CN115341281A - Second-order nonlinear optical crystal of zirconium fluoride monohydrate, preparation and application thereof - Google Patents
Second-order nonlinear optical crystal of zirconium fluoride monohydrate, preparation and application thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 65
- 230000003287 optical effect Effects 0.000 title claims abstract description 45
- GORLMDNEWNWWBP-UHFFFAOYSA-J tetrafluorozirconium;hydrate Chemical compound O.F[Zr](F)(F)F GORLMDNEWNWWBP-UHFFFAOYSA-J 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims abstract description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011282 treatment Methods 0.000 claims description 4
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- 239000000843 powder Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 150000002484 inorganic compounds Chemical class 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- 230000008025 crystallization Effects 0.000 description 4
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- 229910052723 transition metal Inorganic materials 0.000 description 3
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- 229910002483 Cu Ka Inorganic materials 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
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- 238000007689 inspection Methods 0.000 description 1
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- 238000000373 single-crystal X-ray diffraction data Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3551—Crystals
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Abstract
The invention relates to a second-order non-linear optical crystal of monohydrated zirconium fluoride, a preparation method and an application thereof, wherein the chemical formula of the inorganic compound crystal is ZrF 4 ·H 2 O, molecular weight of 185.24, belonging to tetragonal system, space group of I-42d, and unit cell parameter of
α = β = γ =90 °, Z =8. ZrF with millimeter level can be obtained by a hydrothermal method 4 ·H 2 The preparation method of the O nonlinear optical crystal has the advantages of simple operation, low cost, short growth period and the like. Meanwhile, the monohydrate zirconium fluoride nonlinear optical crystal can output 532nm green light under 1064nm laser irradiation, and the powder SHG coefficient of the monohydrate zirconium fluoride nonlinear optical crystal is KH under 1064nm laser irradiation 2 PO 4 2.2 times of (KDP) and can realize phase matching. Compared with the prior art, the ultraviolet absorption cut-off edge of the crystal is below 190nm, can reach a deep ultraviolet region, and has wide application prospect in the field of deep ultraviolet laser.
Description
Technical Field
The invention belongs to the technical field of nonlinear optical crystal materials, and relates to a second-order zirconium fluoride monohydrate nonlinear optical crystal, and preparation and application thereof.
Background
Nonlinear optical crystal materials with Second Harmonic Generation (SHG) characteristics have important applications in precision fabrication such as laser frequency conversion, micromachining, electro-optical modulation, lithography, and semiconductor inspection because they can produce continuously tunable coherent light. In recent years, based on d 0 The second-order nonlinear optical crystal of transition metal is a crystal material which is expected to be practically used. However, existing d 0 Transition metal nonlinear optical materials tend to have relatively large absorption cut-off edges (larger than 200 nm), which prevents their application in the deep ultraviolet (wavelength less than 200 nm) band. Therefore, a novel second-order nonlinear d suitable for deep ultraviolet region was developed 0 Transition metal second-order nonlinear optical crystal materials are an important research direction of current inorganic optical response functional materials.
ZrF 4 ·H 2 O is a known compound, which has been reported since 1960 (Waters, T.N. (1960). J.Inorg.Nucl.chem.15, 320-328.), and its structure was first reported in 1981 (Kojic-prodic.B, et al (1981). Acta Cryst.B37, 1963-1965), but no test studies on the linear and nonlinear optical properties of the crystal have been made, and no application to the nonlinear optical properties has been involved. Meanwhile, most of the existing preparation methods are aqueous solution methods, and the obtained ZrF 4 ·H 2 The smaller O size does not satisfy the crystal size requirements for testing the fundamental physical properties (including nonlinear optical properties) of a crystal, and no reports have been made to date on the preparation of single crystals of zirconium fluoride monohydrate up to several millimeters in size, even though crystals of this size are not commercially available.
Disclosure of Invention
The invention aims to provide a second-order non-linear optical crystal of zirconium fluoride monohydrate, and preparation and application thereof.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides application of a second-order nonlinear optical crystal of zirconium fluoride monohydrate, and the optical crystal is used for outputting 532nm green light under 1064nm laser irradiation. The ZrF 4 ·H 2 The O crystal material has larger frequency doubling effect, and the powder frequency doubling effect is about KH under 1064nm laser irradiation 2 PO 4 2.2 times of the crystal, and is type I phase matching.
The second technical scheme of the invention provides application of the second-order nonlinear optical crystal of the zirconium fluoride monohydrate, and the optical crystal is used for deep ultraviolet laser frequency conversion, photoelectric modulation or laser signal holographic storage.
Further, the ultraviolet absorption cut-off edge of the optical crystal is less than 190nm, and the optical crystal is used in the field of deep ultraviolet nonlinear optics.
