CN113215657B - Scandium iodate second-order nonlinear optical crystal material and preparation and application thereof - Google Patents

Scandium iodate second-order nonlinear optical crystal material and preparation and application thereof Download PDF

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CN113215657B
CN113215657B CN202110389987.0A CN202110389987A CN113215657B CN 113215657 B CN113215657 B CN 113215657B CN 202110389987 A CN202110389987 A CN 202110389987A CN 113215657 B CN113215657 B CN 113215657B
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张弛
徐勤科
吴超
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Tongji University
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Abstract

The invention relates to scandium iodate second-order nonlinear lightChemical crystal material and preparation and application thereof, wherein the chemical formula of the crystal material is alpha-Sc (IO)3)3Molecular weight of 569.66, belonging to hexagonal system, space group of P63Cell parameter of
Figure DDA0003016284710000011
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure DDA0003016284710000012
The scandium iodate crystal material has excellent optical performance, the crystal has extremely strong frequency doubling response, and the powder SHG coefficient is KH under the irradiation of 1064nm laser2PO416 times of (KDP) and a powder SHG coefficient of AgGaS under 2100nm laser irradiation2(AGS) of 1.5 times, and can realize phase matching. The crystal also has a wide optical band gap (4.20eV), a large birefringence (Δ n ═ 0.219@546nm), and extremely strong physicochemical stability.

Description

Scandium iodate second-order nonlinear optical crystal material and preparation and application thereof
Technical Field
The invention belongs to the technical field of nonlinear optical materials, and relates to a scandium iodate second-order nonlinear optical crystal material, and preparation and application thereof.
Background
Nonlinear optical materials that can achieve frequency conversion and produce coherent light have attracted researchers' attention because of their potential for use in laser and photonic technologies. Many efforts have been made to develop nonlinear optical materials for applications in the UV-visible-near-IR region, such as beta-BaB2O4(BBO),LiB3O5(LBO),CsB3O5(CBO),KH2PO4(KDP). In contrast, mid/far infrared (>3 μm) laser technology, and the currently applied infrared nonlinear optical chalcogenide material (e.g. AgGaS like chalcopyrite)2,AgGaSe2,ZnGeP2) With obvious drawbacks such as two-photon absorption or low laser damage threshold. In practical applications such as laser guidance, communication, remote sensing and medical diagnosis, a laser with a size of 3-5 μm (a key atmospheric window) is urgently needed, so that the synthesis of an infrared nonlinear optical material which can meet strict conditions (stable physicochemical property, strong SHG response, wide transmission window and high Laser Damage Threshold (LDT)) is imperative in the current scientific technology.
Commercial crystalline alpha-LiIO3Represents a broad class of compounds that exhibit a variety of properties in piezoelectric, ferroelectric, photoelectric, pyroelectric, and nonlinear optics. alpha-LiIO3The excellent linear and nonlinear optical properties (strong SHG response (10 XKDP), wide bandgap (4.00eV) and wide transmission window (0.28-6 μm)) are derived from [ IO3]Perfect parallel alignment of the groups. However, its severe moisture sensitivity seriously hinders its practical application.
Disclosure of Invention
The invention aims to provide a scandium iodate second-order nonlinear optical crystal material, and preparation and application thereof, and solves the problem that a practically applicable medium/far infrared (>3 μm) nonlinear optical crystal material is lacked at present.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a scandium iodate second-order nonlinear optical crystal material with a chemical formula of alpha-Sc (IO)3)3。
Further, the crystalline material belongs to the hexagonal system, and the space group is P63Cell parameter of
Figure BDA0003016284690000021
Figure BDA0003016284690000022
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure BDA0003016284690000023
Figure BDA0003016284690000024
Further, the crystal material has a unit cell parameter of
Figure BDA0003016284690000025
Figure BDA0003016284690000026
α＝β＝90 deg., gamma 120 deg., Z2, unit cell volume
Figure BDA0003016284690000027
The crystal structure of scandium iodate of the invention is as follows: each Sc3+And [ IO ]3]Six oxygen atoms in the radical coordinate to form [ ScO6]Octahedron, each of [ IO ]3]The radicals passing through two μ2The O atom being bound to two [ ScO ]6]Octahedron, forming 3D [ Sc (IO)3)3]∞A frame.
