Preparation method of multi-component oxide powder
Multi-component oxide powders were synthesized in an open reactor using a solvent evaporation method. Atomic-level mixing and high-temperature calcination were achieved using a magnetic stirrer and oil bath heating. This solved the problems of high energy consumption, low purity, and uneven particle size in the preparation of multi-component oxide powders in the prior art, and produced high-purity, uniformly sized nanocrystals suitable for high-performance functional ceramics.
Patent Information
- Application Number
- CN202511412139.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-29
- Publication Date
- 2026-01-06
AI Technical Summary
Existing methods for preparing multi-component oxide powders suffer from problems such as high energy consumption, low efficiency, large and uneven powder particles, poor component uniformity, and low purity. In particular, they are difficult to meet the requirements of miniaturization, integration, and high reliability of devices when preparing high-performance functional ceramics.
Multi-component oxide powders were synthesized in an open reactor using a solvent evaporation method. Magnetic stirrer and oil bath assisted heating were used to achieve continuous synthesis of multi-component oxide powders with ideal stoichiometry and uniform phase. Nanocrystals with uniform particle size distribution were formed by atomic-level mixing of inorganic salts or metal alkoxides in a liquid environment and high-temperature calcination.
This method enables the preparation of high-purity, uniformly distributed multi-component oxide powders, solving the problems of high energy consumption, low purity, and uneven particle size in traditional methods. It is suitable for large-scale production and meets the needs of high-performance functional ceramics.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of ceramic powder preparation, specifically a method for preparing multi-component oxide powders. It is applicable to the large-scale synthesis of multi-component oxide powders in systems such as titanates, niobates, tantalates, and silicates, and can meet the requirements of high purity, uniform particle size distribution, and ideal stoichiometry of raw material powders for high-performance functional ceramics used in 5G communication, the Internet of Things (IoT), and modern electronic devices. Background Technology
[0002] In recent years, with the rapid development of 5G communication, the Internet of Things (IoT), and modern electronic devices, the demand for high-performance functional ceramics has increased dramatically. As key functional materials, the multi-component oxide powder raw materials used in the preparation of these ceramics must possess characteristics such as low cost, high purity, small size, and uniform particle size distribution to meet the requirements of device miniaturization, integration, and high reliability. Common multi-component oxide powder raw materials mainly belong to systems such as titanates, niobates, tantalates, and silicates, such as LiNbO3 and Li4Ti5O3. 12 CrNbO4, CrTaO4, Zn2SiO4 and Y2Ce2O7, etc. The current mainstream methods for preparing multi-component oxide powders include solid-state method, hydrothermal method, sol-gel method, co-precipitation method, etc.
[0003] Currently, the preparation of industrial multi-component oxide powders mainly relies on solid-state synthesis. Solid-state synthesis has advantages such as simple process, low equipment requirements, small investment, no large amount of organic solvents or toxic reagents involved, large output, and easy scale-up, making it very suitable for large-scale production. However, its application is limited by problems such as high energy consumption, low efficiency, large and uneven powder particles, poor component uniformity, and low purity caused by impurities (ZrO2) introduced by the wear of grinding media (such as zirconia balls).
[0004] The key to solving these problems lies in developing a method for preparing multi-component oxide powders with ideal stoichiometry, uniform particle size distribution, and loose structure. Solvent evaporation is an important method for preparing materials with ideal stoichiometry in liquid-phase reactions. This method involves heating the reaction system in an open reactor using alcohols and organic acids as solvents to form a sol, followed by solvent evaporation to obtain loose multi-component oxide precursor powders. The operation is simple, and the prepared materials have ideal stoichiometry, uniform phase, high purity, and small, evenly distributed particle size. There are currently no reports in China on the production of multi-component oxide powders using solvent evaporation. Domestic methods used include hydrothermal methods, sol-gel methods, and co-precipitation methods; however, these methods have many drawbacks: hydrothermal methods suffer from low raw material utilization and non-stoichiometric ratios caused by washing; sol-gel methods suffer from hard powder agglomeration and long production cycles; and co-precipitation methods easily introduce precipitant impurities and are difficult to control in terms of uniformity.
