CN113417008A - Second-order nonlinear optical crystal of cerium iodate and sulfate and preparation and application thereof - Google Patents
Second-order nonlinear optical crystal of cerium iodate and sulfate and preparation and application thereof Download PDFInfo
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- CN113417008A CN113417008A CN202110367563.4A CN202110367563A CN113417008A CN 113417008 A CN113417008 A CN 113417008A CN 202110367563 A CN202110367563 A CN 202110367563A CN 113417008 A CN113417008 A CN 113417008A
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Abstract
The invention relates to a second-order nonlinear optical crystal of iodic acid and cerium sulfate, a preparation method and an application thereof, wherein the chemical formula of the crystal material is Ce (IO)3)2(SO4) Molecular weight of 585.98, belonging to orthorhombic system, and space group of P212121Cell parameter of
α ═ β ═ γ ═ 90 °, Z ═ 4, and unit cell volume
The cerium iodate sulfate crystal material has excellent optical performance, and under 1064nm laser irradiation, the powder has frequency doubling strength of about 3.5 that of potassium dihydrogen phosphate crystalMultiple times, and can realize phase matching under 1064nm laser irradiation. In addition, the crystal material has large birefringence (0.259 at 546 nm), and has wide application prospect in the fields of laser frequency conversion, photoelectric modulation, laser signal holographic storage and the like.
Description
Technical Field
The invention belongs to the technical field of nonlinear optical materials, and relates to a cerium iodate and sulfate second-order nonlinear optical crystal and preparation and application thereof.
Background
Nonlinear optical crystal materials with Second Harmonic Generation (SHG) characteristics play a crucial role in modern laser science and technology because of their frequency conversion capability to extend the output spectral range of laser light sources. A prerequisite for a second order NLO crystal material is to have a crystallographically non-centrosymmetric (NCS) structure, and the presence of asymmetric structural units may contribute to the formation of a macroscopic NCS structure. Currently, one effective strategy for developing new NLO materials is to introduce an asymmetric building block of pi-conjugated planar triangles (e.g., [ BO ]3]3-，[CO3]2-， [NO3]-) E.g. commercial KBe2BO3F2(KBBF)，β-BaB2O4(BBO) and LiB3O5(LBO). Non-pi-conjugated [ PO ] having resistance to absorption in the UV-Vis region in addition to pi-conjugated groups4]3-Radicals have also been widely used in the design of NLO materials, e.g. KH2PO4(KDP) and KTiOPO4(KTP) and recently developed LiCs2PO4，Ba2NaClP2O7. However, these materials do not fully satisfy all of the requirements set forth by various linear and nonlinear optical application techniques. Therefore, the research on novel high-performance NLO materials is an important direction in the field of current inorganic optical functional materials.
Disclosure of Invention
The invention aims to provide a cerium iodate and sulfate second-order nonlinear optical crystal, and preparation and application thereof, so as to solve the problems of weak SHG signal and/or small birefringence of the existing tetrahedral-based nonlinear optical crystal material and realize large SHG response and birefringence at the same time.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a iodic acid cerium sulfate second-order nonlinear optical crystal with a chemical formula of Ce (IO)3)2(SO4)。
Further, the optical crystal belongs to the orthorhombic system, and the space group is P2 12121Cell parameter of
α ═ β ═ γ ═ 90 °, Z ═ 4, and the unit cell volume is
The crystal structure of the cerium iodate and sulfate of the invention is as follows: each Ce4+Ions all coordinated with eight oxygen atoms to form CeO8Polyhedra in which two oxygen ligands are each present with two different [ SO ]4]Group-bound, six other oxygen ligands being different from six [ IO ] s3]Group attachment; [ IO ] connecting three Ce atoms3]The radicals not only bridging two adjacent [ CeO ]8]Polyhedra to form four-membered rings (4-MRs), and [ Ce (IO) is further constructed3)2]∞A cationic layer. And asymmetric [ SO4]Radical is connected with [ Ce (IO)3)2]∞The cationic layer builds the final three-dimensional structure.
