CN105506743A - Li6Cd5Sn4Se16Nonlinear optical crystal and its preparation method and use - Google Patents
Li6Cd5Sn4Se16Nonlinear optical crystal and its preparation method and use Download PDFInfo
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- CN105506743A CN105506743A CN201511020624.0A CN201511020624A CN105506743A CN 105506743 A CN105506743 A CN 105506743A CN 201511020624 A CN201511020624 A CN 201511020624A CN 105506743 A CN105506743 A CN 105506743A
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- 239000013078 crystal Substances 0.000 title claims abstract description 94
- 230000003287 optical effect Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000002269 spontaneous effect Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 40
- 239000000126 substance Substances 0.000 claims description 36
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 9
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- KBPGBEFNGHFRQN-UHFFFAOYSA-N bis(selanylidene)tin Chemical class [Se]=[Sn]=[Se] KBPGBEFNGHFRQN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052793 cadmium Inorganic materials 0.000 claims description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- PEXNRZDEKZDXPZ-UHFFFAOYSA-N lithium selenidolithium Chemical compound [Li][Se][Li] PEXNRZDEKZDXPZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000005670 electromagnetic radiation Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000003746 solid phase reaction Methods 0.000 claims description 2
- 238000010671 solid-state reaction Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical group [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- 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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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nonlinear Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to Li6Cd5Sn4Se16Nonlinear optical crystal and its preparation method and application; the Li6Cd5Sn4Se16The nonlinear optical crystal has no symmetric center, belongs to an orthorhombic system, and has a space group of Pna21The unit cell parameters are as follows:α ═ β ═ γ ═ 90 °; the nonlinear optical crystal grows by adopting a high-temperature melt spontaneous crystallization method or a Bridgman-Stockbarge method; the nonlinear optical crystal is easy to grow, transparent and free of package in growth, and has the advantages of high growth speed, low cost, easiness in obtaining crystals with larger size and the like; the nonlinear optical crystal has wide light-transmitting wave band, high hardness, good mechanical property, and low liability to cracking and deliquescenceEasy processing and storage; the Li6Cd5Sn4Se16The nonlinear optical crystal can be used for manufacturing nonlinear optical devices.
Description
Technical field
The invention belongs to non-linear optic crystal, preparation and for field, particularly a kind of Li
6cd
5sn
4se
16non-linear optic crystal (Li
6cd
5sn
4se
16monocrystalline) and this SnGa
4se
7the preparation method of monocrystalline and this Li
6cd
5sn
4se
16the purposes of device for non-linear optical of monocrystalline for making.
Background technology
The crystal with non-linear optical effect is called non-linear optic crystal.Here non-linear optical effect refers to the effect such as frequency multiplication and frequency, difference frequency, parameter amplification.Only have the crystal without symmetry centre just may have non-linear optical effect.Utilize the non-linear optical effect of crystal, can second harmonic generator be made, upper and lower frequency converter, the device for non-linear optical such as optical parametric oscillator.The laser that laser apparatus produces carries out frequency inverted by device for non-linear optical, thus obtains the laser of more how useful wavelength, and laser apparatus is more widely used.According to the difference of materials application wave band, ultraviolet region, visible and near-infrared region and mid-infrared light district nonlinear optical material three major types can be divided into.The non-linear optical crystal material of visible region and ultraviolet region can meet the requirement of practical application; KTP (KTiOPO is mainly contained as practical in two frequencys multiplication (532nm) crystal
4), BBO (β-SnB
2o
4), LBO (LiB
3o
5) crystal; In frequency tripling (355nm) crystal, practicality has BBO, LBO, CBO (CsB
3o
5) available.And the nonlinear crystal development of infrared band is slow; The material in infrared light district is ABC mostly
2the chalcopyrite structure semiconductor material of type, as AgGaQ
2(Q=S, Se, Te), the light injury threshold of infrared non-linear crystal is too low and crystal growth difficult, directly affects actual use.Middle-infrared band non-linear optic crystal has important application at optoelectronic areas, and such as the laser (as 1.064 μm) of near-infrared band can be extended to middle infrared by the means such as optical parametric oscillation or optically erasing by it; Also can to the important laser in mid-infrared light district (as CO
2laser, 10.6 μm) carry out frequency multiplication, this is significant for the continuously adjustable laser of acquisition wavelength.Therefore the novel infrared nonlinear optical crystal material finding premium properties has become one of the difficult point and direction, forward position of current nonlinear optical material research field.
