Molten aluminum dislocation reaction process for preparing high-performance alloy material and crystal material

Abstract

The invention relates to the technical field of metal material preparation, in particular to a molten aluminum dislocation reaction process for preparing high-performance alloy materials and crystal materials. A spatial dislocation system is constructed through a microporous inert partition plate, the energy dislocation condition lower than the traditional reaction temperature is controlled, and atomic-scale precise regulation and control are achieved by means of an interface tunneling-lattice self-stitching mechanism. The process is divided into alloy and crystal preparation processes, each process comprises the steps of raw material preparation, dislocation system construction, low-temperature heat preservation reaction and post-treatment, and the material structure is optimized through non-equilibrium nucleation and lattice self-suturing. The process significantly improves the mechanical properties, compactness and purity of the material, reduces energy consumption, can adapt to preparation of various alloys and crystals, and meets the strict requirements of aerospace, semiconductors and other high-end fields for the material.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of metal material preparation, and particularly relates to a molten aluminum dislocation reaction process for preparing high-performance alloy materials and crystal materials. BACKGROUND

[0002] High-performance alloy materials and functional crystal materials are core basic materials in high-end fields such as aerospace, semiconductors and new energy, and their performance directly determines the service life and core indicators of equipment. However, the current preparation technology of the two types of materials still faces an industry bottleneck that is difficult to break through, and cannot meet the comprehensive needs of high-end applications for materials with "high uniformity, low defects and low cost".

[0003] In the field of high-performance alloy preparation, traditional processes have significant limitations. For example, for Ti-Al alloys, the mainstream vacuum melting method is prone to serious composition segregation due to the large difference in melting point between titanium and aluminum (titanium melting point 1668℃, aluminum melting point 660℃), and coarse brittle TiAl3 phases are easily generated at high temperatures, resulting in a significant decrease in alloy plasticity and toughness. The powder metallurgy method needs to go through multiple processes such as pressing and sintering, not only the production cycle is long, but also the density is less than 90% due to powder agglomeration or insufficient sintering, and the alloy oxygen content exceeds the standard during storage and processing, which further deteriorates the mechanical properties. In addition, highly active elements such as zirconium and niobium react violently with aluminum in traditional processes, making it difficult to achieve atomic-level uniform mixing and restricting the performance improvement space of the alloy.

[0004] In the field of high-performance crystal material preparation, traditional technology also faces challenges. For example, for silicon carbide crystals, the widely used solid-phase carbothermal reduction method in industry needs to be carried out at a high temperature of 1800℃ or above, which not only consumes a lot of energy, but also introduces impurities due to carbon diffusion from graphite crucibles. At the same time, the crystal growth rate is difficult to control at high temperatures, and a large number of dislocations and stacking faults are easily generated. The high-temperature melt growth method needs to strictly control the temperature gradient due to the high viscosity and easy decomposition of silicon carbide melt, and the thermal stress generated during the cooling process easily leads to cracking of the crystal, making it difficult to prepare large-size, low-defect crystals. In addition, the traditional preparation processes of aluminum nitride and aluminum oxide crystals also have problems such as high-temperature pollution, high defect density and low production efficiency, which cannot meet the strict requirements of 5G communication and semiconductor packaging for crystal purity and integrity.

[0005] In summary, existing material preparation technologies rely on balanced or near-balanced thermodynamic paths, making it difficult to precisely control atomic-level diffusion, nucleation and growth processes, resulting in shortfalls in material uniformity, density and defect control. Therefore, there is an urgent need in the field for a technical solution that can break through the limitations of traditional processes, achieve precise atomic assembly under mild conditions, and meet the preparation needs of both alloy and crystal materials. SUMMARY

[0006] The object of the present application is to solve the drawbacks existing in the prior art, and the present application provides a molten aluminum misfit reaction process for preparing high-performance alloy materials and crystal materials.

