Preparation method of high-strength aluminum-magnesium-manganese alloy material
By employing techniques such as atomized drying, electromagnetic stirring, and intense plastic deformation, combined with the dispersion of nano-ceramic particles and multiphase synergistic strengthening, the problems of coarse grains and insufficient strength in aluminum-magnesium-manganese alloys have been solved, achieving high strength, high toughness, and corrosion resistance, making them suitable for high-strength applications.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGSU LIZHONG NEW MATERIAL TECH CO LTD
- Filing Date
- 2026-02-10
- Publication Date
- 2026-04-17
AI Technical Summary
Existing aluminum-magnesium-manganese alloy preparation technologies suffer from problems such as coarse grains, insufficient strength, low elongation, uneven distribution of nanoparticles, weak interfacial bonding, high corrosion sensitivity, lack of precise control, and poor environmental performance, making it difficult to meet the application requirements of high strength, high toughness, and extreme environments.
By employing technologies such as atomized drying, electromagnetic stirring, and intense plastic deformation, combined with dispersion strengthening of nano-ceramic particles and multiphase synergistic strengthening, and optimizing the process through machine learning, the grains are refined to the nanoscale, improving mechanical properties and corrosion resistance. Online monitoring and environmentally friendly process optimization are also implemented.
It significantly improves the tensile strength of the alloy to over 450MPa, elongation ≥10%, corrosion resistance and fatigue life are significantly enhanced, the process is precise and controllable, it is suitable for high-strength applications and meets environmental protection requirements.
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Figure CN121674802B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of metal materials technology, specifically, it relates to a method for preparing a high-strength aluminum-magnesium-manganese alloy material. Background Technology
[0002] Aluminum-magnesium-manganese alloys, as a typical non-heat-treatable strengthened aluminum alloy, are widely used in aerospace, automotive manufacturing, electronic equipment, and building structures, especially excelling in components requiring high strength and corrosion resistance, such as inverter housings. This alloy, with aluminum as the matrix and magnesium and manganese as the main alloying elements, offers good weldability, corrosion resistance, and low density, making it a preferred lightweight material. However, with the ever-increasing demands of modern industry for material performance, traditional aluminum-magnesium-manganese alloy preparation methods and performance characteristics are no longer sufficient to meet the requirements of high strength, high toughness, and extreme environmental tolerance. The numerous limitations of existing technologies have become bottlenecks restricting its further application. This invention aims to solve these problems through nanoparticle dispersion strengthening and process optimization.
[0003] Firstly, the preparation of traditional aluminum-magnesium-manganese alloys mainly relies on conventional casting processes, such as semi-continuous casting and subsequent heat treatment. While this method is simple and low-cost, it has significant drawbacks. During the casting process, the alloy melt tends to form coarse grain structures under slow cooling conditions, with average grain sizes often reaching hundreds of micrometers. This leads to severe macroscopic segregation and increased hydrogen inclusions, which in turn affect the material's uniformity and mechanical properties. For example, in the aerospace field, this low strength limits the alloy's use in high-stress components, while in automotive inverter housings, the material's fatigue life and impact resistance fail to meet the stringent standards of electric vehicles. Furthermore, the limited solid solubility of alloying elements in traditional processes, coupled with the high volatility of magnesium, further exacerbates compositional inhomogeneity, making the alloy susceptible to stress corrosion cracking and intergranular corrosion under high-temperature or long-term service conditions. These problems not only reduce the material's reliability and service life but also increase the difficulty of subsequent processing, such as the susceptibility to cracking during hot rolling or extrusion. Nanoparticle strengthening technology, as an emerging means to improve the performance of aluminum-magnesium-manganese alloys, has received widespread attention in recent years. By introducing nano-ceramic particles such as yttrium oxide, zirconium oxide, alumina, or silicon carbide, alloys can achieve dispersion strengthening and grain refinement, thereby significantly improving strength and heat resistance. However, existing nanoparticle strengthening methods still face many challenges. First, there is the problem of particle agglomeration and uneven distribution. Due to their high surface energy, nanoparticles easily aggregate into clusters in the melt, leading to uneven strengthening effects and even forming weak bonding zones at the interface. According to existing research, nano-ceramic particles (such as yttrium oxide) have poor wettability in the aluminum matrix and weak interfacial bonding, making the material prone to cracking under high-temperature deformation or cyclic loading. Second, existing introduction methods, such as mechanical stirring or spray drying, struggle to achieve uniform dispersion, especially in large-scale production, where particle oxidation and agglomeration further deteriorate the alloy's microstructure. Furthermore, existing processes lack online monitoring and precise control of the nanostructure; parameter adjustments rely heavily on experience, which not only reduces production efficiency but also increases scrap rates. Environmental friendliness is also a prominent issue; existing solvent use and waste gas emissions result in a recovery rate of less than 70%, failing to meet the requirements of sustainable development. In the patent field, existing patents on the preparation of aluminum-magnesium-manganese alloys also reveal similar limitations. For example, US patent US11976343B2 describes a high-strength Al-Mn-Sc alloy for rapid solidification manufacturing, but it relies on expensive Sc, resulting in high costs and unsuitability for large-scale applications. Chinese patent CN111575550A proposes a method for preparing a high-strength weldable aluminum alloy by adding Zn and Ti to improve performance, but it fails to address the dispersion problem of nanoparticles, limiting the alloy's application in precision components such as inverter housings. Furthermore, European patent EP3212818B2 relates to the preparation of aluminum alloy products, emphasizing formability under T4 tempering, but neglecting the synergistic effect of high-temperature stability and multiphase strengthening.While these patents have improved the mechanical properties of the alloys to some extent, they have not yet achieved grain refinement to the nanoscale (80-200nm) and multiphase synergistic strengthening. Tensile strength is difficult to exceed 450MPa, while elongation remains above 10%. Further analysis of the corrosion and thermal stability issues in existing technologies reveals that aluminum-magnesium-manganese alloys are prone to pitting and stress corrosion in chloride environments due to the weakening of grain boundaries caused by the network precipitation of the β-phase (Al3Mg2). Environmental and sustainability issues are particularly prominent in existing technologies. Traditional casting processes have high energy consumption, low solvent recovery rates, and exhaust emissions containing harmful substances such as decomposition products of hexachloroethane. Existing green optimizations are limited; for example, patent US5422066A addresses the toughness improvement of Al-Mg-Li alloys but does not consider the overall environmental indicators of the process. Furthermore, while existing applications of intense plastic deformation (such as equal-diameter angular extrusion) and aging treatment can refine grains, the deformation strain control is imprecise, easily leading to cracks. In complex-shaped components such as inverter housings, this instability affects assembly accuracy and long-term reliability.
[0004] In summary, while existing aluminum-magnesium-manganese alloy preparation technologies have made progress in some aspects, they generally suffer from problems such as coarse grains, insufficient strength, low elongation, uneven nanoparticle distribution, corrosion sensitivity, lack of precise control, and poor environmental friendliness. These limitations severely restrict the application of the alloys in extreme environments, such as the high-power inverter casings that need to withstand high temperatures, high humidity, and mechanical vibration. There is an urgent need for an efficient and environmentally friendly nanoparticle dispersion strengthening method that, through multiphase synergy, machine learning optimization, and in-situ phase formation, can achieve grain refinement to the nanoscale, improve overall mechanical properties to a tensile strength of over 450 MPa and an elongation of ≥10%, while ensuring process controllability and sustainability. This invention addresses these pain points by providing an innovative preparation scheme that combines atomized drying, electromagnetic stirring, and intense plastic deformation technologies to achieve a breakthrough in high-strength aluminum-magnesium-manganese alloys. Summary of the Invention
[0005] To address the problems of coarse grains, insufficient strength (typically below 350 MPa), low elongation (less than 8%), easy agglomeration and uneven distribution of nanoparticles, weak interfacial bonding, high corrosion sensitivity, lack of precise control, and poor environmental performance in existing aluminum-magnesium-manganese alloys, this invention provides a method for preparing high-strength aluminum-magnesium-manganese alloy materials. This method uses aluminum as the matrix and adds elements such as magnesium, manganese, zinc, copper, zirconium, and titanium to prepare a master melt. A suspension of yttrium oxide and other nano-ceramic particles is prepared, atomized and dried into powder, and then the nanoparticles are introduced into the melt through electromagnetic stirring and ultrasonic-assisted blowing. Semi-continuous casting combined with electromagnetic field control, homogenization heat treatment, intense plastic deformation (equivalent strain ≥5) such as equal-diameter angular channel extrusion, hot rolling, and two-stage aging treatment are employed to achieve grain refinement to 80-200 nm, uniform dispersion of nanoparticles, and multi-phase synergistic strengthening. Optimization measures include nanoparticle replacement (such as zirconium oxide, alumina, and silicon carbide), in-situ boride phase formation, machine learning parameter optimization (prediction accuracy ≥95%), online characterization and monitoring, and environmentally friendly processes (such as solvent recovery rate ≥90%). Compared with existing technologies, this invention significantly improves the mechanical properties of the alloy, achieving a tensile strength of over 450 MPa, elongation ≥10%, and improved corrosion resistance and fatigue life. The process is precise and controllable, with high production efficiency and environmental friendliness, making it suitable for high-strength applications such as inverter housings.
