CN106192003B - Compound lithium phosphate rubidium nonlinear optical crystal and preparation method and purposes - Google Patents
Compound lithium phosphate rubidium nonlinear optical crystal and preparation method and purposes Download PDFInfo
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Abstract
The present invention relates to a kind of compound lithium phosphate rubidium nonlinear optical crystal and preparation method and purposes, the crystal-chemical formula is LiRb2PO4, space groupCmc21, rhombic system, cell parameter is：a=5.599(18),b=11.32(4),c=7.69(2),Z=4,V=487(3)Å3, molecular weight 272.85.The compound lithium phosphate rubidium is synthesized using solid reaction process；Lithium phosphate rubidium nonlinear optical crystal uses czochralski method, kyropoulos or Bridgman-Stockbarge method for growing, and the lithium phosphate rubidium nonlinear optical crystal mechanical hardness obtained by the method for the invention is big, is easy to cutting, polishing and preservation.Prepare times frequency generator, on be used widely in the device for non-linear optical such as frequency converter, lower frequency converter or optical parametric oscillator.
Description
Technical field
The present invention relates to a kind of compound lithium phosphate rubidium nonlinear optical crystal and its production and use, the compound
Chemical formula be LiRb2PO4。
Background technology
Laser as the coherent monochromatic source of a kind of high intensity, good directionality be widely used in scientific research, industry, traffic,
The association area such as national defence and health care.But the laser wavelength that current various lasers directly export is limited, from ultraviolet waves
Section has remained laser blank wave band to infrared band.Due to the particularity of laser genesis mechanism, it is impossible to be each wavelength
Search out a kind of practical laser medium.So frequency conversion is carried out using nonlinear optical crystal to obtain the various laser of broad tuning
Light source has turned into the advanced subject of Development of Laser Technology.
Interaction of the nonlinear optical effect originating from laser and medium.When laser is with non-zero second order susceptibility
During Propagation, the nonlinear optical effect such as frequency multiplication and frequency, difference frequency, optically erasing can be produced.Nonlinear optical crystal material
Material has been deep into the every field of laser technology, remembers and stores as laser frequency, Electro-optical Modulation and photorefractive crystal
The crystalline material essential etc. technology.Nonlinear optical material main at present has：KDP(KH2PO4)、BBO(β-BaB2O4)、
LBO(LiB3O5) etc., but due to a variety of causes, not yet obtain the applicable various nonlinear optical crystals of each wave band.
According to current inorganic non-linear optical crystal material development, novel inorganic nonlinear optical crystal not only will
Ask with big Clock Multiplier Factor, but also require that its comprehensive performance parameter is good, while easily generate high quality and large size body block crystalline substance
Body, this just needs to carry out a large amount of systems and in-depth study works.Exploring high performance novel nonlinear optical crystal material is
The important topic in photoelectric functional material field, people are still explored in the hope of finding the more preferable nonlinear optical crystal of performance continuous.
The content of the invention
Present invention aims at a kind of compound lithium phosphate rubidium nonlinear optical crystal of offer, the molecular formula of the crystal is
LiRb2PO4, molecular weight 272.85, non-centrosymmetry, space group Cmc21, belong to rhombic system, cell parameter is： Molecular weight 272.85.
Another object of the present invention is to provide using under solid state reaction kinetics compound and czochralski method, kyropoulos or crucible
Drop method grows the preparation method of lithium phosphate rubidium nonlinear optical crystal.
Further object of the present invention is to provide a kind of lithium phosphate rubidium device for non-linear optical and is used to prepare optical communication device, times
Frequency generator, the purposes of upper and lower frequency converter or parametric oscillator.
A kind of compound lithium phosphate rubidium nonlinear optical crystal of the present invention, the molecular formula of the crystal is the crystal
Molecular formula is LiRb2PO4, molecular weight 272.85, non-centrosymmetry, space group Cmc21, belong to rhombic system, cell parameter is：Molecular weight 272.85.