The crystal material of the invention adopts an aliovalent substitution method, selects the radius and Li+Similar Sc3+Substituted alpha-LiIO3Li in the structure of (1)+. Thereby obtaining a special alpha-LiIO-like product which is stable to water3Rare earth iodate alpha-Sc (IO) with structure3)3. Compared with alpha-LiIO3，α-Sc(IO3)3Has enhanced linear and nonlinear properties and exhibits excellent water stability.
The invention uses rare earth cation to replace Li+To modify alpha-LiIO3The novel water-stable mid-infrared nonlinear material is developed. To maintain the alpha-LiIO to the maximum3The rare earth cation should have the structure of (1)+Similar ionic radius and coordination environment and can in principle replace the alkali metal cation Li+And (4) introducing. Rare earth cations with a closed d or f electron shell can cause a large change in the band structure with respect to their optical properties, thereby possibly improving linear and nonlinear properties. Compared with the traditional alkali metal elements, the bonding capability can be enhanced by introducing the high-valence rare earth cations into the iodate system, so that the high-valence rare earth metal elements have higher chemical stability. In particular, the use of rare earth cations with wet stability may improve α -LiIO3The problem of sensitivity to water.
The second technical scheme of the invention provides a preparation method of a scandium iodate second-order nonlinear optical crystal material, which comprises the steps of mixing a scandium source, an iodine source, a lithium source and water to form an initial mixed raw material, and then crystallizing under a hydrothermal condition to obtain a target product.
Further, the scandium source is scandium oxide; the iodine source is iodine oxide; the lithium source is lithium carbonate.
Further, in the initial mixed raw material, the molar ratio of scandium element, iodine element and lithium element is (0.6-1.2): (2.0-4.8): (1.6-3.2). Preferably, the molar ratio of the scandium source, the iodine source and the lithium source in the initial mixed raw material is 0.6: (2-3): 1.6.
furthermore, the temperature of the hydrothermal condition is 180-230 ℃, and the crystallization time is not less than 48 h. Furthermore, the temperature of the hydrothermal condition is 220-230 ℃, and the crystallization time is not less than 48 h.
The third technical scheme of the invention provides application of a scandium iodate second-order nonlinear optical crystal material, and the crystal material is used for infrared laser frequency conversion output. The scandium iodate crystal material has extremely strong frequency doubling effect, and the powder frequency doubling effect is about KH under 1064nm laser irradiation2PO416 times of crystal, and the powder frequency doubling effect is about AgGaS under 2100nm laser irradiation21.5 times of crystal, and can realize phase matching. The scandium iodate crystal material has a large optical band gap (4.2eV) and a large birefringence (Δ n ═ 0.219@546 nm). In addition, it overcomes alpha-LiIO3When immersed in hot water and aqueous solutions having a pH in the range of 3 to 12, the crystal structure remains intact and the NLO activity does not change. Therefore, the crystal material has wide application prospect in the field of nonlinear optics.
Further, the crystal material is used for frequency doubling generators, optical parametric oscillators, optical parametric amplifiers and photoelectric rectifiers. Specifically, the laser frequency converter is used for outputting the middle/far infrared laser beams with double frequency harmonic waves.