[0005] Patent CN116082045A discloses an indium titanium tantalum cerium oxide powder, its preparation method, and a method for improving the properties of indium titanium tantalum cerium oxide. This method employs a co-precipitation method, reacting a solution containing indium, titanium, tantalum, and cerium with an alkaline precipitant, requiring strict pH control to neutral. Subsequent filtration, washing, and grinding are necessary, resulting in low raw material utilization and easy particle agglomeration during grinding. Particle size uniformity relies on mechanical dispersion, making atomic-level mixing difficult. Patent CN119929851A discloses a method for preparing multi-component oxide powder, using water to dissolve a metal source and ethanol to dissolve a silicon source. The silicon source readily hydrolyzes and condenses upon contact with water, leading to uneven mixing of the multiple components. Long aging and drying are required, resulting in a long production cycle. Patent CN103242042A discloses a method for preparing multi-component oxide nanoparticles based on a core-shell structure three-dimensional micro-solid-phase reaction. This method uses a specific spherical oxide as the core, requiring surface charge modification to encapsulate other element ions to form a core-shell precursor, making the process complex. The patent with publication number CN119841345A proposes a multi-component composite doped solid fuel cell zirconium oxide powder and its preparation method. It uses zirconium oxychloride hydrolysis and carbon nanotube modification. However, it is only applicable to zirconium oxide powder and requires special modification materials such as carbon nanotubes and zirconium-based metal-organic frameworks, resulting in high raw material costs. The process involves two calcination steps, which is energy-intensive and cumbersome, and cannot be extended to other multi-component oxides such as titanates and silicates. Summary of the Invention
[0006] To overcome the shortcomings of the prior art, the present invention aims to provide a method for preparing multi-component oxide powders. The method involves synthesizing multi-component oxide powders by solvent evaporation. During the synthesis process, an open reactor, a magnetic stirrer, and oil bath auxiliary heating are used to achieve continuous synthesis of multi-component oxide powders with ideal stoichiometry, uniform phase, and high purity. The magnetic stirrer and oil bath auxiliary heating make the reactants more uniformly heated, enabling the production of substances with ideal stoichiometry that are difficult to generate by conventional methods.
[0007] The technical solution of this invention is:
[0008] A method for preparing a multi-component oxide powder includes the following steps:
[0009] Step 1: Prepare a single-element precursor solution with a concentration of 0.1–5 mol·L⁻¹ using inorganic salts or metal alkoxides as solutes and alcohols and organic acids as solvents. -1 ;
[0010] Step 2: Prepare a multi-element precursor solution from the single-element precursor solution obtained in Step 1, with a concentration of 0.1–5 mol·L⁻¹. -1 ;
[0011] Step 3: The multi-element precursor solution from Step 2 is heated in an oil bath to obtain a uniform multi-element oxide powder precursor.
[0012] Step 4: The synthesized multi-component oxide powder precursor is calcined to obtain multi-component oxide nanocrystals with uniform particle size distribution.
[0013] In the preparation method of the multi-element oxide powder, the concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for inorganic salts are one or more of nitrates and chlorides.
[0014] In the preparation method of the multi-element oxide powder, the concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for alcohol compounds are one or more of the following: ethanol, n-propanol, isopropanol, n-butanol, isobutanol, n-pentanol, and ethylene glycol.
[0015] In the preparation method of the multi-element oxide powder, the concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for organic acids are one or more of formic acid, acetic acid, propionic acid, and acrylic acid.
[0016] In the preparation method of the multi-element oxide powder, when preparing the single-element precursor solution in step 1, the mixture is stirred using a magnetic stirrer and ultrasonically treated for 5 to 15 minutes.
[0017] In the preparation method of the multi-element oxide powder, in step 2, the molar ratio of solute elements in the multi-element precursor solution is the ideal stoichiometric ratio of the target product.
[0018] In the preparation method of the multi-component oxide powder, in step 3, the oil bath temperature is 60-200℃.
[0019] In the preparation method of the multi-component oxide powder, the calcination temperature in step 4 is 800-1500℃.
[0020] The preparation method of the multi-component oxide powder has a particle size range of 0.01 to 10 μm.
[0021] The method for preparing the multi-component oxide powder, wherein the multi-component oxide powder is LiNbO3 or Li4Ti5O 12 CrNbO4, CrTaO4, Zn2SiO4 or Y2Ce2O7 powder.
