A soluble magnesium alloy material and a preparation method thereof based on electromagnetic stirring and heat treatment

Abstract

The application particularly relates to a soluble magnesium alloy material and a preparation method thereof based on electromagnetic stirring and heat treatment. a Al b Zn c Fe d Gd e Y f Ni g alloy; wherein a+b+c+d+e+f+g=100%; 0.5wt.%.

Description

Technical Field

[0001] The present invention relates to the technical field of metal material processing, and specifically relates to a soluble magnesium alloy material and a preparation method thereof based on electromagnetic stirring synergistic heat treatment. Background Art

[0002] In the related art, for magnesium-rare earth alloys (soluble Mg-RE alloys), coarse Mg 12 RE, Mg 41 RE5 and other rare earth-containing cathode phases are easily formed. These phases have high corrosion potential, and as micro-galvanic cathodes, they will accelerate the dissolution of the matrix, form large local cathode regions, induce non-uniform corrosion, and manifest as severe pitting corrosion or local deep pits. Meanwhile, the type, size and distribution of such cathode phases also significantly affect the mechanical properties.

[0003] It should be noted that the information disclosed in the above Background Art section is only for enhancing the understanding of the background of the present invention, and therefore may include information that does not constitute prior art known to a person of ordinary skill in the art. Contents of the Invention

[0004] The present invention provides a soluble magnesium alloy material and a preparation method of the soluble magnesium alloy material based on electromagnetic stirring synergistic heat treatment, which can effectively overcome the defects existing in the prior art.

[0005] Other characteristics and advantages of the present invention will become apparent from the following detailed description, or partially be learned through the practice of the present invention.

[0006] According to a first aspect of the present invention, a soluble magnesium alloy material is provided, and the soluble magnesium alloy material is Mg a Al b Zn c Fe d Gd e Y f Ni g alloy; wherein, based on a+b+c+d+e+f+g=100%; 0.5wt.%<b<5wt.%, 0.2wt.%<c<4.5wt.%, 0.1wt.%<d<1.2wt.%, 3.0wt.%<e<10.0wt.%, 1.0wt.%<f<5.0wt.%, 0.1wt.%<g<1.5wt.%, and the balance is a.

[0007] In some exemplary embodiments, the soluble magnesium alloy material is Mg a Al b Zn c Fe d Gd e Y fNi g Zr h alloy; Of which, 0.2 wt.% <h<0.5wt.%。

[0008] According to a second aspect of the present invention, a method for preparing a soluble magnesium alloy material based on electromagnetic stirring synergistic heat treatment is provided, comprising: 1) Weigh out the magnesium-gadolinium master alloy, magnesium-yttrium master alloy, magnesium-nickel master alloy, Mg particles, Al particles, Zn particles, and aluminum-iron alloy by mass; place the Mg particles, Al particles, Zn particles, Al-Fe alloy, Mg-Ni, Mg-Gd, and Mg-Y master alloys in a copper crucible in a bottom-up order; 2) Fill the electric arc melting equipment with protective gas and control the pressure inside the chamber to stabilize at 1×1 02 Pa ~ 1×10 3 Pa; 3) Melt the material until it is completely melted to obtain a molten liquid; then cool it to obtain an alloy ingot; 4) Melt the alloy ingot until it is completely melted, and then perform multi-stage electromagnetic stirring on the melt; then remove the electromagnetic stirring and cool it to obtain a magnesium alloy ingot. 5) Solution treatment is performed on the magnesium alloy ingots to eliminate component segregation; 6) The alloy material after solution treatment is subjected to aging treatment to obtain soluble magnesium alloy material.

[0009] In some exemplary embodiments, a protective gas is introduced into the arc melting equipment, and the pressure inside the chamber is controlled to be stable at 1×10⁻⁶. 2 Pa ~ 1×10 3 Pa, including: The mechanical pump was used to evacuate the gas pressure inside the arc melting equipment chamber to below 10 Pa, and then high-purity argon gas was introduced to a pressure of 1×10 Pa. 4 Pa; repeat the above process 3 times to stabilize the working pressure inside the cavity at 1×10 Pa. 2 Pa ~ 1×10 3 Between Pa.