Compared with the prior art, the invention has the following advantages:
(1) the invention provides a novel inorganic crystal material scandium iodate, which has extremely strong frequency doubling effect, and the powder frequency doubling effect of the scandium iodate crystal material is about KH under 1064nm laser irradiation2PO416 times of crystal, 21The powder frequency doubling effect of the powder is about AgGaS under the irradiation of 00nm laser21.5 times of crystal, and can realize phase matching. The scandium iodate crystal material has a large optical band gap (4.2eV) and a large birefringence (Δ n ═ 0.219@546 nm). In addition, it overcomes alpha-LiIO3The crystal structure can be kept intact and the NLO activity is not changed after the water sensitive problem of (1) is immersed in hot water and water solution with the pH range of 3 to 12. The method has wide application prospect in the fields of laser frequency conversion, photoelectric modulation, laser signal holographic storage and the like;
(2) the invention provides a preparation method of the scandium iodate crystal material, which adopts a hydrothermal method with mild reaction conditions, can obtain a high-purity crystalline sample at a high yield by hydrothermal crystallization at the temperature of 180-230 ℃, is simple in method and mild in conditions, and is beneficial to large-scale industrial production;
(3) the scandium iodate crystal material can be applied to a laser frequency converter and can be used for outputting medium/far infrared laser beams in double frequency harmonic waves.
Drawings
FIG. 1 is a schematic diagram of the crystal structure of scandium iodate.
FIG. 2 is a comparison of X-ray diffraction patterns, wherein (a) is the crystal structure of sample No. 1 analyzed from single crystal X-ray diffraction data, and the X-ray diffraction patterns obtained by simulation; (b) is a spectrum obtained by grinding the sample No. 1 into powder and then testing the powder by X-ray diffraction.
Fig. 3 is an ultraviolet-visible-near infrared absorption spectrum of sample # 1.
FIG. 4 is an IR spectrum (2.5 to 25 μm) of sample No. 1.
Fig. 5 is a thermogravimetric analysis map of sample # 1.
FIG. 6 shows sample No. 1 and KH2PO4And (3) a second harmonic signal diagram of a sample size in the range of 105-150 mu m.
FIG. 7 is a graph of second harmonic phase matching for sample # 1 in the 1.064 μm band.
Fig. 8 is an optical photograph of sample # 1 under different environments.
Fig. 9 is an XRD pattern of sample # 1 under different circumstances.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, the starting products or process techniques, if not specifically mentioned, are all conventional commercial products or conventional processing techniques in the art.
Example 1
Hydrothermal synthesis of samples
Mixing a scandium source, an iodine source, a lithium source and water according to a certain proportion to form initial raw materials, sealing the initial raw materials in a hydrothermal reaction kettle with a polytetrafluoroethylene lining, heating the initial raw materials to a crystallization temperature, keeping the temperature for a period of time, slowly cooling the temperature of a reaction system to room temperature at a certain speed, filtering and cleaning the reaction system to obtain colorless rod-shaped scandium iodate crystals.
The relationship between the type and ratio of raw materials in the initial mixture, crystallization temperature, crystallization time and sample number is shown in Table 1.
TABLE 1 correspondences between samples and starting materials and Synthesis conditions
Figure BDA0003016284690000041
Figure BDA0003016284690000051
Example 2
Crystal structure analysis
The structure of samples # 1 to # 5 was analyzed by single crystal X-ray diffraction and powder X-ray diffraction methods.
Wherein the single crystal X-ray diffraction test is carried out on a Bruker co D8 VENTURE CMOS X-ray single crystal diffractometer, germany. The crystal size is 0.18X 0.06X 0.05mm3(ii) a The data collection temperature is 293K, and the diffraction light source is Mo-Ka ray monochromized by graphite
Figure BDA0003016284690000052
The scanning mode is omega; the data were subjected to absorption correction processing using the Multi-Scan method. The structure analysis is completed by adopting a SHELXTL-97 program package; determining the position of heavy atom by direct method, and obtaining the coordinates of other atoms by difference Fourier synthesis method; with radicals based on F2The full matrix least square method refines the coordinates and anisotropic thermal parameters of all atoms.
Powder X-ray diffraction test was carried out on an X-ray powder diffractometer of Bruker D8 model, Bruker, Germany, under the conditions of a fixed target monochromatic light source Cu-Ka, wavelength
Figure BDA0003016284690000053
The voltage and current are 40kV/20A, the slit DivSlit/RecSlit/SctSlit is 2.00deg/0.3mm/2.00deg, the scanning range is 5-70 deg, and the scanning step is 0.02 deg.
