Birefringent optical crystal and preparation method and application thereof
By preparing birefringent optical crystals of Mg(C7H3NO4)(H2O)2 compound, the problem of low birefringent index of existing birefringent crystal materials is solved, and efficient optical device applications are achieved, with a large birefringent index and high symmetry. , suitable for a variety of optical devices.
Patent Information
- Application Number
- CN202411364637.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-29
- Publication Date
- 2024-12-20
AI Technical Summary
The existing birefringent crystal materials have generally small birefringence index, limiting the miniaturization of compact and efficient optical devices.
A birefringent optical crystal of Mg(C7H3NO4)(H2O)2 compound was prepared, and the 2D surface was connected to pyridine dicarboxylic acid through Mg-O bond and Mg-N bond, and a 3D spatial structure was formed between layers by hydrogen bonding. The hydrothermal synthesis method was prepared by crystallization at 80~150°C for 6~120 hours.
A large birefringence is obtained, suitable for the preparation of birefringence optics, such as optical polarizers, beam displacements, optical circulators, optical isolators or optical modulators, with high symmetry and a large birefringence , suitable for high-tech fields.
Smart Images
Figure CN119162671A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a Mg(C7H3NO4)(H2O)2 compound, a birefringent crystal and a preparation method and application thereof. Background Art
[0002] Birefringence refers to the phenomenon that when a beam of light wave is incident on an inhomogeneous body, it is decomposed into two beams of linearly polarized light with perpendicular polarization directions. Due to the anisotropy of crystal materials, the angle between the two beams of linearly polarized light is related to the incident direction and polarization state. The ordinary light (o light) obeys the law of refraction, and its refractive index (n) is independent of the incident direction. The extraordinary light (e light) does not obey the law of refraction, and its refractive index (n) is related to the incident direction. The maximum difference in the refractive index of the two beams is the birefringence. Inhomogeneous bodies such as uniaxial and biaxial products that produce birefringence are called birefringent crystals. Birefringent crystals are a very important linear optical material, widely used in the fields of optics and communications, and are key materials for manufacturing components such as polarization polarizing prisms, polarization beam splitters, optical isolators, circulators and optical modulators.
[0003] At present, the commonly used birefringent crystals are mainly YVO4, CaCO3, a-BaB2O4, and MgF2, but the technical application bottleneck they currently face is that the birefringence is generally small, which is not conducive to the miniaturization of compact and efficient optical devices. Therefore, exploring new birefringent crystals with excellent comprehensive performance and large birefringence still has important significance and application value. Summary of the invention
[0004] The purpose of the present invention is to provide a Mg(C7H3NO4)(H2O)2 compound, a birefringent crystal and a preparation method and use thereof. The present invention prepares a Mg(C7H3NO4)(H2O)2 compound and a birefringent optical crystal. The Mg(C7H3NO4)(H2O)2 birefringent crystal prepared by the present invention has a large birefringence and can be used to prepare birefringent crystal devices.
[0005] To achieve the above object, the technical solution of the present invention is as follows: 1. A Mg(C7H3NO4)(H2O)2 compound, wherein the chemical formula of the Mg(C7H3NO4)(H2O)2 compound is Mg(C7H3NO4)(H2O)2.
[0006] 2. The present invention provides a Mg(C7H3NO4)(H2O)2 birefringent optical crystal, the chemical formula of which is Mg(C7H3NO4)(H2O)2, belonging to the monoclinic system, and the space group is C 2 / c , the unit cell parameters are a = 9.9290(3) Å,b = 12.0665(4) Å, c = 7.3261(2) Å, α = 90°, β = 106.157(4)°, γ = 90°, Z = 4.
[0007] The basic structure of the crystal is that Mg in the crystal is connected to pyridine dicarboxylic acid through Mg-O bonds and Mg-N bonds to form a 2D surface (such as Figure 5 As shown in the figure, the layers are connected by hydrogen bonds to form a 3D spatial structure (as shown in the figure). Figure 4 as shown).
