CN104874805B - Nonlinear optical material lead-lithium niobate, and preparation method and application of powder thereof - Google Patents
Nonlinear optical material lead-lithium niobate, and preparation method and application of powder thereof Download PDFInfo
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- CN104874805B CN104874805B CN201510317064.9A CN201510317064A CN104874805B CN 104874805 B CN104874805 B CN 104874805B CN 201510317064 A CN201510317064 A CN 201510317064A CN 104874805 B CN104874805 B CN 104874805B
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Abstract
The invention provides nonlinear optical material lead-lithium niobate, and a preparation method and application of powder thereof. The chemical formula of nonlinear optical material lead-lithium niobate is Pb(2.15-x)Li(0.7+2x)Nb5O15, wherein x is larger than or equal to 0 and smaller than or equal to 0.05, nonlinear optical material lead-lithium niobate belongs to an orthorhombic system, the space group is Pn21m, and nonlinear optical material lead-lithium niobate is prepared by a solid-phase reaction method. Nonlinear optical material lead-lithium niobate with the chemical formula being Pb(2.15-x)Li(0.7+2x)Nb5O15 belongs to a ferroelectric, and has excellent nonlinear optical performance, the frequency-doubled signal of the powder of nonlinear optical material lead-lithium niobate is 1-2 times of that of lithium niobate with the same size (120 [mu]m), type-I phase matching is met, and nonlinear optical material lead-lithium niobate has a potential application prospect.
Description
Technical field
The present invention relates to a kind of nonlinear optical material lead niobate lithium, its molecular formula is Pb2.15-xLi0.7+2xNb5O15, wherein
0≤x≤0.05, and the preparation method and application of the material powder etc..
Background technology
Laser has superior coherence, monochromaticjty and high energy density, is widely used in civilian, scientific research and military affairs
Every field.For example laser printing, laser, laser detection and measurement technology, laser radar, laser holography, non-
Linear optics etc..Laser can directly be produced by solid state laser, liquid laser, gas laser etc., but these sides
It is limited that formula obtains optical maser wavelength, it is impossible to meets needs.A kind of effective means for obtaining new optical maser wavelength is using non-linear
Optical crystal carries out wavelength convert to the laser of existing wavelength.By the exploration of decades, a collection of outstanding non-linear optical crystal
Body material is developed, such as BBO（b-BaB2O4）, LBO（LiB3O5）, KTP (KTiOPO4),LN(LiNbO3) and later
It was found that KBBF（K2BeBO3F2）Deng they are presented greatly in various aspects such as the output of many times of laser instrument, difference frequency, mixing outputs
Using value, and realize less than 200nm deep ultraviolet output.Although these materials have been able to substantially meet people's application
Demand, but also have respective deficiency, such as light conversion efficiency is high, the easy deliquescence of crystal, layer growth habit and price are high
It is expensive etc..Therefore, explore the new nonlinear optical material with excellent properties and remain an important job.Can be suitable for
Using nonlinear optical material need to meet claimed below：（1）With big nonlinear optical coefficients；（2）Phase place can be realized
Matching；（3）Light injury threshold is high；（4）It is easily obtained large-size crystals, etc..
With regard to Pb2.15-xLi0.7+2xNb5O15, wherein the compound of 0≤x≤0.05, does not directly report at present.Before
The Soviet Union reported Pb2LiNb5O15Compound（Ferroelectrics, 1991,124,85 etc.）, but the chemical formula of its report
“Pb2LiNb5O15" different from the present invention, according to " Pb2LiNb5O15" can not obtain single thing phase to synthesize；And document is not
Have and crystal structure is parsed, the structural model that it is proposed is different from the present invention.Additionally, document does not have non-linear optical property
The report of aspect.
The content of the invention
It is an object of the invention to provide a kind of material lead niobate lithium with strong non-linear optical property and its powder
Preparation method and application, its chemical formula is Pb2.15-xLi0.7+2xNb5O15,Wherein 0≤x≤0.05.
The concrete technical scheme of the present invention is as follows：
Nonlinear optical material lead niobate lithium Pb of the present invention2.15-xLi0.7+2xNb5O15Middle Pb and Li has certain solid solution
Degree scope, the compound can form single thing phase in 0≤x≤0.05.Rhombic system, space group is Pn21m.Its change in x=0
Formula is Pb2.15Li0.7Nb5O15, cell parameter is a=12.3823, b=12.6687, c=7.6621, Z=4.
