CN105502329A - RbNaMgP2O7 compound, RbNaMgP2O7 nonlinear optical crystal and preparing method and usage thereof - Google Patents

RbNaMgP2O7 compound, RbNaMgP2O7 nonlinear optical crystal and preparing method and usage thereof Download PDF

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CN105502329A
CN105502329A CN201510898042.6A CN201510898042A CN105502329A CN 105502329 A CN105502329 A CN 105502329A CN 201510898042 A CN201510898042 A CN 201510898042A CN 105502329 A CN105502329 A CN 105502329A
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rbnamgp
crystal
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linear optic
optic crystal
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CN105502329B (en
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罗军华
赵三根
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Fujian Institute of Research on the Structure of Matter of CAS
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/14Phosphates
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL 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
    • G02F1/00Devices 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
    • G02F1/35Non-linear optics
    • G02F1/355Non-linear optics characterised by the materials used
    • G02F1/3551Crystals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams

Abstract

The invention relates to a RbNaMgP2O7 compound, a RbNaMgP2O7 nonlinear optical crystal and a preparing method of the RbNaMgP2O7 crystal and usage of the RbNaMgP2O7 crystal to manufacturing of a nonlinear optical device. The invention has following beneficial effects that the crystal easily grows big and is transparent without an inclosure and has the advantages of fast growth speed, low cost, easiness in obtaining of large size; the obtained crystal has the advantages of shorter ultraviolet absorbing cut-off side, larger nonlinear optical effect, stable physicochemical property, good mechanical property and easiness in machining; the crystal can be used for manufacturing the nonlinear optical device. The nonlinear optical device manufactured by the nonlinear crystal can be used in a plurality of military and civil high-tech fields such as laser blinding weapons, optical disk recording, laser projection television, optical calculation and optical fiber communication.