The third technical scheme of the invention provides a second-order nonlinear optical crystal of zirconium fluoride monohydrate, which has a chemical formula of ZrF 4 ·H 2 O, belonging to the tetragonal system, having a space group of I-42d and a cell parameter of
α＝β＝γ＝90°，Z＝8。
The fourth technical scheme of the invention provides a preparation method of a monohydrate zirconium fluoride second-order nonlinear optical crystal, which comprises the following steps: sealing an initial mixed raw material formed by mixing zirconium fluoride, nitric acid and water in a hydrothermal reaction kettle, heating, performing constant-temperature treatment, cooling, filtering and cleaning to obtain ZrF 4 ·H 2 The O crystal is the target product, namely the zirconium fluoride monohydrate second-order nonlinear optical crystal.
Furthermore, the molar ratio of the zirconium fluoride to the nitric acid to the water is1 (0.5-50) to 1-50.
Furthermore, the molar ratio of the zirconium fluoride to the nitric acid to the water is1 (2-10) to (20-50).
Further, the temperature of constant temperature treatment is 150-230 ℃, and preferably, the temperature of hydrothermal conditions is 180-230 ℃; the constant temperature time is 2-5 days, preferably 3-4 days; the cooling rate is 0.5-5 ℃/h, and preferably, the cooling rate is 1-3 ℃/h.
Furthermore, the heating rate is 5-20 ℃/h.
The method adopted by the invention is a hydrothermal method, namely a synthetic method of mixing the initial raw materials according to a certain proportion and then carrying out chemical reaction in a sealed pressure container by taking water as a solvent under the conditions of high temperature and high pressure. In the hydrothermal reaction process, a high-temperature and high-pressure state is formed in the sealed hydrothermal reaction kettle, natural forming conditions similar to geological rock minerals can be simulated, the dissolution and mixing of insoluble raw materials are facilitated, the chemical reaction rate and the crystallization rate are accelerated, and the millimeter-scale ZrF is obtained through the heterogeneous reaction 4 ·H 2 O crystal material.
Compared with the prior art, the invention has the following advantages:
(1) The invention provides the ZrF 4 ·H 2 The preparation method of the O millimeter-grade crystal adopts a hydrothermal method with mild reaction conditions, and can obtain a high-purity crystalline sample at high yield through hydrothermal crystallization at the temperature of 150-230 ℃, and the length of the produced crystal can reach 2.5mm. The method is simple, has mild conditions, and is beneficial to realizing large-scale industrial production;
(2) The invention provides a novel inorganic crystal material ZrF 4 ·H 2 O, capable of outputting 532nm green light under 1064nm laser irradiation, the crystal material has great frequency doubling effect of KH under 1064nm laser irradiation 2 PO 4 2.2 times of the frequency doubling strength of the crystal can realize I-type phase matching;
(3) The crystal ZrF of the inorganic compound provided by the application 4 ·H 2 The ultraviolet absorption cut-off edge of O is less than 190nm, and the method has wide application prospect in the fields of deep ultraviolet laser frequency conversion, photoelectric modulation, laser signal holographic storage and the like.
Drawings
FIG. 1 is ZrF 4 ·H 2 A crystal photograph of O;
FIG. 2 is a comparison of X-ray diffraction patterns; wherein (a) is an X-ray diffraction pattern obtained by simulating a crystal structure analyzed by sample No. 1 according to single crystal X-ray diffraction data; (b) Is a spectrum obtained by grinding a sample No. 1 into powder and then testing by X-ray diffraction;
FIG. 3 is an ultraviolet-visible-near infrared transmission spectrum of sample # 1;
FIG. 4 is an infrared spectrum (2.5-25 μm) of sample No. 1;
FIG. 5 is a thermogravimetric analysis plot of sample # 1;
FIG. 6 shows sample No. 1 and KH 2 PO 4 Second harmonic signal plots for sample sizes in the range 105-150 μm;
FIG. 7 is a graph of second harmonic phase matching for sample # 1 in the 1.064 μm band.
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, unless otherwise specified, all the conventional commercially available raw materials or conventional processing techniques in the art are indicated.
Example 1:
hydrothermal synthesis of samples
Zirconium fluoride, nitric acid and water are mixed according to a certain proportion to form initial raw materials, the initial raw materials are sealed in a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the temperature is raised to crystallization temperature, the temperature of the reaction system is slowly reduced to room temperature at a certain speed after the constant temperature is kept for a period of time, and filtering and cleaning are carried out, so that transparent blocky ZrF with the thickness of about 2.5mm can be obtained 4 ·H 2 O crystals (as shown in figure 1).
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
Contrast of X-ray diffraction pattern
The powder X-ray diffraction test is carried out on an X-ray powder diffractometer of Bruker D8 type of Germany Bruker company under the conditions of a fixed target monochromatic light source Cu-Ka and the wavelength
The voltage and the 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 powder X-ray diffraction test result shows that the peak positions of all samples are basically the same and the peak intensities are slightly different on the XRD spectrograms of the samples 1# -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 transmission spectrum test
The transmission spectrum test of sample # 1 was performed on an agilent Cary 5000 uv-vis-nir spectrophotometer, usa. As shown in FIG. 3, it can be seen that the compound has a wide optical transmission range, an ultraviolet absorption cut-off edge of less than 190nm, and a corresponding optical band gap of more than 6.53eV.
