Staggered magnet FeAl2Li2O5 and method of making

Abstract

The application discloses a preparation method of staggered magnet FeAl2Li2O5 and belongs to the technical field of inorganic non-metallic materials. The raw materials are crushed to prepare glaze slurry; the obtained glaze slurry is applied to a blank to perform glazing treatment and is dried to prepare a blank containing a glaze layer; the obtained blank containing the glaze layer is sintered at high temperature and is cooled to prepare a solid product; the obtained solid product is washed and dried to obtain novel staggered magnet FeAl2Li2O5; wherein the raw materials comprise the following components: feldspar, quartz, calcite, lepidolite, lithium carbonate, talc, kaolin, aluminum oxide and an iron source, the iron source comprising at least one of purple clay, ferric oxide and ferric oxide. The application can stably synthesize novel staggered magnet FeAl2Li2O5, can obtain particles with uniform size and uniform distribution, and has the advantages of simple preparation method, low cost, non-toxic raw materials and mild preparation conditions.

Description

Technical Field

[0001] This invention relates to the field of inorganic non-metallic materials technology, specifically to an interlaced magnet FeAl2Li2O5 and its preparation method. Background Technology

[0002] Interleaved magnets are a new class of magnetic materials whose spin structures are interconnected through unique spatial rotation operations. While maintaining zero macroscopic net magnetization and crystal centrosymmetry, they can generate huge band spin splitting in momentum space, providing an important direction for symmetry-based engineering design and the discovery of novel spintronic materials. FeAl₂Li₂O₅, as a novel interleaved magnet, has attracted great attention from researchers in ancient ceramics and magnetic materials. In this phase, the magnetic sublattices with opposite spins are interconnected through unique spatial rotation operations, exhibiting magnetic characteristics that are distinctly different from traditional antiferromagnets.

[0003] Currently, the preparation of FeAl₂Li₂O₅ materials mainly relies on crystals that are accidentally formed in the glaze of ancient porcelain, lacking a systematic and controllable synthesis method. Existing preparation techniques face the following technical challenges: first, the raw material ratio is difficult to control precisely, resulting in numerous impurity phases and low purity of the target phase in the reaction products; second, unreasonable sintering process parameters make it difficult to form a single, uniform FeAl₂Li₂O₅ crystal; and third, the products often contain a large amount of amorphous silicon matrix and other impurity phases, making separation and purification difficult. These technical obstacles lead to low yields and poor reproducibility in the preparation of FeAl₂Li₂O₅ materials, severely restricting further research and application of this material. Therefore, developing a simple, low-cost method for the stable preparation of high-purity FeAl₂Li₂O₅ is a key technical problem urgently needing to be solved in this field. Summary of the Invention

[0004] To address the problems existing in the prior art, the present invention provides an interleaved magnet FeAl2Li2O5 and its preparation method, wherein the interleaved magnet FeAl2Li2O5 is constructed through a solid-state reaction.

[0005] This invention is achieved through the following technical solution: A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Mix 7%~24% feldspar, 12.6%~49% quartz, 3.8%~5% calcite, 1%~3% lepidolite, 1.6%~5% talc and 1%~3% lithium carbonate by mass percentage to obtain the glaze. Step 2: Apply the glaze to the surface of the substrate and allow it to dry to form a glaze layer; Step 3: The substrate with the glaze layer is sintered at high temperature to form interlaced FeAl2Li2O5 crystals in the glaze layer.

[0006] Preferably, the glaze in step 1 further includes an iron source, which includes at least one of aluminum oxide, purple clay, kaolin, ferric oxide, and magnetite.

[0007] Preferably, the glaze further comprises, by mass percentage, at least one of the following: 0-15% aluminum oxide, 0-73% purple clay, 0-2% kaolin, 0-5% ferric oxide, and 0-5% magnetite.

[0008] Preferably, after mixing in step 1, wet ball milling is performed at a speed of 300~350 r / min and a time of 30~45 min.

[0009] Preferably, in the wet ball milling process, the volume ratio of raw material to water is 1:0.8~1.