[0007] Based on the above object, the present application provides a molten aluminum misfit reaction process for preparing high-performance alloy materials and crystal materials, comprising the following steps: S1. Reaction process of high-performance alloy materials: S101. Raw material preparation and proportioning: Reactant precursor: composed of at least one high-melting-point metal powder; the high-melting-point metal powder is selected from one or more of titanium, zirconium, niobium, tantalum, nickel, with a purity of not less than 99.5%, and a particle size distribution of 1-100 μm; Aluminum source: high-purity aluminum with a purity of not less than 99.99% is used; S102. Construction of misfit reaction system: In the reaction cavity, high-purity aluminum, microporous inert partition and green body pressed from high-melting-point metal powder are sequentially arranged from top to bottom; the material of the microporous inert partition is boron nitride, aluminum oxide or high-temperature alloy, with a pore size range of 5-50 microns and a porosity of 30%-60%; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 is vacuumed to a pressure of less than 1×10 -2 Pa, then filled with argon, heated to reaction temperature T1 at a heating rate of 5-15 ℃ / min, and kept for 0.5-10 h to obtain a composite material; wherein T1 is a temperature between 50-1000 ℃ above the melting point of aluminum, and T1 is at least 100 ℃ lower than the conventional reaction temperature of the intermetallic compound formed by the high-melting-point metal powder and aluminum; S104. Post-processing: After the reaction is completed, the obtained composite material is cooled, and residual aluminum phase is selectively removed by using an alkaline solution or an acidic solution with a concentration of 5-20 wt% to obtain a high-performance alloy material; S2. Reaction process of high-performance crystal materials: S201. Raw material preparation and proportioning: Reactant precursor: composed of non-metallic powder or compound powder thereof, the non-metallic powder being carbon, silicon, boron powder, and the compound powder being one or more of silicon dioxide, boron nitride, silicon carbide powder, with a purity of not less than 99.9%, and a particle size distribution of 0.1-50 μm; Aluminum source: industrial pure aluminum or aluminum alloy with an aluminum content of not less than 99.0% is used; S202. Construction of misfit reaction system: In the reaction cavity, the aluminum source, the microporous inert partition and the compact pressed by the non-metallic powder or the compound powder of the non-metallic powder are sequentially arranged from top to bottom; the material of the microporous inert partition is boron nitride, graphite or aluminum oxide, the pore size range is 1-20 μm, and the porosity is 20%-50%; S203. Interface tunneling and self-sewing reaction: The reaction cavity in S202 is vacuumized to a pressure lower than 1×10 -2 Pa, then argon is filled, heated to a reaction temperature T2 at a heating rate of 5-20 ℃ / min, and kept for 1-20 h to obtain the crystal material; wherein, T2 is a temperature between 50 ℃ above the melting point of aluminum and 1100 ℃, and T2 is at least 150 ℃ lower than the temperature at which the target crystal is generated by the traditional carbothermal reduction or metallothermic reduction reaction of the non-metallic or the compound thereof; S204. Post-processing: After the reaction, the obtained crystal material is cooled, the generated target crystal material is separated from the aluminum matrix by using an electrochemical stripping method, a physical crushing method or a selective etching method to obtain a high-performance crystal material.

[0008] Preferably, the material of the microporous inert partition is boron nitride.

[0009] Preferably, in S101, the high-melting-point metal powder is a mixture of titanium powder and aluminum powder at a weight ratio of 1:1, a mixture of titanium powder and niobium powder at a weight ratio of 1:1, or a mixture of zirconium powder and nickel powder at a weight ratio of 1:1.

[0010] Preferably, in S102, the compact pressed by the high-melting-point metal powder and the high-purity aluminum are at a weight ratio of 1:1-10.

[0011] Preferably, in S103, T1 is 700-950 ℃.

[0012] Preferably, in S104, a 10wt% NaOH solution is used for selective etching to remove the residual aluminum phase.

[0013] Preferably, in S201, the reactant precursor is a mixture of carbon powder and silicon powder at a weight ratio of 1:0.01-0.1.

[0014] Preferably, in S202, the compact pressed by the non-metallic powder or the compound powder of the non-metallic powder and the aluminum source are at a weight ratio of 1:2-20.

[0015] Preferably, in S203, the reaction temperature T2 is 800-1000 ℃.

[0016] Preferably, in S204, the electrochemical stripping method is used to separate the generated target crystal material from the aluminum matrix to obtain a high-performance crystal material.

[0017] Preferably, the interface tunneling and self-sewing reaction in the present application is explained as follows: The interface tunneling and self-sewing reaction in the present application is a physical and chemical process realized in a non-equilibrium state, which is different from all traditional material synthesis paths, and is not a simple dissolution-diffusion-precipitation, but a kind of atomic scale dynamic self-organization behavior mediated by molten aluminum under the condition of space and energy misalignment, the core mechanism of which can be divided into two stages of pre- and post-connection and mutual promotion.

