A spherical scandium-zirconium powder, a preparation method and application thereof

Abstract

This invention belongs to the field of battery manufacturing technology, specifically relating to a spherical scandium-zirconium powder, its preparation method, and its application. The preparation method includes the following steps: S1: Mixing organic monomers, crosslinking agents, and initiators to carry out a polymerization reaction to obtain a gel; the organic monomers are carbon-carbon double bond monomers; S2: Mixing the gel obtained in S1 with a scandium-zirconium mixed solution, allowing ions in the scandium-zirconium mixed solution to migrate into the gel, and drying to obtain a dry gel; S3: Calcining the dry gel obtained in S2 in two steps to obtain spherical scandium-zirconium powder; wherein, the atmosphere for the first calcination step is a non-reactive atmosphere, and the atmosphere for the second calcination step is an oxygen-containing atmosphere. This preparation method is simple, requires low-level equipment, has low cost, and is easy to industrialize; the obtained spherical scandium-zirconium powder has good dispersibility, ensuring a spherical appearance, a submicron particle size, and high product purity.

Description

Technical Field

[0001] This invention belongs to the field of battery manufacturing technology, specifically relating to a spherical scandium-zirconium powder, its preparation method, and its application. Background Technology

[0002] Solid oxide fuel cells (SOFCs) are electrochemical power generation devices that can directly convert the chemical energy of fuel into electrical energy. If SOFCs are used to process carbon-based fuels, the power generation efficiency can reach 50% to 60% in a single operation, and the pollution is also low.

[0003] In a single SOFC cell, poor thermal matching of the sintering performance of electrode and electrolyte materials, unstable electrolyte conductivity, and structural damage due to weak cell strength can all lead to performance degradation of the entire stack. Therefore, accelerating research on electrolyte materials is crucial for the commercial development of SOFCs. Currently, most commercially available SOFCs use 6–10 mol% yttrium-stabilized zirconium oxide (YSZ) as the solid electrolyte. However, traditional SOFCs using YSZ as the electrolyte suffer from high operating temperatures, adverse interfacial reactions in the battery materials, low conductivity, and difficulty in sealing, all of which hinder further commercial development. Scandium-zirconium powder, due to its excellent oxygen ion conductivity, has been developed as a novel electrolyte material for SOFCs. Existing research has found that spherical morphology is beneficial for increasing powder flowability, which has a significant impact on the quality of the electrolyte membrane obtained by subsequent powder casting. Currently, the main methods for preparing scandium-zirconium powder include solid-phase methods, wet chemical methods, and chemical vapor deposition methods. Wet chemical methods include precipitation, sol-gel methods, hydrothermal methods, and emulsion methods. The most commonly used method is the sol-gel method, a novel approach for preparing inorganic materials developed in the 1960s. This method involves solidifying compounds containing highly chemically active components through processes such as solution, sol, and gel. However, powders obtained using the sol-gel method are prone to agglomeration and irregular morphology. For example, existing patent literature discloses a method for preparing nano-zirconia using an internal gelation method. The steps include preparing a solution containing a zirconium source, a yttrium source, and urea; adding acrylamide and N,N'-methylenebisacrylamide to the solution; adding ammonium persulfate and tetramethylethylenediamine; after complete gelation; washing and filtering; drying; and calcining to obtain nano-zirconia powder. However, acrylamide is prone to chelation with cations such as zirconium salt and yttrium source, which can affect the self-polymerization reaction induced by the initiator in the later stage, making it difficult to control the powder with a specific morphology (such as spherical shape). At the same time, the chelation of acrylamide with cations such as zirconium salt and yttrium source increases the amount of acrylamide added. Moreover, urea and tetramethylethylenediamine need to be added in the experiment, resulting in a variety of raw materials and easy introduction of impurities. Summary of the Invention

[0004] Therefore, the technical problem to be solved by the present invention is to overcome the defects of scandium-zirconium powder prepared by existing technology, such as irregular morphology, difficulty in controlling its spherical shape, excessive types of raw materials used, and low product purity, thereby providing a spherical scandium-zirconium powder, its preparation method and application.

[0005] To this end, the present invention provides the following technical solution.