[0022] The design concept of this invention is:
[0023] This invention introduces a solvent evaporation method to synthesize multi-element oxide powders. Microscopic mixing provides a uniform reaction environment for inorganic salts or metal alkoxides, resulting in a multi-element precursor solution in a liquid phase. This allows for atomic-level mixing, which is more conducive to generating small, uniformly sized particles. Combined with the solvent evaporation approach, high-purity multi-element oxide powder precursors can be rapidly synthesized, and the final multi-element oxide powder is obtained through a high-temperature reaction. Furthermore, this invention uses inorganic salts or organic compounds as raw materials, and there is no residual raw material during the preparation process, thus achieving ideal stoichiometric synthesis. This solves the problem of deviations from stoichiometry caused by traditional solid-phase and hydrothermal synthesis methods. During solvent evaporation, the synthesis of multi-element oxide precursors follows a hydrolysis-condensation mechanism driven by esterification. After the inorganic salt or metal alkoxide dissolves, the reaction between the inorganic salt and alcohol is accompanied by the slow release of H2O from the esterification reaction between the alcohol and the organic acid, as well as the nucleation and growth of the multi-element oxide precursor. Solvent evaporation ensures full utilization of the raw materials, allowing the synthesized multi-element oxide powder to adhere to the ideal stoichiometric ratio.
[0024] The advantages and beneficial effects of this invention are:
[0025] 1. This invention utilizes a solvent evaporation method to synthesize multi-component oxide precursors, producing powders with a loose texture and uniform particle size distribution. Compared to traditional synthesis methods, the solvent evaporation method is less prone to introducing impurities during the mixing process, has high raw material utilization, is simple to operate, and enables large-scale continuous operation.
[0026] 2. This invention utilizes a solid-state calcination method to synthesize multi-component oxide powders, which can solve the problems of high cost and complex production process in the traditional wet chemical synthesis of multi-component oxide powders, and realize the large-scale synthesis of multi-component oxide powders.
[0027] 3. This invention introduces an open reactor and utilizes oil bath-assisted heating, which enables the rapid synthesis of high-purity multi-component oxide powders with ideal stoichiometric ratios.
[0028] 4. This invention uses inorganic salts or metal alkoxides as solutes, and alcohols (providing a dissolution environment) and organic acids (participating in esterification reactions) as mixed solvents. After preparing a single-element precursor solution, it is mixed according to the ideal stoichiometric ratio of the target product to obtain a multi-element precursor solution. The liquid phase environment enables atomic-level uniform mixing of each element, avoiding the particle-level mixing inhomogeneity of solid-phase methods and the local concentration fluctuations of coprecipitation methods.
[0029] 5. In an open reactor, the present invention uses oil bath heating (60-200℃) and magnetic stirring to induce esterification of alcohols and organic acids in the solvent system, slowly releasing H2O. The released H2O uniformly drives the hydrolysis and condensation of inorganic salts or metal alkoxides, avoiding the uneven mixing caused by the rapid hydrolysis of silicon sources in the traditional sol-gel method. At the same time, it achieves complete utilization of raw materials and ensures that the powder meets the ideal stoichiometric ratio. Attached Figure Description
[0030] Figure 1 The image shows the X-ray diffraction (XRD) pattern of Zn₂SiO₄ synthesized in Example 1. In the figure, the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb.unit).
[0031] Figure 2 This is a scanning electron microscope image of Zn2SiO4 synthesized in Example 1.
[0032] Figure 3 The image shows the XRD pattern of CrNbO4 synthesized in Example 2. In the figure, the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb.unit).
[0033] Figure 4 This is a scanning electron microscope image of CrNbO4 synthesized in Example 2.
[0034] Figure 5 The image shows the XRD pattern of CrTaO4 synthesized in Example 3. In the figure, the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb.unit).
[0035] Figure 6 This is a scanning electron microscope image of CrTaO4 synthesized in Example 3.