The single crystal X-ray diffraction test result shows that samples 1# to 5# have the same chemical structural formula and crystal structure, and the chemical formula is alpha-Sc (IO)3)3Molecular weight of 569.66, belonging to hexagonal system, space group of P63Cell parameter of
Figure BDA0003016284690000054
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure BDA0003016284690000055
Represented by sample # 1, whose crystal structure data is
Figure BDA0003016284690000056
Figure BDA0003016284690000057
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure BDA0003016284690000058
The crystal structure is shown in figure 1Shown in the figure.
The powder X-ray diffraction test result shows that the peak positions of the samples are basically the same and the peak intensities are slightly different on the XRD spectrograms of the samples 1# to 6 #.
Typically represented by sample # 1, as shown in FIG. 2. (a) The X-ray diffraction pattern is obtained by simulating a crystal structure analyzed by sample No. 1 according to single crystal X-ray diffraction data; (b) the obtained sample 1# is ground into powder and then is subjected to X-ray diffraction test to obtain a spectrum, and the peak positions are consistent, which indicates that the obtained sample has high purity.
Example 3
Ultraviolet diffuse reflectance spectroscopy test
The diffuse reflectance absorption spectroscopy test of sample # 1 was performed on an agilent Cary 5000 model uv-vis-nir spectrophotometer, usa. As a result, as shown in FIG. 3, it can be seen from FIG. 3 that the compound does not absorb significantly in the range of 295nm to 2500 nm. The compound has a wide optical transmission range and an optical band gap of 4.2 eV.
Example 4
Infrared Spectrum testing
The infrared spectroscopy test of sample # 1 was performed on a Nicolet iS10 model fourier infrared spectrometer, zemer feishol technologies ltd. As shown in FIG. 4, it can be seen from FIG. 4 that the compound has no significant absorption in the range of 2.5 to 6.25 μm and has a wide optical transmission range.
Example 5
Thermogravimetric testing
The thermogravimetric test of sample # 1 was carried out on a thermogravimetric analyzer model Netzsch STA 409PC, a company name of manufacture of equipment resistant to relaxation, germany. The results are shown in FIG. 5, from FIG. 5 it can be seen that the compound remains stable up to a temperature of 450 ℃ and that further heating causes a weight loss of 84.85% total weight loss in the temperature range of 450-2And O2And (4) removing.
Example 6
Frequency doubling test experiment and results
The frequency doubling test experiment of sample # 1 is as follows: production of Nd-YAG solid laser by Q modulationThe generated laser with the wavelength of 1064nm and 2100nm is used as fundamental frequency light to irradiate the tested crystal powder, the generated second harmonic is detected by a photomultiplier, and the harmonic intensity is displayed by an oscilloscope. The crystal sample and the control sample KH are mixed2PO4、AgGaS2And respectively grinding the crystals, and screening out the crystals with different granularity by using a standard screen, wherein the granularity ranges from less than 26, 26-50, 50-74, 74-105, 105-150, 150-200 and 200-280 mu m. And observing the trend of the intensity of the frequency multiplication signal along with the change of granularity, and judging whether the frequency multiplication signal can realize phase matching. Comparison of samples with KH under the same test conditions2PO4、AgGaS2The strength of the second harmonic generated by the sample, and thus the relative magnitude of the frequency doubling effect of the sample.
Test results show that the compound scandium iodate crystal has extremely strong frequency doubling effect, and the frequency doubling signal intensity is KH of a control sample under laser irradiation with the wavelength of 1064nm2PO416 times of the crystal (as shown in FIG. 6a), under 2100nm wavelength laser irradiation, the intensity of the frequency doubling signal is AgGaS of the control sample2Phase matching can be achieved (as in fig. 7) at 1.5 times the crystal (as in fig. 6 b).