[0006] The present invention provides a method for preparing spherical scandium-zirconium powder, comprising the following steps: S1: mixing organic monomers, crosslinking agents, and initiators, and carrying out a polymerization reaction to obtain a gel; wherein the organic monomers are carbon-carbon double bond monomers; S2: mixing the gel obtained in S1 with a scandium-zirconium mixed solution, so that ions in the scandium-zirconium mixed solution migrate into the gel, and drying to obtain a dry gel; S3: calcining the dry gel obtained in S2 in two steps to obtain spherical scandium-zirconium powder; wherein the atmosphere of the first calcination step is an inert atmosphere, and the atmosphere of the second calcination step is an oxygen-containing atmosphere.

[0007] Optionally, in step S1, the mass ratio of organic monomer, crosslinking agent, and initiator is 1:0.01-0.08:0.0005-0.009; preferably, the mass ratio of organic monomer, crosslinking agent, and initiator is 1:0.01-0.06:0.001-0.009.

[0008] Optionally, in step S1, the organic monomer and crosslinking agent are dissolved in deionized water, and an initiator is added at 30-80°C to carry out the reaction; preferably, the initiator is added at 30-45°C to carry out the reaction, specifically, but not limited to, 30°C, 32°C, 34°C, 36°C, 38°C, 40°C, and 42°C.

[0009] Optionally, the liquid-solid mass ratio of deionized water to organic monomer and crosslinking agent is 10 to 35:1; preferably, the liquid-solid mass ratio is 15 to 25:1.

[0010] Optionally, the concentration of metal ions in the scandium-zirconium mixed solution is ≥0.5 mol / L; preferably, the concentration of metal ions in the scandium-zirconium mixed solution is 2.5 to 8 mol / L, which is conducive to the rapid migration of ions into the three-dimensional network structure of the gel. When the concentration is low, the diffusion kinetics are insufficient, which is not conducive to the migration of ions, while when the concentration is high, waste is likely to occur.

[0011] Preferably, the molar ratio of zirconium ions to scandium ions in the scandium-zirconium mixed solution is 89:16 to 22.

[0012] Preferably, the scandium-zirconium mixed solution further includes doped metal ions, the doped metal ions including Y 3+ Ce 3+ Al 3+ Yb 3+ Ca3+ At least one of them.

[0013] Preferably, the molar ratio of zirconium ions to doped metal ions in the scandium-zirconium mixed solution is 89:0.5 to 2.

[0014] Preferably, in step S2, the mass of the organic monomer, crosslinking agent, and initiator is 0.01% to 0.5% of the mass of the solute in the scandium-zirconium mixed solution.

[0015] Optionally, in step S3, the calcination temperature of the first step is 300-500℃, the calcination temperature of the second step is 500-800℃, and the calcination time of each step is 1-10h; preferably, the calcination time of each step is 2-5h.

[0016] Optionally, in step S2, the method for migrating ions from the scandium-zirconium mixed solution into the gel includes one or more of standing, heating, centrifugation, and sonication, for a time of 1–48 h; preferably, the method for migrating ions from the scandium-zirconium mixed solution into the gel includes one or a combination of centrifugation and sonication; preferably, the time for migrating ions from the scandium-zirconium mixed solution into the gel is 3–10 h. Optionally, when using heating to migrate ions from the scandium-zirconium mixed solution into the gel, the heating temperature is 30–55 °C, and should be lower than the temperature at which the initiator is added in step S1 for the reaction; preferably, when using heating to migrate ions from the scandium-zirconium mixed solution into the gel, the heating temperature is 30–45 °C.

[0017] Preferably, the carbon-carbon double bond monomer includes at least one of acrylamide, vinyl alcohol, and vinyl acetic acid.

[0018] Preferably, the crosslinking agent includes at least one of polyethylene glycol, polypropylene glycol, trimethylolpropane, trimethylolethane, N,N-methylenebisacrylamide, hydroxyethyl methacrylate, hydroxypropyl methacrylate, N-hydroxymethylacrylamide, and diacetone acrylamide.

[0019] Preferably, the initiator includes at least one of ammonium persulfate, potassium persulfate, and sodium persulfate.

[0020] The method for preparing spherical scandium-zirconium powder provided by the present invention uses nitrates or chlorides of various metals, preferably nitrates, when preparing the scandium-zirconium mixed solution.

[0021] In the method for preparing spherical scandium-zirconium powder provided by the present invention, optionally, in step S2, the drying temperature is 80-120℃ and the drying time is 1-5h; preferably, the drying time is 1-3h.