[0010] Preferably, the substrate in step 2 is a heat-resistant material with a temperature resistance greater than 1300℃.

[0011] Preferably, in step 2, the glaze is applied to the substrate surface using an immersion glaze method or a drip glaze method, and the thickness of the glaze layer is 1.5~2 mm.

[0012] Preferably, the high-temperature sintering in step 3 employs multi-stage heating: First, raise the temperature to 400-450℃ at a heating rate of 3-5℃ / min, then raise it to 1100-1150℃ at a heating rate of 3℃ / min, then raise it to 1280-1300℃ at a heating rate of 1℃ / min, and finally hold it at 1280-1300℃ for 2-3 hours.

[0013] Preferably, step 3 is followed by an etching process: the sintered product is etched with sodium hydroxide solution to peel off the interlaced magnet from the substrate, and after collection, it is washed and dried to obtain the interlaced magnet FeAl2Li2O5.

[0014] An interleaved magnet FeAl2Li2O5 is prepared using the method described above. The interleaved magnet FeAl2Li2O5 has a butterfly-shaped crystal structure with dendritic crystals encapsulated by an amorphous silicon matrix distributed on the crystal surface. The crystal contains iron, aluminum and lithium elements, and the iron and aluminum elements are uniformly distributed in the crystal.

[0015] Compared with the prior art, the present invention has the following beneficial technical effects: This invention discloses a novel method for preparing interleaved magnet FeAl₂Li₂O₅. Using feldspar, quartz, calcite, or talc as the glaze substrate, an iron source is added and the mixture is sintered at high temperature. Impurities are removed from the product through etching, avoiding complex separation and impurity removal processes. Furthermore, the iron source selected in this invention can be purple clay, iron(III) oxide, or iron(II) oxide, effectively reducing the cost of the preparation method. Therefore, the preparation method described in this invention stably synthesizes FeAl₂Li₂O₅, yielding FeAl₂Li₂O₅ particles. This preparation method has advantages such as simple process, low cost, non-toxic raw materials, and mild preparation conditions.

[0016] Furthermore, adding aluminum oxide to the raw materials can adjust the Al / Si ratio in the reaction and reduce the amount of SiO2 impurities generated.

[0017] Furthermore, by adjusting the amount of water, the ball milling time, and the glaze thickness, the components in the mixed glaze slurry can be evenly distributed, resulting in a thorough sintering reaction and a reduction in the types of impurities in the resulting product.

[0018] Furthermore, by using multi-stage heating, it is possible to obtain uniform and stable single FeAl2Li2O5.

[0019] Furthermore, by using an alkaline sodium hydroxide solution to etch away the main impurity phase SiO2 in the product, a single, stable FeAl2Li2O5 was obtained in a specific embodiment of the present invention. The present invention prepares a single, uniform FeAl2Li2O5 through a solid-state reaction. Attached Figure Description

[0020] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a super-depth-of-field image of the interlaced magnet FeAl2Li2O5 of this invention; Figure 2 This is a SEM image of the interleaved magnet FeAl2Li2O5 of this invention; Figure 3 This is the EDS image of the interleaved magnet FeAl2Li2O5 of this invention; Figure 4 This is an ICP-MS image of the interleaved magnet FeAl2Li2O5 of this invention. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. The components of the embodiments of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0023] Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments of the application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0024] A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Prepare the interlaced magnet glaze; By mass percentage, 7%~24% feldspar, 12.6%~49% quartz, 3.8%~5% calcite, 1%~3% lepidolite, 1.6%~5% talc and 1~3 wt% lithium carbonate are mixed in a certain proportion to obtain the interlaced magnet glaze. Step 2: Load the interlaced magnet glaze onto the substrate; Step 3: The substrate loaded with the interlaced magnet glaze is sintered at high temperature to obtain interlaced magnet FeAl2Li2O5.