[0036] Figure 7 The image shows the XRD pattern of LiTaO3 synthesized in Example 4. In the figure, the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb.unit). Detailed Implementation
[0037] In the specific implementation process, the present invention proposes a method for synthesizing multi-element oxide powder by evaporating solvent, including the following steps: (1) Dissolve inorganic salts or metal alkoxides in stoichiometric ratios in solutions containing alcohols and organic acids respectively, and prepare single-element precursor solutions using a magnetic stirrer. (2) Sonicate the obtained clear solution, and then continuously stir at room temperature, mix the precursor solutions together and continue stirring, and mix the single-element precursor solutions evenly to obtain multi-element precursor solutions. (3) Evaporate the solution using oil bath-assisted heating, and gradually heat the solution under stirring until the solvent is completely evaporated to obtain a solid product, thus obtaining a multi-element oxide powder precursor. (4) Heat-treat the multi-element oxide powder precursor at high temperature, and calcine this solid in an air furnace to determine the formation of the target phase, thereby achieving rapid synthesis of multi-element oxide powder with ideal stoichiometric ratio and uniform particle size distribution.
[0038] To make the contents of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. However, the following embodiments are merely simple examples of this invention and do not represent or limit the scope of protection of this invention. The scope of protection of this invention is determined by the claims.
[0039] The feasibility of the present invention will be further verified below through examples.
[0040] Example 1
[0041] The method for synthesizing Zn₂SiO₄ powder by solvent evaporation in this embodiment is as follows:
[0042] (1) Preparation of single-element precursor solutions: 7.3g Zn(NO3)2·6H2O and 2.5mL tetraethyl orthosilicate were dissolved in solutions containing 150mL ethanol and 50mL formic acid, respectively. The solutions were stirred with a magnetic stirrer and sonicated for 5 minutes to obtain zinc precursor solution and silicon precursor solution, respectively.
[0043] (2) Preparation of multi-element precursor solution: Zinc precursor solution was added dropwise to silicon precursor solution under stirring at room temperature, and the reaction was continued for 2 hours to obtain a mixed solution.
[0044] (3) Preparation of multi-component oxide nanocrystals: The mixed solution was heated to 60°C in an oil bath to evaporate the solvent, forming a viscous gel. Further heating to 180°C transformed it into a solid. A portion of the product was placed in a muffle furnace and calcined at 1100°C for 6 hours to determine the phase formation. Figure 1 As shown. By Figure 1As can be seen, the XRD pattern only shows characteristic diffraction peaks that perfectly match those of the Zn2SiO4 standard PDF card (e.g., PDF#70-1235), and no diffraction peaks of any impurity phases (e.g., unreacted ZnO or SiO2) were detected. The positions and relative intensities of the characteristic diffraction peaks of Zn2SiO4 are completely consistent with those of the standard PDF card, with no peak shifts caused by deviations in stoichiometry. The prepared Zn2SiO4 powder has high purity, high crystallinity, and accurate stoichiometry.
[0045] like Figure 2 As shown in the scanning electron microscope images of Zn2SiO4 synthesized in Example 1, the Zn2SiO4 powder particles are uniformly dispersed, with uniform particle size, and are generally spherical or regular polygonal in shape. The particle surface is smooth, without sharp edges or irregular protrusions, and the overall particle size of Zn2SiO4 powder is 1-5 μm.
[0046] Example 2
[0047] The method for synthesizing CrNbO4 powder by solvent evaporation in this embodiment is as follows:
[0048] (1) Preparation of single-element precursor solutions: 40.01g Cr(NO3)3·9H2O and 27.02g NbCl5 were dissolved in solutions containing 900mL n-propanol and 300mL acetic acid, respectively. The solutions were stirred with a magnetic stirrer and sonicated for 15 minutes to obtain Cr precursor solution and Nb precursor solution, respectively.
[0049] (2) Preparation of multi-element precursor solution: Under stirring at room temperature, Cr precursor solution was added dropwise to Nb precursor solution and the reaction was continued for 2 hours to obtain a mixed solution.