The preparation method of described compound lithium phosphate rubidium nonlinear optical crystal, using solid state reaction kinetics compound,
Czochralski method, kyropoulos or Bridgman-Stockbarge method for growing lithium phosphate rubidium nonlinear optical crystal, concrete operations follow these steps to carry out：
A, it is Rb that will contain rubidium2O、Rb2CO3Or RbF, containing lithium it is Li2O、Li2CO3、LiNO3, LiOH or LiF and phosphorous chemical combination
Thing is NH4H2PO4,(NH4)2HPO4Or P2O5Rb in molar ratio:Li:P=2:1:1 weighs and is put into mortar, mixes and simultaneously carefully grinds
Mill, load corundum crucible, be put into Muffle furnace, be to slowly warm up to 400 DEG C, constant temperature 12 hours, gas drained only as far as possible, treated cold
But crucible is taken out afterwards, sample is ground uniformly, then is placed in crucible, Muffle furnace is warming up to 550 DEG C, constant temperature is after 48 hours by sample
Product take out, and are put into mortar to smash to pieces to grind and produce lithium phosphate rubidium compound single-phase polycrystalline powder, then carry out X to the polycrystal powder and penetrate
Line analysis, gained X-ray spectrogram and finished product LiRb2PO4Monocrystalline last X-ray spectrogram of pulverizing is consistent；
B, the compound lithium phosphate rubidium that step a is obtained is heated to melt in crucible, in 700 DEG C of -750 DEG C of perseverances of temperature
Warm 4-15h, then 680 DEG C -690 DEG C are cooled to, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained is delayed with 0.5-10 DEG C/h of temperature speed
Slow to be down to room temperature, spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface or melt：The crucible for being placed with melt made from step b is placed in list
In brilliant stove, the obtained seed crystals of step c are fixed on seed rod, are down to 660 DEG C -670 DEG C of temperature, seed is put into from single crystal growing furnace top
Crystalline substance, 30-60 minutes are first preheated, then contact seed crystal and liquid level, constant temperature 30-60 minutes；
E, again with the speed slow cooling of 1-5 DEG C/day of temperature, 0-60rpm rotating speed rotary seed crystal rods, 3-15mm/h speed
Upward lifting crystal growth；
F, after crystal growth size needed for, room temperature is down to by crystal lift-off liquid level, and with temperature 1-20 DEG C/h speed,
Then crystal is taken out from single crystal growing furnace, you can obtain LiRb2PO4Nonlinear optical crystal.
Described lithium phosphate rubidium nonlinear optical crystal is preparing optical communication device, times frequency generator, upper and lower frequency conversion
Purposes in device or optical parametric oscillator.
Lithium phosphate rubidium compound provided by the invention, its chemical formula are LiRb2PO4, following chemistry is pressed using solid reaction process
Reaction equation prepares lithium phosphate rubidium compound：
(1)Li2CO3+2NH4H2PO4+2Rb2CO3→2LiRb2PO4+3CO2↑+2H2O↑+2NH4↑+0.5O2↑
(2)LiNO3+NH4H2PO4+Rb2CO3→LiRb2PO4+CO2↑+NO2↑+H2O↑+NH4↑+0.5O2↑
(3)LiOH+NH4H2PO4+Rb2O→LiRb2PO4+1.5H2O↑+NH4↑+0.25O2↑
(4)Li2O+2NH4H2PO4+2Rb2O→2LiRb2PO4+2H2O↑+2NH4↑+0.5O2↑
(5)2LiNO3+P2O5+2Rb2O→2LiRb2PO4+2NO2↑+0.5O2↑
(6)LiF+(NH4)2HPO4+Rb2O→LiRb2PO4+0.5F2↑+0.5H2O↑+2NH4↑+0.25O2↑
(7)LiOH+(NH4)2HPO4+2RbF→LiRb2PO4+H2O↑+F2↑+2NH4↑
(8)Li2CO3+P2O5+4RbF+O2→2LiRb2PO4+CO2↑+2F2↑
In the present invention commercially available reagent and raw material can be used containing Li, containing Rb and containing P-compound.
Brief description of the drawings
Fig. 1 is LiRb of the present invention2PO4The X-ray diffraction figure of powder；
Fig. 2 is LiRb2PO4Crystallogram；
Fig. 3 is LiRb of the present invention2PO4The fundamental diagram for the device for non-linear optical that crystal makes, wherein 1 is laser,
2 is send light beam, and 3 be LiRb2PO4Crystal, 4 be outgoing beam, and 5 be filter plate.