[0006] The present invention adopts the following technical solution: a method for preparing a high-strength aluminum-magnesium-manganese alloy material, which, by weight, includes the following steps: (1) preparing aluminum alloy master melt: based on a total weight of 100 parts of metal element raw materials, with aluminum (CAS No.: 7429-90-5) as the balance, add 2.5-3.5 parts of magnesium (CAS No.: 7439-95-4), 0.8-1.2 parts of manganese (CAS No.: 7439-96-5), 0.4-0.6 parts of zinc (CAS No.: 7440-66-6), 0.1-0.2 parts of copper (CAS No.: 7440-50-8), and zirconium (CAS No.: 7440-67). -7) 0.1-0.2 parts of titanium (CAS No.: 7440-32-6) and 0.03-0.08 parts of titanium were melted at 720-750℃ under argon protection and kept at the temperature for 20-30 min to obtain a uniform aluminum-magnesium-manganese-based melt; (2) Preparation of nano-ceramic precursor suspension: Yttrium oxide nanoparticles (CAS No.: 1314-36-9, average particle size 8-15nm) and anhydrous ethanol (CAS No.: 64-17-5) were weighed at a mass ratio of 1:(8-15), and polyvinylpyrrolidone (CAS No.: 9003-39-8) with a mass ratio of 0.2-0.4 times the mass of nanoparticles was added as a dispersant. Disperse at 300-500W for 15-30 min to obtain a stable suspension; (3) Atomize and dry nanopowder: Atomize the suspension from step (2) and dry it in hot air at 250-350℃. Collect the yttrium oxide nanopowder coated with polyvinylpyrrolidone and pack it into a quartz tube at 0.3-0.8 parts by melt mass for later use; (4) Introduce nanopowder: Cool the melt from step (1) to 650-670℃, stir the electromagnetic stirring at 300-500r / min, blow the nanopowder into the melt through a carrier gas flow rate of 2-4L / min, introduce it for 8-15 min, maintain stirring and temperature, and obtain a composite melt; (5) (6) Refined solidification casting: The billet is formed by semi-continuous casting with a cooling rate of 20-60℃ / s and a thickness of 100-150mm. Then, it is homogenized by heat treatment at 480-500℃ for 5-15h and air-cooled to room temperature to obtain the initial composite alloy ingot; (7) Severe plastic deformation: The billet is subjected to equal diameter angular channel extrusion at 250-380℃ with equivalent deformation ≥5, 3-6 passes, and channel angle of 100-110° to obtain nanocrystalline billet; (8) Hot deformation and aging: The billet is hot-rolled at 320-380℃ with a deformation of 50-70%, then aged at 160-200℃ for 8-18h and air-cooled to obtain the finished material.
[0007] Preferably, in step (2), the yttrium oxide nanoparticles are partially replaced with one or more of zirconium oxide (CAS No.: 1314-23-4, average particle size 5-25 nm), alumina (CAS No.: 1344-28-1, average particle size 10-30 nm), or silicon carbide (CAS No.: 409-21-2, average particle size 5-20 nm), with a total addition amount of 0.2-1.2 parts by melt mass, and the mass ratio of each nanoparticle is yttrium oxide: zirconium oxide: alumina. Silicon carbide = (50-80):(10-30):(5-25):(5-15) to regulate lattice mismatch and interfacial energy, forming stable nanocrystals and multiphase reinforced structures; further add 0.1-0.25 times the mass of nanoparticles of trisodium citrate (CAS No.: 68-04-2) as an electrostatic dispersant, adjust the pH of the suspension to 8-9.5, use circulating microfluidic mixing, Reynolds number 200-800, to ensure that the aggregate size is less than 150nm, Zet The potential is maintained above ±30mV; in step (3), the spray atomization uses a centrifugal atomizer with a rotation speed of 8000-12000rpm and a hot air flow rate of 5-10m / s. After drying, the powder is sieved, and the particle size is controlled at 50-200nm. The powder is then vacuum dried to remove residual solvent; in step (4), before introducing the nanopowder, 0.02-0.08 parts by weight of hexachloroethane (CAS No.: 67-72-1) is added to the melt for 8-12 minutes to refine it. Argon gas (CAS No.: 7440-37-1) at a flow rate of 2.5 L / min is bubbled to reduce hydrogen and inclusions; nitrogen gas (CAS No.: 7727-37-9) with a purity ≥99.999% is introduced simultaneously as an auxiliary carrier gas at a flow rate of 0.5-2 L / min to reduce oxidation and agglomeration; electromagnetic stirring combined with ultrasonic assistance, ultrasonic power 100-300W, frequency 20-40kHz, and action time throughout the entire process, to promote uniform distribution of nanoparticles and interfacial wetting.
[0008] Preferably, in step (5), the semi-continuous casting adopts online electromagnetic field control, with a stirring current of 150-400A, a frequency of 15-40Hz, a stirring zone length of 40-70% of the crystallizer length, and a secondary water cooling rate of 30-80℃ / s to form an initial equiaxed crystal structure with a macroscopic segregation degree ≤0.15 and a secondary dendrite arm spacing ≤15μm; after homogenization heat treatment, the micro-strain is monitored online by X-ray diffraction, and the holding time is adjusted until the grain size is initially refined to 50-100μm; in step (6), the severe plastic deformation adopts a series process: first, equal diameter angular channel extrusion is performed at 320-400℃, with equivalent strain of 3-5 and 4-7 passes; then, room temperature high-pressure torsion is performed with a pressure of 4-5.5GPa and a rotation speed of 8-15 turns; finally, 3-5 passes of multi-directional forging at 220-280℃, with a total strain ≥6, to refine the grain size to 80-200nm, inducing high-density large-angle grain boundaries and non-equilibrium phases; intermediate annealing is used between deformation passes at 300-350℃ for 1-3 hours to prevent cracks; in step (7), the surface oxide layer is removed before hot rolling, and the lubricant between rolling passes is graphite emulsion (CAS No.: 7782-42-5), with a deformation rate of 15-25% per pass; the cold deformation amount before aging is 10-20%, and dislocations are introduced through cold rolling, followed by two-stage aging: the first stage is held at 140-160℃ for 5-8 hours, and the second stage is held at 180-210℃ for 3-6 hours to promote the precipitation of fine second phases and the synergistic strengthening of nanoparticles.
[0009] Preferably, in step (1), the metal raw material is ultrasonically cleaned and rinsed and dried with anhydrous ethanol before melting. The melting process uses induction heating with a power of 10-20kW. During heat preservation, argon gas is introduced at a flow rate of 3-5L / min, and the stirring speed is 100-200r / min to ensure that the composition uniformity deviation is ≤0.1%. In step (2), the suspension is prepared using a high-shear mixer with a speed of 5000-10000rpm. After premixing for 10-20min, it is ultrasonically mixed. The molecular weight of the dispersant polyvinylpyrrolidone is controlled at 10000-40000. In step (3), the dried nanoparticles are surface modified by plasma with a power of 50- 150W, time 5-10min, to improve compatibility with the melt; in step (4), the quartz tube is inserted to a depth of 2 / 3 of the melt height, the melt temperature fluctuates ≤5℃ when it is blown in, and stirring is continued for 5-10min after introduction; in step (5), the casting mold is preheated to 200-300℃, and the ingot is immediately water quenched after demolding at a cooling rate of 50-100℃ / s; in step (6), the material of the equal diameter angular channel extrusion die is a high temperature alloy, the lubricant is a boron nitride coating, and the extrusion speed is 1-5mm / s; in step (7), the temperature of the hot rolling roll is controlled at 150-250℃, and the finished material is polished with a surface roughness Ra≤0.5μm.
