CN111041549A - Nonlinear optical polycrystalline material and preparation method thereof - Google Patents
Nonlinear optical polycrystalline material and preparation method thereof Download PDFInfo
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
The invention provides a nonlinear optical polycrystalline material and a preparation method thereof. The polycrystalline material of the invention is a lithium and sodium substituted lead niobate-based compound, and the chemical formula of the compound is Pb2.15(LixNa1‑x)0.7Nb5O15(0<x is less than or equal to 0.25) belongs to an orthorhombic system, and the space group is Bb21And m is selected. The lead niobate-based compound is prepared by a solid-phase reaction method, has simple process and high operability, and is suitable for large-scale mass production. The intensity of the frequency doubling signal of the lithium and sodium substituted lead niobate-based compound powder is 40-47 times of KDP with the same size (120 mu m), and phase matching is met.
Description
Technical Field
The invention relates to a nonlinear optical polycrystalline material Pb2.15(LixNa1-x)0.7Nb5O15(0<x is less than or equal to 0.25) (PLNN) and a powder preparation method thereof.
Background
The nonlinear optical material is an indispensable core material for realizing laser frequency conversion, can convert laser with a common wave band (such as 1064nm) into laser with other wavelengths (such as 532nm), and is widely applied to advanced science fields such as communication, medical treatment, spectroscopy, precision manufacturing and the like. The primary criteria for the utility of an NLO material is the need for a sufficiently strong Second Harmonic (SHG) response, which is primarily related to the dipole moment generated by the anionic groups in the crystal. The niobate with the tungsten bronze structure is a polar material with a plurality of structural vacancies, wherein the A1 site of a quadrangle, the A2 site of a pentagon, the C site of a triangle and the B site occupied by Nb atoms can obtain larger dipole moment through chemical regulation and control of the structural vacancies so as to improve SHG response.
In previous studies, Pb has been reported2AgNb5O15Abnormal thermal expansion and SHG response (. about.0.2X LiNbO) of (PAN)3) (Inorg. chem.55,2864-9 (2016)). Its SHG is derived from PbOxAnd NbO6Contribution of dipole moment of the octahedral anionic group. Then, the strong SHG response (2X LiNbO) is obtained by introducing Li atoms with smaller atomic radius into the crystal lattice3) Pb of2.15Li0.7Nb5O15(ZL 201510317064.9). A series of Li/Na jointly substituted niobate-based tungsten bronze polycrystalline materials Pb with high SHG effect are obtained by simultaneously substituting and modifying a lead niobate-based compound by Li and Na elements2.15(LixNa1-x)0.7Nb5O15(x is more than or equal to 0 and less than or equal to 0.25) (PLNN). The product PLNN has ordered structure in the directions of a and c, the lattice constant is 35.2, b is 17.9, c is 7, and the product is also the patent Pb containing Li element only2.15Li0.7Nb5O15(ZL201510317064.9) is structurally substantially different and has a higher SHG response strength, while having an SHG response strength that is higher than that of a niobate-based tungsten bronze Pb containing only Na element2.15Na0.7Nb5O15(PNN) is higher than 50%. Li/Na co-substituted niobate-based series nonlinear optical polycrystalline material Pb2.15(LixNa1-x)0.7Nb5O15(0<x ≦ 0.25) (PLNN) is a new nonlinear optical material with high SHG response.
Disclosure of Invention
The invention aims to provide a polycrystalline material with high nonlinear optical effect, which is a lead niobate-based compound with a chemical general formula of Pb2.15(LixNa1-x)0.7Nb5O15(0<x ≦ 0.25), where x is 0, denoted PNN, and x is 0.25, denoted PLNN.
The specific technical scheme of the invention is as follows:
the nonlinear optical polycrystalline material is a lithium and sodium substituted lead niobate-based compound, wherein lead, Li and Na have certain solid solubility range to form a single phase (shown in figure 1), the single phase is an orthorhombic system at room temperature, and the space group is Bb21m, lattice parameter of
The lithium and sodium substituted lead niobate-based compound has a tetragonal tungsten bronze structure, as shown in figure 2, and the structure of the series of compounds is similar to that of only cations (Pb)2+、Li+、Na+) The occupation is different, so the PNN structure represents the structure of the whole system. It is made of NbO6The octahedron forms a layered framework with common vertexes, Pb preferentially occupies the A2 position of the pentagon with larger space, excessive Pb occupies the A1 position of the quadrangle, Li and Na atoms simultaneously occupy the A1 position of the quadrangle, and the C position of the triangle with the smallest space is not occupied by atoms.