[0025] This preparation method achieves element diffusion and crystal structure reconstruction during high-temperature sintering via solid-state reaction, forming a FeAl2Li2O5 phase with interlaced magnetism. Specifically, feldspar, quartz, calcite, and talc are used as glaze substrates, melting at high temperatures to form a liquid silicate glass phase, providing a liquid environment for the reaction. Lithium mica and lithium carbonate decompose during sintering to generate lithium ions, serving as the lithium source in the target phase. Aluminum and iron elements in each component synergistically interact with lithium ions at high temperatures, undergoing diffusion, nucleation, and crystal growth in the silicate glass phase. By controlling the raw material ratio to maintain an appropriate Al / Si ratio in the reaction system, the formation of impurity SiO2 is reduced, ultimately resulting in the precipitation of uniformly sized and well-distributed FeAl2Li2O5 crystals in the glaze layer. This process combines traditional ceramic glaze-making techniques with solid-state synthesis, utilizing the melting and flow characteristics of the glaze at high temperatures to promote uniform element diffusion. By controlling the raw material composition and sintering conditions, the target phase is selectively precipitated in the glass matrix, achieving stable preparation of interlaced magnets.

[0026] In some embodiments, the interlaced magnet glaze further includes an iron source; The iron source includes at least one or more of aluminum oxide, purple clay, kaolin, ferric oxide, and iron(II,III) oxide.

[0027] For example, the interlaced magnet glaze includes 7%~24% feldspar, 12.6%~49% quartz, 3.8%~5% calcite, 1%~3% lepidolite, 1.6%~5% talc, 1~3 wt% lithium carbonate and 0~15% iron source; The iron source includes 0-15% aluminum oxide, 0-73% purple clay, 0-2% kaolin, 0-5% ferric oxide and / or 0-5% iron tetroxide.

[0028] Feldspar, as a basic component of glaze, contains potassium and sodium oxides that form flux at high temperatures, reducing the melting temperature of the glaze, promoting the formation of the liquid phase, and providing a melting medium environment for the solid-phase reaction. At the same time, feldspar provides alumina and silicon oxide, which participate in the lattice construction of the target phase FeAl2Li2O5.

[0029] Quartz primarily provides silicon dioxide, which, after melting at high temperatures, forms a silicate glass phase framework that serves as a reaction carrier. Simultaneously, by controlling the Al / Si ratio, excess SiO2 is prevented from precipitating as an impurity phase, ensuring the purity of the target phase.

[0030] Calcite, as a flux, decomposes into calcium oxide and carbon dioxide at high temperatures. Calcium oxide reacts with quartz to form low-melting-point calcium silicate, which further reduces the melting temperature of the glaze, promotes the formation of the liquid phase, and enhances the diffusion capacity of elements.

[0031] Lithium mica, as a lithium source, decomposes at high temperatures to release lithium ions, which participate in the occupation of Li sites in the target phase FeAl2Li2O5; at the same time, the aluminum and silicon components in lepidolite also participate in lattice construction.

[0032] Talc provides magnesium oxide and silicon oxide. Magnesium oxide acts as a mineralizer to promote crystal growth, while also regulating the viscosity and melting characteristics of the glaze, improving the fluidity and uniformity of the glaze layer.

[0033] Lithium carbonate, as a supplementary lithium source, decomposes at high temperatures to generate lithium oxide and carbon dioxide. The lithium oxide reacts with quartz to form low-melting-point lithium silicate, which enhances the melting effect; at the same time, it provides lithium ions to enter the target phase lattice.

[0034] The core role of the iron source in the preparation of FeAl2Li2O5 is to introduce the magnetic element iron into the reaction system, so that iron ions enter the Fe sites in the target phase lattice and form magnetic sublattices with opposite spins, thereby endowing the material with cross-magnetism.