[0022] The method for preparing spherical scandium-zirconium powder provided by the present invention can be as follows: (1) Weigh organic monomers, crosslinking agents and initiators in a mass ratio of 1:0.01~0.06:0.001~0.009, dissolve organic monomers and crosslinking agents in deionized water, the liquid-solid mass ratio of deionized water to organic monomers and crosslinking agents is 10~35:1, heat to 30~80℃, add initiator to react, and make the solution rapidly polymerize into a transparent polymer gel; (2) Prepare a scandium-zirconium mixed solution in a molar ratio of zirconium ions, anti-ions and doped metal ions of 89:16~22:0.5~2, wherein the concentration of metal ions is ≥0.5mol / L; (3) Mix the gel prepared in (1) and the gel prepared in (2). The obtained scandium-zirconium mixed solution is controlled to have the mass of organic monomer, crosslinking agent and initiator controlled to be 0.01% to 0.5% of the mass of solute in the scandium-zirconium mixed solution. The solution is treated by one or more of the following methods: standing, heating, centrifugation and sonication, so that the ions in the scandium-zirconium mixed solution migrate into the gel. The treatment time is 1 to 48 hours. Then, the solution is dried at 80 to 120°C for 1 to 5 hours to obtain a dry gel. (4) The dry gel obtained in (3) is calcined in two steps. The first step of calcination is carried out in an inactive atmosphere at a temperature of 300 to 500°C for 1 to 10 hours. The second step of calcination is carried out in an oxygen-containing atmosphere at a temperature of 500 to 800°C for 1 to 10 hours to obtain spherical scandium-zirconium powder.

[0023] The present invention also provides a spherical scandium-zirconium powder prepared by the above preparation method.

[0024] The present invention also provides the application of the above-mentioned spherical scandium-zirconium powder in solid oxide fuel cells.

[0025] The beneficial effects of this invention are:

[0026] The present invention provides a method for preparing spherical scandium-zirconium powder, comprising the following steps: S1: mixing organic monomers, crosslinking agents, and initiators, and carrying out a polymerization reaction to obtain a gel; wherein the organic monomers are carbon-carbon double bond monomers; S2: mixing the gel obtained in S1 with a scandium-zirconium mixed solution, allowing ions in the scandium-zirconium mixed solution to migrate into the gel, and drying to obtain a dry gel; S3: calcining the dry gel obtained in S2 in two steps to obtain spherical scandium-zirconium powder; wherein the atmosphere for the first calcination step is an inert atmosphere, and the atmosphere for the second calcination step is an oxygen-containing atmosphere. This preparation method is simple, requires low-level equipment, is low-cost, and is easy to industrialize; it can successfully prepare scandium-zirconium powder with good dispersibility and spherical appearance, with a particle size in the submicron range, and the obtained product has high purity. In the preparation process, under the action of an initiator, organic monomers and cross-linking agents polymerize to form chains. These chains then intertwine and connect to form a three-dimensional network structure of gel. After mixing with a scandium-zirconium mixed solution, ions from the solution migrate into the three-dimensional network structure of the gel, causing it to react within a confined area. This prevents the scandium-zirconium metal salt from agglomerating during calcination and results in spherical powder particles. Forming the gel structure first, followed by the addition of the scandium-zirconium mixed solution, prevents the solution from chelating with the organic monomers and affecting gel formation, thus mitigating the confinement effect and facilitating control of powder morphology. Simultaneously, it avoids the use of other additives and alkaline precipitants, reducing costs and improving product purity. In the final stepwise calcination process, the first calcination is conducted in a non-reactive atmosphere, while the second calcination is conducted in an oxygen-containing atmosphere. This helps prevent rapid oxidation of the gel, which would cause the three-dimensional network structure to disappear quickly, leading to particle agglomeration and the formation of a plate-like structure. Attached Figure Description

[0027] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0028] Figure 1 This is a SEM image of scandium-zirconium powder obtained in Example 1 of the present invention;

[0029] Figure 2 This is a SEM image of scandium-zirconium powder prepared in Comparative Example 1 of this invention;

[0030] Figure 3 This is a SEM image of the scandium-zirconium powder prepared in Comparative Example 2 of this invention. Detailed Implementation

[0031] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0032] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0033] Example 1

[0034] This embodiment provides a spherical scandium-zirconium powder and its preparation method, including the following steps:

[0035] (1) Weigh the organic monomer acrylamide monomer, the crosslinking agent N,N-methylenebisacrylamide and the initiator ammonium persulfate according to the mass ratio of 1:0.05:0.002. Dissolve the organic monomer acrylamide monomer and the crosslinking agent N,N-methylenebisacrylamide in a certain amount of deionized water with a liquid-solid mass ratio of 20:1. Heat to 45℃ and add the initiator ammonium persulfate to react, so that the solution rapidly polymerizes into a transparent polymer gel.