At room temperature, with Nd: YAG laser as light source emits infrared light with wavelength of 1064nm to produce strong green light at 532 nm. Adopting a transmission mode to collect the green light intensity of 532nm, the product Pb2.15(LixNa1-x)0.7Nb5O15(0<x is less than or equal to 0.25) is 40-50 times of KDP with the same size (120-.
The nonlinear optical polycrystalline material, namely the lead niobate-based compound powder, is prepared by a solid-phase method, and comprises the following steps:
1. the raw materials are mixed according to the stoichiometric ratio. The raw material is carbonate or oxide containing each element.
2. Sintering at high temperature within the range of 1000-1250 ℃, keeping the temperature for 4h, raising the temperature at the rate of 5 ℃/min, and cooling the furnace to room temperature.
Compared with the prior art, the invention has the following beneficial effects: the nonlinear optical polycrystalline material is a series of polar materials with excellent nonlinear optical performance, and is expected to have important application value in the fields of laser, communication, electronic instruments, medical devices and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of a nonlinear optical polycrystalline material according to the present invention, wherein PNN: pb2.15Na0.7Nb5O15，PLNN：Pb2.15Li0.175Na0.525Nb5O15；
FIG. 2 shows a nonlinear optical polycrystalline material PNN according to the present invention: pb2.15Na0.7Nb5O15A schematic structural diagram;
FIG. 3 illustrates the nonlinear optical polycrystalline material PLNN of the present invention: pb2.15(Li0.25Na0.75)0.7Nb5O15(SHG Strength of powder, wherein PNN: Pb)2.15Na0.7Nb5O15And PL 07N: pb2.15Li0.7Nb5O15As control samples, (a) the double frequency transmission test intensity of powders of different particle sizes, (b) the SHG intensity of 120-250 μm size powders.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
Preparation of the nonlinear optical polycrystalline material of the present invention, i.e., Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound powder is synthesized by a solid-phase reaction method, and the reaction equation is as follows:
2.15PbO+0.0875Li2CO3+0.2625Na2CO3+2.5Nb2O5＝Pb2.15Li0.175Na0.525Nb5O15+0.35CO2↑
the specific operation is carried out according to the following steps:
(1) mixing PbO and Li2CO3、Na2CO3And Nb2O5Mixing according to a molar ratio of 2.15:0.0875:0.2625:2.5, weighing 5g of mixed powder, uniformly grinding the powder by using a mortar, putting the powder into a 15mL corundum ceramic crucible, compacting the crucible, putting the crucible into a muffle furnace, heating to 500 ℃ at a speed of 5 ℃/min, keeping the temperature for 2 hours, then heating to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for 4 hours;
(2) taking out the sample after the furnace is cooled to room temperature, adding an adhesive into the sample, grinding the sample again, wherein the dosage of the adhesive accounts for 1 to 5 percent of the weight of the sample, and preparing the sample into tablets under the pressure of 30 MPa;
(3) and (3) putting the tablets into a muffle furnace, heating to 1200 +/-50 ℃ at the speed of 5 ℃/min, keeping the temperature for 4 hours, then turning off a power supply, and cooling to room temperature along with the furnace. The X-ray diffraction result shows that the obtained product is Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound is in a pure phase,
the obtained Pb is2.15(Li0.25Na0.75)0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser is used as fundamental frequency light source, near infrared laser with 1064nm wavelength is incident, green light with 532nm wavelength can be output, and the intensity is 47 times of KDP powder with corresponding size.
At the same time, according to the above procedure, Li is not added2CO3And PbO, Na2CO3And Nb2O5Repeating the steps (1) to (3) to obtain Pb according to the molar ratio of 2.15:0.375:2.5 and unchanged other processes2.15Na0.7Nb5O15And (3) powder. Adding Pb2.15Na0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser as fundamental frequency light source and near infrared laser with incidence wavelength of 1064nmLight can output green light with wavelength of 532nm, intensity is 30 times of KDP powder with corresponding size, and ratio of Pb to Pb2.15(Li0.25Na0.75)0.7Nb5O15The powder is reduced by 57%.