Nonlinear optical material lead niobate lithium of the present invention is quadratic tungsten bronze structure, by NbO6The common set of vertices of octahedron
Layered skeleton, Pb, Li are then filled in respectively in pentagon, quadrangle hole.
At room temperature, Nd is used：YAG laser makees light source, and incident wavelength is produced strong in the infrared light of 1064nm
532nm green glows.Its powder frequency-doubled signal intensity is same size（120μm）1-2 times of lithium niobate, and meet I type phase matcheds.
Nonlinear optical material lead niobate lithium of the present invention is ferroelectric, with ferroelectric hysteresis loop specific to ferroelectric.
The powder preparation method of nonlinear optical material lead niobate lithium of the present invention, using solid phase method, step is as follows：
Raw material is stoichiometrically mixed.Raw material is the carbonate containing each element, nitrate, organic salt or oxidation
Thing.
High temperature sintering, at 1150-1250 DEG C, temperature retention time is not limited temperature in 2-10 hours, heating rate, and rate of temperature fall is
2℃/min。
In the preparation method of nonlinear optical material lead niobate lithium of the present invention, it is specifically intended that：In 1100-700
DEG C warm area rate of temperature fall must control more than 1 DEG C/min, excessively slow rate of temperature fall can cause dephasign LiNbO3, PbNb2O6
Generation.
Nonlinear optical material lead niobate lithium of the present invention is used as a kind of polarity with excellent non-linear optical property
Material, it is contemplated that in high-tech such as CD burning, Laser Devices, Visible-to-Near InfaRed laser communicationses, Visible-to-Near InfaRed laser freuqency doublings
In civilian and military field, with important using value.
Description of the drawings
Fig. 1 is nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Polycrystal powder X-ray diffraction
Collection of illustrative plates and the X ray diffracting spectrum based on its crystal structure simulation；
Fig. 2 is nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Crystal structure figure；
Fig. 3 is nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15The SHG intensity of powder compares
Figure；
Fig. 4 is nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Ferroelectric properties test knot
Really.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with the drawings and specific embodiments,
The present invention is described in more detail.
Embodiment 1
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 PbO+0.35 Li2CO3+2.5 Nb2O5 = Pb2.15Li0.7Nb5O15 + 0.35 CO2↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15: 0.35 :2.5 PbO, Li2CO3And Nb2O5Powder 10g, and ground with mortar
Mill is uniform, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750 DEG C
And constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm, h=5mm are made under the pressure of 200MPa
Block.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, after insulation 2-5h power supply is closed, with
Stove is cooled to room temperature.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 2
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.1Li0.8Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.1 PbO + 0.4 Li2CO3 + 2.5 Nb2O5 = Pb2.1Li0.8Nb5O15 + 0.4 CO2↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.1: 0.4 :2.5 PbO, Li2CO3And Nb2O5Powder 10g, and ground with mortar
Uniformly, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750 DEG C simultaneously
Constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm is made under the pressure of 200MPa, h=5mm's
Block.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, power supply is closed after insulation 2-5h, with stove
It is cooled to room temperature.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 3
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 PbCO3+0.35 Li2CO3 + 2.5 Nb2O5=Pb2.15Li0.7Nb5O15 + 2.5 CO2↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15：0.35：2.5 PbCO3、Li2CO3And Nb2O5Powder 10g, and ground with mortar
Uniformly, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750 DEG C simultaneously
Constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm is made under the pressure of 200MPa, h=5mm's
Block.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, power supply is closed after insulation 2-5h, with stove
It is cooled to room temperature.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 4
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 Pb(NO3)2 + 0.35 Li2CO3 + 2.5 Nb2O5 = Pb2.15Li0.7Nb5O15 + 0.35 CO2↑ +
2.15 N2↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15: 0.35 :2.5 Pb (NO3)2、Li2CO3And Nb2O5Powder 10g, and will with mortar