[0010] In some exemplary embodiments, the material is melted until completely melted to obtain a molten liquid; subsequently cooled to obtain an alloy ingot, comprising: Increase the operating current of the electric arc melting equipment to 100 A-200 A to achieve alloy pre-melting; Increase the operating current to 250 A-350 A, and after the alloy is completely melted, cool it to obtain an alloy ingot; Flip the alloy ingot and repeat the above process 2-3 times to obtain an alloy ingot with uniform composition.

[0011] In some exemplary embodiments, the molten metal is subjected to multi-stage electromagnetic stirring, including: In the first stage, the melt temperature is maintained at 680℃-850℃, and electromagnetic stirring is applied; the stirring current is 10-20A, and the time is 30s. In the second stage, the melt temperature is maintained at 550℃-630℃, and electromagnetic stirring is applied; the stirring current is 5-10A, and the holding time is 20s.

[0012] In some exemplary embodiments, solution treatment of magnesium alloy ingots includes: The magnesium alloy ingots were solution treated by controlling the heating temperature to 450-540°C at a rate of 10°C / min and holding for 6-12 hours; then water quenched to room temperature.

[0013] In some exemplary embodiments, aging treatment is performed on the solution-treated alloy material, including: The alloy material is subjected to aging treatment, with the heating temperature controlled to rise to 180-270°C at a rate of 10°C / min, and held for 15-30 hours; then it is air-cooled to room temperature.

[0014] The soluble magnesium alloy material and its preparation method provided in the embodiments of the present invention optimize the composition of the alloy by configuring zinc and iron in the material and combining them with gadolinium and yttrium; while controlling the nickel content to be 0.1-1.5 wt.% and the iron content to be 0.1-1.2 wt.%, and densifying the alloy powder to achieve synergistic regulation of the dissolution rate and mechanical properties of the alloy.

[0015] In the alloy preparation process, the magnesium alloy is prepared in a cast state, allowing the precipitates to be dispersed in the matrix at the micro- and nano-scale. This provides an ideal microstructure basis for achieving uniform and rapid corrosion of the magnesium alloy. Furthermore, by using solution treatment followed by aging to prepare a soluble magnesium alloy, coarse primary precipitates are reduced, and fine precipitates are generated and dispersed, promoting uniform and rapid corrosion, maximizing the galvanic corrosion effect, and simultaneously avoiding the formation of localized corrosion pits.

[0016] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit the invention. Attached Figure Description

[0017] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention. It is obvious that the drawings described below are merely some embodiments of the invention, and those skilled in the art can obtain other drawings based on these drawings without any inventive effort.

[0018] Figure 1 The diagram illustrates an exemplary embodiment of the present invention: a method for preparing a soluble magnesium alloy material based on electromagnetic stirring combined with heat treatment. Figure 2 This schematic diagram illustrates the morphology of an alloy powder according to an exemplary embodiment of the present invention. Figure 3 This diagram illustrates a variation in the compressive properties of an alloy according to an exemplary embodiment of the present invention. Figure 4 A schematic diagram illustrating another alloy powder morphology according to an exemplary embodiment of the present invention is shown. Figure 5 This schematic diagram illustrates another variation in the compressive properties data of an alloy, as per an exemplary embodiment of the present invention. Figure 6 A schematic diagram illustrating another alloy powder morphology according to an exemplary embodiment of the present invention is shown. Figure 7 This schematic diagram illustrates another example of the variation in the compressive properties data of an alloy according to an exemplary embodiment of the present invention. Detailed Implementation

[0019] Exemplary embodiments will now be described more fully with reference to the accompanying drawings. However, these exemplary embodiments can be implemented in many forms and should not be construed as limited to the examples set forth herein; rather, they are provided so that the invention will be more comprehensive and complete, and will fully convey the concept of the exemplary embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.

[0020] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0021] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0022] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.

