of the electromagnetic radiation of described generation canTo comprise 8.0 ~ 12.0 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.06 μ m, and the wavelength of the electromagnetic radiation of described generation is passableComprise 4.3 μ m.
The wavelength of described incidence electromagnetic radiation can be 1.8 ~ 2.2 μ m, and the wavelength of the electromagnetic radiation of described generation canTo comprise 4.3 μ m.
Sulfuration gallium germanium barium nonlinear optical crystal is for the harmonic oscillator of 1.4 ~ 20 μ m middle infrareds, optical parameter with putLarge device and fiber waveguide device.
Sulfuration gallium germanium barium nonlinear optical crystal is for optical parameter and amplifying device from infrared to mid and far infrared district.
Described nonlinear optical crystal can make its cross section be greater than 70mm by splicing.
It is the compound of BaGa2GeS6 that effect of the present invention has been to provide a kind of chemical formula, this compound non-linearOptical crystal and its production and use. Use powder frequency doubling method of testing to measure the phase matched ability of BGGS, confirmBGGS can realize the 2 frequency multiplication outputs that the additional OPO incident wavelength of Nd:YAG laser is 2 μ m, and powder SHG effect is0.8 times of AgGaS2. In addition, BGGS monocrystalline yellow transparent, approximately 870 DEG C of fusing points, hardness is larger, and good mechanical property is not easily brokenAnd deliquescence. BGGS is applicable to the needs of infrared band laser frequency conversion, can make infrared nonlinear optical device with it.
Brief description of the drawings
Fig. 1 is BGGS crystal structure schematic diagram.
Fig. 2 is the x x ray diffraction collection of illustrative plates of BGGS, and wherein 2a is the diffraction pattern of the synthetic BGGS powder sample of solid phase, and 2b isThe BGGS monocrystalline last diffraction pattern of pulverizing.
Fig. 3 is the schematic diagram of BGGS crystal as frequency-doubling crystal application non-linear hour optical effect, and wherein 1 is speculum, 2Q-switch, the 3rd, polarizer, the 4th, Nd:YAG, the 5th, OPO inputs mirror, and the 6th, ktp crystal, the 7th, OPO outgoing mirror and 1064nm rippleLong light total reflection mirror, 8 is light reflection mirrors of 2.1 mum wavelengths, the 9th, through the BGGS monocrystal of crystal post processing and optics processing,The 10th, the outgoing laser beam producing.
Detailed description of the invention
Embodiment 1
Adopt high temperature solid state reaction synthetic compound BaGa2GeS6
Raw materials used: BaS analyzes pure AR0.0687 gram (0.0005mol)
SP0.0697 gram of Ga spectroscopic pure (0.001mol)
SP0.0363 gram of Ge spectroscopic pure (0.0005mol)
S analyzes pure AR0.08017 gram (0.0025mol)
Its chemical equation is:
BaS+2Ga+Ge+5S=BaGa2GeS6
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, put into that mortar mixes and carefullyGrind, then pack in the graphite crucible of Φ 12 × 40mm, with spoon, its compression is added a cover, put into quartz ampoule, through 4-6After hour vacuumizing, when quartz ampoule internal pressure is about 0.1Pa, is placed in Muffle furnace and is slowly warming up to oxyhydrogen flame tube sealing300 DEG C and heated at constant temperature 5 hours, then be warming up to 500 DEG C and heated at constant temperature 5 hours, and then be warming up to 500 DEG C and heated at constant temperature10 hours, be finally warming up to 700 DEG C and constant temperature sintering 48 hours, heating rate must be slow, prevents unreacted sulphur simple substance shapeBecome sulphur steam, quartz ampoule is burst. Cooling rear taking-up crucible, now sample is more loose. Then taking out sample grinds all againEven, then be placed in graphite crucible and add a cover, after vacuumizing, in Muffle furnace, be warming up at 750 DEG C sintering 20 hours, cooling rear taking-up,At this moment sample is formed one, sample is put into mortar and smash grinding to pieces and obtain product. This product is carried out to X-ray analysis, gained(Fig. 2 a) pulverizes with BGGS monocrystalline that (Fig. 2 is b) consistent to last X ray picture to spectrogram.