[0018] The first stage is dynamic molten aluminum interface tunneling. When molten aluminum contacts with the reactant precursor (high melting point metal or non-metal / compound) under the micro-porous partition, a stable solid-liquid interface is formed. Under the condition of "energy misalignment" far below the traditional reaction temperature, the atoms on the surface of the precursor cannot obtain enough energy to dissolve into the aluminum melt in a conventional thermal diffusion manner. Instead, due to its unique metal bond structure and fluidity, molten aluminum forms a dynamic self-adaptive single atomic layer interface with high chemical potential and specific interface potential at a very close distance to the surface of the precursor. In this interface region, the precursor atoms are jointly affected by strong local electronic interaction and thermal vibration fluctuation, and obtain the probability to cross the energy barrier. This process is similar to a kind of "quasi-tunneling effect", which enables the atoms necessary for the reaction to cross the molten aluminum interface layer in single or several forms, continuously and at low speed, into the interior of the aluminum melt. This transport mode avoids the rapid and extensive nucleation caused by the influx of a large number of atoms at once, and creates a prerequisite for the subsequent homogenization process; The second stage is explosive non-steady-state nucleation and lattice self-sewing. The heterogeneous atoms entering the aluminum melt through interface tunneling will gradually disperse and form a "transient atomic cloud" which is macroscopically uniform but microscopically rich, due to the concentration gradient and the convection of the aluminum melt. The system is always in a metastable state. When the atomic cloud concentration in the local region reaches a critical threshold, the Gibbs free energy of the entire aluminum melt volume will change, triggering explosive and global uniform non-steady-state nucleation. In a very short time, a large number of nanoscale crystal nuclei are simultaneously generated in the aluminum melt. These nascent crystal nuclei have very high surface energy and chemical activity, and under the driving of the lubrication and capillary action of molten aluminum, they do not extend layer by layer like traditional growth, but like having self-healing ability, they match and suture the lattices of adjacent grains at the interface through atomic rearrangement; This "lattice self-sewing" mechanism can effectively digest the small misorientation between the crystal nucleus, annihilate most of the grain boundaries and defects, so as to quickly fuse a single block or large size crystal with macroscopically dense, complete and few internal defects from a polycrystalline nanocrystalline assembly at the beginning of formation. Molten aluminum plays an indispensable multiple role in the whole process: it is not only the medium for atomic tunneling, but also the stress buffer layer, the carrier for heat and mass transfer, and finally provides an ideal dynamic environment for lattice self-sewing.

[0019] The beneficial effects of the present application are: 1. The present application constructs a non-equilibrium reaction environment through spatial misorientation and energy misorientation, and realizes atomic-level precise regulation relying on the "interface tunneling-lattice self-sewing" mechanism. High-melting-point metal atoms slowly tunnel into the aluminum melt in the form of single atoms or several atoms, forming a macroscopically uniform and microscopically enriched "transient atomic cloud", which in turn triggers explosive non-steady-state nucleation, and nanoscale crystal nuclei are fused into low-defect organization through lattice self-sewing. This process effectively avoids the composition segregation and grain coarsening problems caused by extensive atomic diffusion in traditional processes, not only can significantly improve the tensile strength and hardness of the alloy through fine-grain strengthening, but also can greatly reduce the hardness fluctuation by virtue of uniform composition distribution, so that the alloy has more stable mechanical response during service, meeting the stringent requirements of aerospace, high-end equipment and other fields for mechanical properties and uniformity of alloy materials.

[0020] 2. The "lattice self-sewing" mechanism of the present application can effectively annihilate grain boundary defects and pores, so that the alloy and crystal material form a macroscopically dense block structure, solving the problem of loose organization caused by insufficient sintering or extensive growth in traditional processes (such as powder metallurgy and high-temperature sintering) from the root. The dense material structure can greatly reduce the penetration channels of corrosion medium (such as chloride ions in salt spray environment), reduce the contact probability between corrosion medium and internal organization of the material, thereby significantly improving the corrosion resistance of the material. Whether it is an alloy component serving in marine environment or industrial corrosion environment, or a crystal material applied in the field of electronic information, the service life can be extended, the maintenance cost can be reduced, and the application scenario range of the material can be widened due to the improvement of density and corrosion resistance.

[0021] 3.The low-temperature reaction system (reaction temperature is at least 150℃ lower than traditional process) designed for the preparation of crystalline materials can effectively avoid the impurity diffusion problem of crucible materials (such as graphite and alumina) in traditional high-temperature process, reducing the risk of external pollution; at the same time, the aluminum source acts as an atomic tunneling medium, which can be completely removed by subsequent electrochemical stripping, selective corrosion and other methods, leaving only a trace amount of impurities; the "interface tunneling-lattice self-sewing" mechanism can also annihilate most dislocations, stacking faults and other defects during crystal nucleation and growth, ensuring that the crystal has excellent structural integrity. This makes the prepared crystalline materials not only meet the high requirements of purity in the fields of semiconductor packaging and 5G communication, but also improve the optical and electrical properties by virtue of low defect characteristics, breaking the technical bottleneck of "high purity and low defect difficult to be considered together" in traditional crystal preparation.