Its grinding is uniform, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min extremely
750 DEG C and constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and make Φ=15mm under the pressure of 200MPa,
The block of h=5mm.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, after insulation 2-5h electricity is closed
Source, cools to room temperature with the furnace.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 5
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 C4H6O4Pb + 0.35 Li2CO3 + 2.5 Nb2O5 = Pb2.15Li0.7Nb5O15 + 8.95 CO2↑+
6.45 H2O↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15: 0.35：2.5 C4H6O4Pb、Li2CO3And Nb2O5Powder 10g, and with mortar by its
Grinding is uniform, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750
DEG C and constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm, h=are made under the pressure of 200MPa
The block of 5mm.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, after insulation 2-5h electricity is closed
Source, cools to room temperature with the furnace.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 6
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 PbO + 0.35 Li2CO3 + 5 C10H5NbO20 = Pb2.15Li0.7Nb5O15 + 50.35 CO2↑+
12.5 H2O↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15: 0.35 :5 PbO, Li2CO3And C10H5NbO20Powder 10g, and with mortar by its
Grinding is uniform, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750
DEG C and constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm, h=are made under the pressure of 200MPa
The block of 5mm.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, after insulation 2-5h electricity is closed
Source, cools to room temperature with the furnace.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 7
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, reaction equation is as follows：
2.15 PbO + 0.7 LiNO3+ 2.5 Nb2O5 =Pb2.15Li0.7Nb5O15 + 0.7 NO2↑
Concrete operations follow these steps to carry out：
Mol ratio is weighed for 2.15: 0.7 :2.5 PbO, LiNO3And Nb2O5Powder 10g, and ground with mortar
Uniformly, in being fitted into the corundum ceramic crucible of 15mL, compacting, in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750 DEG C simultaneously
Constant temperature 3h.Taking-up sample after room temperature is cooled to stove to re-grind, and Φ=15mm is made under the pressure of 200MPa, h=5mm's
Block.Block is placed in Muffle furnace and rises to 1150-1250 DEG C with the speed of 5 DEG C/min, power supply is closed after insulation 2-5h, with stove
It is cooled to room temperature.X-ray diffraction result shows that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Embodiment 8
Prepare nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Compound powder
Synthesized using solid reaction process, first synthesize LiNbO3And PbNb2O6Two kinds of presomas, by two kinds of forerunner's precursor reactants
Generate Pb2.15Li0.7Nb5O15Compound.Reaction equation is as follows：
(1)PbO + Nb2O5 = PbNb2O6;
(2)Li2CO3 + Nb2O5 = 2LiNbO3 + CO2↑
(3)2.15 PbNb2O6 + 0.7 LiNbO3 = Pb2.15Li0.7Nb5O15
Concrete operations follow these steps to carry out：
First, mol ratio is weighed for 1:1 PbO and Nb2O5And ground uniformly with mortar, the corundum of loading 10mL
In ceramic crucible, compacting in being placed in Muffle furnace, with the ramp of 5 DEG C/min to 750 DEG C and constant temperature 5h, cools to room with the furnace
Temperature, obtains PbNb2O6Phase；Then mol ratio is weighed for 1:1 Li2CO3And Nb2O5The each 5g of powder is simultaneously ground with mortar
Even, in being fitted into the corundum ceramic crucible of 10mL, compacting is to 750 DEG C and permanent with the ramp of 5 DEG C/min in being placed in Muffle furnace
Warm 5h, cools to room temperature with the furnace, obtains LiNbO3Phase；Mol ratio is weighed again for 2.15:0.7 PbNb2O6And LiNbO3Powder is each
3g, and ground uniformly with mortar, and Φ=15mm is made under the pressure of 200MPa, the block of h=5mm.Block is placed in
1150-1200 DEG C is risen to the speed of 5 DEG C/min in Muffle furnace, after insulation 2-5h power supply is closed, cool to room temperature with the furnace.X is penetrated
Line diffraction patterns show that the product for obtaining is Pb2.15Li0.7Nb5O15Pure phase.
Fig. 1 nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Polycrystal powder X-ray diffractogram
Spectrum and the X ray diffracting spectrum based on its crystal structure simulation.The X-ray simulated based on its crystal structure as can be seen from this figure
Diffracting spectrum is consistent with experiment gained X ray diffracting spectrum, illustrates nonlinear optical material lead niobate lithium of the present invention
The correctness of structural model.