[0008] 3. A method for preparing a Mg(C7H3NO4)(H2O)2 birefringent optical crystal, comprising the following steps: At room temperature, 3,5-pyridinedicarboxylic acid C7H5NO4 compound, MgO, HNO3 aqueous solution and water are mixed and placed in a polytetrafluoroethylene liner, the liner is installed and placed in a hydrothermal synthesis reactor, the seal is tightened, and then the reactor is placed in a precision blast drying oven connected to an automatic temperature controller, and crystallized at 80~150 ℃ for 6~120 hours to obtain.
[0009] Among them, the input ratio of 3,5-pyridinedicarboxylic acid C7H5NO4 compound, MgO, HNO3 aqueous solution, and water is 0.05-1g:0.05-0.5 g:0.1-2 mL:0.5-10 mL; the mass fraction of HNO3 aqueous solution is 65%-68%.
[0010] Specifically, the Mg(C7H3NO4)(H2O)2 compound is prepared by the following method: 3,5-pyridinedicarboxylic acid C7H5NO4 compound, MgO, HNO3 aqueous solution, and water are put into a polytetrafluoroethylene liner (23 mL) at an input ratio of 0.05-1 g:0.05-0.5 g:0.1-2 mL:0.5-10 mL, and the temperature is raised to 80-150 °C at 10-100 °C / hour and maintained for 10-120 hours, and then cooled to room temperature at a rate of 0.5-3 °C / hour to obtain Mg(C7H3NO4)(H2O)2 compound.
[0011] A use of a Mg(C7H3NO4)(H2O)2 birefringent optical crystal. The Mg(C7H3NO4)(H2O)2 birefringent crystal is used for preparing a birefringent optical device.
[0012] A birefringent optical device comprises the Mg(C7H3NO4)(H2O)2 birefringent optical crystal. The optical device is an optical polarizer, a beam displacer, an optical circulator, an optical isolator or an optical modulator.
[0013] Compared with the prior art, the present invention has the following beneficial effects: The present invention prepares a Mg(C7H3NO4)(H2O)2 compound and a birefringent optical crystal, which has a large birefringence; the Mg(C7H3NO4)(H2O)2 birefringent optical crystal has a large birefringence, and the birefringence of the crystal at 546 nm is 0.44; the Mg(C7H3NO4)(H2O)2 birefringent optical crystal has high symmetry, belongs to a double optical axis crystal, can be used to make birefringent devices, and is expected to be applied in several military and civilian high-tech fields (such as optical polarizers, beam shifters, optical circulators, optical isolators or optical modulators, etc.). BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 This is a working principle diagram of a typical birefringent optical device made of Mg(C7H3NO4)(H2O)2 crystal. When the Mg(C7H3NO4)(H2O)2 crystal is laser processed and optically processed, two laser beams with different polarization directions will be generated.
[0015] Figure 2 It is the UV-visible-near infrared absorption spectrum of Mg(C7H3NO4)(H2O)2 crystals obtained in Example 1 of the present invention.
[0016] Figure 3 This is the powder XRD diffraction pattern of Mg(C7H3NO4)(H2O)2 crystals of Example 1 of the present invention.
[0017] Figure 4 This is a diagram of the crystal structure of Mg(C7H3NO4)(H2O)2 of the present invention.
[0018] Figure 5 It is the bonding mode in Mg(C7H3NO4)(H2O)2 crystal. DETAILED DESCRIPTION
[0019] The present invention is further described below in conjunction with the embodiments and drawings. Those skilled in the art will appreciate that the following embodiments are not intended to limit the scope of protection of the present invention, and any improvements and changes made on the basis of the present invention are within the scope of protection of the present invention.
[0020] Unless otherwise specified, the raw materials in the examples of this application were purchased through commercial channels.
[0021] Example 1 The method for preparing Mg(C7H3NO4)(H2O)2 single crystal comprises the following steps: To prepare Mg(C7H3NO4)(H2O)2 compound, 0.0835 g 3,5-pyridinedicarboxylic acid C7H5NO4 compound, 0.060 g MgO, 0.35 mL HNO3 aqueous solution (concentration of 65wt%) and 1 mL of distilled water were added to a polytetrafluoroethylene liner, the liner was installed and placed in a hydrothermal synthesis reactor, the seal was tightened, and then the reactor was placed in a precision blast drying oven connected to an automatic temperature controller, the temperature was raised to 110°C at a rate of 48°C / hour, constant temperature crystallization was carried out at 110°C for 53 hours, and then the temperature was lowered to 30°C at a rate of 1.67°C / hour, and filtered and dried to obtain a white transparent block of Mg(C7H3NO4)(H2O)2 compound.