[0022] 4.The invention adopts modular design, which can flexibly adapt to the preparation requirements of Ti-Al, Ti-Nb-Al, Zr-Ni-Al and other high-performance alloys, as well as silicon carbide, aluminum nitride, aluminum oxide and other functional crystals by adjusting the raw material ratio, microporous separator parameters and reaction temperature, without the need to reconfigure the reaction device, greatly improving the process adaptability. At the same time, the low-temperature reaction system (alloy reaction temperature 700-950℃, crystal reaction temperature 800-1000℃) can significantly reduce energy consumption compared to traditional high-temperature process; and the preparation process of alloys and crystals does not require complex pretreatment or secondary processing, simplifying the production steps while reducing raw material waste. This "one furnace to adapt to multiple materials, low temperature, low consumption and high efficiency" feature meets the needs of green manufacturing and large-scale industrial production, and has broad industrial application prospects. DETAILED DESCRIPTION

[0023] To make the purpose, technical solutions and advantages of the present invention clearer, the present invention is further described in detail below with specific examples.

[0024] Example 1: Reaction process of high-performance Ti-Al alloy S1. Reaction process of high-performance alloy material S101. Preparation and proportioning of raw materials Reactive precursor: mix titanium powder and aluminum powder in a weight ratio of 1:1, and press into a cylindrical billet; Aluminum source: high-purity aluminum with a purity of not less than 99.99% is used; S102. Construction of misfit reaction system In the reaction cavity, 1kg of high-purity aluminum, boron nitride microporous inert separator and 1kg of billet made by mixing titanium powder and aluminum powder are arranged from top to bottom; S103. Interface tunneling and self-sewing reaction The reaction cavity in S102 is vacuumed to a pressure of less than 1x10-2 Pa, and then filled with argon, heated to a reaction temperature of 700°C at a heating rate of 5°C / min, and kept for 0.5 h to obtain the composite material; S104. Post-processing: After the reaction, the obtained composite material was cooled, and residual aluminum phase was removed by selective corrosion using a 10wt% NaOH solution to obtain the high-performance Ti-Al alloy material.

[0025] Example 2: Reaction process of high-performance Ti-Nb-Al alloy: S1. Reaction process of high-performance alloy material: S101. Preparation and proportioning of raw materials: Reactive precursor: titanium powder and niobium powder were mixed uniformly at a weight ratio of 1:1, and then pressed into a cylindrical blank; Aluminum source: high-purity aluminum with a purity of not less than 99.99%; S102. Construction of misaligned reaction system: In the reaction cavity, 1 kg of high-purity aluminum, a boron nitride microporous inert partition, and 200 g of a blank prepared by mixing titanium powder and niobium powder were sequentially arranged from top to bottom; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 was vacuumed to a pressure of less than 1×10 -2 Pa, and then filled with argon, heated to a reaction temperature of 700°C at a heating rate of 5°C / min, and kept for 0.5 h to obtain the composite material; S104. Post-processing: After the reaction, the obtained composite material was cooled, and residual aluminum phase was removed by selective corrosion using a 10wt% NaOH solution to obtain the high-performance Ti-Nb-Al alloy material Example 3: Reaction process of high-performance Zr-Ni-Al alloy: S1. Reaction process of high-performance alloy material: S101. Preparation and proportioning of raw materials: Reactive precursor: zirconium powder and nickel powder were mixed uniformly at a weight ratio of 1:1, and then pressed into a cylindrical blank; Aluminum source: high-purity aluminum with a purity of not less than 99.99%; S102. Construction of misaligned reaction system: In the reaction cavity, 1 kg of high-purity aluminum, a boron nitride microporous inert partition, and 100 g of a blank prepared by mixing zirconium powder and nickel powder were sequentially arranged from top to bottom; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 was vacuumed to a pressure of less than 1×10 -2Pa, and then filled with argon, heated to the reaction temperature 950℃ at a heating rate of 15℃ / min, and kept for 10h to obtain the composite material; S104. Post-processing: After the reaction, the obtained composite material was cooled, and the residual aluminum phase was selectively removed by etching with a 10wt% NaOH solution to obtain a high-performance Zr-Ni-Al alloy material.

[0026] Example 4: Reaction process of high-performance silicon carbide crystal material: S1. Reaction process of high-performance crystal material: S101. Preparation and proportioning of raw materials: Reactant precursor: mixture of carbon powder and silicon powder in a weight ratio of 1:0.01; Aluminum source: industrial pure aluminum or aluminum alloy with an aluminum content of not less than 99.0%; S102. Construction of misaligned reaction system: In the reaction cavity, 1kg of aluminum source, a boron nitride microporous inert partition, and 500g of a compact prepared by mixing carbon powder and silicon powder were sequentially arranged from top to bottom; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 was vacuumed to a pressure of less than 1×10 -2 Pa, and then filled with argon, heated to the reaction temperature 800℃ at a heating rate of 5℃ / min, and kept for 1h to obtain the crystal material; S104. Post-processing: After the reaction, the obtained crystal material was cooled, and an electrochemical stripping method was used to selectively remove the aluminum matrix by using an electrochemical workstation with the product as the working electrode and anodic dissolution in an HCl electrolyte, and the released silicon carbide crystal was collected to obtain a high-performance silicon carbide crystal material.