Embodiment 2 adopts high temperature solid state reaction synthetic compound BaGa2GeS6
Raw materials used: BaS analyzes pure AR0.1374 gram (0.001mol)
Ga2S3Analyze pure AR0.413 gram (0.001mol)
GeS2Analyze pure AR0.1367 gram (0.001mol)
Its chemical equation is:
BaS+Ga2S3+GeS2=BaGa2GeS6
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, put into that mortar mixes and carefullyGrind, then pack in the graphite crucible of Φ 12 × 40mm, with spoon, its compression is added a cover, put into quartz ampoule, through 4-6After hour vacuumizing, when quartz ampoule internal pressure is about 0.1Pa, is placed in Muffle furnace and slowly heats up with oxyhydrogen flame tube sealingTo 500 DEG C and heated at constant temperature 20 hours, be then warming up to 700 DEG C and constant temperature sintering 48 hours, cooling rear taking-up crucible, this up-to-date styleProduct are more loose. Then take out sample and again grind evenly, then be placed in graphite crucible and add a cover, after vacuumizing, in Muffle furnace, heat upTo sintering at 750 DEG C 20 hours, cooling rear taking-up, at this moment sample is formed one, sample is put into mortar and smash grinding to pieces and get final productProduct. This product is carried out to X-ray analysis, gained spectrogram (Fig. 2 a) with BGGS monocrystalline pulverize last X ray picture (figure2b) consistent.
Embodiment 3 adopts high-temperature fusant slow cooling method grown crystal BaGa2GeS6
Crystal growing apparatus is homemade Resistant heating stove, and temperature controlling instruments is that 908PHK20 type is able to programme temperature automatically controlledInstrument.
Raw materials used: BaS analyzes pure AR0.687 gram (0.005mol)
SP0.697 gram of Ga spectroscopic pure (0.01mol)
SP0.363 gram of Ge spectroscopic pure (0.005mol)
S analyzes pure AR0.8017 gram (0.025mol)
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, then pack Φ 12 × 60 intoIn the graphite crucible of mm, with spoon, its compression is added a cover, put into quartz ampoule, after 4-6 hour vacuumizes, quartz ampouleWhen internal pressure is about 0.1Pa, with oxyhydrogen flame tube sealing be placed in Muffle furnace, be slowly warming up to 300 DEG C and heated at constant temperature 5 littleTime, after be warming up to again 500 DEG C and heated at constant temperature 10 hours, and then be warming up to 700 DEG C and heated at constant temperature 20 hours, finally rise950 DEG C of temperature are to raw material fusing, and constant temperature 20～80 hours, was then cooled to 600 DEG C with 10 hours, closed stove. Treat that sample is coolingAfter, obtain transparent BaGa2GeS6Monocrystalline.
Embodiment 4 adopts Bridgman-Stockbarge method for growing crystal BaGa2GeS6
Crystal growing apparatus is homemade Resistant heating stove, and temperature controlling instruments is that 908PHK20 type is able to programme temperature automatically controlledInstrument.
Raw materials used: BaS analyzes pure AR0.687 gram (0.005mol)
SP0.697 gram of Ga spectroscopic pure (0.01mol)
SP0.363 gram of Ge spectroscopic pure (0.005mol)
S analyzes pure AR0.8017 gram (0.025mol)
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, then pack Φ 12 × 60 intoIn the graphite crucible of mm, with spoon, its compression is added a cover, put into quartz ampoule, after 4-6 hour vacuumizes, quartz ampouleWhen internal pressure is about 0.1Pa, is placed on and in crucible decline stove, is slowly warming up to 300 DEG C and heated at constant temperature 5 with oxyhydrogen flame tube sealingHour, then be warming up to 500 DEG C and heated at constant temperature 5 hours, and then be warming up to 700 DEG C and heated at constant temperature 10 hours, and then riseTemperature, to 900 DEG C and heated at constant temperature 20 hours, finally heats up 950 DEG C to raw material fusing, constant temperature 20～80 hours, and now crucible is pressedBe 2mm/h according to fall off rate, after decline 100mm, be cooled to room temperature with approximately 10 hours, close stove. After sample is cooling,Obtain transparent BaGa2GeS6Monocrystalline.
Embodiment 5
The crystal that example 3,4 is obtained, processes the position that is placed on 9 in Fig. 3 shown device, in room temperature through processingUnder, with adjusting QNd; The additional OPO of YAG laser does input light source, and incident wavelength is 2100nm, receives by photomultiplier tubeThe frequency doubled light output of 1050nm, output intensity is about equal conditions AgGaS20.8 times.
Claims (14)
1. the nonlinear optical crystal of compound sulfuration gallium germanium barium, is characterized in that: its chemical formula is BaGa2GeS6, be center of asymmetryStructure, belongs to trigonal system, and space group is R3, and cell parameter is: α＝β＝90°，γ＝120°，Z＝1，Be of a size of 1-10 millimeter.