Description

RbNaMgP 2o 7compound, RbNaMgP 2o 7non-linear optic crystal and method for making thereof and purposes
Technical field
The present invention relates to a kind of RbNaMgP 2o 7compound, RbNaMgP 2o 7non-linear optic crystal, RbNaMgP 2o 7the preparation method of crystal and RbNaMgP 2o 7crystal is for making the purposes of device for non-linear optical.
Technical background
The non-linear optical effect of crystal refers to so a kind of effect: when a branch of laser with certain polarization direction is in certain direction by one block of non-linear optic crystal, the frequency of this light beam will change.The crystal with non-linear optical effect is called non-linear optic crystal.Utilize the non-linear optical effect of crystal, second harmonic generator and the device for non-linear optical such as upper and lower frequency converter and optical parametric oscillator can be made.The all solid state laser utilizing non-linear optic crystal to carry out frequency transformation is a developing direction of following laser apparatus, and its key is to obtain outstanding non-linear optic crystal.
At present, the non-linear optic crystal being applied to ultraviolet and deep ultraviolet wave band is all borate, mainly contains β-BaB 2o 4(BBO), LiB 3o 5(LBO), RbLiB 6o 10and K (CLBO) 2be 2bO 3f 2etc., but they all exist respective weak point (KBBF).Such as, the degree of birefringence of LBO and CBO is all smaller, and the quadruple that can not realize 1064nm wavelength laser exports; The degree of birefringence of BBO is bigger than normal, there is photorefractive effect, limit its output rating and beam quality when the quadruple for 1064nm wavelength laser exports; And CLBO very easily deliquescence, be difficult to realize commercial applications; KBBF is then because its serious layer growth habit causes it to be difficult to obtain c to the large crystal of thickness.Therefore, to explore the new ultra-violet non-linear optic crystal of excellent combination property and remain urgent and necessity.
Although two kinds of non-linear optic crystal KH of widespread use at present 2pO 4and KTiOPO (KDP) 4(KTP) be phosphoric acid salt, but these two kinds of crystal due to through scope restriction and be not suitable for ultraviolet and deep ultraviolet laser and export.Recently, investigators report two kinds of New Phosphorus hydrochlorate non-linear optic crystal Ba 3p 3o 10x (X=Cl, Br) (see " J.Am.Chem.Soc. ", Vol136,480-487,2014).These two kinds of crystal uv-absorbing cut-off limits reach dark purple outskirt, and powder SHG effect is about 0.6 and 0.5 times of KDP respectively, and in 1064nm and 532nm place phase matched.This achievement in research shows what phosphoric acid salt got a good chance of as ultraviolet deep ultraviolet nonlinear optical material.But regrettably, Ba 3p 3o 10the powder SHG effect of X (X=Cl, Br) is smaller, and this is unfavorable to its application.Therefore, the present inventor, on a large amount of basis explored, has made the present invention.This RbNaMgP invented 2o 7crystal has larger non-linear optical effect.
Summary of the invention
An object of the present invention is to provide a kind of chemical formula to be RbNaMgP 2o 7compound.
An object of the present invention is to provide a kind of RbNaMgP 2o 7the preparation method of compound.
An object of the present invention is to provide a kind of RbNaMgP 2o 7non-linear optic crystal.
An object of the present invention is to provide RbNaMgP 2o 7the preparation method of crystal.
An object of the present invention is to provide RbNaMgP 2o 7the purposes of non-linear optic crystal.
Technical scheme of the present invention is as follows.
(1) a kind of RbNaMgP 2o 7compound, described RbNaMgP 2o 7the chemical formula of compound is RbNaMgP 2o 7.
(2) a kind of RbNaMgP 2o 7the preparation method of compound, adopts the RbNaMgP described in solid reaction process preparation 2o 7compound, described solid reaction process comprises the steps:
Will containing Rb compound, containing Na compound, containing Mg compound and containing P-compound stoichiometrically than after Homogeneous phase mixing, with the ramp of 10-200 DEG C/h to 400-500 DEG C, then heat preservation sintering more than 24 hours, grinding is taken out evenly after being down to room temperature, again to be greater than the ramp of 10-200 DEG C/h to 600-700 DEG C of sintering more than 24 hours, grinding more than 1 time is taken out in midway, obtains the RbNaMgP of pure phase 2o 7compound.
Below severally typically can obtain RbNaMgP 2o 7the reaction of compound:
(a)Rb 2CO 3+Na 2CO 3+2MgO+4NH 4H 2PO 4=2RbNaMgP 2O 7+2CO 2↑+6H 2O↑+4NH 3
(b)Rb 2CO 3+2NaHCO 3+2MgO+4(NH 4) 2HPO 4=2RbNaMgP 2O 7+5H 2O↑+3CO 2↑+8NH 3↑+O 2
(c)3RbNO 3+3NaOH+3MgO+6NH 4H 2PO 4=3RbNaMgP 2O 7+18H 2O↑+NH 3↑+4N 2↑。
(3) a kind of RbNaMgP 2o 7non-linear optic crystal, described RbNaMgP 2o 7non-linear optic crystal containing symmetry centre, does not belong to rhombic system Pna2 1spacer, unit cell parameters is z=4.
(4) one prepares RbNaMgP 2o 7the method of non-linear optic crystal, adopts the RbNaMgP described in melt method for growing 2o 7non-linear optic crystal.
(5) melting method described in comprises the steps:
RbNaMgP is put in crucible 2o 7raw materials of compound, then will fill RbNaMgP 2o 7the crucible of raw materials of compound is placed in crystal growing furnace, is warmed up to more than 800 DEG C, is incubated more than 12 hours, then slow cooling, growing crystal in high-temperature fusant surface or melt;
Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed being not more than 50 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