We have studied Li first
6cd
5sn
4se
16crystalline structure, and find Li
6cd
5sn
4se
16there is non-linear optical property.
Summary of the invention
The object of the invention is to provide a kind of Li
6cd
5sn
4se
16non-linear optic crystal.
Another object of the present invention is to provide Li
6cd
5sn
4se
16the preparation method of non-linear optic crystal.
Still a further object of the present invention is to provide Li
6cd
5sn
4se
16the purposes of non-linear optic crystal.
Technical scheme of the present invention is as follows:
Li provided by the invention
6cd
5sn
4se
16non-linear optic crystal, this Li
6cd
5sn
4se
16non-linear optic crystal does not have symmetry centre, and belong to rhombic system, spacer is Pna2
1, its unit cell parameters is:
α=β=γ=90 °.
Li provided by the invention
6cd
5sn
4se
16the preparation method of non-linear optic crystal, it is high-temperature fusant spontaneous crystallization method growth Li
6cd
5sn
4se
16non-linear optic crystal, the steps include:
By Powdered Li
6cd
5sn
4se
16compound or according to mol ratio Li:Cd:Sn
4: the mixture of Se=6:5:4:16 ratio mixing is heated to melt to obtain high temperature solution, and keeps 24-96 hour under this high temperature solution state, afterwards, is cooled to room temperature, obtains Li with the rate of temperature fall of 1-10 DEG C/h
6cd
5sn
4se
16crystal;
Described Powdered Li
6cd
5sn
4se
16being prepared as follows of compound:
By Li source material, Cd source material, Sn
4source material and simple substance Se simple substance are according to mol ratio Li:Cd:Sn
4: after the ratio of Se=6:5:4:16 mixes, be heated to 800-1050 DEG C and carry out chemosynthesis, obtaining chemical formula is Li
6cd
5sn
4se
16compound, grinds to obtain Powdered Li through smashing to pieces
6cd
5sn
4se
16compound;
Described Li source material is lithium simple substance or lithium selenide;
Described Cd source material is cadmium simple substance or cadmium selenide:
Described Sn
4source material is tin simple substance or two Tin diselenides.
Described chemosynthesis is solid state reaction.
Described Powdered Li
6cd
5sn
4se
16being prepared according to the following reaction formula of compound:
(1)6Li+5Cd+4Sn+16Se＝Li
6Cd
5Sn
4Se
16；
(2)3Li
2Se+5Cd+4Sn+13Se＝Li
6Cd
5Sn
4Se
16；
(3)6Li+5CdSe+4Sn+11Se＝Li
6Cd
5Sn
4Se
16；
(4)6Li+5Cd+4SnSe
2+8Se＝Li
6Cd
5Sn
4Se
16；
(5)3Li
2Se+5CdSe+4SnSe
2＝Li
6Cd
5Sn
4Se
16；
Li provided by the invention
6cd
5sn
4se
16the another kind of preparation method of non-linear optic crystal, it is Bridgman-Stockbarge method for growing Li
6cd
5sn
4se
16non-linear optic crystal, its step is as follows:
By Powdered Li
6cd
5sn
4se
16compound or according to mol ratio Li:Cd:Sn
4: the mixture of Se=6:5:4:16 ratio mixing puts into crystal growing apparatus, and be warming up to melting sources, after raw material melts completely, crystal growing apparatus vertically declines with the speed of 0.1-10mm/h, in crystal growing apparatus decline process, carry out Li
6cd
5sn
4se
16non-linear optic crystal grows, and obtains Li
6cd
5sn
4se
16crystal; Its growth cycle is 5-20 days;
Described Powdered Li
6cd
5sn
4se
16being prepared as follows of compound:
By Li source material, Cd source material, Sn
4source material and simple substance Se simple substance are according to mol ratio Li:Cd:Sn
4: after the ratio of Se=6:5:4:16 mixes, be heated to 800-1050 DEG C and carry out chemosynthesis, obtaining chemical formula is Li
6cd
5sn
4se
16compound, grinds to obtain Powdered Li through smashing to pieces
6cd
5sn
4se
16compound;
Described Li source material is lithium simple substance or lithium selenide;
Described Cd source material is cadmium simple substance or cadmium selenide:
Described Sn
4source material is tin simple substance or two Tin diselenides.