[0035] Iron sources include purple clay, kaolin, ferric oxide, and magnetite. Purple clay and kaolin are natural iron-bearing minerals, inexpensive, and also provide auxiliary components such as aluminum and silicon. Ferric oxide provides high-valence iron ions, while magnetite provides mixed-valence iron ions. The combination of multiple iron sources can regulate the redox balance of the reaction system and promote the stable precipitation of the target phase. During high-temperature sintering, iron ions diffuse in the silicate glass phase and synergistically interact with aluminum and lithium ions to induce selective growth of FeAl2Li2O5 crystals, while suppressing the formation of impurity phases such as olivine and magnetite, ensuring the purity and crystal quality of the target phase.

[0036] In some embodiments, after the raw materials are mixed evenly in proportion in step 1, wet ball milling is performed to obtain the interlaced magnet glaze.

[0037] Specifically, the process of preparing glaze slurry from raw materials after crushing includes: After the components in the raw materials are mixed evenly, water is added and ball milling is performed to obtain the interlaced magnet glaze. The volume ratio of raw materials to water is 1:0.8~1, the ball mill speed is 300~350 r / min, and the ball milling time is 30~45 min.

[0038] In some embodiments, the substrate is a heat-resistant material with a temperature greater than 1300°C.

[0039] The interlaced magnet glaze is loaded onto a heat-resistant substrate and sintered at high temperature to form interlaced magnets on the substrate.

[0040] The substrate must meet a temperature resistance of over 1300℃ to ensure that it does not soften, deform or decompose during high-temperature sintering at 1280-1300℃.

[0041] The heat-resistant matrix includes: clay body, mullite refractories, corundum refractories, high-alumina ceramic plates, zirconia ceramic plates, etc. Selecting a matrix material with a coefficient of thermal expansion similar to that of the glaze can effectively reduce thermal stress and improve the yield rate.

[0042] For example, the glaze of the interlaced magnets is applied to the clay body by dipping or dripping, and the thickness of the glaze layer is 1.5~2mm.

[0043] In some embodiments, the high-temperature sintering in step 3 employs multi-stage heating, as follows: First, raise the temperature to 400℃~450℃ at a heating rate of 3~5℃ / min, then raise it to 1100℃~1150℃ at a heating rate of 3℃ / min, then raise it to 1280~1300℃ at a heating rate of 1℃ / min, and finally hold it at 1280~1300℃ for 2h~3h.

[0044] This multi-stage heating and sintering process achieves the gradual reaction of various components in the glaze and the directional precipitation of the target phase by controlling the heating rate and holding time in stages. The functions of each stage are as follows: The first stage (room temperature to 400℃~450℃, heating rate 3~5℃ / min): This stage is a low-temperature preheating stage. Its main purpose is to slowly expel adsorbed water, crystal water, and gases produced by the decomposition of carbonates and organic matter in the raw materials from the glaze. The slower heating rate can avoid rapid gas release that could cause blistering and cracking of the glaze, while also ensuring a uniform temperature distribution inside the body and reducing the accumulation of thermal stress.

[0045] The second stage (heating from 400℃~450℃ to 1100℃~1150℃ at a rate of 3℃ / min): This stage is the intermediate-temperature melting stage, where raw materials such as feldspar, quartz, calcite, and talc begin to soften and melt, forming a silicate glass liquid phase. The heating rate is controlled at 3℃ / min to ensure that all components are fully melted and uniformly mixed, providing a homogeneous liquid phase environment for subsequent solid-phase reactions, while also promoting the diffusion of lithium ions generated from the decomposition of lepidolite and lithium carbonate in the liquid phase.

[0046] The third stage (heating from 1100℃~1150℃ to 1280~1300℃ at a heating rate of 1℃ / min): This stage is the high-temperature crystallization stage, using an extremely slow heating rate of 1℃ / min to provide sufficient time for the nucleation and growth of FeAl2Li2O5 crystals. Slow heating allows for precise control of supercooling, enabling the crystal to grow slowly within the optimal temperature range, avoiding multiphase co-deposition or coarse grains caused by excessively rapid heating, and ensuring the purity of the target phase and the uniformity of grain size.