The condition of described growing crystal is for being rate of temperature fall: 0.2 ~ 5 DEG C/day, preferably 0.2 ~ 1 DEG C/day; Rotating speed: 0 ~ 50 rev/min, preferably 10 ~ 40 revs/min; Sense of rotation: single direction rotation or bidirectional rotation; Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed being not more than 50 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
(6) the described Rb compound that contains is selected from cesium carbonate (Rb 2cO 3) or cesium nitrate (RbNO 3); The described Na compound that contains is selected from sodium carbonate (Na 2cO 3), sodium hydroxide (NaOH) or sodium bicarbonate (NaHCO 3); The described Mg compound that contains is selected from MgO; The described P-compound that contains is selected from NH 4h 2pO 4or (NH 4) 2hPO 4.
(7) aforesaid method is adopted can to obtain the RbNaMgP being of a size of centimetre-sized 2o 7single crystal; Use large size crucible, and extend vegetative period, then can obtain the crystal of corresponding large-size.
(8) crystal aftertreatment and optical manufacturing method as follows: after crystal growth terminates, promote seed rod, make crystal depart from liquid level, will stay and anneal in a furnace by crystal, room temperature is cooled to, preferred rate of temperature fall 10 – 30 DEG C/h with the speed being not more than 50 DEG C/h; According to the crystallography data of crystal, crystal boule is directed, by required angle, sectional dimension and thickness sliced crystal, crystal is led to light mirror polish, namely can be used as device for non-linear optical and use.
(9) RbNaMgP of the present invention 2o 7the purposes of non-linear optic crystal, comprises and using as device for non-linear optical.
Preferably, prepared device for non-linear optical comprises at least a branch of incidence electromagnetic radiation by least one piece of RbNaMgP 2o 7after non-linear optic crystal, produce the device that at least a branch of frequency is different from the output radiation of incidence electromagnetic radiation.
This RbNaMgP 2o 7non-linear optic crystal has that physical and chemical performance is stable, hardness is moderate, good mechanical property, not easily broken, be easy to the advantages such as processing; So this invention also provides RbNaMgP further 2o 7the purposes of non-linear optic crystal, it is this RbNaMgP 2o 7non-linear optic crystal is for the preparation of device for non-linear optical.
RbNaMgP of the present invention 2o 7non-linear optic crystal of compound, this compound and its production and use has following beneficial effect:
(1) at this RbNaMgP 2o 7the growing crystals of non-linear optic crystal is easily grown up and transparent in inclusion, has that the speed of growth is very fast, cost is low, is easy to obtain the advantages such as large-size crystal;
(2) RbNaMgP obtained 2o 7non-linear optic crystal has that shorter uv-absorbing cut-off limit, larger non-linear optical effect, physical and chemical performance are stable, good mechanical property, be easy to the advantages such as processing;
(3) this RbNaMgP 2o 7non-linear optic crystal can be used for making device for non-linear optical;
(4) device for non-linear optical that non-linear optic crystal of the present invention makes can be used in some military and civilian high-tech areas, such as blinding laser weapons, video disc recording, laser projection tv, optical oomputing and optical-fibre communications etc.
Accompanying drawing explanation
Fig. 1 uses RbNaMgP 2o 7the fundamental diagram of a kind of typical device for non-linear optical that crystal is made, wherein 1 is laser apparatus, and 2 is incoming laser beams, and 3 is the RbNaMgP through crystal aftertreatment and optical manufacturing 2o 7crystal, 4 is produced laser beams, and 5 is spectral filters.
Fig. 2 is RbNaMgP of the present invention 2o 7polycrystal powder X ray diffracting spectrum with based on RbNaMgP 2o 7the X ray diffracting spectrum of crystalline structure simulation.
Fig. 3 is RbNaMgP of the present invention 2o 7crystalline structure figure.
Embodiment
The present invention is further described below in conjunction with embodiment and accompanying drawing.Those skilled in the art know, and following embodiment is not limiting the scope of the invention, and any improvement of making on basis of the present invention and change are all within protection scope of the present invention.
Embodiment 1-3 is about Powdered RbNaMgP 2o 7the preparation of compound.
Embodiment 1
Adopt solid reaction process, reaction equation is as follows:
(a)Rb 2CO 3+Na 2CO 3+2MgO+4NH 4H 2PO 4=2RbNaMgP 2O 7+4CO 2↑+6H 2O↑+4NH 3
Above-mentioned three kinds of reagent charging capacity: Rb 2cO 311.55 grams (0.05mol), Na 2cO 35.30 grams (0.05mol), MgO4.03 gram (0.1mol), NH 4h 2pO 423.01 grams (0.2mol).
Concrete operation step is: take reagent respectively by above-mentioned dosage, they are put into mortar, mixes and grind evenly, then loading in corundum ceramic crucible, by its compacting, put into retort furnace, with the ramp of 20 DEG C/h to 400 DEG C, then heat preservation sintering 24 hours, then grinding is taken out after being down to room temperature evenly, sinter 24 hours with the ramp of 200 DEG C/h to 600 DEG C again, grinding 2 times is taken out in midway, obtains the RbNaMgP of pure phase 2o 7compound.
As shown in Figure 2, the x-ray diffractogram of powder spectrum testing gained is consistent with according to the collection of illustrative plates of its single crystal structure matching gained.
Embodiment 2
Prepare Powdered RbNaMgP 2o 7compound
Adopt solid reaction process, reaction equation is as follows:
(b)Rb 2CO 3+2NaHCO 3+2MgO+4(NH 4) 2HPO 4=2RbNaMgP 2O 7+5H 2O↑+3CO 2↑+8NH 3↑+O 2