[0010] Preferably, the entire process involves online characterization and monitoring of the nanostructure: transmission electron microscopy is used to observe grain size and nanoparticle distribution, scanning electron microscopy combined with electron backscatter diffraction is used to determine grain orientation, X-ray diffraction is used to analyze grain size and strain, and differential scanning calorimetry is used to characterize aging behavior; in step (2), the stability of the suspension is monitored using a dynamic light scattering instrument with an average particle size ≤50nm; in step (4), the composite melt is sampled and analyzed to determine the uniformity of nanoparticle dispersion with a deviation ≤5%; in step (6), the deformed sample is electrolytically polished, and the dislocation density is observed to be ≥10 14 m -2 Based on the monitoring results, the amount of nanoparticles added was adjusted by 0.1-0.2 parts, the deformation strain was adjusted by 0.5-1 parts, and the aging temperature was adjusted by 5-10℃ to achieve a nanocrystal size of 80-150nm and a particle spacing of 30-100nm. Further in-situ nanophase formation was introduced: after the introduction in step (4), 0.05-0.15 parts of boric acid (CAS No.: 10043-35-3) by the melt mass was added, and the reaction was carried out at 660-680℃ for 10-15min to form in-situ boride nanoparticles (average particle size 10-30nm), with a mass ratio of 20-40% of the introduced nanoparticles.
[0011] Preferably, machine learning is used to optimize the process: collect parameters and microstructure data such as nanoparticle type and content (0.2-1.0 parts), melting temperature (710-760℃), cooling rate (15-70℃ / s), deformation strain (4-7), aging temperature (150-220℃) and time (6-20h), construct a support vector machine model, train a dataset of ≥500 sets, predict the process window of target grain size 60-180nm and particle spacing 25-120nm, with an accuracy of ≥95%; the prediction results guide the adjustment of the holding time in step (1) by 5-10min, the change of the carrier gas flow rate in step (4) by 0.5-1L / min, the increase or decrease of the number of passes in step (6) by 1-2, and the change of the deformation amount in step (7) by 5-10%; the model input includes alloy composition deviation and the influence of environmental humidity, and the output is an optimized parameter combination to achieve precise control; in addition, after homogenization in step (5), pulse current processing is introduced, with a current density of 50-150A / cm 2 The pulse frequency is 10-50Hz and the duration is 10-30min, which promotes diffusion and refines the initial tissue.
[0012] Preferably, in step (2), the nanoparticles are pretreated by ball milling with yttrium oxide and other materials at a ball-to-material ratio of 5:1-10:1, a rotation speed of 300-400 r / min, and a time of 2-4 h, resulting in the attachment of hydroxyl groups on the surface; 0.05-0.15 times the mass of silane coupling agent (CAS No.: 2530-85-0) is added to the suspension and stirred for 30-60 min to improve hydrophilicity; in step (3), drying is assisted by vacuum freeze drying at a temperature of -50~-30℃ for 4-8 h, removing residual water. The content is ≤0.5%; in step (4), the surface of the melt is covered with an argon protective layer of 5-10cm thickness, and 0.01-0.05 parts of calcium fluoride (CAS No.: 7789-75-5) by mass of the melt is injected simultaneously as a flux when introducing nanopowder; in step (5), the melt viscosity is monitored during the casting process and adjusted to 1.5-2.5mPa·s; in step (6), deformation is combined with finite element simulation to predict stress distribution and adjust channel geometric parameters; in step (7), aging is carried out in a vacuum furnace with a pressure ≤10. -3 Pa prevents oxidation; the finished material is tested by ultrasound and found to be defect-free, with a density ≥99.5%.
[0013] Preferably, a mixed carrier gas system is introduced: in step (4), the carrier gas is a mixture of argon and helium (CAS No.: 7440-59-7) with a volume ratio of 1:0.2-0.5 and a total flow rate of 2.5-4.5L / min to improve the transport efficiency of nanoparticles; in step (5), the ingot is subjected to magnetic levitation vibration treatment with a frequency of 20-50Hz, an amplitude of 1-3mm, and a time of 5-10min to refine the solidification structure; in step (6), the high-pressure torsion mold is lined with a diamond coating to reduce the friction coefficient to 0.1-0.2; in step (7), after hot deformation, the ingot is immediately oil-quenched at a cooling rate of 100-200℃ / s, followed by low-temperature cryogenic treatment at -196℃ for 2-4h to induce nanotwins; two-stage aging gap insertion stress relaxation annealing is performed at a temperature of 100-120℃ for 1-2h; the overall process is environmentally optimized: the solvent recovery rate is ≥90%, and the waste gas is adsorbed by activated carbon (CAS No.: 7440-44-0).
[0014] Preferably, in step (1), the order of adding alloying elements is as follows: first melt aluminum, then add manganese, zirconium, and titanium, and then add magnesium, zinc, and copper to avoid volatilization; in step (2), the suspension is treated by a high-pressure homogenizer at a pressure of 100-200 MPa and circulated 3-5 times; in step (3), the powder is stored in a vacuum seal with a humidity of ≤20%; in step (4), after introduction, the melt is stirred by a rotating magnetic field with a magnetic field strength of 0.1-0.3T, a rotation speed of 50-100 r / min, and a time of 10-20 min; in step (5), the cross-sectional shape of the ingot is optimized to be rectangular with a width-to-thickness ratio of 1.5-2.5; in step (6), the hardness distribution of the deformed sample is tested by nano-indentation, and the uniformity is ≥95%; in step (7), the finished product is subjected to tensile pre-deformation of 1-5% to improve fatigue life.
[0015] Compared to existing technologies, this invention provides a method for preparing high-strength aluminum-magnesium-manganese alloy materials. This method, through innovative process design and optimization measures, significantly overcomes many limitations in traditional aluminum-magnesium-manganese alloy preparation, achieving a comprehensive improvement in material performance and sustainable development of the production process. Specifically, this invention systematically improves alloy composition ratios, nanoparticle introduction methods, solidification casting control, severe plastic deformation, hot deformation, and aging treatment. Combined with machine learning optimization, in-situ phase formation, and online monitoring technologies, the alloy grain size is refined to 80-200 nm, achieving a tensile strength of over 450 MPa and an elongation of not less than 10%. Simultaneously, it improves corrosion resistance and fatigue life, making it suitable for high-strength, high-corrosion-resistant applications such as inverter housings. The beneficial effects of this invention are described in detail below from multiple dimensions. First, in terms of mechanical properties, this invention achieves a significant improvement in strength and toughness. In existing technologies, the tensile strength of traditional aluminum-magnesium-manganese alloys is typically below 350 MPa, and the elongation is less than 8%. This is mainly due to the coarse grains (hundreds of micrometers) formed during the casting process and the limited solid solution of alloying elements, leading to easy fracture and low plasticity under high stress environments. For example, literature reports show that conventional semi-continuous casting alloys suffer from severe macroscopic segregation and large secondary dendrite arm spacing, limiting their application in aerospace or automotive inverter housings. This invention introduces nano-ceramic particles such as yttrium oxide, zirconium oxide, alumina, or silicon carbide (average particle size 5-30 nm, total addition 0.2-1.2 parts), and employs a combination of atomized drying, electromagnetic stirring, and ultrasonic assistance to ensure uniform dispersion of the particles in the melt, forming a stable nanocrystalline structure and multiphase strengthening microstructure. Simultaneously, by combining angular channel extrusion (equivalent strain ≥5, 3-6 passes) and high-pressure torsion, high-density, large-angle grain boundaries and dislocation densities are induced, refining the grain size to 80-200 nm and controlling the intergranular spacing to 25-120 nm. This not only enhances the dispersion strengthening effect but also significantly improves the yield strength and tensile strength of the material through the Orowan mechanism and Hall-Petch relationship.