[0047] The fourth stage (holding at 1280~1300℃ for 2~3 hours): This stage is the holding and crystallization stage. Holding at the optimal growth temperature of the target phase for an extended period allows the FeAl2Li2O5 crystals to grow fully. Simultaneously, atomic diffusion and grain boundary migration eliminate internal crystal defects, improving crystal integrity and phase purity. Holding for 2~3 hours ensures the reaction proceeds fully, maximizing the target phase content in the glaze while preventing over-sintering that could lead to crystal coarsening or decomposition.

[0048] This multi-stage heating process achieves coordinated regulation of glaze melting, element diffusion, and crystal growth by precisely controlling the heating rate and holding time at each stage. It is a key process guarantee for obtaining high-purity, high-quality FeAl2Li2O5 crystals.

[0049] In some embodiments, step 4 is further included, separating the interlaced magnets from the substrate, as follows: The substrate is etched to separate it from the interlaced magnet. The separated interlaced magnet is washed and dried to obtain the final interlaced magnet FeAl2Li2O5. For example, sodium hydroxide solution is used to etch the sintered products, allowing the interlaced magnets to be collected after peeling off from the substrate.

[0050] The concentration of the sodium hydroxide solution is 4 mol·L⁻¹. -1 The etching time is 2-3 hours.

[0051] The washing and drying process includes washing 3 to 5 times with water and then drying at 60 to 65°C.

[0052] Example 1 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 7% feldspar, 12.6% quartz, 3.8% calcite, 1% lepidolite, 1% lithium carbonate, 1.6% talc, and 73% purple clay by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of material, grinding stone, and water is 1:2:1. Place the mixture in a planetary ball mill and ball mill at 350 r / min for 30 min to obtain the glaze slurry.

[0053] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 2 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0054] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 450℃ at a heating rate of 5℃ / min, then heat to 1150℃ at a heating rate of 3℃ / min, and then heat to 1300℃ at a heating rate of 1℃ / min. Hold at this temperature for 2 hours and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0055] Example 2 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 23% feldspar, 49% quartz, 4% calcite, 1% lepidolite, 1% lithium carbonate, 4% talc, 2% kaolin, 11% alumina and 5% ferric oxide by mass percentage, mix them evenly, add Al2O3 grinding stone and water, the volume ratio of material, grinding stone and water is 1:2:0.8, place in a planetary ball mill and ball mill at 300 r / min for 30 min to obtain glaze slurry.

[0056] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.5 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0057] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 450℃ at a heating rate of 5℃ / min, then heat to 1150℃ at a heating rate of 3℃ / min, then heat to 1300℃ at a heating rate of 1℃ / min, hold for 3 h, and then cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0058] Example 3 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 19% feldspar, 48% quartz, 5% calcite, 2% lepidolite, 2% lithium carbonate, 5% talc, 14% alumina, 2% kaolin, and 3% ferric oxide by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of the material, grinding stone, and water is 1:2:0.9. Place the mixture in a planetary ball mill and ball mill at 320 r / min for 45 min to obtain the glaze slurry.

[0059] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 2 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0060] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 400℃ at a heating rate of 3℃ / min, then heat to 1100℃ at a heating rate of 3℃ / min, and then heat to 1290℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0061] Example 4 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 8% feldspar, 14% quartz, 4% calcite, 1% lepidolite, 1% lithium carbonate, 2% talc, and 70% purple clay by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of material, grinding stone, and water is 1:2:0.9. Place the mixture in a planetary ball mill and ball mill at 320 r / min for 40 min to obtain a glaze slurry.

[0062] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.7 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0063] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 430℃ at a heating rate of 4℃ / min, then heat to 1120℃ at a heating rate of 3℃ / min, and then heat to 1280℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0064] Example 5 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 20% feldspar, 47% quartz, 5% calcite, 1% lepidolite, 3% lithium carbonate, 5% talc, 13% alumina, 1% kaolin, and 5% ferric oxide by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of the material, grinding stone, and water is 1:2:0.85. Place the mixture in a planetary ball mill and ball mill at 330 r / min for 35 min to obtain the glaze slurry.