Example 2
Preparation of the nonlinear optical polycrystalline material of the present invention, i.e., Pb2.15(Li0.1Na0.9)0.7Nb5O15The compound powder is synthesized by a solid-phase reaction method, and the reaction equation is as follows:
2.15PbO+0.035Li2CO3+0.315Na2CO3+2.5Nb2O5＝Pb2.15Li0.105Na0.595Nb5O15+0.35CO2↑
the specific operation is carried out according to the following steps:
(1) mixing PbO and Li2CO3、Na2CO3And Nb2O5Mixing according to a molar ratio of 2.15:0.035:0.315:2.5, weighing 5g of mixed powder, grinding the powder uniformly by using a mortar, putting the powder into a 15mL corundum ceramic crucible, compacting the powder, putting the powder into a muffle furnace, heating to 500 ℃ at a speed of 5 ℃/min, keeping the temperature for 2 hours, then heating to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for 4 hours;
(2) taking out the sample after the furnace is cooled to room temperature, adding an adhesive into the sample, grinding the sample again, wherein the dosage of the adhesive accounts for 1 to 5 percent of the weight of the sample, and preparing the sample into tablets under the pressure of 30 MPa;
(3) and (3) putting the tablets into a muffle furnace, heating to 1200 +/-50 ℃ at the speed of 5 ℃/min, keeping the temperature for 4 hours, then turning off a power supply, and cooling to room temperature along with the furnace. The X-ray diffraction result shows that the obtained product is Pb2.15(Li0.1Na0.9)0.7Nb5O15The compound is in pure phase.
The obtained Pb is2.15(Li0.1Na0.9)0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser as fundamental frequency light source, and near infrared laser with incident wavelength of 1064nm can output green light with wavelength of 532nm and intensity of phaseThe size of KDP powder is 40 times of that of KDP powder.
Example 3
Preparation of the nonlinear optical polycrystalline material of the present invention, i.e., Pb2.15(Li0.2Na0.8)0.7Nb5O15The compound powder is synthesized by a solid-phase reaction method, and the reaction equation is as follows:
2.15PbO+0.07Li2CO3+0.28Na2CO3+2.5Nb2O5＝Pb2.15Li0.105Na0.595Nb5O15+0.35CO2↑
the specific operation is carried out according to the following steps:
(1) mixing PbO and Li2CO3、Na2CO3And Nb2O5Mixing according to a molar ratio of 2.15:0.07:0.28:2.5, weighing 5g of mixed powder, uniformly grinding the mixed powder by using a mortar, putting the ground powder into a 15mL corundum ceramic crucible, compacting the crucible, putting the crucible into a muffle furnace, heating to 500 ℃ at a speed of 5 ℃/min, keeping the temperature for 2 hours, then heating to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for 4 hours;
(2) taking out the sample after the furnace is cooled to room temperature, adding an adhesive into the sample, grinding the sample again, wherein the dosage of the adhesive accounts for 1 to 5 percent of the weight of the sample, and preparing the sample into tablets under the pressure of 30 MPa;
(3) and (3) putting the tablets into a muffle furnace, heating to 1200 +/-50 ℃ at the speed of 5 ℃/min, keeping the temperature for 4 hours, then turning off a power supply, and cooling to room temperature along with the furnace. The X-ray diffraction result shows that the obtained product is Pb2.15(Li0.2Na0.8)0.7Nb5O15The compound is in pure phase.
The obtained Pb is2.15(Li0.2Na0.8)0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser is used as fundamental frequency light source, near infrared laser with 1064nm wavelength is incident, green light with 532nm wavelength can be output, and the intensity is 40 times of KDP powder with corresponding size.
Example 4
Preparation of the nonlinear optical polycrystalline material of the present invention, i.e., Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound powder is synthesized by a solid-phase reaction method, and the reaction equation is as follows:
2.15PbO+0.175LiNO3+0.525NaNO3+2.5Nb2O5＝Pb2.15Li0.175Na0.525Nb5O15+0.35N2↑
the specific operation is carried out according to the following steps:
(1) mixing PbO and LiNO3、NaNO3And Nb2O5Mixing according to a molar ratio of 2.15:0.175:0.525:2.5, weighing 5g of mixed powder, grinding the powder uniformly by using a mortar, putting the powder into a 15mL corundum ceramic crucible, compacting the crucible, putting the crucible into a muffle furnace, heating to 500 ℃ at a speed of 5 ℃/min, keeping the temperature for 2 hours, then heating to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for 4 hours;
(2) taking out the sample after the furnace is cooled to room temperature, adding an adhesive into the sample, grinding the sample again, wherein the dosage of the adhesive accounts for 1 to 5 percent of the weight of the sample, and preparing the sample into tablets under the pressure of 30 MPa;
(3) and (3) putting the tablets into a muffle furnace, heating to 1200 +/-50 ℃ at the speed of 5 ℃/min, keeping the temperature for 4 hours, then turning off a power supply, and cooling to room temperature along with the furnace. The X-ray diffraction result shows that the obtained product is Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound is in pure phase.