Described Li
6cd
5sn
4se
16prepare by following chemical equation:
(1)6Li+5Cd+4Sn+16Se＝Li
6Cd
5Sn
4Se
16；
(2)3Li
2Se+5Cd+4Sn+13Se＝Li
6Cd
5Sn
4Se
16；
(3)6Li+5CdSe+4Sn+11Se＝Li
6Cd
5Sn
4Se
16；
(4)6Li+5Cd+4SnSe
2+8Se＝Li
6Cd
5Sn
4Se
16；
(5)3Li
2Se+5CdSe+4SnSe
2＝Li
6Cd
5Sn
4Se
16。
Adopt above-mentioned two kinds of methods all can obtain the Li being of a size of centimetre-sized
6cd
5sn
4se
16non-linear optic crystal; Use large size crucible, and extend vegetative period, then can obtain corresponding large-size Li
6cd
5sn
4se
16non-linear optic crystal.
According to the crystallography data of crystal, crystal boule is directed, by required angle, thickness and sectional dimension sliced crystal, crystal is led to light mirror polish, namely can be used as device for non-linear optical and use, this Li
6cd
5sn
4se
16non-linear optic crystal has physical and chemical performance and stablizes, and hardness is comparatively large, and good mechanical property is not easily broken, not easily deliquescence, is easy to the advantages such as processing and preservation; The present invention also provides Li further for this reason
6cd
5sn
4se
16the purposes of non-linear optic crystal, this Li
6cd
5sn
4se
16non-linear optic crystal is for the preparation of device for non-linear optical, and this device for non-linear optical comprises at least a branch of incidence electromagnetic radiation by least one piece of this Li
6cd
5sn
4se
16the device that at least a branch of frequency is different from the output radiation of incidence electromagnetic radiation is produced after non-linear optic crystal.
Li of the present invention
6cd
5sn
4se
16compound, this compound non-linear optic crystal and its production and use there is following effect:
At this Li
6cd
5sn
4se
16the growing crystals of non-linear optic crystal is easily grown up and the transparent advantages such as have the speed of growth very fast, cost is low without wrapping up, easy acquisition large-size crystal; The Li obtained
6cd
5sn
4se
16non-linear optic crystal has wider transmission region, and hardness is comparatively large, good mechanical property, and not easily broken and deliquescence is easy to the advantages such as processing and preservation; This Li
6cd
5sn
4se
16non-linear optic crystal can be used for making device for non-linear optical.
Accompanying drawing explanation
Fig. 1 adopts Li of the present invention
6cd
5sn
4se
16the fundamental diagram of a kind of typical device for non-linear optical that non-linear optic crystal is made, wherein 1 is laser apparatus, and 2 is incoming laser beams, and 3 is the Li after crystal aftertreatment and optical manufacturing
6cd
5sn
4se
16non-linear optic crystal, 4 is produced outgoing laser beams, and 5 is filter plates.
Fig. 2 is Li
6cd
5sn
4se
16the structural representation of non-linear optic crystal.
Embodiment
Embodiment 1, adopts high-temperature fusant spontaneous crystallization legal system for Li
6cd
5sn
4se
16crystal:
Take 2.785 grams of Li
2se, 9.568 grams of CdSe and 11.065 gram SnSe
2(i.e. Li
2se:CdSe:SnSe
2=0.03mol:0.05mol:0.04mol), after Homogeneous phase mixing, load in the quartz glass tube of Φ 12mm × 20mm, be evacuated to 10
-3after handkerchief, be placed in tubular type growth furnace with oxyhydrogen flame encapsulation, rise to 900 DEG C, constant temperature 72 hours, with the speed slow cooling of 5 DEG C/h to room temperature, close tubular type growth furnace; Cut after silica tube cooling, transparent Li can be obtained
6cd
5sn
4se
16crystal.
Embodiment 2, adopts falling crucible method to prepare Li
6cd
5sn
4se
16crystal:
Take 0.417 gram of Li, 5.621 grams of Cd, 4.748 grams of Sn and 12.634 gram Se (Li:Cd:Sn:Se=0.06mol:0.05mol:0.04mol:0.16mol), after Homogeneous phase mixing, load in the quartz glass tube of Φ 20mm × 30mm, be evacuated to 10
-3after handkerchief, be placed in crystal growing furnace with oxyhydrogen flame encapsulation, rise to 900 DEG C and make melting sources, after raw material melts completely, growing apparatus vertically declines with the speed of 0.1-10mm/ hour; After crystal growth terminates, growing apparatus was down to room temperature with 20 hours, obtained transparent Li
6cd
5sn
4se
16crystal.