[0036] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxynitrate solution, scandium nitrate solution and cerium nitrate solution at a metal ion molar ratio of 89:20:1, wherein the concentration of metal ions is 8 mol / L;

[0037] (3) Mix the gel prepared in (1) and the scandium-zirconium mixed solution prepared in (2), and control the mass of organic monomer, crosslinking agent and initiator to be 0.01% of the mass of solute in the scandium-zirconium mixed solution; heat at 35°C for 3 hours and let stand for 5 hours to allow ions in the scandium-zirconium mixed solution to migrate into the gel; then dry at 100°C for 3 hours to obtain a dry gel;

[0038] (4) The dry gel obtained in (3) was calcined in two steps. The atmosphere of the first step was nitrogen, the temperature was 400℃ and the time was 4h. The atmosphere of the second step was air, the temperature was 650℃ and the time was 4h, to obtain spherical scandium zirconium powder.

[0039] Example 2

[0040] This embodiment provides a spherical scandium-zirconium powder and its preparation method, including the following steps:

[0041] (1) Weigh the organic monomer ethylene alcohol monomer, the crosslinking agent polyethylene glycol and the initiator ammonium persulfate according to the mass ratio of 1:0.01:0.001. Dissolve the organic monomer ethylene alcohol monomer and the crosslinking agent polyethylene glycol in a certain amount of deionized water. The liquid-solid mass ratio is 25:1. Heat to 30°C and add the initiator ammonium persulfate to react, so that the solution is rapidly polymerized into a transparent polymer gel.

[0042] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxynitrate solution, scandium nitrate solution and yttrium nitrate solution at a metal ion molar ratio of 89:19:1.5, wherein the concentration of metal ions is 2.5 mol / L;

[0043] (3) Mix the gel prepared in (1) and the scandium-zirconium mixed solution prepared in (2), and control the mass of organic monomer, crosslinking agent and initiator to be 0.1% of the mass of solute in the scandium-zirconium mixed solution; sonicate for 3 h to allow ions in the scandium-zirconium mixed solution to migrate into the gel; then dry at 80 °C for 5 h to obtain dry gel;

[0044] (4) The dry gel obtained in (3) was calcined in two steps. The first step of calcination was carried out in an argon atmosphere at a temperature of 500℃ for 1 hour. The second step of calcination was carried out in an air atmosphere at a temperature of 800℃ for 1 hour to obtain spherical scandium zirconium powder.

[0045] Example 3

[0046] This embodiment provides a spherical scandium-zirconium powder and its preparation method, including the following steps:

[0047] (1) Weigh the organic monomer vinylacetic acid monomer, the crosslinking agent trimethylol ethane and the initiator potassium persulfate according to the mass ratio of 1:0.06:0.009. Dissolve the organic monomer vinylacetic acid monomer and the crosslinking agent trimethylol ethane in a certain amount of deionized water with a liquid-solid mass ratio of 35:1. Heat to 40°C and add the initiator potassium persulfate to react, so that the solution can be rapidly polymerized into a transparent polymer gel.

[0048] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxychloride solution, scandium chloride solution and aluminum chloride solution at a metal ion molar ratio of 89:20:1, wherein the concentration of metal ions is 3 mol / L;

[0049] (3) Mix the gel prepared in (1) and the scandium-zirconium mixed solution prepared in (2), and control the mass of organic monomer, crosslinking agent and initiator to be 0.5% of the mass of solute in the scandium-zirconium mixed solution; centrifuge for 1 h to allow the ions in the scandium-zirconium mixed solution to migrate into the gel; then dry at 120°C for 1 h to obtain dry gel;

[0050] (4) The dry gel obtained in (3) is calcined in two steps. The atmosphere of the first step is nitrogen, the temperature is 300℃ and the time is 10h. The oxygen volume fraction in the atmosphere of the second step is ≥99.5%, the temperature is 500℃ and the time is 8h, to obtain spherical scandium zirconium powder.