Example 7
Water stability test and results
The water stability test experiment for sample # 1 is as follows: approximately 50mg of the sample was immersed at a certain temperature in 10mL of deionized water, aqueous NaOH (pH 9,12) and aqueous HCl (pH 3, 5). Left at a temperature of 20 ℃ to 100 ℃ for 24 hours and then filtered to dry. PXRD data were collected to analyze its crystallinity.
The test results show that alpha-Sc (IO)3)3The weight of (a) was not changed and the crystals remained transparent (fig. 8). XRD pattern and pure alpha-Sc (IO) after immersion of sample in water3)3The spectra of the powders were consistent as shown in FIG. 9, where (a) is the conversion of alpha-Sc (IO) at 35 ℃3)3Powder X-ray diffraction patterns of samples after being soaked in aqueous solutions with pH values of 3,5, 9 and 12 for 24 hours; (b) alpha-Sc (IO) at 50 DEG C3)3Powder X-ray diffraction patterns of samples after being soaked in aqueous solutions with pH values of 3,5, 9 and 12 for 24 hours; (c) at 65 deg.Calpha-Sc (IO)3)3Powder X-ray diffraction patterns of samples after being soaked in aqueous solutions with pH values of 3,5, 9 and 12 for 24 hours; (d) alpha-Sc (IO) at 80 DEG C3)3Powder X-ray diffraction pattern of sample soaked in water solution with pH values of 3,5, 9 and 12 for 24 hr; (e) is alpha-Sc (IO) soaked in boiling water with pH values of 3,5, 9 and 12 for 24 hours3)3Powder X-ray diffraction pattern of the sample.
Example 3:
compared to sample # 1 in example 1, the temperature was mostly the same except that in this example, the hydrothermal conditions were 210 ℃.
Example 4:
compared to sample # 1 in example 1, the temperature was largely the same except that in this example the hydrothermal conditions were at 220 ℃.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (9)

1. A scandium iodate second-order nonlinear optical crystal material is characterized in that the chemical formula of the scandium iodate second-order nonlinear optical crystal material is alpha-Sc (IO)3)3(ii) a The crystal material belongs to a hexagonal system and has a space group of P63Cell parameter of
Figure FDA0003436979630000011
Figure FDA0003436979630000012
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure FDA0003436979630000013
2. The scandium iodate second-order nonlinear optical crystal material of claim 1, wherein the crystal material has a unit cell parameter of
Figure FDA0003436979630000014
α ═ β ═ 90 °, γ ═ 120 °, Z ═ 2, and unit cell volume
Figure FDA0003436979630000015
3. The method for preparing a scandium iodate second-order nonlinear optical crystal material as claimed in any one of claims 1-2, wherein a scandium source, an iodine source, a lithium source and water are mixed to form an initial mixed raw material, and then crystallization is carried out under hydrothermal conditions to obtain a target product.
4. The method for preparing a scandium iodate second-order nonlinear optical crystal material according to claim 3, wherein the scandium source is scandium oxide; the iodine source is iodine oxide; the lithium source is lithium carbonate.
5. The method for preparing a scandium iodate second-order nonlinear optical crystal material according to claim 3, wherein the molar ratio of scandium element, iodine element and lithium element in the initial mixed raw material is (0.6-1.2): (2.0-4.8): (1.6-3.2).
6. The method for preparing the scandium iodate second-order nonlinear optical crystal material as claimed in claim 3, wherein the temperature of the hydrothermal condition is 180-230 ℃ and the crystallization time is not less than 48 h.
7. The method for preparing the scandium iodate second-order nonlinear optical crystal material according to claim 6, wherein the temperature of the hydrothermal condition is 220-230 ℃, and the crystallization time is not less than 48 h.
8. Use of a scandium iodate second order nonlinear optical crystal material as in any one of claims 1-2 for conversion of the output of infrared laser light.
9. The use of a scandium iodate second-order nonlinear optical crystal material as claimed in claim 8, wherein the crystal material is used in frequency doubling generators, optical parametric oscillators, optical parametric amplifiers and photoelectric rectifiers.
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