Nano rare earth garnet-based material and preparation method thereof

The preparation of nano-rare earth garnet-based materials by hydrothermal method solves the problem of the inability to synthesize pure phase Y3Al2Ga3O12 in existing technologies, and realizes efficient and environmentally friendly preparation of nanomaterials, which are suitable for the bio- and pharmaceutical industries and LED lighting.

CN121377103APending Publication Date: 2026-01-23SHANGHAI NAT ENG RES CENT FORNANOTECH +1
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Patent Information

Application Number
CN202511792419.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-01
Publication Date
2026-01-23

AI Technical Summary

Technical Problem

No method for hydrothermal synthesis of pure-phase Y3Al2Ga3O12 nano-rare earth garnet-based materials has been reported in the existing technology.

Method used

A hydrothermal method was used to prepare nano-rare earth garnet-based materials by adding Y(NO3)3, Al(NO3)2, and Ga(NO3)3 to deionized water, stirring and mixing, adjusting the pH, heating and reacting, washing, centrifuging and drying.

Benefits of technology

The preparation of pure-phase Y3Al2Ga3O12 nano-rare earth garnet-based materials was achieved. The method is simple, environmentally friendly, green and non-toxic, and the process is convenient. The synthesized materials have high sintering activity.

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Abstract

The invention relates to a nano rare earth garnet-based material and a preparation method thereof. The invention relates to a nano rare earth garnet-based material. The chemical formula of the nano rare earth garnet-based material is Y3Al2Ga3O12. The preparation method solves the problem that in the prior art, a pure-phase Y3Al2Ga3O12 nano rare earth garnet-based material cannot be temporarily subjected to hydro-thermal synthesis. According to the preparation method, a simple hydrothermal method is adopted, nitrate is taken as a main material, and the preparation of the pure-phase Y3Al2Ga3O12 nano rare earth garnet-based material is realized by adjusting conditions and parameters such as the pH value, the reaction time and the reaction temperature of a system.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of luminescent materials, in particular to a nanometer rare earth garnet-based material and a preparation method thereof. BACKGROUND

[0002] The core of the garnet-based material lies in its unique crystal structure. Its general chemical formula is A3B2C3O 12 , wherein: A site: usually larger divalent or trivalent cations, such as Mg²⁺, Ca²⁺, Y³⁺, Gd³⁺, Lu³⁺, etc. A-site cations are located in the dodecahedron coordination center. B site: usually medium-sized trivalent cations, such as Al³⁺, Fe³⁺, Ga³⁺, Cr³⁺, etc. B-site cations are located in the octahedral coordination center. C site: usually smaller trivalent cations, such as Al³⁺, Fe³⁺, Ga³⁺, etc. C-site cations are located in the tetrahedral coordination center. This stable, cubic symmetric lattice structure allows flexible component regulation through element substitution, thereby deriving a variety of material systems with different properties.

[0003] The hydrothermal method refers to a method for preparing materials by dissolving and recrystallizing powders with water as a solvent in a sealed pressure container. Compared with other powder preparation methods, the powder prepared by the hydrothermal method has the advantages of complete grain development, small particle size, uniform distribution, light particle agglomeration, use of relatively inexpensive raw materials, easy obtaining of appropriate stoichiometric materials and crystal shape, etc. Especially, the hydrothermal method for preparing ceramic powder does not require high-temperature calcination, thereby avoiding grain growth, defect formation and impurity introduction in the calcination process, and thus the prepared powder has high sintering activity. Hydrothermal and solvothermal synthesis chemistry is different from solution chemistry, which is a branch of chemistry that studies the chemical behavior and law of substances in solution under high temperature and sealed or high pressure conditions. It is extended to reactions that are difficult to perform at normal temperature and pressure.

[0004] Initially, the hydrothermal method was mainly used for synthesizing water crystals, so the definition of the hydrothermal method is: the hydrothermal method is to use an aqueous solution as a reaction medium in a specially designed sealed reaction container (autoclave), heat the reaction container to create a high-temperature (100-1000℃) and high-pressure (1-100 MPa) reaction environment, and make normally difficultly soluble or insoluble substances dissolve and recrystallize. The hydrothermal method has been widely used in material preparation, chemical reaction and treatment, and has become a very active research field. Its definition is: the hydrothermal process refers to a general term for chemical reactions carried out in water, aqueous solution or steam under high temperature and high pressure. This method uses water as the main solvent, reducing the use of organic solvents, which is beneficial to environmental protection. However, there is no report on the hydrothermal synthesis of Y3Al2Ga3O 12 There is no report on the hydrothermal synthesis of nanometer rare earth garnet-based materials. SUMMARY

[0005] In view of the deficiencies of the prior art, the present application aims to provide a nanometer rare earth garnet-based material.