After tested, the Li prepared by above-described embodiment 1-2
6cd
5sn
4se
16non-linear optic crystal belongs to rhombic system, and spacer is Pna2
1, its unit cell parameters is:
α=β=γ=90 °, Z=7,
density: 5.453g/cm
3, there is frequency-doubled effect; Fig. 2 is this Li
6cd
5sn
4se
16the structural representation of non-linear optic crystal.
Embodiment 3:
The Li of embodiment 1-2 gained
6cd
5sn
4se
16crystal is not easily broken, is easy to cutting, polishing and preservation, not deliquescence; By the Li of embodiment 1-2 gained
6cd
5sn
4se
16crystal, being placed on accompanying drawing 1 shown device label is the position of 3, and at room temperature, with the Ho:Tm:Cr:YAG laser light source adjusting Q, incident wavelength is the infrared light of 2090nm, and output wavelength is the frequency doubled light of 1045nm, and laser intensity is and AgGaSe
2quite.
Accompanying drawing 1 adopts Li of the present invention
6cd
5sn
4se
16the fundamental diagram of a kind of typical device for non-linear optical that non-linear optic crystal is made, wherein 1 is laser apparatus, and 2 is incoming laser beams, and 3 is the Li after crystal aftertreatment and optical manufacturing
6cd
5sn
4se
16non-linear optic crystal, 4 is produced outgoing laser beams, and 5 is filter plates; Send incoming laser beam 2 by laser apparatus 1 and inject Li
6cd
5sn
4se
16single crystal 3, the outgoing laser beam 4 produced is by filter plate 5, and the laser beam required for obtaining;
Use Li of the present invention
6cd
5sn
4se
16the device that non-linear optic crystal makes can be a times frequency generator, upper and lower frequency converter, optical parametric oscillator.Photoparametric amplifier etc.
It should be noted that, the present invention also can directly use Powdered Li
6cd
5sn
4se
16the preparation Li of compound
6cd
5sn
4se
16single crystal: Powdered Li
6cd
5sn
4se
16the preparation of compound: by Li source material, Cd source material, Sn
4source material and simple substance Se simple substance are according to mol ratio Li:Cd:Sn
4: after the ratio of Se=7:4.5:4:16 mixes, be heated to 800-1050 DEG C and carry out chemosynthesis, obtaining chemical formula is Li
6cd
5sn
4se
16compound, grind to obtain Powdered Li through smashing to pieces
6cd
5sn
4se
16compound; The preferred solid reaction process of chemical synthesis process of the present invention; Li of the present invention
6cd
5sn
4se
16compound can be prepared according to the following reaction formula:
(1)6Li+5Cd+4Sn+16Se＝Li
6Cd
5Sn
4Se
16；
(2)3Li
2Se+5Cd+4Sn+13Se＝Li
6Cd
5Sn
4Se
16；
(3)6Li+5CdSe+4Sn+11Se＝Li
6Cd
5Sn
4Se
16；
(4)6Li+5Cd+4SnSe
2+8Se＝Li
6Cd
5Sn
4Se
16；
(5)3Li
2Se+5CdSe+4SnSe
2＝Li
6Cd
5Sn
4Se
16；
Above-mentioned Powdered Li
6cd
5sn
4se
16li source material in compound and nonlinear chemical crystal preparation thereof can be lithium simple substance or lithium selenide; Cd source material can be cadmium simple substance or cadmium selenide; Sn
4source material can be tin simple substance or two Tin diselenides.
Claims (7)
1. a Li
6cd
5sn
4se
16non-linear optic crystal, this Li
6cd
5sn
4se
16non-linear optic crystal does not have symmetry centre, and belong to rhombic system, spacer is Pna2
1, its unit cell parameters is:
α=β=γ=90 °.