[0065] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.9 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0066] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 440℃ at a heating rate of 4℃ / min, then heat to 1130℃ at a heating rate of 3℃ / min, and then heat to 1285℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0067] Example 6 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 22% feldspar, 49% quartz, 4% calcite, 2% lepidolite, 1% lithium carbonate, 4% talc, 11% alumina, 2% kaolinite, and 5% iron oxide by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of the material, grinding stone, and water is 1:2:1. Place the mixture in a planetary ball mill and ball mill at 340 r / min for 38 min to obtain the glaze slurry.

[0068] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.5 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0069] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 400℃ at a heating rate of 4℃ / min, then heat to 1140℃ at a heating rate of 3℃ / min, and then heat to 1280℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0070] Example 7 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 20% feldspar, 48% quartz, 5% calcite, 1% lepidolite, 2% lithium carbonate, 5% talc, 14% alumina, 2% kaolinite, and 3% iron oxide by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of the material, grinding stone, and water is 1:2:0.8. Place the mixture in a planetary ball mill and ball mill at 300 r / min for 43 min to obtain the glaze slurry.

[0071] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.7 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0072] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 400℃ at a heating rate of 3℃ / min, then heat to 1100℃ at a heating rate of 3℃ / min, then heat to 1300℃ at a heating rate of 1℃ / min, hold for 3 h, and then cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0073] Example 8 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 15% feldspar, 30% quartz, 4% calcite, 3% lepidolite, 2% lithium carbonate, 3% talc, and 43% purple clay by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of material, grinding stone, and water is 1:2:0.9. Place the mixture in a planetary ball mill and ball mill at 320 r / min for 40 min to obtain the glaze slurry.

[0074] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.8 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0075] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 420℃ at a heating rate of 4℃ / min, then heat to 1120℃ at a heating rate of 3℃ / min, and then heat to 1290℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0076] Example 9 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 12% feldspar, 35% quartz, 4.5% calcite, 2% lepidolite, 2% lithium carbonate, 3% talc, 5% alumina, 1% kaolin, and 2% ferric oxide by mass percentage, with the remainder being purple clay (33.5%). Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of the material, grinding stone, and water is 1:2:0.9. Place the mixture in a planetary ball mill and ball mill at 330 r / min for 42 min to obtain the glaze slurry.

[0077] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.8 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0078] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 430℃ at a heating rate of 4℃ / min, then heat to 1130℃ at a heating rate of 3℃ / min, and then heat to 1295℃ at a heating rate of 1℃ / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0079] Example 10 A method for preparing interleaved magnet FeAl2Li2O5 includes the following steps: Step 1: Weigh out 10% feldspar, 25% quartz, 4% calcite, 2% lepidolite, 2% lithium carbonate, 3% talc, 5% alumina, 1% kaolin, 2% ferric oxide, and 46% purple clay by mass percentage. Mix them evenly, then add Al2O3 grinding stone and water. The volume ratio of material, grinding stone, and water is 1:2:0.9. Place the mixture in a planetary ball mill and ball mill at 320 r / min for 40 min to obtain the glaze slurry.

[0080] Step 2: Apply the glaze slurry obtained in Step 1 to the surface of the unglazed body using either the dipping or dripping method. Repeat the glazing process until the glaze layer reaches a thickness of 1.8 mm. Allow it to dry naturally to obtain a body containing a glaze layer.

[0081] Step 3: Place the dried billet from Step 2 into a muffle furnace and perform high-temperature sintering according to the following multi-stage heating program: start from room temperature and heat to 425°C at a heating rate of 4°C / min, then heat to 1125°C at a heating rate of 3°C / min, and then heat to 1290°C at a heating rate of 1°C / min. Hold at this temperature for 2.5 h and allow to cool naturally with the furnace to obtain interlaced magnet FeAl2Li2O5.

[0082] Example 11 An interleaved magnet, FeAl2Li2O5, has a butterfly-shaped crystal structure with dendritic crystals encapsulated by an amorphous silicon matrix distributed on the crystal surface. The crystal contains iron, aluminum, and lithium elements, with the iron and aluminum elements being uniformly distributed within the crystal.