[0006] The present application further aims to provide a preparation method of the above material, which solves the problem that pure-phase Y3Al2Ga3O 12 nanometer rare earth garnet-based material.

[0007] To achieve the above-mentioned purposes, the present application is implemented by the following technical solutions: The present application discloses a nanometer rare earth garnet-based material, which has a chemical formula of Y3Al2Ga3O 12 .

[0008] The present application provides a preparation method of the nanometer rare earth garnet-based material, which comprises the following steps: adding Y(NO3)3, Al(NO3)2 and Ga(NO3)3 into deionized water, stirring and mixing, adjusting pH, performing a heating reaction, washing, centrifuging and drying, and then obtaining the nanometer rare earth garnet-based material.

[0009] Preferably, the concentrations of Y(NO3)3, Al(NO3)2 and Ga(NO3)3 are 0.8 mol / L respectively.

[0010] Preferably, the volume ratio of Y(NO3)3, Al(NO3)2 and Ga(NO3)3 is 3:2:3.

[0011] Preferably, the pH is adjusted to 7-8 by using NaOH with a concentration of 5M.

[0012] Preferably, the heating reaction temperature is 180℃, and the reaction time is 12h.

[0013] The present application has the following advantages: 1. The present application adopts a simple hydrothermal method, uses nitrate as the main material, and realizes the preparation of pure-phase Y3Al2Ga3O 12 nanometer rare earth garnet-based material by adjusting conditions and parameters such as pH value of the system, reaction time and reaction temperature.

[0014] 2. The present application synthesizes the pure-phase Y3Al2Ga3O 12 nanometer rare earth garnet-based material by using a hydrothermal method, which is safe. The preparation method disclosed by the present application is environmentally friendly, green, non-toxic and inexpensive, and has a simple process. 12 The present application first synthesizes Y3Al2Ga3O 12 nanometer rare earth garnet-based material by using a hydrothermal method. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 Y3Al2Ga3O 12 XRD pattern of the nanometer rare earth garnet-based material; Figure 2 Y3Al2Ga3O 12 SEM pattern of the nanometer rare earth garnet-based material. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0017] If not specifically indicated, the technical means used in the embodiments is the conventional means well known to those skilled in the art.

[0018] The present application discloses a Y3Al2Ga3O 12 The preparation method of the nanometer rare earth garnet-based material comprises the following steps: (1) Y(NO3)3, Al(NO3)2 and Ga(NO3)3 are respectively prepared into liquid reagents with a concentration of 0.8 mol / L.

[0019] (2) Deionized water is added into a beaker, and Y(NO3)3, Al(NO3)2 and Ga(NO3)3 prepared in step (1) are added into the deionized water according to the ion concentration, and the volume ratio is 3:2:3, and the mixture is stirred by a magnetic force, and the pH is adjusted to 7-8 by using 5M NaOH, and then the stirring is performed for 30 min.

[0020] (3) The solution in the beaker is transferred to a 100ml polytetrafluoroethylene liner, heated at 180℃ for 12h, and then the hydrothermal kettle is taken out to reduce the temperature to room temperature, and the content is taken out, washed by using deionized water and anhydrous ethanol, centrifuged (8000r / min) several times, and the solid substance is dried at 60℃, and the obtained sample is ground in an agate mortar, and Y3Al2Ga3O 12 nanometer rare earth garnet-based material.

[0021] The present application will be further described below in combination with specific embodiments.

[0022] Embodiment 1 Y3Al2Ga3O 12 The nanometer rare earth garnet-based material is prepared according to the following steps: (1) Prepare 0.8 mol / L liquid reagents of Y(NO3)3, Al(NO3)2 and Ga(NO3)3 respectively for later use; (2) Add 10ml of deionized water to a beaker, then add 15mL of Y(NO3)3, 10mL of Al(NO3)2 and 15mL of Ga(NO3)3 and stir magnetically until well mixed. Adjust the pH to 7-8 with 5M NaOH and stir for 30min. (3) Transfer the solution in the beaker to a 100ml polytetrafluoroethylene liner and react at 180℃ for 12h. After the reaction is complete, remove the hydrothermal reactor and cool it to room temperature. Take out the contents, wash with deionized water and anhydrous ethanol, centrifuge several times at 8000r / min, dry the solid at 60℃, and grind the obtained sample in an agate mortar to obtain the final sample Y3Al2Ga3O. 12 Nano-rare earth garnet-based materials.