[0051] Example 4

[0052] This embodiment provides a spherical scandium-zirconium powder and its preparation method, including the following steps:

[0053] (1) Weigh the organic monomer acrylamide monomer, the crosslinking agent hydroxypropyl methacrylate and the initiator sodium persulfate according to the mass ratio of 1:0.03:0.005. Dissolve the organic monomer acrylamide monomer and the crosslinking agent hydroxypropyl methacrylate in a certain amount of deionized water with a liquid-solid mass ratio of 10:1. Heat to 45°C and add the initiator sodium persulfate to react, so that the solution can be rapidly polymerized into a transparent polymer gel.

[0054] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxynitrate solution, scandium nitrate solution and cerium nitrate solution at a metal ion molar ratio of 89:18:2, wherein the concentration of metal ions is 5 mol / L;

[0055] (3) Mix the gel prepared in (1) and the scandium-zirconium mixed solution prepared in (2), and control the mass of organic monomer, crosslinking agent and initiator to be 0.3% of the mass of solute in the scandium-zirconium mixed solution; let stand for 48 h to allow the ions in the scandium-zirconium mixed solution to migrate into the gel; then dry at 90 °C for 4 h to obtain dry gel;

[0056] (4) The dry gel obtained in (3) was calcined in two steps. The atmosphere of the first step was nitrogen, the temperature was 450℃ and the time was 3h. The atmosphere of the second step was air, the temperature was 700℃ and the time was 4h, to obtain spherical scandium zirconium powder.

[0057] Example 5

[0058] This embodiment provides a spherical scandium-zirconium powder and its preparation method. The difference from Embodiment 1 is that the concentration of metal ions in the scandium-zirconium mixed solution prepared in step (2) is 0.5 mol / L.

[0059] Example 6

[0060] This embodiment provides a spherical scandium-zirconium powder and its preparation method. The difference from Embodiment 1 is that in step (1), the organic monomer acrylamide monomer, the crosslinking agent N,N-methylenebisacrylamide and the initiator ammonium persulfate are weighed in a mass ratio of 1:0.08:0.0005. After dissolving the organic monomer and the crosslinking agent, the temperature is raised to 80°C and the initiator ammonium persulfate is added to carry out the reaction.

[0061] Example 7

[0062] This embodiment provides a spherical scandium-zirconium powder and its preparation method, including the following steps:

[0063] (1) Weigh acrylamide monomer, crosslinking agent N,N-methylenebisacrylamide and initiator ammonium persulfate in a mass ratio of 1:0.03:0.002. Dissolve acrylamide monomer and crosslinking agent N,N-methylenebisacrylamide in a certain amount of deionized water with a liquid-solid mass ratio of 15:1. Heat to 55°C and add initiator ammonium persulfate to react, so that the solution rapidly polymerizes into a transparent polymer gel.

[0064] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxynitrate solution and scandium nitrate solution at a metal ion molar ratio of 9:2, wherein the concentration of metal ions is 6 mol / L;

[0065] (3) Mix the gel prepared in (1) and the scandium-zirconium mixed solution prepared in (2), and control the mass of organic monomer, crosslinking agent and initiator to be 0.05% of the mass of solute in the scandium-zirconium mixed solution; heat at 40°C for 3 hours and let stand for 7 hours to allow ions in the scandium-zirconium mixed solution to migrate into the gel; then dry at 100°C for 3 hours to obtain a dry gel;

[0066] (4) The dry gel obtained in (3) was calcined in two steps. The atmosphere of the first step was nitrogen, the temperature was 400℃ and the time was 4h. The atmosphere of the second step was air, the temperature was 650℃ and the time was 4h, to obtain spherical scandium zirconium powder.

[0067] Comparative Example 1

[0068] This comparative example provides a scandium-zirconium powder and its preparation method, including the following steps:

[0069] (1) Weigh the organic monomer acrylamide monomer, the crosslinking agent N,N-methylenebisacrylamide and the initiator ammonium persulfate according to the mass ratio of 1:0.05:0.002. Dissolve the organic monomer acrylamide monomer and the crosslinking agent N,N-methylenebisacrylamide in a certain amount of deionized water with a liquid-solid mass ratio of 20:1 and heat to 45℃.

[0070] (2) Prepare a scandium-zirconium mixed solution by mixing zirconium oxynitrate solution, scandium nitrate solution and cerium nitrate solution at a metal ion molar ratio of 89:20:1, wherein the concentration of metal ions is 8 mol / L;

[0071] (3) Mix the mixture obtained in (1) and the scandium-zirconium mixed solution prepared in (2), add ammonium persulfate as an initiator to react, and rapidly polymerize it into a transparent polymer gel. Control the mass of organic monomer, crosslinking agent, initiator gel to be 0.01% of the mass of solute in the scandium-zirconium mixed solution, and then dry it at 100°C for 3 hours to obtain a dry gel.