[0016] Secondly, this invention demonstrates excellent corrosion resistance and thermal stability. Existing aluminum-magnesium-manganese alloys are susceptible to chloride environments, leading to pitting corrosion and stress corrosion cracking, primarily due to the weakening of grain boundaries caused by the network precipitation of the β-phase (Al3Mg2), and salt spray testing time is typically less than 800 hours. Furthermore, under high-temperature service, the alloy exhibits poor thermal stability and is prone to softening and deformation. This invention optimizes lattice mismatch and interfacial energy by controlling alloying elements (e.g., 0.4-0.6 parts zinc, 0.1-0.2 parts copper) and nanoparticle substitution (mass ratio of yttrium oxide:zirconia: aluminum oxide: silicon carbide = 50-80:10-30:5-25:5-15), forming a stable interfacial layer and inhibiting the precipitation of harmful phases. Simultaneously, the in-situ formation of boride nanoparticles (adding 0.05-0.15 parts boric acid, reacting to form particles with a diameter of 10-30 nm, mass ratio 20-40%) further enhances grain boundary strengthening and the corrosion barrier. By combining two-stage aging treatment (holding at 140-160℃ for 5-8 hours followed by holding at 180-210℃ for 3-6 hours) and cryogenic treatment (holding at -196℃ for 2-4 hours), nanotwins and fine second-phase precipitation are induced, improving the alloy's heat resistance and corrosion resistance. Test results show that the salt spray test time in the example was 1120.9-1380.4 hours, with an average of 1250 hours, which is more than 50% longer than existing technologies; the fatigue life reached 9.8 × 10⁻⁶. 5 -1.4×10 6 The average number of cycles is 1.2 × 10⁻⁶. 6 The efficiency is improved by 2-3 times. This is due to the synergistic effect of nanoparticles, which reduces interfacial element segregation (≤5at%), making the alloy more stable in humid, salt spray, or high-temperature environments. It is particularly suitable for applications such as inverter housings for electric vehicles, reducing maintenance costs and environmental risks.
[0017] Third, this invention provides a precise and controllable solution for microstructure control and uniformity. Existing technologies rely on empirical adjustments, leading to easy agglomeration of nanoparticles (aggregate size >200nm), large distribution deviations, resulting in uneven strengthening and a high scrap rate (>10%). This invention employs optimized suspension preparation (e.g., adding 0.2-0.4 times polyvinylpyrrolidone and 0.1-0.25 times trisodium citrate, pH 8-9.5, Zeta potential ±30mV or higher), combined with circulating microfluidic mixing (Reynolds number 200-800) and high-pressure homogenization (100-200MPa, 3-5 times) to ensure aggregate size <150nm. The introduction process uses a mixed carrier gas (argon:helium = 1:0.2-0.5) and rotating magnetic field stirring (0.1-0.3T, 50-100r / min), combined with ultrasonic assistance (100-300W, 20-40kHz), to achieve uniform nanoparticle distribution with a deviation ≤5%. Furthermore, real-time feedback from online characterization monitoring (such as transmission electron microscopy, X-ray diffraction, and dynamic light scattering) allows for reverse parameter adjustments (e.g., increasing or decreasing the amount of nanoparticles by 0.1-0.2 parts). This results in a highly uniform microstructure, optimized grain orientation, macroscopic segregation ≤0.15, and secondary dendrite arm spacing ≤15μm. Compared to Comparative Example 3 (low melting temperature leading to grain coarsening to 410.8nm), the examples exhibit grain sizes of 82.1-198.5nm, particle spacing of 28.6-118.3nm, and more than double the uniformity, thus improving the material's reliability and processability.
[0018] Fourth, in terms of production efficiency and process optimization, this invention introduces intelligent control. Existing technologies rely on trial-and-error adjustments of parameters, resulting in low efficiency, narrow process windows, and long production cycles (>20h / batch). This invention constructs a support vector machine model based on ≥500 datasets (including nanoparticle content of 0.2-1.0 parts, melting temperature of 710-760℃, etc.) to predict grain size of 60-180nm and particle spacing of 25-120nm with an accuracy of ≥95%. The prediction guides parameter changes (such as adjusting holding time by 5-10min, increasing or decreasing the number of passes by 1-2), combined with finite element simulation to predict stress distribution, optimizing channel geometry and deformation paths. Digital twin simulation of the entire process achieves a prediction error of ≤10% for microstructure evolution, shortening the optimization cycle by 30%. This data-driven method not only increases output but also reduces energy consumption (optimizing induction heating power from 10-20kW), making it suitable for large-scale industrial production.
[0019] Fifth, regarding environmental protection and sustainability, this invention emphasizes green process design. Existing technologies have solvent recovery rates of <70%, harmful waste gas emissions (such as hexachloroethane decomposition products), and high energy consumption. This invention optimizes solvent use (e.g., anhydrous ethanol recovery rate ≥90%), treats waste gas with activated carbon adsorption, and introduces vacuum freeze-drying (-50 to -30°C) and pulsed current treatment (50-150 A / cm). 2 This reduces oxidation and hydrogen inclusions without requiring additional harmful additives. Overall process energy efficiency is improved by 20%, and scrap rate is reduced to <5%. For example, Example 1 reduces exhaust emissions by 50%, while Comparative Example 5 (low power leading to prolonged heating) increases energy consumption. This promotes sustainable development in alloy production and complies with international environmental standards.
[0020] Furthermore, this invention also offers advantages in cost control and application expansion. Existing technologies rely on rare elements (such as Sc), resulting in high costs; this invention uses common nanoparticles and optimized alloying elements, reducing costs by 15-20%. The alloy is suitable for use outside inverter housings and can also be extended to fields such as aerospace and construction, enhancing industrial competitiveness.
[0021] In summary, this invention, through innovations such as nanoparticle dispersion strengthening and multiphase synergy, comprehensively surpasses existing technologies, achieving breakthroughs in strength, corrosion resistance, production efficiency, and environmental friendliness. The exemplary embodiments demonstrate excellent performance, and comparative examples verify the importance of key parameters. This method not only solves the pain points of aluminum-magnesium-manganese alloys but also provides a new paradigm for the preparation of high-performance materials, driving industry progress. Attached Figure Description
[0022] Figure 1 This is a transmission electron microscope (TEM) image of the high-strength aluminum-magnesium-manganese alloy material prepared in Example 1.
[0023] Figure 2 This is the energy dispersive X-ray spectrum (10,000x magnification) of aluminum in the high-strength aluminum-magnesium-manganese alloy material prepared in Example 1.
[0024] Figure 3 This is the energy dispersive X-ray spectrum (10,000x magnification) of magnesium in the high-strength aluminum-magnesium-manganese alloy material prepared in Example 1.
[0025] Figure 4 This is the energy dispersive X-ray spectrum (10,000x magnification) of manganese in the high-strength aluminum-magnesium-manganese alloy material prepared in Example 1. Detailed Implementation
[0026] The present invention will now be described in detail through specific embodiments. However, these illustrative embodiments are for purposes and uses only to illustrate the invention and do not constitute any limitation on the actual scope of protection of the invention, nor are they intended to restrict the scope of protection of the invention to these embodiments. For parameter ranges not mentioned, intermediate values are selected. Also, for mass ratios not explicitly stated or mentioned, the mass ratio after addition generally refers to the mass ratio. Furthermore, in the present invention, the unit of mass is grams (g).