[0027] Example 5: Reaction process of high-performance silicon carbide crystal material: S1. Reaction process of high-performance crystal material: S101. Preparation and proportioning of raw materials: Reactant precursor: mixture of carbon powder and silicon powder in a weight ratio of 1:0.05; Aluminum source: industrial pure aluminum or aluminum alloy with an aluminum content of not less than 99.0%; S102. Construction of misaligned reaction system: In the reaction cavity, 1kg of aluminum source, a boron nitride microporous inert partition, and 100g of a compact prepared by mixing carbon powder and silicon powder were sequentially arranged from top to bottom; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 is vacuumed to a pressure lower than 1x10 -2 Pa, then filled with argon, heated to a reaction temperature of 950°C at a temperature increasing rate of 10°C / min, and kept for 10h to obtain the crystal material; S104. Post-processing: After the reaction, the obtained crystal material is cooled, and an electrochemical stripping method is used to selectively remove the aluminum matrix by using an electrochemical workstation to perform anodic dissolution of the product as a working electrode in an HCl electrolyte, and the released silicon carbide crystal is collected to obtain a high-performance silicon carbide crystal material.

[0028] Example 6: Reaction process of high-performance silicon carbide crystal material: S1. Reaction process of high-performance crystal material: S101. Preparation and proportioning of raw materials: Reactive precursor: a mixture of carbon powder and silicon powder in a weight ratio of 1:0.1; Aluminum source: industrial pure aluminum or aluminum alloy with an aluminum content of not less than 99.0%; S102. Construction of misfit reaction system: In the reaction cavity, 1kg of aluminum source, a boron nitride microporous inert partition, and 50g of a compact prepared by mixing carbon powder and silicon powder are sequentially arranged from top to bottom; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 is vacuumed to a pressure lower than 1x10 -2 Pa, then filled with argon, heated to a reaction temperature of 1100°C at a temperature increasing rate of 20°C / min, and kept for 20h to obtain the crystal material; S104. Post-processing: After the reaction, the obtained crystal material is cooled, and an electrochemical stripping method is used to selectively remove the aluminum matrix by using an electrochemical workstation to perform anodic dissolution of the product as a working electrode in an HCl electrolyte, and the released silicon carbide crystal is collected to obtain a high-performance silicon carbide crystal material.

[0029] Comparative Example 1: The difference between Comparative Example 1 and Example 1 is that titanium powder and niobium powder are uniformly mixed in a weight ratio of 1:1, and then pressed into a cylindrical compact. The compact is sintered at a high temperature of 1200°C for 2h in a vacuum environment, and then cooled in the furnace to obtain an alloy material.

[0030] Comparative Example 2: The difference between Comparative Example 2 and Example 2 is that titanium powder, niobium powder, and high-purity aluminum with the same composition and weight as in Example 2 are directly placed in contact with the aluminum block at the bottom of the crucible without any partition. Melting is carried out at the same temperature (850°C) and atmosphere as in Example 2, and kept for 6h, and then cooled in the furnace to obtain an alloy material.

[0031] Comparative Example 3: Comparative Example 3 is different from Example 2 in that the boron nitride microporous separator is replaced by a dense boron nitride separator.

[0032] Comparative Example 4: Comparative Example 4 is different from Example 4 in that the same high-purity carbon powder and silicon powder (weight ratio 1:0.01) as in Example 4 are used as raw materials, the green body is uniformly mixed, the green body is placed in a graphite crucible, and a traditional solid-phase carbothermic reduction reaction is carried out by directly heating to 1800°C under argon protection for 4h, without using an aluminum source and a boron nitride microporous separator.

[0033] Comparative Example 5: Comparative Example 5 is different from Example 5 in that the steps of Example 5 are repeated, including the use of the same raw materials, proportions, separators, and spatial structures, but the reaction temperature is increased to 1400°C and the holding time is 10h.