[0072] (4) The dry gel obtained in (3) was calcined in two steps. The first step was calcined in a nitrogen atmosphere at a temperature of 400℃ for 4 hours. The second step was calcined in an air atmosphere at a temperature of 650℃ for 4 hours to obtain scandium zirconium powder with irregular morphology.

[0073] Comparative Example 2

[0074] This comparative example provides a scandium-zirconium powder and its preparation method. The difference from Example 1 is that the atmosphere for calcination in the first step (4) is also air.

[0075] Test Example 1

[0076] The scandium-zirconium powders obtained in the examples and comparative examples were subjected to SEM observation. The SEM image of the scandium-zirconium powder obtained in Example 1 is shown below. Figure 1 As shown, the SEM images of scandium-zirconium powder obtained in the other embodiments are similar to those in Example 1, and will not be listed here one by one; Figure 2 The image shows a SEM image of scandium-zirconium powder obtained in Comparative Example 1. Figure 3 This is for comparative example 2.

[0077] As can be seen, the scandium-zirconium powder prepared using the method of this invention with optimized parameters in the examples exhibits good dispersibility and a perfect spherical shape. In contrast, the scandium-zirconium powder prepared in Comparative Example 1 without following the preparation steps of this invention has a completely irregular morphology; the scandium-zirconium powder prepared in Comparative Example 2 without distinguishing between the two calcination atmospheres is directly in the form of flakes with a length and width of approximately several micrometers and a thickness of tens of nanometers. The preparation method of this invention can produce well-dispersed spherical scandium-zirconium powder.

[0078] Test Example 2

[0079] The particle size D50 of the scandium-zirconium powder prepared in the examples and comparative examples was tested using a Malvern MASTERSIZER3000 laser particle size analyzer. The results are shown in Table 1.

[0080] Test Example 3

[0081] The content of impurity elements was determined by inductively coupled plasma (ICP) to calculate the purity of scandium-zirconium powder prepared in the test examples and comparative examples. The results are shown in Table 1.

[0082] Test Example 4

[0083] Weigh and calculate the yield, yield = actual output / theoretical output. The results are shown in Table 1.

[0084] Table 1

[0085] Particle size D50 (μm) purity(%) Yield (%) Example 1 0.40 99.99 98.5 Example 2 0.51 99.97 97.5 Example 3 0.43 99.95 97.8 Example 4 0.58 99.99 98.0 Example 5 0.48 99.99 40 Example 6 0.55 99.92 98.3 Example 7 0.45 99.98 98.4 Comparative Example 1 0.9 97 98.1 Comparative Example 2 - 99.95 98.2

[0086] Analysis of the data in Table 1 shows that the scandium-zirconium powder prepared using the method of the present invention in the examples has a small particle size and very high purity. In particular, the preparation parameters used in Example 1 are all optimal values, resulting in the smallest particle size, highest purity, and highest yield of the scandium-zirconium powder. Comparing Example 5 and Example 1, it can be seen that compared with the scandium-zirconium powder prepared using the optimal parameters in Example 1, the concentration of metal ions in the scandium-zirconium mixed solution used in Example 5 is only 0.5 mol / L. This results in insufficient diffusion kinetics during preparation, which is not conducive to ion migration, ultimately leading to a yield of only 40%. In Comparative Example 1, a scandium-zirconium mixed solution is first added to a mixture of organic monomers and crosslinking agents, and then an initiator is added to react and form a gel. The resulting scandium-zirconium powder has a larger particle size, irregular morphology, and contains some impurities, resulting in lower purity. In Comparative Example 2, during the stepwise calcination, the calcination atmosphere in the first step was also air. While the purity of the resulting scandium-zirconium powder remained unaffected, its morphology was flake-like and its size was extremely large, failing to meet application requirements. The scandium-zirconium powder preparation method provided by this invention can successfully prepare scandium-zirconium powder with good dispersibility and a spherical morphology, with a submicron particle size, and the obtained product has very high purity.