Embodiment
Below in conjunction with accompanying drawing and the example implemented, the present invention is described in detail：
Embodiment 1：
By reaction equation Li2CO3+2NH4H2PO4+2Rb2CO3→2LiRb2PO4+3CO2↑+2H2O↑+2NH4↑+0.5O2↑ synthesis
Compound L iRb2PO4；Using solid phase synthesis process：
A, by Li2CO3、NH4H2PO4、Rb2CO3In molar ratio 1:2:2 weigh and are put into mortar, mix and simultaneously carefully grind, so
It is fitted into afterwards in Φ 100mm × 100mm open corundum crucible, is put into Muffle furnace, is to slowly warm up to 400 DEG C, constant temperature 12 hours,
Crucible is taken out after cooling, and now sample is more loose, then takes out sample and re-grinds uniformly, then is placed in crucible, in Muffle
550 DEG C of constant temperature 48 hours, is drawn off, produces LiRb in stove2PO4Powder, it is put into grinding in mortar and carries out X-ray analysis, gained
X-ray spectrogram and LiRb2PO4The X-ray spectrogram that mono-crystalline structures obtain is consistent；
LiRb is prepared using czochralski method in the melt2PO4Crystal：
B, by the LiRb of synthesis2PO4Compound is fitted into Φ 100mm × 100mm opening platinum crucible, and crucible is put into crystalline substance
In body growth furnace, 720 DEG C are warming up to, constant temperature 15 hours, then 690 DEG C are cooled to, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained is slowly dropped to 2 DEG C/h of temperature speed
Room temperature, small crystals is obtained in temperature-fall period using suspension platinum filament method, and spontaneous crystallization obtains seed crystal；
D, the crucible for being placed with lithium phosphate rubidium melt made from step b is placed in single crystal growing furnace, the obtained seed crystals of step c is consolidated
It is scheduled on seed rod, is down to 670 DEG C of temperature, is put into seed crystal from single crystal growing furnace top, first preheats 30 minutes, then connect seed crystal and liquid level
Touch, constant temperature 30 minutes；
E, it is upward with 10rpm rotating speed rotary seed crystal rods, 3mm/h speed again with the speed slow cooling of DEG C/day of temperature 2
Lifting crystal growth；
F, after crystal growth size needed for, room temperature is down to by crystal lift-off liquid level, and with temperature 5 DEG C/h speed, so
Crystal is taken out from single crystal growing furnace afterwards, you can obtain 20mm × 15mm × 16mm LiRb2PO4Nonlinear optical crystal.
Oxide spinel lithium in reaction equation can be substituted by lithium hydroxide, lithia, lithium fluoride or lithium nitrate, and rubidium carbonate can
Can be replaced by rubidium fluoride RbF, rubidium oxide replacement, phosphoric acid dihydro amine by phosphorus pentoxide, diammonium hydrogen phosphate.
Embodiment 2：
By reaction equation LiNO3+NH4H2PO4+Rb2CO3→LiRb2PO4+CO2↑+NO2↑+H2O↑+NH4↑+0.5O2↑ synthesisization
Compound LiRb2PO4, concrete operation step is according to the step a of embodiment 1 progress：
LiRb is prepared using czochralski method2PO4Crystal：
B, the LiRb for synthesizing step a2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, with temperature
20 DEG C/h of degree heating rate is heated to 750 DEG C, constant temperature 10h of temperature, then is cooled to 690 DEG C, obtains lithium phosphate rubidium liquation；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained slowly is dropped with 0.5 DEG C/h of temperature speed
To room temperature, small crystals is obtained using suspension platinum filament method in temperature-fall period, spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface：The crucible for being placed with lithium phosphate rubidium melt made from step b is placed in list
In brilliant stove, obtained seed crystal is fixed on seed rod, is cooled to 665 DEG C, seed crystal is put into from single crystal growing furnace top, first preheats 40 points
Clock, then seed crystal and liquid level are contacted, constant temperature 35 minutes；
E, cooled again with the speed of DEG C/day of temperature 1, it is upward with 5mm/h speed with 15rpm rotating speed rotary seed crystal rod
Lifting crystal growth；
F, after crystal stops growing, by crystal lift-off liquid level, room temperature is down to 5 DEG C/h of temperature speed, then taken out
Crystal, that is, obtain 12mm × 10mm × 11mm LiRb2PO4Nonlinear optical crystal.
Raw material lithium nitrate in reaction equation can be substituted by lithium hydroxide, lithia, lithium fluoride or lithium carbonate, and rubidium carbonate can
Can be replaced by rubidium fluoride RbF, rubidium oxide replacement, phosphoric acid dihydro amine by phosphorus pentoxide, diammonium hydrogen phosphate.
