CN103290480B - Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal and method for making and purposes - Google Patents

Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal and method for making and purposes Download PDF

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CN103290480B
CN103290480B CN201210048486.7A CN201210048486A CN103290480B CN 103290480 B CN103290480 B CN 103290480B CN 201210048486 A CN201210048486 A CN 201210048486A CN 103290480 B CN103290480 B CN 103290480B
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optic crystal
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姚吉勇
尹文龙
冯凯
郝文钰
傅佩珍
吴以成
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The present invention relates to Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal and method for making and purposes; This Li 2in 2siS 6compound adopts solid state reaction preparation; Li 2in 2siS 6non-linear optic crystal adopts high-temperature fusant spontaneous crystallization method or Bridgman-Stockbarge method for growing; At this Li 2in 2siS 6the 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; Gained Li 2in 2siS 6non-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 2in 2siS 6non-linear optic crystal can be used for making device for non-linear optical.

Description

Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal and method for making and purposes
Technical field
The present invention relates to a kind of Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal (Li 2in 2siS 6monocrystalline) and this Li 2in 2siS 6the preparation method of monocrystalline and use Li 2in 2siS 6the purposes of the device for non-linear optical that monocrystalline makes.
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-BaB 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.
Summary of the invention
The object of the invention is to provide a kind of chemical formula to be Li 2in 2siS 6compound.
Another object of the present invention is to provide a kind of Li 2in 2siS 6non-linear optic crystal.
Still a further object of the present invention is to provide Li 2in 2siS 6the preparation method of non-linear optic crystal.
A further object of the invention is to provide Li 2in 2siS 6the purposes of non-linear optic crystal.
Technical scheme of the present invention is as follows:
The invention provides a kind of chemical formula is Li 2in 2siS 6compound.
Li provided by the invention 2in 2siS 6the preparation method of compound, its step is as follows:
By containing Li material, containing In material, containing Si material and S according to mol ratio Li: In: Si: S=2: 2: 1: 6 ratio to prepare burden and after mixing, be heated to 800-900 DEG C carry out solid state reaction and (in principle, adopt general chemical synthesis process to prepare Li 2in 2siS 6compound; The preferred solid reaction process of the present invention), obtaining chemical formula is Li 2in 2siS 6compound; Described is lithium sulfide or sulphur indium lithium containing Li material; Described is elementary silicon or silicon disulfide containing Si material; Described is indium simple substance or indium trisulfide or sulphur indium lithium containing In material.
The step that solid state reaction is carried out in described heating is: by loading in silica tube after above-mentioned batching grinding, be evacuated to 10 to silica tube -3pa also carries out fusing encapsulation, and put into retort furnace, with the ramp of 10-50 DEG C/h to 800-900 DEG C, constant temperature 48-72 hour, takes out sample after cooling; The sample taken out is reground and is placed in silica tube again and is evacuated to 10 -3pa also carries out fusing encapsulation, then puts into retort furnace and be warming up to 800-900 DEG C of sintering 48 hours; Sample is taken out, and smashs to pieces and grind to obtain Powdered Li 2in 2siS 6compound.
Described Li 2in 2siS 6compound can be prepared by following chemical equation:
(1)Li 2S+In 2S 3+SiS 2＝Li 2In 2SiS 6；
(2)Li 2S+2In+Si+5S＝Li 2In 2SiS 6；
(3)Li 2S+In 2S 3+Si+2S＝Li 2In 2SiS 6；
(4)Li 2S+2In+3S+SiS 2＝Li 2In 2SiS 6；
(5)2LiInS 2+SiS 2＝Li 2In 2SiS 6；
(6)2LiInS 2+Si+2S＝Li 2In 2SiS 6。
Li provided by the invention 2in 2siS 6non-linear optic crystal does not have symmetry centre, and belong to oblique system, spacer is Cc, and its unit cell parameters is: β=110.06 °.
Li provided by the invention 2in 2siS 6the preparation method of non-linear optic crystal, it is high-temperature fusant spontaneous crystallization method growth Li 2in 2siS 6non-linear optic crystal, the steps include: Powdered Li 2in 2siS 6compound is heated to melt to obtain high temperature solution after keeping 24-96 hour, be cooled to room temperature with the rate of temperature fall of 1-10 DEG C/h, obtains the Li of pale yellow transparent 2in 2siS 6crystal.
Described Powdered Li 2in 2siS 6being prepared as follows of compound:
By containing Li material, containing In material, containing Si material and simple substance S according to mol ratio Li: In: Si: S=2: 2: 1: 6 ratio to prepare burden and after mixing, be heated to 800-900 DEG C carry out solid state reaction and (in principle, adopt general chemical synthesis process to prepare Li 2in 2siS 6compound; The preferred solid reaction process of the present invention), obtaining chemical formula is Li 2in 2siS 6compound; Described is lithium sulfide or sulphur indium lithium containing Li material; Described is elementary silicon or silicon disulfide containing Si material; Described is indium simple substance or indium trisulfide or sulphur indium lithium containing In material.
Described Li 2in 2siS 6compound can be prepared by following chemical equation:
(1)Li 2S+In 2S 3+SiS 2＝Li 2In 2SiS 6；
(2)Li 2S+2In+Si+5S＝Li 2In 2SiS 6；
(3)Li 2S+In 2S 3+Si+2S＝Li 2In 2SiS 6；
(4)Li 2S+2In+3S+SiS 2＝Li 2In 2SiS 6；
(5)2LiInS 2+SiS 2＝Li 2In 2SiS 6；
(6)2LiInS 2+Si+2S＝Li 2In 2SiS 6。
Li provided by the invention 2in 2siS 6a preparation method again of non-linear optic crystal, it is Bridgman-Stockbarge method for growing Li 2in 2siS 6non-linear optic crystal, its step is as follows:
By Powdered Li 2in 2siS 6compound puts into crystal growing apparatus, and be slowly warming up to its fusing, after it melts completely, crystal growing apparatus vertically declines with the speed of 0.1-10mm/h, in crystal growing apparatus decline process, carry out Li 2in 2siS 6non-linear optic crystal grows, and its growth cycle is 5-20 days;
Bridgman-Stockbarge method for growing Li of the present invention 2in 2siS 6non-linear optic crystal also comprises Li 2in 2siS 6the aftertreatment of non-linear optic crystal: after crystal growth terminates, will stay in growth furnace and anneals by crystal, be cooled to room temperature (preferred rate of temperature fall 20 ~ 50 DEG C/h) with the speed of 20 ~ 100 DEG C/h.
Adopt above-mentioned two kinds of methods all can obtain the Li being of a size of centimetre-sized 2in 2siS 6non-linear optic crystal; Use large size crucible, and extend vegetative period, then can obtain corresponding large-size Li 2in 2siS 6non-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 2in 2siS 6non-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; So the present invention also provides Li further 2in 2siS 6the purposes of non-linear optic crystal, this Li 2in 2siS 6non-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 Li 2in 2siS 6the 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 2in 2siS 6compound, this compound non-linear optic crystal and its production and use there is following effect:
At this Li 2in 2siS 6the 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 2in 2siS 6non-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 2in 2siS 6non-linear optic crystal can be used for making device for non-linear optical.
Accompanying drawing explanation
Fig. 1 adopts Li of the present invention 2in 2siS 6the 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 2in 2siS 6non-linear optic crystal, 4 is produced outgoing laser beams, and 5 is filter plates.
Fig. 2 is Li 2in 2siS 6the structural representation of non-linear optic crystal.
Embodiment
Embodiment 1, prepares Powdered Li 2in 2siS 6compound:
Adopt (1) Li 2s+In 2s 3+ SiS 2=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described Li 2s is 1.379 grams, described In 2s 3be 9.775 grams, described SiS 2it is 2.767 grams; I.e. Li 2s: In 2s 3: SiS 2=0.03mol: 0.03mol: 0.03mol;
Concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with oxyhydrogen flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 800 DEG C, constant temperature 48-72 hour, takes out after cooling, takes out sample and is reground, be placed in silica tube again and vacuumize encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar and smash to pieces and grind to obtain Powdered Li 2in 2siS 6compound.
Embodiment 2, prepares Powdered Li 2in 2siS 6compound:
Adopt Li 2s+2In+Si+5S=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described Li 2s is 1.379 grams, and described In is 6.889 grams, and described Si is 0.843 gram, and described S is 4.811 grams, i.e. Li 2s: In: Si: S=0.03mol: 0.06mol: 0.03mol: 0.15mol;
Its concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 900 DEG C, its temperature rise rate is 10 DEG C/h, constant temperature 48 hours, take out after cooling, taking-up sample is reground, then is placed in silica tube and vacuumizes encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar smash to pieces grind to obtain preparation Powdered Li 2in 2siS 6compound.
Embodiment 3, prepares Powdered Li 2in 2siS 6compound:
Adopt Li 2s+In 2s 3+ Si+2S=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described Li 2s is 1.379 grams, described In 2s 3be 9.775 grams, described Si is 0.843 gram, and described S is 1.924 grams, i.e. Li 2s: In 2s 3: Si: S=0.03mol: 0.03mol: 0.03mol: 0.06mol;
Concrete operation step is, concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 800 DEG C, its temperature rise rate is 20 DEG C/h, constant temperature 72 hours, take out after cooling, taking-up sample is reground, then is placed in silica tube and vacuumizes encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar and smash to pieces and grind to obtain Powdered Li 2in 2siS 6compound.
Embodiment 4, prepares Powdered Li 2in 2siS 6compound:
Adopt Li 2s+2In+3S+SiS 2=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described Li 2s is 1.379 grams, and described In is 6.889 grams, and described S is 2.886 grams, described SiS 2be 2.767 grams, i.e. Li 2s: In: S: SiS 2=0.03mol: 0.06mol: 0.09mol: 0.03mol;
Its concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 900 DEG C, its temperature rise rate is 10 DEG C/h, constant temperature 48 hours, take out after cooling, taking-up sample is reground, then is placed in silica tube and vacuumizes encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar smash to pieces grind to obtain preparation Powdered Li 2in 2siS 6compound.
Embodiment 5, prepares Powdered Li 2in 2siS 6compound:
Adopt 2LiInS 2+ SiS 2=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described LiInS 2be 11.153 grams, described SiS 2be 2.767 grams, i.e. LiInS 2: SiS 2=0.06mol: 0.03mol;
Its concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 800 DEG C, its temperature rise rate is 30 DEG C/h, constant temperature 48 hours, take out after cooling, taking-up sample is reground, then is placed in silica tube and vacuumizes encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar smash to pieces grind to obtain preparation Powdered Li 2in 2siS 6compound products.
Embodiment 6, prepares Powdered Li 2in 2siS 6compound:
Adopt 2LiInS 2+ Si+2S=Li 2in 2siS 6reaction formula solid reaction process prepares Li 2in 2siS 6compound; Described LiInS 2be 11.153 grams, described Si is 0.843 gram, and described S is 1.924 grams, i.e. LiInS 2: Si: S=0.06mol: 0.03mol: 0.06mol;
Its concrete operation step is, takes reagent respectively, they are put into mortar in glove box by above-mentioned dosage, and mixing is also carefully ground, and then loads in the silica tube of Φ 12mm × 16mm, is evacuated to 10 -3with flame, silica tube fusing is encapsulated after pa, put into retort furnace, slowly rise to 900 DEG C, its temperature rise rate is 10 DEG C/h, constant temperature 48 hours, take out after cooling, taking-up sample is reground, then is placed in silica tube and vacuumizes encapsulation, in 800 DEG C of sintering 48 hours in retort furnace, taken out, put into mortar smash to pieces grind to obtain preparation Powdered Li 2in 2siS 6compound.
Embodiment 7, adopts high-temperature fusant spontaneous crystallization legal system for Li 2in 2siS 6crystal:
By the Li obtained in embodiment 1 to 6 2in 2siS 6powder loads in the quartz glass tube of Φ 12mm × 16mm, is evacuated to 10 -3after handkerchief, be placed in tubular type growth furnace with oxyhydrogen flame encapsulation, slowly 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, the Li of pale yellow transparent can be obtained 2in 2siS 6crystal.
Embodiment 8, adopts falling crucible method to prepare Li 2in 2siS 6crystal:
By the Li obtained in embodiment 1 to 6 2in 2siS 6powder loads in the quartz glass tube of Φ 12mm × 16mm, is evacuated to 10 -3after handkerchief, with oxyhydrogen flame encapsulation be placed in crystal growing furnace, slowly rise to 900 DEG C raw material is melted completely after, growing apparatus vertically declines with the speed of 0.1-10mm/ hour; After crystal growth terminates, growing apparatus was down to room temperature with 30 hours, obtained the Li of pale yellow transparent 2in 2siS 6crystal.
After tested, the Li prepared by above-described embodiment 7-8 2in 2siS 6non-linear optic crystal belongs to oblique system, and spacer is Cc, and its unit cell parameters is: β=110.06 °, Z=4, there is frequency-doubled effect; Fig. 2 is this Li 2in 2siS 6the structural representation of non-linear optic crystal.
Embodiment 9:
By the Li of embodiment 7 and 8 gained 2in 2siS 6crystal is done through spectrometry, and this crystal is transparent within the scope of 0.35 μm of-18 mum wavelength; Not easily broken, be easy to cutting, polishing and preservation, not deliquescence; By the Li of embodiment 7,8 gained 2in 2siS 6crystal, being placed on accompanying drawing 1 shown device label is the position of 3, and at room temperature, with tune Q Ho:YAG laser light source, incident wavelength is the infrared light of 2090nm, and output wavelength is the frequency doubled light of 1045nm, and laser intensity is about AgGaS 2half.
Accompanying drawing 1 adopts Li of the present invention 2in 2siS 6the 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 2in 2siS 6non-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 2in 2siS 6single 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 2in 2siS 6the device that non-linear optic crystal makes can be a times frequency generator, upper and lower frequency converter, optical parametric oscillator etc.Laser apparatus 1 can be mix ream yttrium aluminum garnet (Ho:YAG) laser apparatus or other laser apparatus, and concerning the frequency doubling device using Ho:YAG laser light source, the infrared light of incoming beam 2 to be wavelength be 2090nm, passes through Li 2in 2siS 6it is the frequency doubled light of 1045 that non-linear optic crystal produces wavelength, and outgoing beam 4 is the fundamental frequency light of 2090nm and the frequency doubled light of 1045nm containing wavelength, and the effect of filter plate 5 is elimination fundamental frequency light compositions, only allows frequency doubled light to pass through.