Above-mentioned three kinds of reagent charging capacity: Rb 2cO 32.31 grams (0.01mol), NaHCO 31.68 grams (0.02mol), MgO0.81 gram (0.02mol), (NH 4) 2hPO 45.28 grams (0.04mol).
Concrete operation step is: take reagent respectively by above-mentioned dosage, they are put into mortar, mixes and grind evenly, then loading in corundum ceramic crucible, by its compacting, put into retort furnace, with the ramp of 200 DEG C/h to 500 DEG C, then heat preservation sintering more than 24 hours, then grinding is taken out after being down to room temperature evenly, sinter 48 hours with the ramp of 100 DEG C/h to 700 DEG C again, grinding 2 times is taken out in midway, obtains the RbNaMgP of pure phase 2o 7compound.
Embodiment 3
Prepare Powdered RbNaMgP 2o 7compound
Adopt solid reaction process, reaction equation is as follows:
(c)3RbNO 3+3NaOH+3MgO+6NH 4H 2PO 4=3RbNaMgP 2O 7+18H 2O↑+NH 3↑+4N 2↑。
Above-mentioned three kinds of reagent charging capacity: RbNO 37.37 grams (0.05mol), NaOH2.00 gram (0.05mol), MgO2.02 gram (0.05mol), NH 4h 2pO 411.50 grams (0.1mol).
Concrete operation step is: take reagent respectively by above-mentioned dosage, they are put into mortar, mixes and grind evenly, then loading in corundum ceramic crucible, by its compacting, put into retort furnace, with the ramp of 50 DEG C/h to 450 DEG C, then heat preservation sintering 72 hours, then grinding is taken out after being down to room temperature evenly, sinter 72 hours with the ramp of 50 DEG C/h to 700 DEG C again, grinding 4 times is taken out in midway, obtains the RbNaMgP of pure phase 2o 7compound.
Embodiment 4-6 is preparation RbNaMgP 2o 7crystal
Embodiment 4
Melting method comprises the steps:
At room temperature, put in crucible according to stoichiometric ratio configuration and pretreated raw materials of compound, then the crucible filling material is placed in crystal growing furnace, 850 DEG C are warmed up to the temperature rise rate of 20 DEG C/h, be incubated 24 hours, then slow prompt drop temperature, under following growth conditions from high-temperature fusant growing crystal surperficial or melt;
The condition of described growing crystal is for being rate of temperature fall: 0.2 DEG C/day, rotating speed: 10 revs/min; Sense of rotation: single direction rotation;
Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed of 10 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
Embodiment 5
At room temperature, put in crucible according to stoichiometric ratio configuration and pretreated raw materials of compound, then the crucible filling material is placed in crystal growing furnace, 900 DEG C are warmed up to the temperature rise rate of 50 DEG C/h, be incubated 36 hours, then slow cooling, under following growth conditions from high-temperature fusant surface or melt growing crystal;
The condition of described growing crystal is for being rate of temperature fall: 3 DEG C/day; Rotating speed: 50 revs/min, sense of rotation: bidirectional rotation;
Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed of 30 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
Embodiment 6
At room temperature, put in crucible according to stoichiometric ratio configuration and pretreated raw materials of compound, then the crucible filling material is placed in crystal growing furnace, 850 DEG C are warmed up to the temperature rise rate of 20-50 DEG C/h, be incubated 24 hours, then slow cooling, under following growth conditions from high-temperature fusant surface or melt growing crystal;
The condition of described growing crystal is for being rate of temperature fall: 1 DEG C/day; Rotating speed: 40 revs/min; Sense of rotation: single direction rotation;
Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed of 30 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
After tested, the RbNaMgP prepared by embodiment 4-6 2o 7non-linear optic crystal containing symmetry centre, does not belong to rhombic system Pna2 1spacer, unit cell parameters is z=4; There is frequency-doubled effect; Fig. 3 is this RbNaMgP 2o 7the structural representation of non-linear optic crystal.
Embodiment 7
By the RbNaMgP of embodiment 4 gained 2o 7non-linear optic crystal is done through spectrum test, the uv-absorbing of this crystal cut-off limit lower than 190nm, and in 190 – 1100nm wavelength regions through; This crystal is not easily broken, is easy to cutting and polishing; By the RbNaMgP of embodiment 6 gained 2o 7non-linear optic crystal, being placed on accompanying drawing 1 shown device label is the position of 3, at room temperature, fundamental frequency light source is made with tune QNd:YAG laser apparatus, incident wavelength is the near infrared light of 1064nm, and output wavelength is the green laser of 532nm, and laser intensity is about equivalent to 0.9 times of KDP.
Accompanying drawing 1 is for adopt RbNaMgP to the present invention 2o 7the simple declaration of the device for non-linear optical that crystal makes.Send light beam 2 by laser apparatus 1 and inject RbNaMgP 2o 7crystal 3, the outgoing beam 4 produced is by filter plate 5, thus the laser beam required for obtaining.This nonlinear optics laser apparatus can be times frequency generator or upper and lower frequency converter or optical parametric oscillator etc.
Above-mentioned embodiment is just explained in detail technical scheme of the present invention; the present invention has more than and is only confined to above-described embodiment; those skilled in the art should be understood that; every improvement on basis of the present invention according to above-mentioned principle and spirit, substitute, all should within protection scope of the present invention.