[0050] (3) Preparation of multi-component oxide nanocrystals: The mixed solution was heated to 80°C in an oil bath to evaporate the solvent, forming a viscous gel. Further heating to 180°C transformed it into a solid. A portion of the product was placed in a muffle furnace and calcined at 1000°C for 6 hours to determine the phase formation. Figure 3 As shown. By Figure 3 As can be seen, the XRD pattern only shows characteristic diffraction peaks that perfectly match those of the CrNbO4 standard PDF card (e.g., PDF#71-0951). No diffraction signals from any impurity phases were detected, including unreacted Cr-based oxides (e.g., Cr2O3) and Nb-based oxides (e.g., Nb2O5). The positions and relative intensities of the characteristic diffraction peaks of CrNbO4 are completely consistent with those of the standard PDF card, with no peak shifts or abnormal peak intensity ratios caused by deviations in stoichiometry. This confirms that the ratio of Cr to Nb precisely matches the ideal stoichiometry of CrNbO4 (Cr:Nb = 1:1).
[0051] like Figure 4 As shown in the scanning electron microscope images of CrNbO4 synthesized in Example 2, the CrNbO4 powder particles are in a stable dispersion state. The CrNbO4 particles are generally spherical or regular polygonal in shape, with smooth particle surfaces and no sharp edges, depressions or irregular protrusions. The overall particle size of the CrNbO4 powder is 10-500 nm.
[0052] Example 3
[0053] The method for synthesizing CrTaO4 powder by solvent evaporation in this embodiment is as follows:
[0054] (1) Preparation of single-element precursor solutions: 4g Cr(NO3)3·9H2O and 3.58g TaCl5 were dissolved in solutions containing 3.5mL ethylene glycol and 1.5mL propionic acid, respectively. The solutions were stirred with a magnetic stirrer and sonicated for 5 minutes to obtain Cr precursor solution and Ta precursor solution, respectively.
[0055] (2) Preparation of multi-element precursor solution: Then, under stirring at room temperature, the Cr precursor solution was added dropwise to the Ta precursor solution, and the reaction was continued for 2 hours to obtain a mixed solution.
[0056] (3) Preparation of multi-component oxide nanocrystals: The mixed solution was heated to 60°C in an oil bath to evaporate the solvent, forming a viscous gel. Further heating to 120°C transformed it into a solid. A portion of the product was placed in a muffle furnace and calcined at 1300°C for 6 hours to determine the phase formation. Figure 5 As shown. By Figure 5 As can be seen, the XRD pattern only shows characteristic diffraction peaks that perfectly match those of the standard PDF card for CrTaO4 (e.g., PDF#81-0910). No diffraction signals of any impurity phases were detected, including unreacted Cr-based oxides (e.g., Cr2O3) and Ta-based oxides (e.g., Ta2O5). The positions and relative intensities of the characteristic diffraction peaks of CrTaO4 are completely consistent with those of the standard PDF card. There are no peak position shifts or abnormal peak intensity ratios caused by deviations in stoichiometry, confirming that the ratio of Cr to Ta precisely matches the ideal stoichiometry of CrTaO4 (Cr:Ta = 1:1).
[0057] like Figure 6 As shown in the scanning electron microscope images of CrTaO4 synthesized in Example 3, the CrTaO4 powder particles are in a stable and highly consistent dispersion state. The CrTaO4 particles are generally spherical or regular polygonal in shape, with smooth particle surfaces and no sharp edges, depressions or irregular protrusions. The overall particle size of the CrTaO4 powder is 10-500 nm.
[0058] Example 4
[0059] The method for synthesizing LiTaO3 powder by solvent evaporation in this embodiment is as follows:
[0060] (1) Preparation of single-element precursor solutions: 6.9g LiNO3 and 35.82g TaCl5 were dissolved in solutions containing 60mL isopropanol and 40mL propionic acid, respectively. The solutions were stirred with a magnetic stirrer and sonicated for 5 minutes to obtain Li precursor solution and Ta precursor solution, respectively.
[0061] (2) Preparation of multi-element precursor solution: The Li precursor solution was then added dropwise to the Ta precursor solution under stirring at room temperature, and the reaction was continued for 2 hours to obtain a mixed solution.