[0034] Performance Test: 1. Room temperature tensile strength test: According to GB / T 228.1-2021 "Metallic Materials-Tensile Testing-Part 1: Method of Test at Room Temperature", the alloy products from Examples 1-3 and Comparative Examples 1-3 are processed into round bar tensile specimens with a diameter of 5mm and a gauge length of 25mm, a universal material testing machine is used to perform room temperature tensile testing at a loading rate of 2mm / min, the maximum load of each specimen is recorded, the tensile strength of each group of specimens is calculated according to the formula: tensile strength = maximum load / specimen cross-sectional area, and the experimental results are shown in Table 1.

[0035] 2. Brinell hardness test: According to GB / T 231.1-2018 "Metallic Materials-Brinell Hardness Test-Part 1: Test Method", five evenly distributed test points (avoiding edges and obvious defects) are selected from the surface of the alloy products from Examples 1-3 and Comparative Examples 1-3, a Brinell hardness tester is used, a 2.5mm diameter hard alloy indenter is selected, a test force of 187.5kgf is applied, the pressure is maintained for 30s and then unloaded, the diameter of each indentation is measured, the hardness value of each test point is obtained from the Brinell hardness conversion table, the average hardness and standard deviation of the five points are calculated, and the experimental results are shown in Table 1.

[0036] 3. Density test: The alloys and crystals obtained from Examples 1-6 and Comparative Examples 1-5 are first weighed in air using an electronic balance (accuracy 0.001g), denoted as m1, then the sample is completely immersed in distilled water (ensuring no air bubbles are attached, and the container can be gently shaken to remove air bubbles), the mass of the sample in water is measured, denoted as m2, and the actual density (p) of the sample is calculated according to the formula: actual density p = m1 x p 水 / (m1-m2) (pwater is the density of distilled water at room temperature, taken as 1g / cm 3); Consult the theoretical density of the corresponding material, and calculate the density of each group of samples according to "density = (actual density / theoretical density) × 100%". The experimental results are shown in Table 2.

[0037] 4. Neutral Salt Spray Corrosion Test: Referring to GB / T 10125-2021 "Artificial Atmosphere Corrosion Test - Salt Spray Test", the materials obtained in Examples 1-6 and Comparative Examples 1-5 were processed into 50mm×50mm×5mm sheets. The surface was polished with 400# sandpaper until there were no obvious scratches, wiped with alcohol, and then dried. The samples were placed in a salt spray test chamber, the temperature of which was adjusted to 35℃, the spray medium was a 5wt% NaCl aqueous solution (pH=6.5-7.2), the spray pressure was 0.07-0.1MPa, and the salt spray deposition rate was 1-2mL / (h·80cm). 2 After continuous spraying for 240 hours, the samples were removed, the surface salt was rinsed with clean water, and after drying, the mass of the sample after corrosion was weighed using an electronic balance and recorded as m3. The corrosion rate of each group of samples was calculated according to the formula: Corrosion rate = (m1 - m3) / (sample surface area × corrosion time). (Unit: g / (m3)) 2 The experimental results are shown in Table 2.

[0038] 5. Crystal Material Purity Test: Accurately weigh 0.5g of the crystal powder samples ground in Examples 4-6 and Comparative Examples 4-5, add 50mL of concentrated nitric acid and 10mL of hydrofluoric acid mixed solution, heat to 80℃ for 30min to dissolve, cool, add 20mL of distilled water, add 2 drops of phenolphthalein indicator, and titrate with 0.1mol / L NaOH standard solution until the solution turns pink and does not fade for 30s. Record the volume of NaOH consumed, V1, and calculate the Al content in the sample according to the reaction equation (Al reacts with NaOH in a 1:3 molar ratio). Take another 0.5g of sample, add 10mL of dilute sulfuric acid (1:1 volume ratio), heat to dissolve, add 5mL of starch indicator, and titrate with 0.01mol / L iodine standard solution until the solution turns blue. Calculate the O content based on the volume of iodine consumed. The total impurity content is the sum of Al, O and other trace elements (estimated according to titration deviation). The experimental results are shown in Table 3.