Example 4
Infrared Spectrum testing
The infrared spectroscopy test of sample # 1 was performed on a Nicolet iS10 type fourier infrared spectrometer, zemer feishol technologies ltd. The results are shown in FIG. 4, and it can be seen that the compound 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 a result, as shown in FIG. 5, it can be seen that the compound was stable up to 200 ℃ 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, the photomultiplier is used to detect the generated second harmonic, and oscilloscope is used to display the harmonic intensity. The crystal sample and the control sample KH are mixed 2 PO 4 Grinding the crystals respectively, and sieving with standard sieve to obtain crystals with different particle sizes of less than 26, 26-50, 50-74, 74-105, 105-150, 150-200, and 200-280 μm. 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 conditions 2 PO 4 The strength of the second harmonic generated by the sample, and thus the relative magnitude of the frequency doubling effect of the sample.
The test result shows that the compound ZrF 4 ·H 2 The O crystal has larger frequency doubling effect, and the frequency doubling signal intensity is KH of a reference sample under the irradiation of laser with the wavelength of 1064nm 2 PO 4 2.2 times of the crystal (as in FIG. 6), and I-type phase matching (as in FIG. 7) can be realized.
The embodiments described above are intended to facilitate a person of ordinary skill in the art in understanding and using the invention. 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 (10)
1. The application of the second-order nonlinear optical crystal of zirconium fluoride monohydrate is characterized in that the optical crystal is used for outputting 532nm green light under 1064nm laser irradiation.
2. The application of a second-order nonlinear optical crystal of zirconium fluoride monohydrate is characterized in that the optical crystal is used for deep ultraviolet laser frequency conversion, photoelectric modulation or laser signal holographic storage.
3. The use of a second-order nonlinear optical crystal of zirconium fluoride monohydrate according to claim 2, characterized in that the optical crystal is used in the deep ultraviolet nonlinear optical field.
4. A second-order non-linear optical crystal of zirconium fluoride monohydrate is characterized in that the chemical formula of the optical crystal is ZrF 4 ·H 2 O, belonging to the tetragonal system, having a space group of I-42d and a cell parameter of
α＝β＝γ＝90°，Z＝8。
5. The method for preparing a second-order nonlinear optical crystal of zirconium fluoride monohydrate of claim 4, wherein the method comprises: sealing an initial mixed raw material formed by mixing zirconium fluoride, nitric acid and water in a hydrothermal reaction kettle, heating, performing constant-temperature treatment, cooling, filtering and cleaning to obtain ZrF 4 ·H 2 O crystal is the target product, namely the second-order non-linear optical crystal of zirconium fluoride monohydrate.
6. The method for preparing a second-order nonlinear optical crystal of zirconium fluoride monohydrate of claim 5, wherein the molar ratio of zirconium fluoride, nitric acid and water is1 (0.5-50) to 1-50.
7. The method for preparing a second-order nonlinear optical crystal of zirconium fluoride monohydrate according to claim 5, wherein the molar ratio of zirconium fluoride to nitric acid to water is1 (2-10) to (20-50).
8. The method for preparing a second order nonlinear optical crystal of zirconium fluoride monohydrate of claim 5, wherein the temperature of the constant temperature treatment is 150-230 ℃ and the time is 2-5 days.
9. The method for preparing a second-order nonlinear optical crystal of zirconium fluoride monohydrate according to claim 5, wherein the temperature rise rate is 5 to 20 ℃/h.
10. The method for preparing a second-order nonlinear optical crystal of zirconium fluoride monohydrate according to claim 5, wherein the cooling rate in the cooling process is 0.5-5 ℃/h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015058477A1 (en) * | 2013-10-23 | 2015-04-30 | 中国科学院新疆理化技术研究所 | Deep ultraviolet non-linear optical crystal of barium borate hydrate, preparation method therefor and use thereof |
| CN111719182A (en) * | 2020-03-12 | 2020-09-29 | 同济大学 | Europium iodate monohydrate infrared nonlinear optical crystal material and preparation and application thereof |
| CN113235160A (en) * | 2021-04-12 | 2021-08-10 | 同济大学 | Cerium fluoroiodate second-order nonlinear optical crystal material and preparation and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015058477A1 (en) * | 2013-10-23 | 2015-04-30 | 中国科学院新疆理化技术研究所 | Deep ultraviolet non-linear optical crystal of barium borate hydrate, preparation method therefor and use thereof |
| US20160145769A1 (en) * | 2013-10-23 | 2016-05-26 | Xinjiang Technical Institute Of Physics And Chemistry, Chinese Academy Of Sciences | Deep ultraviolet non-linear optical crystal of barium borate hydrate, preparation method therefor and use thereof |
| CN111719182A (en) * | 2020-03-12 | 2020-09-29 | 同济大学 | Europium iodate monohydrate infrared nonlinear optical crystal material and preparation and application thereof |
| CN113235160A (en) * | 2021-04-12 | 2021-08-10 | 同济大学 | Cerium fluoroiodate second-order nonlinear optical crystal material and preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| J.A. SOMMERS ET AL.: "Research and development for commercial production of high-purity ZrF4 and HfF4", 《MATERLALS SCIENCE FORUM》, vol. 32, pages 629 - 634 * |
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