[0023] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0024] In related technologies, magnesium alloys, with their low density, high specific strength, and excellent processing performance, while also being prone to corrosion, have become one of the ideal materials for preparing soluble pressure bridge plugs. However, their low absolute strength and insufficient dissolution rate severely limit their practical application in the oil and gas field. To overcome this bottleneck, researchers have adopted a strategy combining alloying and thermomechanical treatment to finely control the microstructure. For example, adding elements such as Al and Zn can effectively improve mechanical strength, while introducing elements such as Cu and Ni will generate a large number of intermetallic compound particles (such as Mg2Ni, Al2Cu, MgAlCu, and LPSO phases) in the matrix. These particles, acting as cathode phases, can accelerate alloy dissolution but are prone to inducing uneven corrosion. It is worth noting that existing research shows that the improvement of the mechanical properties of magnesium alloys is often accompanied by a decrease in the dissolution rate, and vice versa. This trade-off between properties poses a significant challenge to the synergistic control of overall performance. Therefore, how to significantly improve the dissolution rate while maintaining sufficient strength has become a core problem that urgently needs to be solved in the current oil and gas field.

[0025] The development of soluble magnesium alloys focuses on the synergistic matching of mechanical load-bearing capacity and corrosion dissolution. Current performance improvements primarily revolve around three directions. First, composition optimization based on alloying involves the targeted addition of elements such as Zn, Ca, Al, and rare earth elements to precisely control the electrochemical potential of the magnesium matrix and the type, quantity, and distribution of precipitated phases, seeking a balance between mechanical strength and dissolution rate to meet performance requirements under different working conditions. Second, combining thermoplastic deformation with heat treatment, comprehensively utilizing plastic processing techniques such as extrusion, rolling, and forging, as well as heat treatment methods such as solution treatment and aging, to effectively refine matrix grains, disperse agglomerated precipitates, and optimize the morphology and size distribution of the second phase, thereby improving the problems of excessively rapid localized corrosion and uneven degradation in traditional magnesium alloys. Third, focusing on developing novel multi-component alloy systems, breaking through the limitations of traditional binary and ternary compositions, and leveraging the synergistic effect of multiple components to compensate for the performance shortcomings caused by the addition of a single element, further improving dissolution controllability and structural stability.

[0026] Although the three main R&D paths for current soluble magnesium alloys can achieve basic performance regulation, they still have common shortcomings in accurately matching the core goal of mechanical load bearing and corrosion dissolution. Alloying optimization faces the problem of insufficient element synergy, and single or multiple additions are difficult to take into account the precise balance between strength and dissolution rate. Excessive introduction of rare earth and other elements not only drives up costs, but also easily causes agglomeration of precipitated phases, which instead increases the risk of local corrosion. The coupled regulation of thermoplastic deformation and heat treatment is restricted by process compatibility defects. It is difficult to match the parameters of plastic processing and heat treatment, which easily causes uneven grain size and residual stress fluctuation, affects the degradation uniformity, and at the same time, the complex process also increases energy consumption and production costs. The development of new multi-component alloy systems is still in the exploratory stage, with insufficient understanding of multi-component interaction mechanisms and precipitation rules, prominent problems of component segregation and uneven structure, and a long R&D cycle, making it difficult to quickly respond to the demands of practical scenarios such as oil and gas engineering. On the whole, the three types of technical paths generally have common problems such as insufficient performance regulation accuracy, imbalance between cost and efficiency, and lack of industrialization adaptability, which restrict the technical leap of soluble magnesium alloys from laboratory controllability to engineering reliability.

[0027] Aiming at the problems existing in the prior art, the present invention provides a soluble magnesium alloy material which is Mg a Al b Zn c Fe d Gd e Y f Ni g alloy; wherein, based on a+b+c+d+e+f+g=100%; 0.5wt.%<b<5wt.%, 0.2wt.%<c<4.5wt.%, 0.1wt.%<d<1.2wt.%, 3.0wt.%<e<10.0wt.%, 1.0wt.%<f<5.0wt.%, 0.1wt.%<g<1.5wt.%, and the balance is a.

[0028] In an exemplary embodiment, the soluble magnesium alloy material further includes zirconium Zr. The soluble magnesium alloy material is Mg a Al b Zn c Fe d Gd e Y f Ni g Zr h alloy; wherein 0.2wt.%<h<0.5wt.%.