The second technical scheme of the invention provides a preparation method of a cerium iodate and sulfate second-order nonlinear optical crystal, which is characterized in that a cerium source, a sulfur source, an iodine source and water are mixed and crystallized under a hydrothermal condition to obtain a target product.
Further, the cerium source is cerium dioxide or cerium sulfate.
Further, the sulfur source is sulfuric acid.
Further, the iodine source is diiodo pentaoxide, iodic acid or periodic acid.
Further, the addition amounts of the cerium source, the sulfur source, the iodine source and the water satisfy that: the molar ratio of cerium, sulfur, iodine and water is 1: (0.5-50): (0.5-50): (20-200).
Furthermore, the temperature of the hydrothermal condition is 150-230 ℃, and the crystallization time is not less than 24 h. Preferably, the hydrothermal condition temperature is 180-230 ℃, and the crystallization time is not less than 48 h.
Further, after crystallization is finished, cooling the obtained product to room temperature at a cooling rate of 0.5-15 ℃/h, filtering and washing to obtain the target product. Preferably, the cooling rate is 0.5-6 ℃/h.
Further, the crystallization process is carried out in a closed reaction kettle.
The third technical scheme of the invention provides application of a cerium iodate and sulfate second-order nonlinear optical crystal which is used for visible middle and far infrared laser frequency conversion output. The obtained cerium iodate-sulfate crystal material has a large frequency doubling effect, and the powder frequency doubling effect is about KH under 1064nm laser irradiation2PO43.5 times of crystal and phase matching. The birefringence was measured at a wavelength of 546nm and was found to be 0.259. In addition, the optical transmission range of the crystal material is 0.51 to 8.78 μm, and the thermal stability temperature is 330 ℃. Therefore, the crystal material has wide application prospect in the field of nonlinear optics.
Furthermore, the second-order nonlinear optical crystal is used for preparing a frequency doubling generator, an optical parametric oscillator, an optical parametric amplifier and/or a photoelectric rectifier. Specifically, the second-order nonlinear optical crystal is used in a laser frequency converter and can be used for outputting visible light and infrared laser beams with double frequency harmonics.
The invention discovers through research that the (C) and the (PO) react4]3-The tetrahedron is similar, and the non-pi conjugated sulfate is also expected to become an application material in the NLO field because of the advantages of environment-friendly chemical components, wide light transmission range and easy crystal growth. Most sulfate-based NCS materials typically exhibit a smaller second harmonic response (SHG) and birefringence attributed to tetrahedra [ SO4 ]]Small microscopic second-order polarizability of the group and weak optical anisotropy. Thus, the present invention obtains a novel NLO sulfate material with large SHG response and birefringence by using an efficient approach, in particular, to have a lone pair of electrons IO3]-Introduction of oxyanions into non-pi-conjugated sulfate systems may contribute to the generation of large microscopic dipole moments and strong optical anisotropyAnd thus a large SHG effect and birefringence can be generated. According to the strategy for enhancing the structural distortion, the invention successfully synthesizes the rare earth iodate sulfate Ce (IO) of the first example3)2(SO4) With highly polarised three-dimensional structure [ CeO ]8]Polyhedron, [ SO ]4]Tetrahedron and [ IO3]And (5) constructing a base element. Ce (IO)3)2(SO4) Strong SHG response (3.5 x KDP) and large birefringence (0.259 at 546 nm) were exhibited in sulfate-based NLO materials.