Embodiment 3：
By reaction equation LiOH+NH4H2PO4+Rb2O→LiRb2PO4+1.5H2O↑+NH4↑+0.25O2↑ synthesis compound
LiRb2PO4, concrete operation step is according to the step a of embodiment 1 progress：
LiRb is prepared using kyropoulos2PO4Crystal：
B, by the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, with temperature 20
DEG C/h heating rate is heated to 700 DEG C, constant temperature 4h of temperature, then is cooled to 680 DEG C, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained slowly is dropped with 1.5 DEG C/h of temperature speed
To room temperature, small crystals is obtained using suspension platinum filament method in temperature-fall period, spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface：The crucible for being placed with lithium phosphate rubidium melt made from step b is placed in list
In brilliant stove, obtained seed crystal is fixed on seed rod, is cooled to 660 DEG C, seed crystal is put into from single crystal growing furnace top, first preheats 45 points
Clock, then seed crystal and liquid level are contacted, constant temperature 40 minutes；
E, cooled again with the speed of DEG C/day of temperature 3, with 25rpm rotating speed rotary seed crystal rod；
F, after crystal stops growing, by crystal lift-off liquid level, room temperature is down to 10 DEG C/h of temperature speed, then taken out
Crystal, that is, obtain 10mm × 14mm × 8mm LiRb2PO4Nonlinear optical crystal.
Raw material lithium hydroxide in reaction equation can be substituted by lithium nitrate, lithia, lithium fluoride or lithium carbonate, and rubidium oxide can
Can be replaced by rubidium fluoride RbF, rubidium carbonate replacement, phosphoric acid dihydro amine by phosphorus pentoxide, diammonium hydrogen phosphate.
Embodiment 4：
By reaction equation Li2O+2NH4H2PO4+2Rb2O→2LiRb2PO4+2H2O↑+2NH4↑+0.5O2↑ synthesis compound
LiRb2PO4, concrete operation step is according to the step a of embodiment 1 progress：
LiRb is prepared using kyropoulos2PO4Crystal：
B, by the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, with temperature 20
DEG C/h heating rate is heated to 710 DEG C, constant temperature 6h of temperature, then is cooled to 681 DEG C, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained is slowly dropped to 5 DEG C/h of temperature speed
Room temperature, small crystals is obtained in temperature-fall period using suspension platinum filament method, and spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound melt：The crucible for being placed with lithium phosphate rubidium melt made from step b is placed in monocrystalline
In stove, obtained seed crystal is fixed on seed rod, is cooled to 667 DEG C, seed crystal is put into from single crystal growing furnace top, first preheats 50 points
Clock, then seed crystal is completely soaked in the melt, constant temperature 45 minutes；
E, cooled again with the speed of DEG C/day of temperature 4, with 0rpm rotating speed not rotary seed crystal rod；
F, after crystal stops growing, by crystal lift-off liquid level, room temperature is down to 15 DEG C/h of temperature speed, then taken out
Crystal, that is, obtain 15mm × 10mm × 12mm LiRb2PO4Nonlinear optical crystal.
Raw material lithia in reaction equation can be substituted by lithium nitrate, lithium hydroxide, lithium fluoride or lithium carbonate, and rubidium oxide can
Can be replaced by rubidium fluoride RbF, rubidium carbonate replacement, phosphoric acid dihydro amine by phosphorus pentoxide, diammonium hydrogen phosphate.
Embodiment 5：
By reaction equation 2LiNO3+P2O5+2Rb2O→2LiRb2PO4+2NO2↑+0.5O2↑ synthesis compound L iRb2PO4, specifically
Operating procedure is carried out according to the step a of embodiment 1：
LiRb is prepared using czochralski method2PO4Crystal：
B, by the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, with temperature 20
DEG C/h heating rate is heated to 730 DEG C, constant temperature 15h of temperature, then is cooled to 685 DEG C, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained slowly is dropped with 10 DEG C/h of temperature speed
To room temperature, small crystals is obtained using suspension platinum filament method in temperature-fall period, spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface：The crucible for being placed with lithium phosphate rubidium melt made from step b is placed in list
In brilliant stove, obtained seed crystal is fixed on seed rod, 660 DEG C is cooled to and is put into seed crystal at the top of single crystal growing furnace, first preheat 60 points
Clock, then seed crystal and liquid level are contacted, constant temperature 50 minutes；
E, cooled again with the speed of DEG C/day of temperature 5, it is upward with 15mm/h speed with 60rpm rotating speed rotary seed crystal rod
Lifting crystal growth；
F, after crystal stops growing, by crystal lift-off liquid level, room temperature is down to 20 DEG C/h of temperature speed, then taken out
Crystal, that is, obtain 10mm × 12mm × 8mm LiRb2PO4Nonlinear optical crystal.