[0039] Table 1. Results of tensile strength and Brinell hardness tests

[0040] Table 2. Results of density and neutral salt spray corrosion tests

[0041] Table 3. Results of purity test for crystal materials

[0042] Performance Analysis: From the experimental data in Table 1, the high-performance alloys (Ti-Al, Ti-Nb-Al, Zr-Ni-Al alloys) prepared by the embodiments of the present application are significantly superior to the comparative examples in terms of room temperature tensile strength and Brinell hardness. This advantage is due to the unique "interface tunneling-lattice self-sewing" mechanism of the present application: under the synergistic effect of spatial misplacement (microporous partition) and energy misplacement (low-temperature reaction), high-melting-point metal atoms slowly tunnel into the aluminum melt in the form of single atoms or several atoms, forming a macroscopically uniform and microscopically enriched "transient atomic cloud", which in turn triggers explosive unsteady nucleation, and the generated nanoscale crystal nuclei are fused into a low-defect structure through lattice self-sewing, the fine-grained structure greatly improves the tensile strength through the Hall-Petch effect, and the uniform composition distribution ensures that the Brinell hardness remains at a high level with minimal fluctuations; in contrast, the traditional high-temperature sintering process in the comparative examples lacks the aluminum-mediated tunneling effect, resulting in coarse-grained atomic diffusion, which not only leads to the formation of brittle intermetallic compounds, but also significantly reduces the tensile strength and hardness; the comparative example without a partition has no spatial misplacement restriction, and high-melting-point metal atoms quickly dissolve into the aluminum melt, causing severe composition segregation, which not only reduces the mechanical properties, but also significantly deteriorates the hardness uniformity; and the comparative example using a dense partition blocks the atomic tunneling channel, allowing only surface local reactions to occur, resulting in a loose and porous structure, and the mechanical properties and uniformity are at the worst level.

[0043] As can be seen from the experimental data in Table 2, the density of the alloy of the embodiments is much higher than that of the comparative examples, and the corrosion rate is significantly lower, because the "lattice self-sewing" mechanism can effectively annihilate grain boundary defects and pores, forming a macroscopically dense bulk structure, and the dense structure can greatly reduce the penetration channel of the corrosion medium, thereby improving corrosion resistance; the comparative examples lack this mechanism, and traditional sintering, non-partition melting, or dense partition blocking reactions will all result in a large number of pores remaining in the structure, which become channels for rapid diffusion of corrosion media, greatly increasing the corrosion rate, among which the comparative example using a dense partition has the most porous structure and the lowest density, and the highest corrosion rate; For crystalline materials (silicon carbide crystals), the embodiments also exhibit obvious advantages in density and corrosion resistance. The embodiments use aluminum-mediated interface tunneling to allow carbon and silicon atoms to enter the aluminum melt in an orderly manner at low temperatures, and then form low-defect crystals through lattice self-sewing, with very few internal pores and high density; at the same time, the dense crystal structure and the subsequent complete removal of the aluminum source result in excellent chemical stability of the crystal and a low corrosion rate. In the comparative examples, the traditional solid-phase carbon thermal reduction process lacks the aluminum-mediated self-sewing mechanism, and the crystal growth is coarse at high temperatures, leaving a large number of grain boundary pores inside, resulting in low density and the easy introduction of impurities from the crucible, further reducing the corrosion resistance of the crystal; and the comparative example that only increases the reaction temperature destroys the interface tunneling-self-sewing mechanism by exceeding the "energy misplacement" window, resulting in thermal stress cracks in the crystal at high temperatures, a decrease in density, and an increase in corrosion rate.

[0044] From the experimental data in Table 3, it can be seen that the purity of the examples is much higher than that of the comparative examples. The low-temperature reaction conditions of the examples can avoid the diffusion of impurities of the crucible material (such as graphite and alumina) at a traditional high temperature, and the aluminum source can be completely removed by an electrochemical stripping method, leaving only a trace amount of impurities. At the same time, sufficient holding time can allow the unreacted precursor powder to diffuse fully, further reducing the impurity content. The comparative examples have high residual amounts of unreacted precursors due to the diffusion of crucible impurities caused by the traditional high-temperature process and the absence of aluminum source-assisted purification, resulting in a significant reduction in purity. The comparative example with only an increased reaction temperature will induce a side reaction between the aluminum source and the crystal at high temperature, generating new impurity phases and promoting the diffusion of elements of the separator material, so that the purity is higher than that of the traditional carbothermic reduction comparative example, but still much lower than that of the examples.

[0045] In summary, the overall advantages of the example materials in mechanical properties, density, corrosion resistance, and purity are all derived from the core innovation of spatial misplacement, energy misplacement, and interface tunneling-lattice self-sewing. This innovation breaks through the traditional material preparation path that relies on equilibrium thermodynamics, and realizes the fine-grained, uniform, and dense organization of the material through atomic-level dynamic self-organization in a non-equilibrium state, thereby improving various properties. The comparative examples cannot rely on the interface tunneling-lattice self-sewing mechanism due to the destruction of spatial misplacement (no separator, dense separator) or energy misplacement (high temperature), and can only rely on traditional dissolution-diffusion, high-temperature sintering, and other methods to prepare materials. Ultimately, due to coarse organization, composition segregation, residual porosity, or impurity introduction, the various properties are far inferior to those of the examples, fully demonstrating the advancement and necessity of the technical solutions of the present application.