[0029] This invention improves the heat resistance of soluble magnesium alloys by using Zn and Fe in combination with gadolinium (Gd), yttrium (Y), and nickel (Ni), utilizing the combination of Gd and Y and controlling their composition. Simultaneously, the solid solution and aging process precipitates Mg5Gd and β'-Y phases, thereby enhancing tensile strength. Furthermore, it forms a long-period ordered LPSO phase, refining the microstructure. Additionally, the addition of trace amounts of iron suppresses localized pitting corrosion. Moreover, it offers advantages such as higher strength, more uniform dissolution, less breakage, and lower cost.

[0030] Furthermore, adding an appropriate amount of zirconium (Zr) to the alloy can improve yield strength and microstructure uniformity. It can also significantly refine grains, greatly improve toughness and strength, reduce grain boundary corrosion, and promote more uniform dissolution, without affecting the Ni / Fe acceleration effect.

[0031] The soluble magnesium alloy provided by this invention has the following alloy properties: compressive strength of 360-420 MPa, elongation of 4-12%, and corrosion rate of 90-135 mg / cm2.h (93℃, 3% KCl solution).

[0032] For example, the content of each element can be any value within the above-mentioned mass percentage range. Specifically, by mass percentage, the soluble magnesium alloy material comprises the following components: aluminum (Al): 0.5-5.0 wt.%; zinc (Zn): 0.2-4.5 wt.%; iron (Fe): 0.1-1.2 wt.%; nickel (Ni): 0.1-1.5 wt.%; yttrium (Y): 1.0-5.0 wt.%; gadolinium (Gd): 3.0-10.0 wt.%. The balance is magnesium (Mg): 82-93 wt.%.

[0033] In addition, it may also include: zirconium (Zr): 0.2-0.5 wt.%; the balance being magnesium (Mg).

[0034] In one embodiment, the Al component in the soluble magnesium alloy may be 0.5%, 1%, 2%, 3%, 4%, 4.5%, or 5% by mass. Preferably, the Al component may be 2.6-3.6 wt.% by mass.

[0035] In one embodiment, the Zn component in the soluble magnesium alloy may be 0.2%, 0.8%, 1%, 2%, 3%, 4%, or 4.5% by mass. Preferably, the Zn component may be 1.5%-2.0% by mass.

[0036] In one embodiment, the Fe component in the soluble magnesium alloy may be 0.1 wt.%, 0.4 wt.%, 0.6 wt.%, 0.2 wt.%, 0.8 wt.%, 1.0 wt.%, and 1.2 wt.% by mass. Preferably, the Al component may be 0.15-0.2 wt.% by mass.

[0037] In one embodiment, the Ni component in the soluble magnesium alloy may be 0.1 wt.%, 0.3 wt.%, 0.5 wt.%, 0.8 wt.%, 1 wt.%, 1.2 wt.%, or 1.5 wt.% by mass. Preferably, the Al component may be 0.8-1.2 wt.% by mass.

[0038] In one embodiment, the Y component in the soluble magnesium alloy may be 1%, 1.5%, 2%, 3%, 4%, 4.5%, or 5% by mass. Preferably, the Y component may be 2.4-3.0 wt.% by mass.

[0039] In one embodiment, the Gd component in the soluble magnesium alloy may be 3%, 4%, 5%, 6%, 7.5%, 9%, or 10% by mass. Preferably, the Y component may be 6-6.8 wt.% by mass.

[0040] In one embodiment, the Zr component in the soluble magnesium alloy may be 0.2 wt.%, 0.25 wt.%, 0.3 wt.%, 0.35 wt.%, 0.4 wt.%, 0.45 wt.%, and 0.5 wt.% by mass. Preferably, the Al component may be 0.35-0.42 wt.% by mass.

[0041] In one exemplary embodiment, a method for preparing a soluble magnesium alloy material based on electromagnetic stirring synergistic heat treatment is provided, which can be applied to the preparation of the soluble magnesium alloy in the above embodiments. (Reference) Figure 1 As shown, the method includes: Step S11: Weigh out the magnesium-gadolinium master alloy, magnesium-yttrium master alloy, magnesium-nickel master alloy, Mg particles, Al particles, Zn particles, and aluminum-iron alloy by mass; place the Mg particles, Al particles, Zn particles, Al-Fe alloy, Mg-Ni, Mg-Gd, and Mg-Y master alloys into a copper crucible in a bottom-up order; Step S12: Fill the electric arc melting equipment with protective gas and control the pressure inside the cavity to stabilize at 1×10⁻⁶. 2 Pa ~ 1×10 3 Pa, pre-melting the material; Step S13: Melt the material until it is completely melted to obtain a molten liquid; then cool it to obtain an alloy ingot. Step S14: Melt the alloy ingot until it is completely melted, and perform multi-stage electromagnetic stirring on the melt; then remove the electromagnetic stirring and cool it to obtain a magnesium alloy ingot. Step S15: The magnesium alloy ingot is subjected to solution treatment to eliminate compositional segregation; Step S16: The alloy material after solution treatment is subjected to aging treatment to obtain soluble magnesium alloy material.