Claims (8)

1.RbNaMgP 2o 7compound, is characterized in that: described RbNaMgP 2o 7the chemical formula of compound is RbNaMgP 2o 7.
2. RbNaMgP according to claim 1 2o 7the preparation method of compound, is characterized in that: adopt the RbNaMgP described in solid reaction process preparation 2o 7compound, described solid reaction process comprises the steps:
Will containing Rb compound, containing Na compound, containing Mg compound and containing P-compound stoichiometrically than after Homogeneous phase mixing, with the ramp of 10-200 DEG C/h to 400-500 DEG C, then heat preservation sintering more than 24 hours, grinding is taken out evenly after being down to room temperature, again to be greater than the ramp of 10-200 DEG C/h to 600-700 DEG C of sintering more than 24 hours, grinding more than 1 time is taken out in midway, obtains the RbNaMgP of pure phase 2o 7compound.
3. RbNaMgP according to claim 2 2o 7the preparation method of compound, is characterized in that: described is Rb containing Rb compound 2cO 3or RbNO 3; Described is Na containing Na compound 2cO 3, NaOH or NaHCO 3; Described is MgO containing Mg compound; Described is NH containing P-compound 4h 2pO 4or (NH 4) 2hPO 4.
4.RbNaMgP 2o 7non-linear optic crystal, is characterized in that: described RbNaMgP 2o 7non-linear optic crystal containing symmetry centre, does not belong to rhombic system Pna2 1spacer, unit cell parameters is
5. RbNaMgP according to claim 4 2o 7the preparation method of non-linear optic crystal: adopt the RbNaMgP described in melt method for growing 2o 7non-linear optic crystal, described melting method comprises the steps:
RbNaMgP is put in crucible 2o 7raw materials of compound, then will fill RbNaMgP 2o 7the crucible of raw materials of compound is placed in crystal growing furnace, is warmed up to more than 800 DEG C, is incubated more than 12 hours, then slow cooling, growing crystal in high-temperature fusant surface or melt;
Arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, arrive after required yardstick until crystal growth, promote seed rod, make crystal depart from liquid level, be cooled to room temperature with the speed being not more than 50 DEG C/h, obtain RbNaMgP 2o 7non-linear optic crystal.
6. RbNaMgP according to claim 5 2o 7the preparation method of non-linear optic crystal: the described growth conditions of growing crystal from high-temperature fusant surface or melt is: rate of temperature fall is 0.2 ~ 5 DEG C/day; Seed rod rotating speed is 0 ~ 50 rev/min; Seed rod sense of rotation is single direction rotation or bidirectional rotation.
7. RbNaMgP according to claim 5 2o 7the preparation method of non-linear optic crystal: the described growth conditions of growing crystal from high-temperature fusant surface or melt is: rate of temperature fall is 0.2 ~ 1 DEG C/day; Seed rod rotating speed is 10 ~ 40 revs/min; Sense of rotation is single direction rotation or bidirectional rotation.
8.RbNaMgP 2o 7the purposes of non-linear optic crystal, is characterized in that, described RbNaMgP 2o 7non-linear optic crystal can be used as device for non-linear optical and uses.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106495121A (en) * 2016-10-14 2017-03-15 中国科学院福建物质结构研究所 CsLiCdP2O7Compound, CsLiCdP2O7Nonlinear optical crystal and its preparation method and purposes
CN107059123A (en) * 2017-01-18 2017-08-18 南开大学 The preparation method and its usage of four metaphosphoric acid dipotassium strontium crystals
CN109208078A (en) * 2018-01-15 2019-01-15 北京师范大学 Deep ultraviolet nonlinear optics phosphate crystal NaBa2P2O7Cl and preparation method thereof and purposes