[0027] Example 1
[0028] The preparation method of high-strength aluminum-magnesium-manganese alloy material includes the following steps: (1) Preparation of aluminum alloy master melt: with aluminum (CAS No.: 7429-90-5) as the balance, add 3 parts of magnesium (CAS No.: 7439-95-4), 1 part of manganese (CAS No.: 7439-96-5), 0.5 parts of zinc (CAS No.: 7440-66-6), 0.15 parts of copper (CAS No.: 7440-50-8), 0.15 parts of zirconium (CAS No.: 7440-67-7), and 0.15 parts of titanium (CAS No.: 7440-32- 6) 0.055 parts (total mass of 100g, i.e., aluminum 95.145g, magnesium 3g, manganese 1g, zinc 0.5g, copper 0.15g, zirconium 0.15g, titanium 0.055g), the metal raw materials were ultrasonically cleaned and rinsed and dried with anhydrous ethanol before melting. They were melted at 735℃ under argon protection and held for 25min. Induction heating was used during the melting process with a power of 15kW. Argon gas flow rate was 4L / min during the holding period, and stirring speed was 150r / min to ensure that the composition uniformity deviation was ≤0.1%, so as to obtain a uniform aluminum-magnesium-manganese-based melt.(2) Preparation of nano-ceramic precursor suspension: Yttrium oxide nanoparticles (CAS No.: 1314-36-9, average particle size 11.5 nm) and anhydrous ethanol (CAS No.: 64-17-5) were weighed at a mass ratio of 1:11.5 (total mass of 115 g, i.e. 10 g of yttrium oxide nanoparticles and 105 g of anhydrous ethanol). Polyvinylpyrrolidone (CAS No.: 9003-39-8) (0.3 times the mass of nanoparticles) was added as a dispersant (3 g), and the mixture was dispersed at an ultrasonic power of 400 W for 22.5 min. A stable suspension was obtained. The yttrium oxide nanoparticles were partially replaced with one or more of the following: zirconium oxide (CAS No.: 1314-23-4, average particle size 15 nm), alumina (CAS No.: 1344-28-1, average particle size 20 nm), or silicon carbide (CAS No.: 409-21-2, average particle size 12.5 nm). The total amount added was 0.7 parts (70 g) of the melt mass, and the mass ratio of each nanoparticle was yttrium oxide:zirconia:alumina:silicon carbide = 65:20:15:10 (i.e., yttrium oxide 4...). 5.5g of zinc oxide, 14g of zirconium oxide, 10.5g of alumina, and 7g of silicon carbide were added to regulate lattice mismatch and interfacial energy, forming stable nanocrystals and multiphase reinforced structures. Trisodium citrate (CAS No.: 68-04-2), at 0.175 times the mass of the nanoparticles, was further added as an electrostatic dispersant (12.25g). The pH of the suspension was adjusted to 8.75, and microfluidic mixing was employed with a Reynolds number of 500 to ensure that the aggregate size was less than 150nm and the Zeta potential remained above ±30mV. Nanoparticle pretreatment was also performed. Yttrium oxide and other materials were activated by ball milling at a ball-to-material ratio of 7.5:1, a rotation speed of 350 r / min, and a time of 3 h, resulting in the adhesion of hydroxyl groups to the surface. 0.1 times the mass of silane coupling agent (CAS No.: 2530-85-0, 7 g) was added to the suspension, and the mixture was stirred for 45 min to improve hydrophilicity. The suspension was prepared using a high-shear mixer at 7500 rpm, premixed for 15 min, and then sonicated. The molecular weight of the dispersant, polyvinylpyrrolidone, was controlled at 25000. The stability of the suspension was monitored using a dynamic light scattering instrument, with an average particle size ≤50 nm. (3) Atomization and drying of nanopowder: The suspension in step (2) is atomized by spray and dried in hot air at 300℃. Yttrium oxide nanopowder coated with polyvinylpyrrolidone is collected and loaded into a quartz tube (55g) at 0.55 parts by melt mass. The atomization is carried out by a centrifugal atomizer with a rotation speed of 10000rpm and a hot air flow rate of 7.5m / s. After drying, the powder is sieved and the particle size is controlled at 125nm. The residual solvent is removed by vacuum drying. After drying, the nanopowder is surface modified by plasma at a power of 100W for 7.5min to improve its compatibility with the melt. The drying is assisted by vacuum freeze drying at a temperature of -40℃ for 6h. The residual moisture content is ≤0.5%.(4) Introduction of nanopowder: The melt from step (1) was cooled to 660℃, and the electromagnetic stirring speed was 400r / min. Nanopowder was blown into the melt through a carrier gas flow rate of 3L / min for 11.5min. Stirring and temperature were maintained to obtain a composite melt. Before introducing the nanopowder, 0.05 parts by weight of hexachloroethane (CAS No.: 67-72-1) was added to the melt for 10min (5g). Argon gas (CAS No.: 7440-37-1) was bubbled at 1.75L / min to reduce hydrogen and inclusions. Nitrogen gas (CAS No.: 7727-37-9) with a purity ≥99.999% was introduced simultaneously as an auxiliary carrier gas at a flow rate of 1.25L / min to reduce oxidation and agglomeration. Electromagnetic stirring was combined with ultrasonic assistance at an ultrasonic power of 200W and a frequency of 30kHz. The entire process was time-inducing to promote uniform distribution of nanoparticles and interfacial wetting. The quartz tube was inserted to a depth of 2 / 3 of the melt height, and the melt temperature fluctuation during introduction was ≤5℃. After introduction, stirring continued for 7.5 min. The melt surface was covered with an argon protective layer with a thickness of 7.5 cm. When introducing the nanoparticles, 0.03 parts by weight of calcium fluoride (CAS No.: 7789-75-5) was injected simultaneously as a flux (3g). A mixed carrier gas system was introduced: the carrier gas was a mixture of argon and helium (CAS No.: 7440-59-7) with a volume ratio of 1:0.35 and a total flow rate of 3.5 L / min to improve the nanoparticle delivery efficiency. After introduction, the melt was stirred by a rotating magnetic field with a magnetic field strength of 0.2T, a rotation speed of 75 r / min, and a time of 15 min. The composite melt was sampled and analyzed to determine the uniformity of nanoparticle dispersion, with a deviation of ≤5%. (5) Refining solidification casting: The billet was formed by semi-continuous casting with a cooling rate of 40℃ / s and a thickness of 125mm. Then, it was homogenized and heat-treated at 490℃ for 10h and air-cooled to room temperature to obtain the initial composite alloy ingot. The semi-continuous casting was controlled by online electromagnetic field with a stirring current of 275A and a frequency of 27.5Hz. The length of the stirring zone was 55% of the length of the crystallizer. The secondary water cooling rate was 55℃ / s to form the initial equiaxed crystal structure with a macroscopic segregation of ≤0.15 and a secondary dendrite arm spacing of ≤15μm. The homogenization heat treatment After treatment, X-ray diffraction was used to monitor micro-strain online, and the holding time was adjusted until the grain size was initially refined to 75 μm. The casting mold was preheated to 250℃, and the ingot was immediately water-quenched after demolding at a cooling rate of 75℃ / s. The melt viscosity was monitored during the casting process and adjusted to 2 mPa·s. The ingot was subjected to magnetic levitation vibration treatment at a frequency of 35 Hz, an amplitude of 2 mm, and a time of 7.5 min to refine the solidification structure. The cross-sectional shape of the ingot was optimized to be rectangular with a width-to-thickness ratio of 2. After homogenization, pulsed current treatment was introduced with a current density of 100 A / cm. 2The pulse frequency was 30 Hz and the time was 20 min to promote diffusion and refine the initial structure; further in-situ nanophase formation was introduced: after the introduction in step (4), 0.1 parts of boric acid (CAS No.: 10043-35-3) (10 g) by melt mass was added and reacted at 670℃ for 12.5 min to form in-situ boride nanoparticles (average particle size 20 nm), with a mass ratio of 30% of the introduced nanoparticles. (6) Severe plastic deformation: Equal diameter angular channel extrusion was used, with equivalent strain of 5.5 at 315℃, 4.5 passes, and a channel angle of 105° to obtain nanocrystalline billets; severe plastic deformation was carried out in series: first, equal diameter angular channel extrusion was performed at 360℃, with equivalent strain of 4 and 5.5 passes; then, room temperature high-pressure torsion was performed at a pressure of 4.75 GPa and a rotation of 11.5 revolutions; finally, multi-directional forging was performed at 250℃ for 4 passes, with a total strain of 6.5, which refined the grain size to 140 nm and induced high-density large-angle grain boundaries and non-equilibrium phases; intermediate annealing was used in the deformation gap at a temperature of 325℃ for 2 hours to prevent cracking; the equal diameter angular channel extrusion die was made of high-temperature alloy, lubricated with boron nitride coating, and the extrusion speed was 3 mm / s; the high-pressure torsion die was lined with diamond coating to reduce the friction coefficient to 0.15; deformation was combined with finite element simulation to predict stress distribution and adjust channel geometry parameters; after deformation, the sample was electrolytically polished and the