[0042] For example, in step S11, zirconium can also be weighed by mass.

[0043] For example, in step S11, Mg particles, Al particles, Zn particles, Al-Fe, Mg-Ni, Mg-Gd and Mg-Y master alloys are placed in a copper crucible in a bottom-up order.

[0044] For example, step S12 specifically includes: The mechanical pump was used to evacuate the gas pressure inside the arc melting equipment chamber to below 10 Pa, and then high-purity argon gas was introduced to a pressure of 1×10 Pa. 4 Pa; repeat the above process 3 times to stabilize the working pressure inside the cavity between 1×102 Pa and 1×103 Pa.

[0045] For example, step S13 specifically includes: Increase the operating current of the electric arc melting equipment to 100 A-200 A to achieve alloy pre-melting; Increase the operating current to 250 A-350 A, and after the alloy is completely melted, cool it to obtain an alloy ingot; Flip the alloy ingot and repeat the above process 2-3 times to obtain an alloy ingot with uniform composition.

[0046] For example, multi-stage electromagnetic stirring of the molten metal includes: In the first stage, the melt temperature is maintained at 680℃-850℃, and electromagnetic stirring is applied; the stirring current is 10-20A, and the time is 30s. In the second stage, the melt temperature is maintained at 550℃-630℃, and electromagnetic stirring is applied; the stirring current is 5-10A, and the holding time is 20s.

[0047] For example, solution treatment of magnesium alloy ingots includes: The magnesium alloy ingots were solution treated by controlling the heating temperature to 450-540°C at a rate of 10°C / min and holding for 6-12 hours; then water quenched to room temperature.

[0048] For example, aging treatment of alloy materials after solution treatment includes: The alloy material is subjected to aging treatment, with the heating temperature controlled to rise to 180-270°C at a rate of 10°C / min, and held for 15-30 hours; then it is air-cooled to room temperature.

[0049] The preparation method will be described in detail below with reference to the embodiments.

[0050] In a first exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.1-1.2 wt.%; Al: 0.5-5.0 wt.%; Zn: 0.2-4.5 wt.%; Gd: 3.0-10.0 wt.%; Y: 1.0-5.0 wt.%; Ni: 0.1-1.5 wt.%; the balance is Mg. It may also contain trace impurities. Among them, impurities may include Mn and Cu.

[0051] (2) Place Mg particles, Al particles, Zn particles, Al-Fe, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order, so that the low melting point material is at the bottom and the high melting point material is at the top.

[0052] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 2 Pa ~ 1×10 3 Between Pa.

[0053] (4) Turn on the melting function, increase the working current to 100 A-200 A to achieve alloy pre-melting, and then increase the working current to 250 A-350 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0054] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated 2-3 times, with the aim of obtaining a uniform alloy ingot through multiple melting and mixing.

[0055] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 680℃-850℃, apply electromagnetic stirring with a stirring current of 10-20A, and hold for 30s. Then reduce the working current to maintain the melt temperature at 550℃-630℃, continue applying electromagnetic stirring with a stirring current of 5-10A, and hold for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0056] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 450-540°C, the heating rate is 10°C / min, and the temperature is held for 6-12 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0057] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 180-270°C, the heating rate is 10°C / min, the holding time is 15-30h, and then air cooling is performed.

[0058] In a second exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.1wt.%; Al: 0.5wt.%; Zn: 0.2wt.%; Gd: 3.0wt.%; Y: 1.0wt.%; Ni: 0.1wt.%; the balance is Mg.