2. Li described in a claim 1
6cd
5sn
4se
16the preparation method of non-linear optic crystal, it is high-temperature fusant spontaneous crystallization method growth Li
6cd
5sn
4se
16non-linear optic crystal, the steps include:
By Li
6cd
5sn
4se
16compound or according to mol ratio Li:Cd:Sn
4: Li source material, Cd source material, the Sn of the mixing of Se=6:5:4:16 ratio
4the mixture of source material and simple substance Se simple substance is heated to melt to obtain high temperature solution, and this high temperature solution is kept 24-96 hour, afterwards, is cooled to room temperature, obtains Li with the rate of temperature fall of 1-10 DEG C/h
6cd
5sn
4se
16crystal;
Described Powdered Li
6cd
5sn
4se
16being prepared as follows of compound:
By Li source material, Cd source material, Sn
4source material and simple substance Se simple substance are according to mol ratio Li:Cd:Sn
4: after the ratio of Se=6:5:4:16 mixes, be heated to 800-1050 DEG C and carry out chemosynthesis, obtaining chemical formula is Li
6cd
5sn
4se
16compound, grinds to obtain Powdered Li through smashing to pieces
6cd
5sn
4se
16compound;
Described Li source material is lithium simple substance or lithium selenide;
Described Cd source material is cadmium simple substance or cadmium selenide:
Described Sn
4source material is tin simple substance or two Tin diselenides.
3. by Li according to claim 1
6cd
5sn
4se
16the preparation method of non-linear optic crystal, is characterized in that, described chemosynthesis is solid state reaction.
4. by Li according to claim 1
6cd
5sn
4se
16the preparation method of non-linear optic crystal, is characterized in that, described Powdered Li
6cd
5sn
4se
16compound is prepared according to the following reaction formula:
(1)6Li+5Cd+4Sn+16Se＝Li
6Cd
5Sn
4Se
16；
(2)3Li
2Se+5Cd+4Sn+13Se＝Li
6Cd
5Sn
4Se
16；
(3)6Li+5CdSe+4Sn+11Se＝Li
6Cd
5Sn
4Se
16；
(4)6Li+5Cd+4SnSe
2+8Se＝Li
6Cd
5Sn
4Se
16；
(5)3Li
2Se+5CdSe+4SnSe
2＝Li
6Cd
5Sn
4Se
16。
5. Li described in a claim 1
6cd
5sn
4se
16the preparation method of non-linear optic crystal, it is Bridgman-Stockbarge method for growing Li
6cd
5sn
4se
16non-linear optic crystal, its step is as follows:
By Li
6cd
5sn
4se
16compound or according to mol ratio Li:Cd:Sn
4: the mixture of Se=6:5:4:16 ratio mixing puts into crystal growing apparatus, and be warming up to melting sources, after raw material melts completely, crystal growing apparatus vertically declines with the speed of 0.1-10mm/h, in crystal growing apparatus decline process, carry out Li
6cd
5sn
4se
16non-linear optic crystal grows, and obtains Li
6cd
5sn
4se
16non-linear optical crystal; Its growth cycle is 5-20 days;
Described Powdered Li
6cd
5sn
4se
16being prepared as follows of compound:
By Li source material, Cd source material, Sn
4source material and simple substance Se simple substance are according to mol ratio Li:Cd:Sn
4: after the ratio of Se=6:5:4:16 mixes, be heated to 800-1050 DEG C and carry out chemosynthesis, obtaining chemical formula is Li
6cd
5sn
4se
16compound, grinds to obtain Powdered Li through smashing to pieces
6cd
5sn
4se
16compound;
Described Li source material is lithium simple substance or lithium selenide;
Described Cd source material is cadmium simple substance or cadmium selenide:
Described Sn
4source material is tin simple substance or two Tin diselenides.
6. by Li according to claim 5
6cd
5sn
4se
16the preparation method of non-linear optic crystal, is characterized in that, described Li
6cd
5sn
4se
16prepare by following chemical equation:
(1)6Li+5Cd+4Sn+16Se＝Li
6Cd
5Sn
4Se
16；
(2)3Li
2Se+5Cd+4Sn+13Se＝Li
6Cd
5Sn
4Se
16；
(3)6Li+5CdSe+4Sn+11Se＝Li
6Cd
5Sn
4Se
16；
(4)6Li+5Cd+4SnSe
2+8Se＝Li
6Cd
5Sn
4Se
16；
(5)3Li
2Se+5CdSe+4SnSe
2＝Li
6Cd
5Sn
4Se
16。
7. a Li according to claim 1
6cd
5sn
4se
16the purposes of non-linear optic crystal, is characterized in that, this Li
6cd
5sn
4se
16non-linear optic crystal is for the preparation of device for non-linear optical, and prepared device for non-linear optical comprises at least a branch of incidence electromagnetic radiation by least one piece of this Li
6cd
5sn
4se
16the device that at least a branch of frequency is different from the output radiation of incidence electromagnetic radiation is produced after non-linear optic crystal.
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