[0023] Figure 1 Y3Al2Ga3O prepared in Example 1 12 XRD pattern of nano-rare earth garnet-based material, the results show: the prepared Y3Al2Ga3O 12 XRD patterns of nano-rare earth garnet-based materials and Y3Al2Ga3O 12 The standard card (PDF#75-0555) is a perfect match, proving the successful synthesis of pure-phase Y3Al2Ga3O by hydrothermal synthesis. 12 .

[0024] Figure 2 Y3Al2Ga3O prepared in Example 1 12 SEM images of nano-rare earth garnet-based materials show that the prepared Y3Al2Ga3O 12 The nano-rare earth garnet-based material has a microstructure of cubic particles with a size of approximately 500 nm.

[0025] The Y3Al2Ga3O prepared by this invention 12 Nano-rare earth garnet-based materials have applications in the biotechnology and pharmaceutical industries, serving as catalysts, LED light sources, and sensors. This invention is the first to synthesize Y3Al2Ga3O using a simple hydrothermal method. 12 The crystal structure of the nano-rare earth garnet-based material was characterized by X-ray diffraction (XRD), and the morphology was characterized by scanning electron microscopy (SEM). A cubic nanoscale pure-phase Y3Al2Ga3O3 material was obtained. 12 Material..

[0026] The results are as follows: Figure 1 Y3Al2Ga3O prepared for the example 12XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O

[0027] Figure 2 XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 SEM pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 SEM pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O

[0028] XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O 12 XRD pattern of the nanometer rare earth garnet-based material prepared by hydrothermal synthesis, the result shows that the prepared Y3Al2Ga3O

[0029] The above-described embodiments are merely preferred modes of the present application, and are not intended to limit the scope of the present application. Various modifications and improvements to the technical solutions of the present application made by those skilled in the art without departing from the design spirit of the present application shall fall within the protection scope of the present application as defined by the claims.

Claims

1. A nano-rare earth garnet-based material, characterized in that, The chemical formula of the nano-rare earth garnet-based material is Y3Al2Ga3O 12 .

2. A method for preparing a nano-rare earth garnet-based material as described in claim 1, characterized in that, Add Y(NO3)3, Al(NO3)2, and Ga(NO3)3 solutions of equal molar concentration to deionized water in a volume ratio of 3:2:3, stir and mix well, adjust the pH to weakly alkaline, heat and react, wash, centrifuge and dry to obtain nano-rare earth garnet-based materials.

3. The method for preparing nano-rare earth garnet-based materials according to claim 2, characterized in that, The concentrations of Y(NO3)3, Al(NO3)2, and Ga(NO3)3 were 0.8 mol / L.

4. The method for preparing nano-rare earth garnet-based materials according to claim 2, characterized in that... Adjust the pH to 7-8 using 5M NaOH.

5. The method for preparing nano-rare earth garnet-based materials according to claim 2, characterized in that, The heating reaction temperature is 180℃, and the reaction time is 12h.

6. The method for preparing the nano-rare earth garnet-based material according to any one of claims 2 to 5, characterized in that, Prepare according to the following steps: (1) Prepare 0.8 mol / L liquid reagents of Y(NO3)3, Al(NO3)2 and Ga(NO3)3 respectively for later use; (2) Add 10ml of deionized water to a beaker, then add 15mL of Y(NO3)3, 10mL of Al(NO3)2 and 15mL of Ga(NO3)3 and stir magnetically until well mixed. Adjust the pH to 7-8 with 5M NaOH and stir for 30min. (3) Transfer the solution in the beaker to a 100ml polytetrafluoroethylene liner and react at 180℃ for 12h. After the reaction is complete, remove the hydrothermal reactor and cool it to room temperature. Take out the contents, wash with deionized water and anhydrous ethanol, centrifuge several times at 8000r / min, dry the solid at 60℃, and grind the obtained sample in an agate mortar to obtain the final sample Y3Al2Ga3O. 12 Nano-rare earth garnet-based materials.