2. the growing method of nonlinear optical crystal claimed in claim 1, is characterized in that containing Ba, Ga, the raw material of GeCompare in the compound melt for 1:2:1:6 and adopt the growth of high-temperature fusant slow cooling method with the amount of substance of simple substance S, 0.1Pa'sUnder pressure, raw material is encapsulated in quartz ampoule, then ampoule is put into grower, be slowly warming up to raw material fusing, treat formerAfter material melts completely, quartz ampoule carries out crystal growth with the speed slow cooling of 1～3 DEG C/h, can obtain sulfuration gallium germaniumBarium nonlinear optical crystal; The raw material of described Ba are Ba simple substance or BaS compound; The raw material of described Ga are Ga simple substanceOr GaS compound; The raw material of described Ge are Ge simple substance or GeS compound.
3. the growing method of nonlinear optical crystal claimed in claim 1, is characterized in that containing Ba, Ga, the raw material of GeCompare in the compound melt for 1:2:1:6 and adopt Bridgman technology grown crystal with the amount of substance of simple substance S, at 0.1PaPressure under, raw material is encapsulated in quartz ampoule, then ampoule is put into grower, be slowly warming up to raw material fusing, treatAfter raw material melts completely, quartz ampoule with 0～5 milli m/h speed vertically decline, carry out crystal growth; Crystal has been grownCheng Hou, is down to room temperature with the speed of 10～30 DEG C/h, can obtain sulfuration gallium germanium barium nonlinear optical crystal; Described Ba'sRaw material are Ba simple substance or BaS compound; The raw material of described Ga are Ga simple substance or GaS compound; Described Ge'sRaw material are Ge simple substance or GeS compound.
4. the purposes of nonlinear optical crystal claimed in claim 1, is characterized in that: for infrared nonlinear optical device,This device for non-linear optical comprises makes at least a branch of incidence electromagnetic radiation by producing extremely after at least one block of nonlinear optical crystalFew a branch of frequency is different from the device of the output radiation of incidence electromagnetic radiation.
5. purposes as claimed in claim 4, is characterized in that: the wave-length coverage of the electromagnetic radiation of described generation is 1.4～20 μm。
6. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.0～1.1 μ m, producesThe wavelength of raw electromagnetic radiation comprises 3.0～6.0 μ m.
7. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.8～2.5 μ m, producesThe wavelength of raw electromagnetic radiation comprises 3.0～6.0 μ m.
8. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.0～1.1 μ m, producesThe wavelength of raw electromagnetic radiation comprises 8.0～12.0 μ m.
9. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.8～2.5 μ m, producesThe wavelength of raw electromagnetic radiation comprises 8.0～12.0 μ m.
10. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.06 μ m, generationThe wavelength of electromagnetic radiation comprises 4.3 μ m.
11. purposes as claimed in claim 4, is characterized in that: the wavelength of described incidence electromagnetic radiation is 1.8～2.2 μ m, produceThe wavelength of raw electromagnetic radiation comprises 4.3 μ m.
12. purposes as claimed in claim 4, is characterized in that: described nonlinear optical crystal makes its section by splicingFace is greater than 70mm.
The purposes of 13. nonlinear optical crystals claimed in claim 1, is characterized in that: described nonlinear optical crystal is usedIn the harmonic oscillator of 1.4～20 μ m middle infrareds, optical parameter and amplifying device and fiber waveguide device.
The purposes of 14. nonlinear optical crystals claimed in claim 1, is characterized in that: described nonlinear optical crystal is usedIn the optical parameter from infrared to mid and far infrared district and amplifying device.
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| CN103058266A (en) * | 2011-10-20 | 2013-04-24 | 中国科学院理化技术研究所 | BaGa2GeS6 compound, BaGa2GeS6 nonlinear optical crystal, and preparation method and application thereof |
| CN102644117A (en) * | 2012-04-27 | 2012-08-22 | 中国科学院福建物质结构研究所 | Selenium indium bismuth barium single crystal, preparation and application thereof |
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| CN109853039B (en) * | 2019-02-01 | 2021-04-06 | 中国科学院福建物质结构研究所 | Single crystal material Ba13In12Zn7S38Preparation method and application thereof |
| CN111041559B (en) * | 2019-12-13 | 2021-07-20 | 四川大学 | Synthetic container and synthetic method of quaternary sulfur lithium compound polycrystal |
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