dislocation density was observed to be ≥10 14 m -2 The hardness distribution of the deformed sample was tested by nanoindentation, and the uniformity was ≥95%. (7) Hot deformation and aging: The billet was hot-rolled at 350℃ with a deformation of 60%, and then aged at 180℃ for 13h, followed by air cooling to obtain the finished material; the surface oxide layer was removed before hot rolling, and the lubricant between rolling passes was graphite emulsion (CAS No.: 7782-42-5), with a deformation rate of 20% per pass; the cold deformation before aging was 15%, and dislocations were introduced through cold rolling, followed by two-stage aging: the first stage was held at 150℃ for 6.5h, and the second stage was held at 195℃ for 4.5h to promote the precipitation of fine second phase and the synergistic strengthening of nanoparticles; the hot rolling roll temperature was controlled at 200℃, and the finished material was polished with a surface roughness Ra≤0.5μm; after hot deformation, it was immediately oil quenched at a cooling rate of 150℃ / s, followed by low-temperature deep cryogenic treatment at -196℃ for 3h to induce nanotwins; stress relaxation annealing was inserted between the two-stage aging, at a temperature of 110℃ for 1.5h; aging was carried out in a vacuum furnace with a pressure ≤10 -3Pa prevents oxidation; the finished material is tested for defects by ultrasound and has a density ≥99.5%; the finished product undergoes tensile pre-deformation of 3% to improve fatigue life. The entire process involves online characterization and monitoring of the nanostructure: transmission electron microscopy is used to observe grain size and nanoparticle distribution, scanning electron microscopy combined with electron backscatter diffraction is used to determine grain orientation, X-ray diffraction is used to analyze grain size and strain, and differential scanning calorimetry is used to characterize aging behavior; based on the monitoring results, the amount of nanoparticles added is adjusted by 0.15 parts, the deformation strain is adjusted by 0.75 parts, and the aging temperature is adjusted by 7.5℃ to achieve a nanocrystal size of 115nm and a particle spacing of 65nm; machine learning is used to optimize the process: parameters and microstructure characteristics such as nanoparticle type and content (0.6 parts), melting temperature (735℃), cooling rate (40℃ / s), deformation strain (5.5), aging temperature (180℃), and time (13h) are collected to construct a support vector machine model, train a dataset of 750 sets, and predict the target grain size. A process window of 120nm and a particle spacing of 72.5nm was achieved with an accuracy of 96%. The predicted results guided adjustments to the holding time in step (1) by 7.5min, the carrier gas flow rate in step (4) by 0.75L / min, the number of passes in step (6) by 1.5, and the deformation amount in step (7) by 7.5%. The model input included alloy composition deviation and the influence of environmental humidity, and the output optimized parameter combination to achieve precise control. Multi-scale characterization included atomic probe tomography to analyze the elemental segregation at the nanoparticle interface ≤5at%. The process integrated digital twin model simulated the entire process and predicted the microstructure evolution error ≤10%. Overall process environmental optimization: solvent recovery rate of 95%, and waste gas adsorption by activated carbon (CAS No.: 7440-44-0). The parameters were optimized based on literature, referring to the existing literature "Nature Communications". (2023) on nano-dispersion in Al alloys, Advanced Materials (2025) on hybrid reinforcements, Nano Today (2024) on in-situ phases, Materials & Design (2024) on Mg-Mn synergies, Acta Materialia (2023) on severe deformation” and reference patent US20210238729A1 to ensure innovation; Step (1) The order of adding alloying elements: first melt aluminum, then add manganese, zirconium, titanium, then add magnesium, zinc, copper to avoid volatilization; Step (2) The suspension is treated by a high-pressure homogenizer at a pressure of 150MPa and circulated 4 times; Step (3) The powder is stored in a vacuum seal with a humidity of ≤20%. The obtained high-strength aluminum-magnesium-manganese alloy material has the following physical parameters: grain size 140nm, tensile strength 480MPa, elongation 12%.In addition, the properties of the prepared high-strength aluminum-magnesium-manganese alloy materials are as follows. Figure 1 , Figure 2 , Figure 3 and Figure 4 As shown.
[0029] The specific parameters for Examples 2-12 and Comparative Examples 1-12 are listed in the following tables. The tables are designed according to the progression of the steps, with each table reflecting different parameter values for the examples / comparative examples, covering all endpoint and intermediate values. Only the parameters that have changed from those in Example 1 are listed in the tables; the descriptions of the remaining parameters are the same as in Example 1.
[0030] Table 1: Parameters for preparing aluminum alloy master melt in step (1)
[0031]
[0032] Table 2: Parameters for preparing the nano-ceramic precursor suspension in step (2)
[0033]
[0034] Table 3: Parameters for preparing the nano-ceramic precursor suspension in step (2)
[0035]
[0036] Table 4: Parameters of atomized and dried nanopowder in step (3)
[0037]
[0038] Table 5: Parameters for introducing nanopowder in step (4)
[0039]
[0040] Table 6: Parameter 2 for introducing nanopowder in step (4)
[0041]
[0042] Table 7: Step (5) Refining the parameters of solidification casting
[0043]
[0044] Table 8: Step (5) Refining the parameters of solidification casting
[0045]
[0046] Table 9: Parameters of severe plastic deformation in step (6)
[0047]
[0048] Table 10: Parameters of the second step (6) of intense plastic deformation
[0049]
[0050] Table 11: Parameters for heat deformation and aging in step (7)
[0051]
[0052] Table 12: Parameters for heat deformation and aging in step (7)
[0053]
[0054] Table 13: Other optimization parameters (machine learning, in-situ equivalence, etc.)
[0055]
[0056] Table 14: Parameters for Comparative Example Step (1)
[0057]
[0058] Table 15: Parameters of Comparative Example Step (2)
[0059]
[0060] To verify the performance of the high-strength aluminum-magnesium-manganese alloy material described in this invention, multi-dimensional tests were conducted on the products prepared in Examples 1-12 and Comparative Examples 1-12. The tests included tensile strength (MPa), elongation (%), grain size (nm), particle spacing (nm), corrosion resistance (salt spray test time h), and fatigue life (number of cycles). The test methods are as follows: Tensile strength and elongation test: According to GB / T228.1-2021 standard, an electronic universal testing machine (model: WDW-100) was used. The sample size was a standard dog bone shape, the tensile speed was 2 mm / min, and the maximum strength and elongation percentage before fracture were recorded. Grain size and particle spacing test: A transmission electron microscope (model: JEM-2100F) and an X-ray diffractometer (model: XRD-7000) were used, combined with ImageJ software analysis. The samples were prepared by electrolytic polishing, and the average values were measured. Corrosion resistance test: According to GB / T10125-2012 standard, a salt spray test chamber (model: YWX / Q-250) was used with 5% NaCl solution at a constant temperature of 35℃. The time (h) until obvious rust spots appeared was recorded. Fatigue life test: According to GB / T3075-2008 standard, a high-frequency fatigue testing machine (model: PLG-100C) was used with a stress ratio of 0.1 and a frequency of 100Hz. The number of cycles until fracture was recorded.
[0061] Table 16: Performance Test Results 1 (Example)
[0062]
[0063] Table 17: Performance Test Results II (Example)
[0064]
[0065] Table 18: Performance Test Results 1 (Comparative Example)
[0066]
[0067] Table 19: Performance Test Results II (Comparative Example)
[0068]
[0069] The test results show that the tensile strength of the products in the examples is 452.6-498.7 MPa, the elongation is 10.4-13.8%, and the grain size is 82.1-198.5 nm, demonstrating excellent performance. In contrast, the comparative examples, due to the absence of key raw materials (such as magnesium, which weakens solid solution strengthening and reduces strength by about 30%) or parameter deviations (such as low temperature leading to grain coarsening and a 2-3 fold increase in size), exhibited significantly reduced performance (e.g., strength decreased to 305.4-342.5 MPa, and grain size increased to 405.6-480.6 nm). For example, Example 3, by increasing the nanoparticle content and deformation strain, improved dispersion strengthening, resulting in increased strength but a slight increase in elongation (due to finer grains balancing dislocations). Comparative Example 1, lacking magnesium, weakened solid solution strengthening, leading to decreased strength and elongation. Comparative Example 3, with its low temperature inhibiting grain refinement, resulted in larger grains and a halved fatigue life. This demonstrates the superiority of the preparation method of this invention.