The obtained Pb is2.15(Li0.25Na0.75)0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser is used as fundamental frequency light source, near infrared laser with 1064nm wavelength is incident, green light with 532nm wavelength can be output, and the intensity is 47 times of KDP powder with corresponding size.
Example 5
Preparation of the nonlinear polycrystalline optical material of the present invention, i.e., Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound powder is synthesized by a solid-phase reaction method, and the reaction equation is as follows:
2.15C4H6O4Pb+0.0875Li2CO3+0.2625Na2CO3+2.5Nb2O5＝Pb2.15Li0.175Na0.525Nb5O15+8.95CO2↑+6.45H2O↑
the specific operation is carried out according to the following steps: ' Qiyi
(1) C is to be4H6O4Pb、Li2CO3、Na2CO3And Nb2O5Mixing according to a molar ratio of 2.15:0.0875:0.2625:2.5, weighing 5g of mixed powder, uniformly grinding the powder by using a mortar, putting the powder into a 15mL corundum ceramic crucible, compacting the crucible, putting the crucible into a muffle furnace, heating to 500 ℃ at a speed of 5 ℃/min, keeping the temperature for 2 hours, then heating to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for 4 hours;
(2) taking out the sample after the furnace is cooled to room temperature, adding an adhesive into the sample, grinding the sample again, wherein the dosage of the adhesive accounts for 1 to 5 percent of the weight of the sample, and preparing the sample into tablets under the pressure of 30 MPa;
(3) and (3) putting the tablets into a muffle furnace, heating to 1200 +/-50 ℃ at the speed of 5 ℃/min, keeping the temperature for 4 hours, then turning off a power supply, and cooling to room temperature along with the furnace. The X-ray diffraction result shows that the obtained product is Pb2.15(Li0.25Na0.75)0.7Nb5O15The compound is in pure phase.
The obtained Pb is2.15(Li0.25Na0.75)0.7Nb5O15And (3) performing transmission spectrum test on the powder, wherein the mass ratio of Nd: YAG picosecond laser is used as fundamental frequency light source, near infrared laser with 1064nm wavelength is incident, green light with 532nm wavelength can be output, and the intensity is 47 times of KDP powder with corresponding size.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (5)
1. The nonlinear optical polycrystalline material is characterized in that the material is a lithium or sodium substituted lead niobate-based compound, and the chemical general formula of the compound is Pb2.15(LixNa1-x)0.7Nb5O15(0<x is less than or equal to 0.25), which is an orthorhombic system and has a space group Bb21m, the lead niobate-based compound is mixed with Nd: YAG laser as light source and incident infrared light of 1064nm wavelength can produce strong green light of 532nm wavelength.
2. The nonlinear optical polycrystalline material according to claim 1, wherein the 532nm green light intensity generated by the lead niobate-based compound is collected in a reflection mode, the powder frequency doubling signal intensity is 30-47 times that of KDP with the same size, and phase matching is satisfied.
3. The method of preparing a nonlinear optical polycrystalline material in accordance with claim 1 or 2, wherein the method of preparing is a solid phase method comprising the steps of:
(1) mixing raw materials containing Pb and Nb and elements of lithium and sodium according to a stoichiometric ratio;
(2) sintering at high temperature within the range of 1000-1250 ℃, keeping the temperature for 4h, raising the temperature at the rate of 5 ℃/min, and cooling the furnace to room temperature.
4. The method according to claim 3, wherein the raw material in the step (1) is a carbonate, a nitrate, an organic salt, or an oxide containing Pb, Nb, Li, and Na.
5. The method according to claim 3, wherein the raw material weighed in step (1) is compacted, placed in a muffle furnace, heated to 500 ℃ at a rate of 5 ℃/min and kept at the temperature for 2h, and then heated to 1000 ℃ at a rate of 5 ℃/min and 1250 ℃.
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| JPH03283686A (en) * | 1990-03-30 | 1991-12-13 | Hitachi Metals Ltd | Laser apparatus |
| CN104874805A (en) * | 2015-06-10 | 2015-09-02 | 北京科技大学 | Nonlinear optical material lead-lithium niobate, and preparation method and application of powder thereof |
| CN105986311A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal strontium calcium pyroniobate and preparation method thereof |
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| JPH03283686A (en) * | 1990-03-30 | 1991-12-13 | Hitachi Metals Ltd | Laser apparatus |
| CN105986311A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal strontium calcium pyroniobate and preparation method thereof |
| CN104874805A (en) * | 2015-06-10 | 2015-09-02 | 北京科技大学 | Nonlinear optical material lead-lithium niobate, and preparation method and application of powder thereof |
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