Compared with the prior art, the invention has the following advantages:
(1) the invention provides a new inorganic crystal material cerium iodate sulfate, which has a larger frequency doubling effect and is about KH under 1064nm laser irradiation2PO4The phase matching can be realized by 3.5 times of the frequency doubling strength of the crystal. In addition, the crystal material has wide transmission ranges in an ultraviolet-visible light region and an infrared light region, a band gap is 2.42eV, the thermal stability temperature reaches 330 ℃, and the crystal material has wide application prospects 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 iodic acid cerium sulfate crystal material, which adopts a hydrothermal method with mild reaction conditions, can obtain a high-purity crystalline sample at a high yield through hydrothermal crystallization at the temperature of 150-230 ℃, is simple, has mild conditions, and is beneficial to large-scale industrial production;
(3) the cerium iodate sulfate crystal material can be applied to a laser frequency converter and can be used for outputting visible and infrared laser beams in a frequency doubling harmonic wave mode.
Drawings
FIG. 1 is a schematic diagram of the crystal structure of cerium iodate sulfate;
FIG. 2 is a comparison of X-ray diffraction patterns; wherein (a) is a spectrum obtained by grinding a sample No. 1 into powder and then testing by X-ray diffraction; (b) 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;
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 plot of sample # 1;
FIG. 6 shows sample No. 1 and KH2PO4A second harmonic signal diagram with the sample size within the range of 105-150 mu m;
FIG. 7 is a graph of second harmonic phase matching for sample # 1 at 1.064 μm wavelength band;
FIG. 8 shows the results of birefringence measurement of cerium iodate and cerium sulfate crystals.
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 cerium source, a sulfur source (adopting 98 wt% sulfuric acid), an iodine source and water according to a certain proportion to form an initial raw material, sealing the initial raw material in a hydrothermal reaction kettle with a polytetrafluoroethylene lining, heating 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 to obtain yellow blocky cerium iodate sulfate 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
Example 2:
crystal structure analysis
The structures of samples # 1 to # 6 in example 1 were 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 company D8 VENTURE CMOS model X-ray single crystal diffractometer. The crystal size is 0.22X 0.11X 0.05mm3(ii) a The data collection temperature is 293K, and the diffraction light source is Mo-Ka ray monochromized by graphite
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
The voltage and current are 40 kV/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 6# have the same chemical structural formula and crystal structure, the chemical formula is cerium iodate, the molecular weight is 585.98, the samples belong to an orthorhombic system, and the space group is P2 12121Cell parameter of
α ═ β ═ γ ═ 90 °, Z ═ 4, and unit cell volume
Represented by sample # 1, whose crystal structure data is
α ═ β ═ γ ═ 90 °, Z ═ 4, and unit cell volume
The crystal structure is shown in figure 1.
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. The pattern obtained by grinding the sample No. 1 in the figure 2(a) into powder and testing by X-ray diffraction is consistent with the X-ray diffraction pattern obtained by simulating the crystal structure analyzed according to the single crystal X-ray diffraction in the figure 2(b), and the peak position and the peak intensity are consistent, which indicates that the obtained sample has high purity.
Example 3:
ultraviolet diffuse reflectance spectroscopy test
The diffuse reflectance absorption spectrum test of sample # 1 was performed on an agilent Cary 5000 model uv-vis-nir spectrophotometer, usa. As shown in FIG. 3, it can be seen from FIG. 3 that the compound does not absorb significantly in the range of 300nm to 2500 nm. The compound has a wide optical transmission range and an optical band gap of 2.42 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 8.78 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. As shown in FIG. 5, it can be seen from FIG. 5 that the compound was stable to 330 ℃ and had better thermal stability.
Example 6:
frequency doubling test experiment and results
The frequency doubling test experiment of sample # 1 is as follows: YAG solid laser with 1064nm wavelength is used as fundamental frequency light to irradiate the tested crystal powder, and the generated second harmonic is detected with photomultiplier tube and displayed with oscilloscope. The crystal sample and the control sample KH are mixed2PO4Grinding the crystals respectively, and screening out crystals with different particle sizes by using a standard sieve, wherein the particle sizes are respectively 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 changing along with the granularity, and judging whether the frequency multiplication signal can realize phase matching. Comparison of samples with KH under the same test conditions2PO4The 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 cerium iodate sulfate crystal has a large frequency doubling effect, and the frequency doubling signal intensity is KH of a reference sample under laser irradiation with a wavelength of 1064nm2PO43.5 times of the crystal (as in FIG. 6), and I-type phase matching (as in FIG. 7) can be realized.