[0070] Overall, the performance indicators of the embodiments are superior to those of the comparative examples, which is consistent with the principles of materials science: uniform dispersion of nanoparticles, grain refinement, and multiphase synergistic strengthening can significantly improve the strength, toughness, and corrosion resistance of alloys. The performance decline of the comparative examples reasonably reflects the sensitivity of key parameters, such as solid solution weakening due to the lack of strengthening elements and grain coarsening caused by temperature deviations. These changes verify the innovation and reliability of the patented method, proving that the optimization window of process parameters (such as melting temperature 720-750℃, nanoparticle addition amount 0.2-1.2 parts) is key to achieving the target performance (tensile strength ≥450MPa, elongation ≥10%, grain size 80-200nm). The following analysis of the changing trends by indicator category, combined with the explanation of the rationality in conjunction with specific comparative examples, further illustrates this.
[0071] Tensile strength (MPa): Examples: 452.6-498.7 MPa (average approximately 480 MPa). The highest value was observed in Example 3 (498.7 MPa), thanks to a higher amount of nanoparticles (1.2 parts), optimized multiphase substitution ratio (80:30:25:15), and large deformation strain (7), which promoted Orowan dispersion strengthening and Hall-Petch grain refinement effects. Comparative examples: 305.4-342.5 MPa (average approximately 325 MPa), a decrease of approximately 30-35%. Trend and rationale: The strength of the comparative examples decreased significantly because: Comparative example 1 (magnesium deficiency): Magnesium is the main solid solution strengthening element, and its deficiency led to a decrease in matrix strength, down to 320.7 MPa (solid solution strengthening contributes approximately 20-30% of the total strength). Comparative example 2 (manganese deficiency, replaced by iron): Iron introduced a harmful phase, increasing brittleness, and the strength decreased to 305.4 MPa (iron contamination is common in existing technologies, leading to strengthening failure). Comparative Example 3 (melting temperature 680℃, below the range): Low temperature hinders uniform diffusion of alloying elements, causing segregation and reducing strength to 340.2 MPa. Other comparative examples (such as Comparative Example 5 with low power, and Comparative Example 9 with excessive zinc) resulted in abnormal melt viscosity or precipitation of harmful phases, further weakening interfacial bonding. The overall decrease verifies the necessity of the melting parameters (710-760℃) and element ratios in the patent, avoiding the strength bottleneck of existing technologies (<350 MPa). Elongation (%): Examples show: 10.4-13.8% (average about 12%). Example 3 has the highest (13.8%), due to the fine grains (82.1 nm) and uniform particle distribution improving dislocation slip capability, balancing strength and toughness. Comparative examples show: 5.8-7.0% (average about 6.3%), a decrease of about 40-50%. Trends and Justification: The significant decrease in elongation in the comparative examples reasonably reflects the deterioration of the microstructure: Comparative Example 1 (Magnesium deficiency): Magnesium enhances plasticity, but its absence weakens grain boundaries, reducing elongation to 6.2% (Mg promotes dynamic recovery in Al-Mg-Mn alloys). Comparative Example 7 (Stirring speed 50 r / min, low range): Insufficient stirring causes compositional inhomogeneity, introducing stress concentration points, reducing elongation to 6.3%. Comparative Example 8 (pH 7, low range): Poor suspension stability leads to nanoparticle agglomeration (aggregates > 200 nm), forming crack initiation points, reducing elongation to 5.9%. In-situ phase and dispersion optimization are key to maintaining toughness; the deviations in the comparative examples simulate the low plasticity problem (<8%) in existing technologies, demonstrating that the patented pH adjustment (8-9.5) and stirring optimization improve uniformity. Grain size (nm): Examples show: 82.1-198.5 nm (average approximately 140 nm). The lowest value was in Example 3 (82.1 nm), thanks to the high cooling rate (70 °C / s), large strain (7) and pulsed current treatment, which promoted the formation and refinement of equiaxed crystals.Comparative examples: 405.6-480.6 nm (average approximately 440 nm), an increase of about 2-3 times. Trend and rationality: The significant increase in grain size (coarsening) in the comparative examples is reasonable, as grain refinement depends on drastic deformation and nanopinning. Comparative Example 3 (low melting temperature): Low temperature slows solidification kinetics, increasing dendrite arm spacing (>15 μm), resulting in grain coarsening to 410.8 nm. Comparative Example 10 (copper content less than 0.05 parts): Copper promotes finer nuclei; its absence leads to insufficient nucleation, resulting in grain size increasing to 455.2 nm. Comparative Example 12 (compositional deviation 0.2%): Inhomogeneity leads to localized supersaturation, resulting in grain coarsening to 440.1 nm. The upward trend verifies the effectiveness of the patented electromagnetic field control (current 150-400 A) and deformation series (equal diameter angular extrusion + high-pressure torsion), simulating the grain coarsening problem (hundreds of μm) in existing technologies. Particle spacing (nm): Examples show: 28.6-118.3nm (average approximately 65nm). Example 3 shows the lowest spacing (28.6nm), due to multiphase substitution and ultrasonic assistance (300W) ensuring uniform dispersion, reducing spacing and enhancing pinning effect. Comparative examples show: 190.7-245.7nm (average approximately 215nm), an increase of approximately 2-3 times. Trend and rationality: The comparative examples show increased spacing and weakened enhancement effect, which is reasonable due to dispersion failure: Comparative example 5 (low power): Insufficient heating leads to unstable suspension, particle agglomeration, and spacing increases to 230.8nm. Comparative example 6 (low argon flow rate): Increased oxidation and poor particle adhesion, spacing increases to 200.6nm (carrier gas optimization reduces oxidation in the patent). Comparative example 11 (missing ball milling activation): Low nanoparticle surface activity and poor wetting, spacing increases to 205.4nm. Mixed carrier gas and surface modification are key to controlling spacing; the comparative examples simulate the uneven distribution problem in existing technologies. Salt spray test time (h): Example 1 performance: 1120.9-1380.4h (average about 1250h). Example 3 had the highest time (1380.4h) due to in-situ boride (40%) and interface optimization inhibiting β-phase precipitation, thus improving the corrosion barrier. Comparative example performance: 620.9-685.3h (average about 650h), a decrease of about 45-50%. Trend and rationality: The decrease in corrosion resistance in the comparative examples reasonably reflects grain boundary weakening: Comparative example 2 (iron replacement): iron phase promotes pitting corrosion, time decreased to 620.9h. Comparative example 9 (excess zinc): excessive zinc forms a harmful phase, time decreased to 685.3h (patented ratio control avoids corrosion sensitivity). Comparative example 4 (short holding time): insufficient diffusion, segregation aggravates corrosion, time decreased to 660.2h. The decrease verifies the corrosion resistance effect of the patented two-stage aging and pH adjustment, surpassing existing technologies (<800h). Fatigue life (number of cycles): Example result: 9.8 × 10. 5 -1.4×10 6 (Average 1.2×10) 6 Example 3 showed the highest result (1.4 × 10⁻⁶).6 Due to the high density of nanotwins and dislocations, crack propagation is delayed. Comparative example: 4.1 × 10⁻⁶ 5 -5.1×10 5 (Average 4.6×10) 5 The lifespan decreased by approximately 60%. The trend and rationale: The shortened lifespan in the comparative example is reasonable due to stress concentration. Comparative Example 1 (magnesium deficiency): Low toughness, easy crack propagation, reduced to 4.5 × 10⁻⁶. 5 Comparative Example 7 (low stirring): Uneven distribution forms fatigue sources, reducing fatigue intensity to 4.6 × 10⁻⁶. 5 Comparative Example 10 (low copper): Insufficient grain refinement reduced lifetime to 4.4 × 10⁻⁶. 5 .
[0072] The embodiments show a comprehensive increase in performance metrics (strength, elongation, corrosion resistance, lifespan) or a slight decrease (grain size, particle spacing), demonstrating the systematic nature of the patented method: nano-introduction (atomization + stirring) ensures dispersion, deformation + aging achieves refinement, and machine learning provides precise control (accuracy ≥95%). Negative changes in the comparative examples (e.g., a 30% decrease in strength, a 2-fold increase in grain size) reasonably stem from parameter deviations, simulating pain points in existing technologies (e.g., agglomeration, segregation), and highlighting the innovations of this invention through comparison (e.g., multiphase ratio, in-situ borides). For example, the low temperature / power in comparative examples 3-5 leads to a deterioration in all metrics, verifying the threshold effect of energy input; the elemental deficiencies in comparative examples 1-2 emphasize the synergistic effect of the proportions. This not only proves the rationality of the method but also provides guidance for industrial applications: deviations from the optimization window will significantly reduce performance.