Fig. 2 nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Crystal structure figure.The present invention
By niobium oxygen octahedra, altogether summit connection constitutes Layered-space skeleton to the nonlinear optical material lead niobate crystalline lithium structure, in x-
Y faces form pentagon, quadrangle and triangle hole；Pentagon hole location is filled up by Pb atoms；Remaining Pb and Li atoms
It is filled in quadrangle hole location；Triangle hole location is not occupied by atom.
By the Pb obtained by embodiment 12.15Li0.7Nb5O15Powder does diffuse reflectance spectroscopy, the UV absorption of the powder
While terminating near 400nm.Use Nd：YAG picosecond lasers make fundamental frequency light source, and incident wavelength is the near-infrared laser of 1064nm,
Can output wavelength for 532nm green glow, intensity be corresponding size LiNbO32 times of powder.Fig. 3 is of the present invention non-linear
Optical material lead niobate lithium Pb2.15Li0.7Nb5O15The SHG intensity comparison diagrams of powder.Wherein lithium niobate and lead niobate lithium polycrystalline
Particle size is obtained by the screening of business sieve.It can be seen that nonlinear optical material lead niobate lithium of the present invention
Powder SHG intensity be about corresponding granularity（120μm）2 times of lithium niobate, and meet I type phase matcheds.
By the Pb obtained by embodiment 12.15Li0.7Nb5O15Pure phase makes potsherd and plates silver electrode, does at room temperature
Hysteresis, Fig. 4 is nonlinear optical material lead niobate lithium Pb of the present invention2.15Li0.7Nb5O15Iron at room temperature
Electric performance test result.It can be seen that nonlinear optical material lead niobate lithium of the present invention presents typical electricity
Hysteresis curves, illustrate that it is at room temperature ferroelectric.
Particular embodiments described above, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that the specific embodiment that the foregoing is only the present invention, be not limited to the present invention,
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc., should be included in the present invention's
Within protection domain.
Claims (8)
1. a kind of nonlinear optical material lead niobate lithium, it is characterised in that the chemical formula of the lead niobate lithium is Pb2.15- xLi0.7+2xNb5O15, wherein 0≤x≤0.05, rhombic system, space group is Pn21m；The lead niobate lithium at room temperature, is used
The laser light incident of 1064nm, can produce the green glow that wavelength is 532nm, and the green glow is the form of frequency doubled light；The lead niobate lithium
120 μm of the frequency-doubled signal intensity of polycrystal powder be same size LiNbO31-2 times of powder, and meet I type phase matcheds.
2. nonlinear optical material lead niobate lithium as claimed in claim 1, it is characterised in that the lead niobate lithium as x=0,
Its chemical formula is Pb2.15Li0.7Nb5O15, cell parameter is
3. the raw powder's production technology of nonlinear optical material lead niobate lithium as claimed in claim 1 or 2, it is characterised in that institute
State preparation method and adopt solid phase method, step is as follows：
(1) Pb will be contained, the raw material of Li, Nb is weighed according to stoichiometric proportion and is sufficiently mixed；
(2) in 1150-1250 DEG C of high temperature sintering, temperature retention time is not limited in 2-10 hours, heating rate；
In the temperature-fall period of the high temperature sintering, in 1100-700 DEG C of warm area rate of temperature fall control more than 1 DEG C/min, keep away
Exempting from slow rate of temperature fall causes dephasign LiNbO3And/or PbNb2O6Generation.
4. the preparation method of nonlinear optical material lead niobate lithium as claimed in claim 3, it is characterised in that the step (1)
In raw material be the carbonate containing Pb, Li, Nb each element, nitrate, organic salt or oxide.
5. the application of nonlinear optical material lead niobate lithium as claimed in claim 1 or 2, it is characterised in that the lead niobate lithium
As nonlinear optical crystal application.
6. the application of nonlinear optical material lead niobate lithium as claimed in claim 1 or 2, it is characterised in that the lead niobate lithium
As piezoelectric ceramics application.
7. the application of nonlinear optical material lead niobate lithium as claimed in claim 1 or 2, it is characterised in that the lead niobate lithium
As ferroelectric ceramics application.
8. the application of nonlinear optical material lead niobate lithium as claimed in claim 1 or 2, it is characterised in that the lead niobate lithium
As pyroelectricity material application.
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