[0046] The above describes only the preferred specific embodiments of the present application, but the protection scope of the present application is not limited thereto. Any person skilled in the art can make equivalent substitutions or changes to the technical solutions and inventive concepts of the present application within the technical scope disclosed by the present application, which should be covered within the protection scope of the present application.

Claims

1. A melt aluminum dislocation reaction process for producing high performance alloy and crystalline materials, characterized by, The method comprises the following steps: S1. Reaction process of high-performance alloy material: S101. Preparation and proportioning of raw materials: Reactant precursor: composed of at least one high-melting-point metal powder; the high-melting-point metal powder is selected from one or more of titanium, zirconium, niobium, tantalum and nickel, with a purity of not less than 99.5% and a particle size distribution of 1-100 μm; Aluminum source: high-purity aluminum with a purity of not less than 99.99% is used; S102. Construction of staggered reaction system: In the reaction cavity, high-purity aluminum, a microporous inert partition plate and a compact pressed from high-melting-point metal powder are sequentially arranged from top to bottom; the material of the microporous inert partition plate is boron nitride, aluminum oxide or high-temperature alloy, with a pore size range of 5-50 microns and a porosity of 30%-60%; S103. Interface tunneling and self-sewing reaction: The reaction cavity in S102 is vacuumed to a pressure lower than 1x10 -2 Pa, then argon is filled, heated to a reaction temperature T1 at a temperature increasing rate of 5-15 ℃ / min, and kept for 0.5-10 h to obtain a composite material; wherein, T1 is a temperature between 50-1000 ℃ above the melting point of aluminum, and T1 is at least 100 ℃ lower than the traditional reaction temperature of the high-melting-point metal powder and aluminum to form intermetallic compounds. S104. Post-processing: After the reaction is completed, the obtained composite material is cooled, and residual aluminum phase is selectively removed by using an alkaline solution or an acidic solution with a concentration of 5-20 wt%, thereby obtaining a high-performance alloy material; S2. Reaction process of high-performance crystal material: S201. Preparation and proportioning of raw materials: Reactant precursor: composed of non-metal powder or compound powder thereof, the non-metal powder being carbon, silicon or boron powder, and the compound powder being one or more of silicon dioxide, boron nitride and silicon carbide powder, with a purity of not less than 99.9% and a particle size distribution of 0.1-50 μm; Aluminum source: industrial pure aluminum or aluminum alloy with an aluminum content of not less than 99.0% is used; S202. Construction of staggered reaction system: In the reaction cavity, the aluminum source, a microporous inert partition plate and a compact pressed from non-metal powder or compound powder thereof are sequentially arranged from top to bottom; the material of the microporous inert partition plate is boron nitride, graphite or aluminum oxide, with a pore size range of 1-20 μm and a porosity of 20%-50%; S203. Interface tunneling and self-sewing reaction: The reaction cavity in S202 is vacuumed to a pressure lower than 1 x 10 -2 Pa, then argon is filled, heated to a reaction temperature T2 at a temperature increasing rate of 5-20 ℃ / min, and kept for 1-20 h to obtain a crystal material; wherein, T2 is a temperature between 50 ℃ above the melting point of aluminum and 1100 ℃, and T2 is at least 150 ℃ lower than the temperature at which the non-metal or its compound generates a target crystal through a traditional carbothermal reduction or metallothermic reduction reaction. S204. Post-processing: After the reaction is completed, the obtained crystal material is cooled, and the generated target crystal material is separated from the aluminum matrix by using an electrochemical stripping method, a physical crushing method or a selective corrosion method, thereby obtaining a high-performance crystal material.

2. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The material of the microporous inert partition plate is boron nitride.

3. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The high-melting-point metal powder in S101 is a mixture of titanium powder and aluminum powder with a weight ratio of 1:1, a mixture of titanium powder and niobium powder with a weight ratio of 1:1 or a mixture of zirconium powder and nickel powder with a weight ratio of 1:

1.

4. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The compact pressed from high-melting-point metal powder in S102 and the high-purity aluminum have a weight ratio of 1:1-10.

5. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, T1 in S103 is 700-950 ℃.

6. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, In S104, a NaOH solution with a concentration of 10 wt% is used to selectively remove residual aluminum phase.

7. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The reactant precursor in S201 is a mixture of carbon powder and silicon powder with a weight ratio of 1:0.01-0.

1.

8. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The compact pressed from non-metal powder or compound powder thereof in S202 and the aluminum source have a weight ratio of 1:2-20.

9. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, The reaction temperature T2 in S203 is 800-1000 ℃.

10. The melt aluminum dislocation reaction process for making high performance alloy and crystal materials of claim 1, wherein, In S204, the electrochemical stripping method is used to separate the generated target crystal material from the aluminum matrix, thereby obtaining a high-performance crystal material.

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