CN113862774A - Praseodymium lithium niobate scandate magneto-optical crystal and preparation method thereof - Google Patents
Praseodymium lithium niobate scandate magneto-optical crystal and preparation method thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 99
- POAXSRDNOWKSLD-UHFFFAOYSA-N [Li].[Pr] Chemical compound [Li].[Pr] POAXSRDNOWKSLD-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 239000000155 melt Substances 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 4
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 13
- 230000005291 magnetic effect Effects 0.000 abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 7
- -1 rare earth ions Chemical class 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000005090 crystal field Methods 0.000 abstract description 3
- 230000005669 field effect Effects 0.000 abstract description 3
- 230000007704 transition Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000006698 induction Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 230000008859 change Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002223 garnet Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000010431 corundum Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 229910052741 iridium Inorganic materials 0.000 description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000005304 optical glass Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000000411 transmission spectrum Methods 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- FNCIDSNKNZQJTJ-UHFFFAOYSA-N alumane;terbium Chemical compound [AlH3].[Tb] FNCIDSNKNZQJTJ-UHFFFAOYSA-N 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
The invention discloses a praseodymium lithium niobate scandate magneto-optical crystal applicable to a visible-near infrared region and a preparation method thereof. The magneto-optical crystal has a chemical formula of Li(5+2x)Pr3Nb(2‑x)ScxO12Wherein x is 0.5 to 1.0. The crystal belongs to a cubic system and has a space group of
Description
Technical Field
The invention belongs to the technical field of magneto-optical materials and crystal growth, and particularly relates to a praseodymium niobate scandate lithium magneto-optical crystal and a preparation method and application thereof.
Background
Magneto-optical materials are indispensable key functional materials in the information industry of the new generation. Devices such as an optical isolator, an optical fiber current sensor, an optical circulator, a magneto-optical modulator and the like which take magneto-optical materials as cores are important basic devices in the fields of optical communication, the Internet of things, a smart grid, a mobile internet and the like, and play a key role in information technology. The optical isolator is one of indispensable key components in the technical field of modern optical communication, and is called as a diode in an optical path. And the optical fiber current sensor is the most basic sensing device in the smart grid. Therefore, in order to meet the strategic requirements of the national modern information industry development, the research on novel high-quality magneto-optical materials in the visible-near infrared band is imperative.
In the magneto-optical material, the magneto-optical glass is used as an amorphous magneto-optical material, has higher transmittance and isotropy in a visible-near infrared band, and is easy to prepare large-size products. However, the verdet constant of magneto-optical glass is small, which is not favorable for miniaturization and integration of devices. Meanwhile, magneto-optical glass has poor thermal conductivity and small laser damage resistance threshold, and is not suitable for being applied to a high-power laser system. Currently, the crystalline magneto-optical materials commercially available in the visible-near infrared band are mainly Terbium Gallium Garnet (TGG) crystals. However, the growth process of the crystal is not easy to control, the domestic growth of high-quality and large-size TGG crystal is difficult, and compared with the foreign TGG product, the two indexes of absorption loss and extinction ratio are still different. In addition, TGG crystal synthesis raw materials are expensive, and the growth cost is high. Terbium-aluminum garnet (TAG) crystals are paramagnetic magneto-optical crystals with excellent comprehensive performance in visible-near infrared bands, the verdet constant is about 1.5 times of TGG, but the terbium-aluminum garnet (TAG) crystals are non-homoconstituent molten compounds, cannot be subjected to crystal growth by a pulling method, are expensive in growth cost, and are difficult to grow large-size massive single crystals. Therefore, the search for a novel magneto-optic crystal material with a cubic structure and stronger magneto-optic effect and capable of being grown by a Czochralski method is an urgent need for the development of information technology.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a praseodymium lithium niobate scandate magneto-optical crystal applicable to a visible-near infrared region and a preparation method thereof. The magneto-optical crystal prepared has cubic high symmetry, and can effectively eliminate the limitation of birefringence effect on magneto-optical application. Meanwhile, the magnetic rare earth material has the structural characteristics of high content of magnetic rare earth ions, large electron exchange effect, strong crystal field effect, large effective electron transition wavelength of the magnetic rare earth ions in the crystal and the like, is favorable for generating a strong magneto-optical effect, and is expected to provide a novel high-quality magneto-optical material for developing a new visible-near infrared light area magneto-optical device.
In order to achieve the purpose, the invention adopts the following technical scheme:
a magneto-optical crystal of praseodymium lithium niobate scandate has a chemical formula of Li(5+2x)Pr3Nb(2-x)ScxO12Wherein x is 0.5 to 1.0, belonging to the cubic system, and the space group is
。
The cubic system praseodymium lithium niobate scandate magneto-optical crystal adopts a melt pulling (Czochralski) method to carry out single crystal growth, and the preparation method comprises the following steps:
1) and (4) synthesizing high-purity initial raw materials. According to the synthesis of Li(5+2x)Pr3Nb(2-x)ScxO12(x is 0.5 to 1.0) the stoichiometric ratio of the drug (Pr) is accurately weighed6O11Purity 99.99% and Li2CO3Purity 99.95% and Nb2O5Purity of 99.95% and Sc2O3Purity 99.95%) and willThe weighed medicines are put into a corundum mortar for even grinding and tabletting, and then high-temperature sintering is carried out to obtain the initial raw materials required by crystal growth.