[0073] The above description, in conjunction with specific embodiments, provides a further detailed explanation of the present invention. It should not be construed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, several simple deductions or substitutions can be made without departing from the concept of the present invention, and all such deductions or substitutions should be considered to fall within the scope of protection defined by the claims submitted herein.
Claims
1. A method of producing a high-strength aluminum-magnesium-manganese alloy material, characterized by: The steps are as follows, by weight: (1) Based on 100 parts of total metal element raw materials, with aluminum as the balance, add 2.5-3.5 parts of magnesium, 0.8-1.2 parts of manganese, 0.4-0.6 parts of zinc, 0.1-0.2 parts of copper, 0.1-0.2 parts of zirconium, and 0.03-0.08 parts of titanium, melt them at 720-750℃ under argon protection and hold for 20-30 minutes to obtain an aluminum-magnesium-manganese based melt; (2) Weigh according to a mass ratio of 1:(8-15) Take yttrium oxide nanoparticles and anhydrous ethanol, add 0.2-0.4 times the mass of yttrium oxide nanoparticles of polyvinylpyrrolidone, and disperse under ultrasonic power of 300-500W for 15-30min to obtain a suspension; (3) Spray atomize the suspension of step (2), dry it in hot air at 250-350℃, collect the yttrium oxide nanoparticles coated with polyvinylpyrrolidone, and pack them into a quartz tube at a melt mass of 0.3-0.8 parts for later use; (4) Take the suspension of step (1) The aluminum-magnesium-manganese-based melt is cooled to 650-670℃, the electromagnetic stirring speed is 300-500r / min, and the nanopowder is blown into the aluminum-magnesium-manganese-based melt through a carrier gas flow rate of 2-4L / min for 8-15min. The stirring and temperature are maintained to obtain a composite melt; (5) a semi-continuous casting billet with a cooling rate of 20-60℃ / s is formed with a thickness of 100-150mm, followed by homogenization heat treatment at 480-500℃ for 5-15h, and then air-cooled to At room temperature, an initial composite alloy ingot is obtained; (6) the initial composite alloy ingot is subjected to intense plastic deformation by extrusion through equal diameter channels, and equivalent deformation ≥5 is applied at 250-380℃, with 3-6 passes and a channel angle of 100-110° to obtain a nanocrystalline billet; (7) hot deformation and aging: the nanocrystalline billet is hot rolled at 320-380℃ with a deformation of 50-70%, and then aged at 160-200℃ for 8-18 hours, and air-cooled to obtain the finished material.
2. The method of producing a high-strength aluminum-magnesium-manganese alloy material according to claim 1, characterized by: In step (3), the spray atomization uses a centrifugal atomizer with a rotation speed of 8000-12000 rpm and a hot air flow rate of 5-10 m / s. After drying, the powder is sieved, and the particle size is controlled at 50-200 nm. The powder is then vacuum dried to remove residual solvent. In step (4), before introducing the nanopowder, 0.02-0.08 parts of hexachloroethane are added to the aluminum-magnesium-manganese-based melt for 8-12 min of refining. Nitrogen gas is simultaneously introduced as an auxiliary carrier gas with 1-2.5 L / min of argon bubbling and a flow rate of 0.5-2 L / min.
3. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (5), the semi-continuous casting adopts online electromagnetic field control, with a stirring current of 150-400A, a frequency of 15-40Hz, a stirring zone length of 40-70% of the crystallizer length, and a secondary water cooling rate of 30-80℃ / s to form an initial equiaxed crystal structure with a macroscopic segregation degree ≤0.15 and a secondary dendrite arm spacing ≤15μm. After the homogenization heat treatment in step (5), the micro-strain is monitored online by X-ray diffraction, and the holding time is adjusted until the grain size is initially refined to 50-100μm.
4. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (6), the intense plastic deformation adopts a series process: first, equal diameter angular channel extrusion is carried out at 320-400℃, with equivalent strain of 3-5 and 4-7 passes; then, room temperature high-pressure torsion is carried out at a pressure of 4-5.5GPa and a rotation of 8-15 revolutions; finally, multi-directional forging is carried out at 220-280℃ for 3-5 passes, with a total strain ≥6, so that the grain size is refined to 80-200nm, inducing high-density large-angle grain boundaries and non-equilibrium phases. At the same time, intermediate annealing is carried out between deformations at a temperature of 300-350℃ for 1-3h. In step (7), the surface oxide layer is removed before hot rolling, and the lubricant between rolling passes is graphite emulsion, with a deformation rate of 15-25% per pass; the cold deformation amount before aging is 10-20%, and dislocations are introduced through cold rolling, followed by two-stage aging: the first stage is held at 140-160℃ for 5-8h, and the second stage is held at 180-210℃ for 3-6h.
5. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (1), the metal raw material is ultrasonically cleaned and rinsed and dried with anhydrous ethanol before melting. The melting process is carried out by induction heating with a power of 10-20kW. Argon gas is introduced at a flow rate of 3-5L / min during heat preservation and the stirring speed is 100-200r / min to ensure that the uniformity deviation of the composition is ≤0.1%. In step (2), the suspension is prepared by a high-shear mixer with a speed of 5000-10000rpm. After premixing for 10-20min, it is ultrasonically mixed. The molecular weight of the dispersant polyvinylpyrrolidone is controlled at 10000-40000.
6. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (3), the dried nanopowder is subjected to plasma surface modification with a power of 50-150W and a time of 5-10min to improve its compatibility with the melt; in step (4), the quartz tube is inserted to a depth of 2 / 3 of the melt height, and the melt temperature fluctuation is ≤5℃ when it is blown in. After introduction, it is stirred for 5-10min; in step (5), the casting mold is preheated to 200-300℃, and the ingot is immediately water-quenched after demolding at a rate of 50-100℃ / s; in step (6), the material of the equal diameter angular channel extrusion die is a high-temperature alloy, the lubricant is a boron nitride coating, and the extrusion speed is 1-5mm / s; in step (7), the temperature of the hot rolling roll is controlled at 150-250℃, and the finished material is polished with a surface roughness Ra≤0.5μm.
7. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (2), the nanoparticles are pretreated by ball milling with yttrium oxide and other materials at a ball-to-material ratio of 5:1-10:1, a rotation speed of 300-400 r / min, and a time of 2-4 h, resulting in the attachment of hydroxyl groups on the surface. 0.05-0.15 times the mass of silane coupling agent is added to the suspension and stirred for 30-60 min. In step (3), the drying is assisted by vacuum freeze drying at a temperature of -50~-30℃ for 4-8 h, with residual moisture ≤0.5%.
8. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: In step (4), the surface of the melt is covered with an argon protective layer of 5-10 cm thickness. When introducing the nanopowder, 0.01-0.05 parts by weight of calcium fluoride as a flux is simultaneously injected into the aluminum-magnesium-manganese-based melt. In step (5), the melt viscosity is monitored during the casting process and adjusted to 1.5-2.5 mPa·s. In step (7), aging is carried out in a vacuum furnace with a pressure ≤10. -3 Pa.
9. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: Introducing a mixed carrier gas system: In step (4), the carrier gas is a mixture of argon and helium with a volume ratio of 1:0.2-0.5 and a total flow rate of 2.5-4.5 L / min, which improves the transport efficiency of nanoparticles; In step (5), the ingot is subjected to magnetic levitation vibration treatment with a frequency of 20-50 Hz, an amplitude of 1-3 mm, and a time of 5-10 min, which refines the solidification structure; In step (6), the high-pressure torsion mold is lined with a diamond coating to reduce the friction coefficient to 0.1-0.
2.
10. The method of producing a high-strength Al-Mg-Mn alloy material according to claim 1, characterized by: Step (1) Order of alloying elements added: first melt aluminum, then add manganese, zirconium, titanium, then add magnesium, zinc, and copper; Step (2) The suspension is treated by a high-pressure homogenizer at a pressure of 100-200 MPa and circulated 3-5 times; Step (3) The powder is stored in a vacuum seal with a humidity of ≤20%; Step (4) After introduction, the melt is stirred by a rotating magnetic field with a magnetic field strength of 0.1-0.3T, a rotation speed of 50-100 r / min, and a time of 10-20 min; Step (5) The cross-sectional shape of the ingot is optimized to be rectangular with a width-to-thickness ratio of 1.5-2.5.
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