Raw material lithium nitrate in reaction equation can be substituted by lithia, lithium hydroxide, lithium fluoride or lithium carbonate, and rubidium oxide can
Can be replaced by rubidium fluoride RbF, rubidium carbonate replacement, phosphorus pentoxide by phosphoric acid dihydro amine, diammonium hydrogen phosphate.
Embodiment 6：
By reaction equation LiF+ (NH4)2HPO4+Rb2O→LiRb2PO4+0.5F2↑+0.5H2O↑+2NH4↑+0.5O2↑ synthesisization
Compound LiRb2PO4, concrete operation step is according to the step a of embodiment 1 progress：
LiRb is prepared using czochralski method2PO4Crystal：
B, by the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, with temperature 20
DEG C/h heating rate is heated to 735 DEG C, constant temperature 12h of temperature, then is cooled to 683 DEG C, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained is slowly dropped to 8 DEG C/h of temperature speed
Room temperature, small crystals is obtained in temperature-fall period using suspension platinum filament method, and spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface：The crucible for being placed with lithium phosphate rubidium melt made from step b is placed in list
In brilliant stove, obtained seed crystal is fixed on seed rod, is cooled to 662 DEG C, seed crystal is put into from single crystal growing furnace top, first preheats 50 points
Clock, then seed crystal and liquid level are contacted, constant temperature 60 minutes；
E is cooled with the speed of DEG C/day of temperature 3 again, upward with 10mm/h speed with 50rpm rotating speed rotary seed crystal rod
Lifting crystal growth；
F, after crystal stops growing, by crystal lift-off liquid level, room temperature is down to 15 DEG C/h of temperature speed, then taken out
Crystal, that is, obtain 15mm × 8mm × 15mm LiRb2PO4Nonlinear optical crystal.
Raw material fluorinated lithium in reaction equation can be substituted by lithia, lithium hydroxide, lithium nitrate or lithium carbonate, and rubidium oxide can
Can be replaced by rubidium fluoride RbF, rubidium carbonate replacement, diammonium hydrogen phosphate by phosphoric acid dihydro amine, phosphorus pentoxide.
Embodiment 7：
By reaction equation LiOH+ (NH4)2HPO4+2RbF→LiRb2PO4+H2O↑+F2↑+2NH4↑ synthesis compound L iRb2PO4,
Concrete operation step is carried out according to the step a of embodiment 1：
LiRb is prepared using Bridgman-Stockbarger method2PO4Crystal：
By the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, crucible bottom band circle
Taper wedge angle, seed crystal is placed in crucible bottom, crucible is put into vertical heating furnace, be warming up to after raw material is completely melt, protect
It is constant to hold heating power；
Crucible is declined with 1mm/h speed, melt is solidified generation crystal from bottom to top；
After crystal stops growing, room temperature is down to 5 DEG C/h of temperature speed, then takes out crystal, that is, obtain 15mm ×
11mm × 5mm LiRb2PO4Nonlinear optical crystal.
Raw material lithium hydroxide in reaction equation can be substituted by lithia, lithium fluoride, lithium nitrate or lithium carbonate, and rubidium fluoride RbF can
Can be replaced by rubidium oxide, rubidium carbonate replacement, diammonium hydrogen phosphate by phosphoric acid dihydro amine, phosphorus pentoxide.
Embodiment 8：
By reaction equation Li2CO3+P2O5+4RbF+O2→2LiRb2PO4+CO2↑+2F2↑ synthesis compound L iRb2PO4, specific behaviour
Make step to carry out according to embodiment 1：
LiRb is prepared using Bridgman-Stockbarger method2PO4Crystal：
By the LiRb of synthesis2PO4Compound, it is fitted into Φ 100mm × 100mm open platinum crucible, crucible bottom band circle
Taper wedge angle, seed crystal is placed in crucible bottom, crucible is put into vertical heating furnace, be warming up to after raw material is completely melt, protect
It is constant to hold heating power；
Crucible is declined with 3mm/h speed, melt is solidified generation crystal from bottom to top；
After crystal stops growing, by crystal lift-off liquid level, room temperature is down to 10 DEG C/h of temperature speed, then takes out crystalline substance
Body, that is, obtain 10mm × 8mm × 9mm LiRb2PO4Nonlinear optical crystal.