[0062] (3) Preparation of multi-component oxide nanocrystals: The mixed solution was heated to 80°C in an oil bath to evaporate the solvent, forming a viscous gel. Further heating to 120°C transformed it into a solid. A portion of the product was calcined at 1100°C for 6 hours to determine the phase formation, such as... Figure 7 As shown. By Figure 7 As can be seen, the XRD pattern only shows characteristic diffraction peaks that perfectly match those of the LiTaO3 standard PDF card (e.g., PDF#71-0951). No diffraction signals of any impurity phases were detected, including unreacted Li-based oxides (e.g., Li2O) and Ta-based oxides (e.g., Ta2O5). The positions and relative intensities of the characteristic diffraction peaks of LiTaO3 are completely consistent with those of the standard PDF card, without any peak position shift or abnormal peak intensity ratio caused by deviations in stoichiometry. This confirms that the Li to Ta ratio precisely matches the ideal stoichiometry of LiTaO3 (Li:Ta = 1:1). In this embodiment, the LiTaO3 powder particles are stably dispersed and highly consistent. The LiTaO3 particles are generally spherical or regular polygonal, with smooth surfaces, no sharp edges, depressions, or irregular protrusions, and the overall particle size of the LiTaO3 powder is 1–10 μm.
[0063] The results of the examples show that the XRD patterns of Zn2SiO4, CrNbO4, CrTaO4, and LiTaO3 in Examples 1-4 (e.g., Figure 1 , 3 No impurity peaks were observed in peaks 5 and 7, perfectly matching the standard PDF card, confirming high purity and accurate stoichiometry. The atomically mixed solvent evaporated slowly, resulting in a loose precursor state. The nanocrystals formed after calcination exhibited uniform particle size (SEM images as shown). Figure 2 , 4As shown in Figures 6 and 7, this method avoids hard agglomeration. The method of this invention enables the synthesis of high-purity, uniformly sized multi-component oxide nanocrystals without raw material loss. This method is simple, rapid, and low-cost, not only solving the problem of incomplete stoichiometry in traditional wet chemical synthesis, but also producing a loose and fluffy multi-component oxide powder. This invention is applicable to the preparation of various multi-component oxides, especially for powder materials requiring high purity, ideal stoichiometry, and no hard agglomeration, and has broad application prospects.
[0064] The above description is only a preferred embodiment of the present invention, but the implementation of the present invention is not limited to the above embodiments. Any obvious improvements, substitutions or modifications made by those skilled in the art based on the present invention shall fall within the protection scope of the present invention.
Claims
1. A method for preparing a multi-component oxide powder, characterized in that, Includes the following steps: Step 1: Prepare a single-element precursor solution with a concentration of 0.1–5 mol·L⁻¹ using inorganic salts or metal alkoxides as solutes and alcohols and organic acids as solvents. -1 ; Step 2: Prepare a multi-element precursor solution from the single-element precursor solution obtained in Step 1, with a concentration of 0.1–5 mol·L⁻¹. -1 ; Step 3: The multi-element precursor solution from Step 2 is heated in an oil bath to obtain a uniform multi-element oxide powder precursor. Step 4: The synthesized multi-component oxide powder precursor is calcined to obtain multi-component oxide nanocrystals with uniform particle size distribution.
2. The method for preparing a multi-component oxide powder according to claim 1, characterized in that, The concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for inorganic salts are one or more of nitrates and chlorides.
3. The method for preparing a multi-component oxide powder according to claim 1, characterized in that, The concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for alcohol compounds are one or more of the following: ethanol, n-propanol, isopropanol, n-butanol, isobutanol, n-pentanol, and ethylene glycol.
4. The method for preparing a multi-component oxide powder according to claim 1, characterized in that, The concentration of the single-element precursor solution prepared in step 1 is preferably 0.1–2.0 mol·L⁻¹. -1 The raw materials for organic acids are one or more of formic acid, acetic acid, propionic acid, and acrylic acid.
5. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, When preparing the single-element precursor solution in step 1, use a magnetic stirrer to stir and sonicate for 5 to 15 minutes.
6. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, In step 2, the molar ratio of solute elements in the multi-element precursor solution is the ideal stoichiometric ratio of the target product.
7. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, In step 3, the oil bath temperature is 60–200℃.
8. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, In step 4, the roasting temperature is 800–1500℃.
9. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, The particle size range of the multi-component oxide powder is 0.01–10 μm.
10. A method for preparing a multi-component oxide powder according to claim 1, characterized in that, The multi-component oxide powders are LiNbO3 and Li4Ti5O. 12 CrNbO4, CrTaO4, Zn2SiO4 or Y2Ce2O7 powder.
Citation Information
Patent Citations
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