2) And (4) growing a single crystal. The iridium crucible is used as a container for crystal growth, and the synthesized starting material is charged into the container and placed in a single crystal pulling furnace under an inert gas (e.g., N)2Ar, etc.) at the growth temperature of 1300-1550 ℃, the growth speed of 0.5-2.0 mm/h and the crystal rotation speed of 10-20 r/min. The change conditions of the aperture and the growth trend during the crystal growth are observed through a quartz observation window on the single crystal pulling furnace, and the growth form of the crystal is controlled by adjusting the rise and fall of the potential and the change rate of the potential through an European land surface.
3) And (5) annealing the crystal. After the crystal growth is finished, lifting the crystal and separating the crystal from the melt, adjusting the height of the crystal to be 2-5 mm higher than the surface of the melt, and then slowly annealing to room temperature at a cooling rate of 10-100 ℃/h. Thus obtaining the cubic system Li(5+2x)Pr3Nb(2-x)ScxO12Magneto-optical crystal blank.
The invention has the following remarkable advantages: the cubic system praseodymium lithium niobate scandate magneto-optical crystal with excellent physical and chemical properties can be obtained by the method. The magneto-optical crystal has good light transmission performance in a visible-near infrared region, has the characteristic of cubic crystal system isotropy, and can effectively eliminate the limitation of a birefringence effect on magneto-optical application. Meanwhile, the crystal also has the structural characteristics of high content of magnetic rare earth ions, large electron exchange effect, strong crystal field effect, large effective electron transition wavelength of the magnetic rare earth ions in the crystal and the like, and is favorable for generating strong magneto-optical effect. Tested by a Faraday magneto-optical effect test system, the magneto-optical crystal Li of the invention(5+2x)Pr3Nb(2-x)ScxO12The Verdet constant is 115-125 rad/T.m (633 nm), which is much higher than that of the terbium-doped glass in commercial application at present and is equivalent to that of Terbium Gallium Garnet (TGG) crystal in commercial application. In addition, the magneto-optical crystal is a consistent melting compound, the growth temperature is 1300-1550 ℃, the magneto-optical crystal can be grown by adopting a medium-frequency induction Czochralski method, the growth process is simple,The period is short, the crystal integrity is high, and large-scale low-cost batch production can be realized.
Drawings
FIG. 1 shows a magneto-optical crystal Li according to the invention6Pr3Nb1.5Sc0.5O12The Rietveld fine modification of (1).
FIG. 2 shows a magneto-optical crystal Li according to the invention6Pr3Nb1.5Sc0.5O12A transmission spectrum of (a).
FIG. 3 is a schematic diagram of a Faraday magneto-optical effect testing system for detection according to the present invention: 1-a laser; 2-a polarizer; 3-an electromagnet; 4-sample; 5-an analyzer; 6-rotating the mirror holder by an angle; 7-optical power meter.
FIG. 4 shows a magneto-optical crystal Li according to the invention6Pr3Nb1.5Sc0.5O12Faraday rotation diagram of (a).
Detailed Description
Example 1: melt Czochralski method for growing cubic system Li6Pr3Nb1.5Sc0.5O12A magneto-optical crystal.
Will press Li6Pr3Nb1.5Sc0.5O12Pr with accurately weighed stoichiometric ratio6O11（99.99%）、Li2CO3（99.95%）、Nb2O5（99.95%）、Sc2O3(99.95%) are put into a corundum mortar and are mixed and ground uniformly, and after tabletting, the mixture is put into a muffle furnace to be calcined for 2 hours at 200 ℃, and then the mixture is heated to 730 ℃ to be calcined for 5 hours, and finally the mixture is heated to 1000 ℃ to carry out solid phase reaction for 12 hours. And cooling, taking out, grinding, tabletting, heating to 1050 ℃, and carrying out solid phase reaction again for 12 hours to obtain the initial raw material for crystal growth. The adopted size is phi 60 mm multiplied by 43mm3The iridium crucible of (1) is used as a container for crystal growth, and the synthesized polycrystalline powder raw material is charged into the container, and is placed in a single crystal pulling furnace, and single crystal pulling is performed under an Ar atmosphere. The growth temperature is 1430 ℃, the growth speed is 1.0mm/h, and the crystal rotation speed is 12 r/min. During the growth process, the change of the aperture and the growth trend of the crystal during growth is observed through a quartz observation windowAnd the rising and falling of the potential and the change rate thereof are adjusted through the continental surface so as to control the crystal growth form. After the growth is finished, the crystal is lifted and separated from the melt, and the height of the crystal is adjusted to be 2-3 mm higher than the surface of the melt. Then setting a cooling program, slowly annealing to room temperature at a cooling rate of 10-100 ℃/h for 32 hours to obtain Li with the size of 12mm multiplied by 12mm (equal diameter part)6Pr3Nb1.5Sc0.5O12And (4) crystals.