[0022] Figure 3 This is the powder XRD diffraction spectrum of the Mg(C7H3NO4)(H2O)2 crystal of Example 1, indicating that Mg(C7H3NO4)(H2O)2 crystals were obtained.
[0023] Example 2 The method for preparing Mg(C7H3NO4)(H2O)2 single crystal comprises the following steps: Preparation of Mg(C7H3NO4)(H2O)2 compound: add 0.167 g 3,5-pyridinedicarboxylic acid C7H5NO4 compound, 0.080 g MgO, 0.35 mL HNO3 aqueous solution (concentration of 65wt%) and 1 mL of distilled water into a polytetrafluoroethylene liner, install the liner and put it into a hydrothermal synthesis reactor, tighten the seal, and then put the reactor into a precision blast drying oven connected to an automatic temperature controller, heat it to 110°C at a rate of 48°C / hour, crystallize it at a constant temperature at 110°C for 53 hours, then cool it to 30°C at a rate of 1.67°C / hour, filter and dry it, and you can get a white transparent block of Mg(C7H3NO4)(H2O)2 compound.
[0024] The powder XRD diffraction spectrum of the crystal in this example is Figure 3 Basically the same.
[0025] Figure 4 This is the crystal structure diagram of Mg(C7H3NO4)(H2O)2 of the present invention. As can be seen from the figure, Mg in the crystal is connected to pyridinedicarboxylic acid through Mg-O bonds and Mg-N bonds to form a 2D surface, and the layers are connected by hydrogen bonds to form a 3D spatial structure.
[0026] Figure 2The UV-visible-near infrared diffuse reflectance spectrum of the crystal obtained in Example 1 of the present invention shows that the light absorption cutoff edge of the crystal is 273 nm. The first principle theoretical calculation results show that the theoretical value of the birefringence of the crystal is about 0.44 @ 546 nm, and the experimental value of the birefringence of the crystal tested using a polarizing microscope is 0.44 @ 546 nm, indicating that the experimental value of the birefringence matches the calculated value well.
[0027] The crystal working principle diagram obtained by the present invention is as follows Figure 1 As shown, a laser beam is incident on the treated and optically processed Mg(C7H3NO4)(H2O)2 crystal of the present invention, which can generate two laser beams with different polarization directions.
[0028] The above specific implementation methods are only detailed explanations of the technical solutions of the present invention. The present invention is not limited to the above embodiments. Those skilled in the art should understand that any improvements and substitutions based on the above principles and spirits on the basis of the present invention should be within the protection scope of the present invention.
Claims
1. A birefringent optical crystal, characterized in that: The chemical formula of the crystal is Mg(C7H3NO4)(H2O)2, it belongs to the monoclinic system, and its space group is C 2 / c , the unit cell parameters are a = 9.9290(3) Å, b = 12.0665(4) Å, c = 7.3261(2) Å, α = 90°, β = 106.157(4)°, γ = 90°, Z = 4.
2. The method for preparing a birefringent optical crystal according to claim 1, characterized in that: The steps include: At room temperature, 3,5-pyridinedicarboxylic acid, MgO, HNO3 solution and water are mixed and placed in a polytetrafluoroethylene liner, the liner is installed and placed in a hydrothermal synthesis reactor, and crystallized at 80-150°C for 6-120 hours to obtain the Mg(C7H3NO4)(H2O)2 birefringent optical crystal; Among them, the input ratio of 3,5-pyridinedicarboxylic acid, MgO, HNO3 solution, and water is 0.05-1 g: 0.05-0.5 g: 0.1-2 mL: 0.5-10 mL.
3. The method for preparing a birefringent optical crystal according to claim 2, characterized in that: The mass fraction of HNO3 solution is 65%-68%.
4. The use of a birefringent optical crystal according to claim 1, characterized in that: The Mg(C7H3NO4)(H2O)2 birefringent optical crystal is used for preparing birefringent optical devices.