[0087] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for producing a spherical scandium zirconium powder, characterized by, Includes the following steps: S1: Mix organic monomers, crosslinking agents, and initiators to carry out a polymerization reaction and obtain a gel; The organic monomer is a carbon-carbon double bond monomer; S2: The gel obtained in S1 is mixed with a scandium-zirconium mixed solution to allow ions in the scandium-zirconium mixed solution to migrate into the gel. The mixture is then dried to obtain a dry gel. S3: The dry gel obtained in S2 by two-step calcination yields spherical scandium-zirconium powder; The first calcination step is conducted in an inert atmosphere, while the second calcination step is conducted in an oxygen-containing atmosphere.

2. The method for preparing spherical scandium-zirconium powder according to claim 1, characterized in that, In step S1, the mass ratio of organic monomer, crosslinking agent, and initiator is 1:0.01~0.08:0.0005~0.

009.

3. The method for preparing spherical scandium-zirconium powder according to claim 2, characterized in that, The mass ratio of organic monomer, crosslinking agent, and initiator is 1:0.01~0.06:0.001~0.

009.

4. The method for preparing spherical scandium-zirconium powder according to any one of claims 1 to 3, characterized in that, In step S1, the organic monomer and crosslinking agent are dissolved in deionized water, and an initiator is added at 30~80°C to carry out the reaction.

5. The method for preparing spherical scandium-zirconium powder according to claim 4, characterized in that, An initiator is added at 30-45℃ to carry out the reaction.

6. The method for preparing spherical scandium-zirconium powder according to claim 4, characterized in that, The liquid-solid mass ratio of deionized water to organic monomers and crosslinking agents is 10~35:

1.

7. The method for preparing spherical scandium-zirconium powder according to claim 6, characterized in that, The liquid-to-solid mass ratio is 15~25:

1.

8. The method for preparing spherical scandium-zirconium powder according to claim 1, characterized in that, The concentration of metal ions in the scandium-zirconium mixed solution is ≥0.5 mol / L; And / or, the molar ratio of zirconium ions to scandium ions in the scandium-zirconium mixed solution is 89:16~22; and / or, the scandium-zirconium mixed solution further comprises a dopant metal ion, the dopant metal ion comprising at least one of Y 3+ , Ce 3+ , Al 3 + , Yb 3+ , Ca 2+ .

9. The method for preparing spherical scandium-zirconium powder according to claim 8, characterized in that, The concentration of metal ions in the scandium-zirconium mixed solution is 2.5~8 mol / L.

10. The method for preparing spherical scandium-zirconium powder according to claim 8, characterized in that, The molar ratio of zirconium ions to doped metal ions in the scandium-zirconium mixed solution is 89:0.5~2.

11. The method for preparing spherical scandium-zirconium powder according to any one of claims 1 to 3, characterized in that, In step S2, the mass of the organic monomer, crosslinking agent, and initiator is 0.01% to 0.5% of the mass of the solute in the scandium-zirconium mixed solution.

12. The method for preparing spherical scandium-zirconium powder according to any one of claims 1 to 3, characterized in that, In step S3, the first calcination temperature is 300~500℃, the second calcination temperature is 500~800℃, and the calcination time for each step is 1~10h. And / or, in step S2, the method for migrating ions in the scandium-zirconium mixed solution to the gel includes one or more of the following: standing, heating, centrifugation, and sonication, for a time of 1 to 48 hours.

13. The method for preparing spherical scandium-zirconium powder according to claim 12, characterized in that, In step S3, the calcination time for each step is 2-5 hours.

14. The method for preparing spherical scandium-zirconium powder according to claim 12, characterized in that, In step S2, the method for migrating ions from the scandium-zirconium mixed solution into the gel includes one or both of centrifugation and sonication.

15. The method for preparing spherical scandium-zirconium powder according to claim 12, characterized in that, In step S2, the time for ions in the scandium-zirconium mixed solution to migrate into the gel is 3 to 10 hours.

16. The method for preparing spherical scandium-zirconium powder according to any one of claims 1 to 3, characterized in that, The carbon-carbon double bond monomers include at least one of acrylamide and vinylacetic acid; And / or, the crosslinking agent includes polyethylene glycol, polypropylene glycol, trimethylolpropane, trimethylolpropane, N,N At least one of methylenebisacrylamide, hydroxyethyl methacrylate, hydroxypropyl methacrylate, N-hydroxymethylacrylamide, and diacetone acrylamide; And / or, the initiator includes at least one of ammonium persulfate, potassium persulfate, and sodium persulfate.

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