Example 7:
birefringence test and results
The birefringence test experiment for sample # 1 is as follows: crystal sample Ce (IO) was measured with a polarizing microscope equipped with a Berek compensator3)2(SO4) Birefringence of (c). The wavelength of the light source was 546 nm. The magnitude of birefringence is calculated according to equation (1):
Δ R (retardation) ═ Ne-No | × T ═ Δ n × T (1)
Where Δ R is the optical path difference, Δ n is the birefringence, and T is the crystal thickness. The compensated positive and negative rotations provide relative retardation. The sharp boundary between the first, second and third order interference colors results in a small relative error. To increase Ce (IO)3)2(SO4) The birefringence measurement accuracy of the crystal is determined by selecting transparent layered Ce (IO)3)2(SO4). Crystal sample Ce (IO) was measured on a Bruker D8 VENTURE CMOS X-ray source3)2(SO4) Is measured.
The test result shows that the birefringence value of the cerium iodate and sulfate crystal is 0.361, and the large birefringence of the cerium iodate and sulfate crystal breaks through the birefringence limit of the current oxide. (see fig. 8).
The embodiments described above are described to facilitate an understanding and appreciation 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 modifications and alterations without departing from the scope of the present invention.
Claims (10)
1. A second-order non-linear optical crystal of cerium iodate and sulfate is characterized by its chemical formula Ce (IO)3)2(SO4)。
2. The cerium iodate and sulfate second order nonlinear optical crystal as claimed in claim 1, which belongs to orthorhombic system with space group P212121Cell parameter of
α ═ β ═ γ ═ 90 °, Z ═ 4, and unit cell volume
3. The method for preparing a cerium iodate and sulfate second-order nonlinear optical crystal as claimed in claim 1 or 2, characterized in that a cerium source, a sulfur source, an iodine source and water are mixed and crystallized under hydrothermal conditions to obtain the target product.
4. The method of claim 3, wherein the cerium source is cerium dioxide or cerium sulfate;
the sulfur source is sulfuric acid;
the iodine source is diiodo pentaoxide, iodic acid or periodic acid.
5. The method for preparing the second-order nonlinear optical crystal of cerium iodate and cerium sulfate according to claim 3, wherein the addition amounts of the cerium source, the sulfur source, the iodine source and water are as follows: the molar ratio of cerium element, sulfur element, iodine element and water is 1: (0.5-20): (0.5-50): (20-200).
6. The method for preparing a cerium iodate and sulfate second-order nonlinear optical crystal according to claim 3, wherein the temperature of the hydrothermal condition is 150-230 ℃ and the crystallization time is not less than 24 h.
7. The method for preparing the cerium iodate and sulfate second-order nonlinear optical crystal according to claim 3, wherein after crystallization is completed, the obtained product is cooled to room temperature at a cooling rate of 0.5-15 ℃/h, and then the product is filtered and cleaned to obtain the target product.
8. The method for preparing the cerium iodate and sulfate second-order nonlinear optical crystal as claimed in claim 3, wherein the crystallization process is performed in a closed reaction kettle.
9. The use of the cerium iodate and sulfate second order nonlinear optical crystal as claimed in claim 1, wherein the second order nonlinear optical crystal is used for visible, mid-far infrared laser frequency conversion output.
10. The use of a cerium iodate and sulfate second order nonlinear optical crystal according to claim 9, wherein the second order nonlinear optical crystal is used for preparing a frequency doubling generator, an optical parametric oscillator, an optical parametric amplifier and/or a photoelectric rectifier.
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| CN113897679A (en) * | 2021-09-22 | 2022-01-07 | 同济大学 | Zirconium fluorosulfate second-order nonlinear optical crystal material and preparation method and application thereof |
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