Recording of Li prepared in example 1 by X-pert powder diffractometer6Pr3Nb1.5Sc0.5O12And (3) performing X-ray diffraction spectrum on the crystal powder, and refining the crystal structure by using a Rietveld method, wherein the computer program is DBWS-9411. The results of the function fitting were compared to the experimental results of the crystal, as shown in fig. 1. The result shows that the curve of the function calculation is well matched with the experimental result, the final refinement factor reaches Rwp =5.23%, and the grown crystal is in a cubic phase garnet structure, and the space group is
No other hetero-phase substances are present. Mixing Li6Pr3Nb1.5Sc0.5O12After the crystal is oriented, cut and polished, the transmission spectrum of the crystal at room temperature is tested on a Perkin-Elmer Lambda UV/Vis/NIR spectrometer and is shown in figure 2, wherein the transmission spectrum is 200-1400 nm. The result shows that the ultraviolet absorption cut-off edge is about 300 nm, and the ultraviolet absorption cut-off edge is in the wave band range of 300-1400 nm except Pr3+No other absorption is carried out outside the characteristic absorption peak of the ions, and the total transmittance is higher. The extinction method is adopted to test the magneto-optical crystal Li in the self-made Faraday magneto-optical effect test system (figure 3)6Pr3Nb1.5Sc0.5O12The faraday rotation angle of (a) as shown in figure 4. As a result, it was found that the Verdet constant (Verdet constant) was about 183 rad/T.m (633 nm), which was equivalent to that of a commercial TGG crystal.
Example 2: melt Czochralski method for growing cubic system Li7Pr3NbScO12A magneto-optical crystal.
Will press Li7Pr3NbScO12Pr with accurately weighed stoichiometric ratio6O11（99.99%）、Li2CO3（99.95%）、Nb2O5（99.95%）、Sc2O3(99.95%) are put into a corundum mortar and mixed and ground uniformly, and after tabletting, the mixture is put into a muffle furnace to be calcined for 2 hours at 200 ℃, and then the mixture is heated to 730 ℃ to be calcined for 5 hours, and finally the mixture is heated to 950 ℃ to carry out solid phase reaction for 12 hours. And cooling, taking out, grinding, tabletting, heating to 1000 ℃, and carrying out solid phase reaction for 12 hours again to obtain the initial raw material for crystal growth. The adopted size is phi 60 mm multiplied by 43mm3The iridium crucible of (1) is used as a container for crystal growth, and the synthesized polycrystalline powder raw material is charged into the container and put into a single crystal pulling furnace, and N is added2And (4) carrying out single crystal pulling under the atmosphere. The growth temperature is 1380 ℃, the growth speed is 1.5mm/h, and the crystal rotation speed is 20 r/min. In the growth process, the change conditions of the aperture and the growth trend during the crystal growth are observed through the quartz observation window, and the growth form of the crystal is controlled by adjusting the rise and fall of the potential and the change rate of the potential through the European land surface. After the growth is finished, the crystal is lifted and separated from the melt, and the height of the crystal is adjusted to be 2-3 mm higher than the surface of the melt. Then setting a cooling program, slowly annealing to room temperature at a cooling rate of 10-80 ℃/h for 36 hours to obtain Li with the size of 11mm multiplied by 11mm (equal diameter part)7Pr3NbScO12The Verdet constant of the crystal at 633nm band is about 181 rad/T.m, which is equivalent to that of a commercial TGG crystal.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (3)
1. A praseodymium lithium niobate scandate magneto-optical crystal is characterized in that: the crystal has a chemical formula of Li(5+2x)Pr3Nb(2-x)ScxO12Wherein x is 0.5 to 1.0, belonging to the cubic system, and the space group is
。
2. A method of preparing the praseodymium lithium niobate scandate magneto-optical crystal of claim 1, wherein: the method comprises the following steps:
(1) synthesizing a high-purity polycrystalline raw material: according to Li(5+2x)Pr3Nb(2-x)ScxO12Wherein x is 0.5-1.0 stoichiometric ratio and Pr is accurately weighed6O11、Li2CO3、Nb2O5And Sc2O3Grinding them uniformly, tabletting, then making high-temp. sintering so as to obtain the initial raw material required for crystal growth;
(2) growing a single crystal: carrying out single crystal pulling on the initial raw material in the atmosphere of inert gas, wherein the growth temperature is 1300-1550 ℃, the growth speed is 0.5-2.0 mm/h, and the crystal rotation speed is 10-20 r/min;
(3) crystal annealing: after the crystal growth is finished, lifting the crystal to be 2-5 mm higher than the surface of the melt, then slowly annealing to room temperature at a cooling rate of 10-100 ℃/h to obtain cubic system Li(5+2x)Pr3Nb(2-x)ScxO12Magneto-optical crystal blank.
3. Use of the praseodymium lithium niobate scandate magneto-optical crystal of claim 1 or the praseodymium lithium niobate scandate magneto-optical crystal prepared by the method of claim 2 in a magneto-optical material in the visible-near infrared region.
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