Claims (6)

1. a Li 2in 2siS 6non-linear optic crystal, this Li 2in 2siS 6non-linear optic crystal does not have symmetry centre, and belong to oblique system, spacer is Cc, and its unit cell parameters is: β=110.06 °.
2. Li described in a claim 1 2in 2siS 6the preparation method of non-linear optic crystal, it is high-temperature fusant spontaneous crystallization method growth Li 2in 2siS 6non-linear optic crystal, the steps include: Powdered Li 2in 2siS 6compound is heated to melt to obtain high temperature solution after keeping 24-96 hour, be cooled to room temperature with the rate of temperature fall of 1-10 DEG C/h, obtains the Li of pale yellow transparent 2in 2siS 6crystal.
3. by Li described in claim 2 2in 2siS 6the preparation method of non-linear optic crystal, is characterized in that, described Powdered Li 2in 2siS 6being prepared as follows of compound:
By containing Li material, containing In material, mix according to the ratio of mol ratio Li:In:Si:S=2:2:1:6 containing Si material and S after, heating carry out solid state reaction, obtaining chemical formula is Li 2in 2siS 6compound, grind to obtain Powdered Li through smashing to pieces 2in 2siS 6compound; Described is lithium sulfide or sulphur indium lithium containing Li material; Described is elementary silicon or silicon disulfide containing Si material; Described is indium simple substance or indium trisulfide or sulphur indium lithium containing In material.
4. Li described in a claim 1 2in 2siS 6the preparation method of non-linear optic crystal, it is Bridgman-Stockbarge method for growing Li 2in 2siS 6non-linear optic crystal, its step is as follows:
By Li 2in 2siS 6powder puts into crystal growing apparatus, is slowly warming up to powder smelting, and after powder melts completely, crystal growing apparatus vertically declines with the speed of 0.1-10mm/h, in crystal growing apparatus decline process, carry out Li 2in 2siS 6non-linear optic crystal grows, and its growth cycle is 5-20 days.
5. by Li described in claim 4 2in 2siS 6the preparation method of non-linear optic crystal, is characterized in that, also comprises Li 2in 2siS 6the aftertreatment of non-linear optic crystal: after crystal growth terminates, will stay in growth furnace and anneals by crystal, be cooled to room temperature with the speed of 20 ~ 50 DEG C/h.
6. a Li according to claim 1 2in 2siS 6the purposes of non-linear optic crystal, is characterized in that, this Li 2in 2siS 6non-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 Li 2in 2siS 6the 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.
CN201210048486.7A 2012-02-27 2012-02-27 Li 2in 2siS 6compound, Li 2in 2siS 6non-linear optic crystal and method for making and purposes Expired - Fee Related CN103290480B (en)

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