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009179692A (en) * 2008-01-30 2009-08-13 Nagoya Institute Of Technology Metal phosphate
CN103848409A (en) * 2014-03-07 2014-06-11 河南理工大学 Barium phosphate potassium compound crystal and preparation method and use thereof
CN103950912A (en) * 2014-04-29 2014-07-30 中国科学院福建物质结构研究所 RbBa2(PO3)5 compound, RbBa2(PO3)5 nonlinear optical crystal as well as preparation method and application of crystal

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009179692A (en) * 2008-01-30 2009-08-13 Nagoya Institute Of Technology Metal phosphate
CN103848409A (en) * 2014-03-07 2014-06-11 河南理工大学 Barium phosphate potassium compound crystal and preparation method and use thereof
CN103950912A (en) * 2014-04-29 2014-07-30 中国科学院福建物质结构研究所 RbBa2(PO3)5 compound, RbBa2(PO3)5 nonlinear optical crystal as well as preparation method and application of crystal

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SANGEN ZHAO等: "Deep-Ultraviolet Transparent Phosphates RbBa2(PO3)5 and Rb2Ba3(P2O7)2 Show Nonlinear Optical Activity from Condensation of [PO4]3− Units", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106495121A (en) * 2016-10-14 2017-03-15 中国科学院福建物质结构研究所 CsLiCdP2O7Compound, CsLiCdP2O7Nonlinear optical crystal and its preparation method and purposes
CN106495121B (en) * 2016-10-14 2018-08-28 中国科学院福建物质结构研究所 CsLiCdP2O7Compound, CsLiCdP2O7Nonlinear optical crystal and its preparation method and purposes
CN107059123A (en) * 2017-01-18 2017-08-18 南开大学 The preparation method and its usage of four metaphosphoric acid dipotassium strontium crystals
CN109208078A (en) * 2018-01-15 2019-01-15 北京师范大学 Deep ultraviolet nonlinear optics phosphate crystal NaBa2P2O7Cl and preparation method thereof and purposes
CN109208078B (en) * 2018-01-15 2020-05-22 北京师范大学 Deep ultraviolet nonlinear optical phosphate crystal NaBa2P2O7Cl, preparation method and application thereof

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