Oxide spinel lithium in reaction equation can be substituted by lithia, lithium fluoride, lithium nitrate or lithium hydroxide, and rubidium fluoride RbF can
Can be replaced by rubidium oxide, rubidium carbonate replacement, phosphorus pentoxide by phosphoric acid dihydro amine, diammonium hydrogen phosphate.
Embodiment 9：
By arbitrary LiRb obtained by embodiment 1-82PO4Crystal by match direction process a block size 5mm × 5mm ×
3mm frequency doubling device, it is placed in as shown in accompanying drawing 3 on 3 position, at room temperature, with the Nd for adjusting Q:YAG laser makees light source,
Incident wavelength is 1064nm, by adjusting Q Nd:YAG laser 1 sends the infrared beam 2 that wavelength is 1064nm and injects LiRb2PO4It is single
Crystalline substance 3, produces the green frequency doubled light that wavelength is 532nm, and outgoing beam 4 is green containing the infrared light and 532nm that wavelength is 1064nm
Light, the green laser that wavelength is 532nm is obtained after filtered 5 elimination.
Claims (3)
1. a kind of compound lithium phosphate rubidium nonlinear optical crystal, it is characterised in that the molecular formula of the crystal is LiRb2PO4, molecule
Amount 272.85, non-centrosymmetry, space groupCmc21, belong to rhombic system, cell parameter is：A=5.599 (18), b=11.32
(4), c=7.69 (2), Z=4, V=487 (3)3。
2. the preparation method of compound lithium phosphate rubidium nonlinear optical crystal according to claim 1, it is characterised in that adopt
With solid state reaction kinetics compound, czochralski method, kyropoulos or Bridgman-Stockbarge method for growing crystal, concrete operations follow these steps into
OK：
A, it is Rb that will contain rubidium2O、Rb2CO3Or RbF, containing lithium it is Li2O、Li2CO3、LiNO3, LiOH or LiF and phosphorus-containing compound be
NH4H2PO4,(NH4)2HPO4Or P2O5Rb in molar ratio:Li:P = 2:1:1 weighs and is put into mortar, mixes and carefully grinds, dress
Enter corundum crucible, be put into Muffle furnace, be to slowly warm up to 400 DEG C, constant temperature 12 hours, as far as possible drain gas only, after cooling
Crucible is taken out, sample is ground uniformly, then is placed in crucible, Muffle furnace is warming up to 550 DEG C, constant temperature took sample after 48 hours
Go out, be put into mortar to smash to pieces to grind and produce lithium phosphate rubidium compound single-phase polycrystalline powder, then X ray point is carried out to the polycrystal powder
Analysis, gained X-ray spectrogram and finished product LiRb2PO4Monocrystalline last X-ray spectrogram of pulverizing is consistent；
B, the compound lithium phosphate rubidium that step a is obtained is heated to melt in crucible, in 700 DEG C of -750 DEG C of constant temperature 4- of temperature
15h, then 680 DEG C -690 DEG C are cooled to, obtain lithium phosphate rubidium melt；
C, lithium phosphate rubidium seed crystal is prepared：The lithium phosphate rubidium melt that step b is obtained slowly is dropped with 0.5-10 DEG C/h of temperature speed
To room temperature, spontaneous crystallization obtains seed crystal；
D, crystal is grown in compound bath surface or melt：The crucible for being placed with melt made from step b is placed in single crystal growing furnace
In, the obtained seed crystals of step c are fixed on seed rod, are down to 660 DEG C -670 DEG C of temperature, seed crystal is put into from single crystal growing furnace top,
30-60 minutes are first preheated, then contact seed crystal and liquid level, constant temperature 30-60 minutes；
E, it is upward with the speed slow cooling of 1-5 DEG C/day of temperature, 0-60rpm rotating speed rotary seed crystal rods, 3-15mm/h speed again
Lifting crystal growth；
F, after crystal growth size needed for, room temperature is down to by crystal lift-off liquid level, and with temperature 1-20 DEG C/h speed, then
Crystal is taken out from single crystal growing furnace, you can obtain LiRb2PO4Nonlinear optical crystal.
3. lithium phosphate rubidium nonlinear optical crystal according to claim 1 is preparing optical communication device, times frequency generator,
Purposes in upper and lower frequency converter or optical parametric oscillator.
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