[0083] Figure 1 This is a super-depth-of-field image of the interlaced magnet FeAl2Li2O5 prepared in an embodiment of the present invention. The image shows a large number of dendritic crystals precipitated on the sample surface. Compositional analysis confirmed that the dendritic crystals are crystalline phases encapsulated in an amorphous silicon matrix.

[0084] Figure 2 The image shows a scanning electron microscope (SEM) image of the interlaced magnet FeAl2Li2O5 prepared according to an embodiment of the present invention. The image shows that the crystals have a butterfly-shaped morphology, and the crystal size is uniform and well distributed.

[0085] Figure 3 The image shows the energy dispersive spectroscopy (EDS) diagram of the interlaced magnet FeAl2Li2O5 prepared in an embodiment of the present invention. The diagram shows that the precipitated butterfly-shaped crystals contain a large amount of iron and aluminum elements, which is consistent with the composition of the target phase FeAl2Li2O5.

[0086] Figure 4 The image shows an inductively coupled plasma mass spectrometry (ICP-MS) spectrum of the interleaved magnet FeAl2Li2O5 prepared in an embodiment of the present invention. The image shows that the sample contains trace amounts of lithium, further verifying the presence of lithium in the target phase.

[0087] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A method for preparing an interlaced magnet FeAl2Li2O5, characterized in that, Includes the following steps: Step 1: Mix 7%~24% feldspar, 12.6%~49% quartz, 3.8%~5% calcite, 1%~3% lepidolite, 1.6%~5% talc and 1%~3% lithium carbonate by mass percentage to obtain the glaze. Step 2: Apply the glaze to the surface of the substrate and allow it to dry to form a glaze layer; Step 3: The substrate with the glaze layer is sintered at high temperature to form interlaced FeAl2Li2O5 crystals in the glaze layer.

2. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 1, characterized in that, The glaze in step 1 also includes an iron source, which includes at least one of aluminum oxide, purple clay, kaolin, ferric oxide, and iron oxide.

3. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 2, characterized in that, The glaze, by mass percentage, also includes at least one of the following: 0-15% aluminum oxide, 0-73% purple clay, 0-2% kaolin, 0-5% ferric oxide, and 0-5% iron oxide.

4. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 1, characterized in that, After mixing as described in step 1, wet ball milling is performed at a speed of 300-350 r / min for a time of 30-45 min.

5. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 4, characterized in that, In the wet ball milling process, the volume ratio of raw material to water is 1:0.8~1.

6. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 1, characterized in that, The substrate mentioned in step 2 is a heat-resistant material with a temperature resistance greater than 1300℃.

7. A method for preparing an interlaced magnet FeAl2Li2O5 according to claim 6, characterized in that, In step 2, the glaze is applied to the substrate surface using either an immersion glaze method or a drip glaze method, and the thickness of the glaze layer is 1.5~2 mm.

8. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 1, characterized in that, The high-temperature sintering described in step 3 employs a multi-stage heating method: First, raise the temperature to 400-450℃ at a heating rate of 3-5℃ / min, then raise it to 1100-1150℃ at a heating rate of 3℃ / min, then raise it to 1280-1300℃ at a heating rate of 1℃ / min, and finally hold it at 1280-1300℃ for 2-3 hours.

9. The method for preparing an interlaced magnet FeAl2Li2O5 according to claim 1, characterized in that, Step 3 is followed by an etching process: the sintered product is etched with sodium hydroxide solution to peel off the interlaced magnet from the substrate. After collection, it is washed and dried to obtain the interlaced magnet FeAl2Li2O5.

10. An interleaved magnet FeAl2Li2O5, characterized in that, The interlaced magnet FeAl2Li2O5, prepared by any one of claims 1 to 9, has a butterfly-shaped crystal structure, with dendritic crystals encapsulated by an amorphous silicon matrix distributed on the crystal surface. The crystal contains iron, aluminum, and lithium elements, and the iron and aluminum elements are uniformly distributed in the crystal.

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