[0059] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0060] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 2 Between PaPa.

[0061] (4) Turn on the melting function, increase the working current to 100 A to achieve alloy pre-melting, and then increase the working current to 250 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0062] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated 3 times, with the aim of obtaining a uniform alloy ingot through multiple melting and mixing.

[0063] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 680°C, apply electromagnetic stirring with a stirring current of 10A for 30s. Then reduce the working current to maintain the melt temperature at 630°C, continue applying electromagnetic stirring with a stirring current of 10A for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0064] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 450°C, the heating rate is 10°C / min, and the temperature is held for 6 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0065] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 180°C, the heating rate is 10°C / min, the temperature is held for 15 hours, and then air-cooled.

[0066] refer to Figure 2 , Figure 3 The figure shows the morphology and compressibility of the alloy powder.

[0067] In a third exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 1.2 wt.%; Al: 5.0 wt.%; Zn: 4.5 wt.%; Gd: 10.0 wt.%; Y: 5.0 wt.%; Ni: 1.5 wt.%; the balance is Mg.

[0068] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0069] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 3 Between Pa.

[0070] (4) Turn on the melting function, increase the working current to 200 A to achieve alloy pre-melting, and then increase the working current to 350 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0071] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated twice to obtain a uniform alloy ingot through multiple melting and mixing.

[0072] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 850°C, apply electromagnetic stirring with a stirring current of 20A for 30s. Then reduce the working current to maintain the melt temperature at 630°C, continue applying electromagnetic stirring with a stirring current of 10A for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0073] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 540°C, the heating rate is 10°C / min, and the temperature is held for 6 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0074] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 270°C, the heating rate is 10°C / min, the holding time is 30h, and then it is air cooled.

[0075] refer to Figure 4 , Figure 5 The figure shows the morphology and compressibility of the alloy powder.

[0076] In a fourth exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.15 wt.%; Al: 3.0 wt.%; Zn: 2.0 wt.%; Gd: 6.5 wt.%; Y: 0.5 wt.%; Ni: 1.2 wt.%; the balance is Mg.

[0077] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0078] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 3 Between Pa.

[0079] (4) Turn on the melting function, increase the working current to 160A to achieve alloy pre-melting, and then increase the working current to 300A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0080] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated twice to obtain a uniform alloy ingot through multiple melting and mixing.

[0081] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 800°C, apply electromagnetic stirring with a stirring current of 16A for 30s. Then reduce the working current to maintain the melt temperature at 600°C, continue applying electromagnetic stirring with a stirring current of 8A for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0082] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 500°C, the heating rate is 10°C / min, and the temperature is held for 12 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0083] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 240°C, the heating rate is 10°C / min, the temperature is held for 24 hours, and then air-cooled.

[0084] refer to Figure 6 , Figure 7 The figure shows the morphology and compressibility of the alloy powder.

[0085] In a fifth exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.1-1.2 wt.%; Al: 0.5-5.0 wt.%; Zn: 0.2-4.5 wt.%; Gd: 3.0-10.0 wt.%; Y: 1.0-5.0 wt.%; Ni: 0.1-1.5 wt.%; Zr: 0.2-0.5 wt.%; the balance is Mg.

[0086] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Zr, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0087] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 2 Pa ~ 1×10 3 Between Pa.

[0088] (4) Turn on the melting function, increase the working current to 100 A-200 A to achieve alloy pre-melting, and then increase the working current to 250 A-350 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0089] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated 2-3 times, with the aim of obtaining a uniform alloy ingot through multiple melting and mixing.

[0090] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 680℃-850℃, apply electromagnetic stirring with a stirring current of 10-20A, and hold for 30s. Then reduce the working current to maintain the melt temperature at 550℃-630℃, continue applying electromagnetic stirring with a stirring current of 5-10A, and hold for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0091] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 450-540°C, the heating rate is 10°C / min, and the temperature is held for 6-12 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0092] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 180-270°C, the heating rate is 10°C / min, the holding time is 15-30h, and then air cooling is performed.

[0093] In a sixth exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.12wt.%; Al: 3.5wt.%; Zn: 1.8wt.%; Gd: 6.6wt.%; Y: 2.4wt.%; Ni: 1.0wt.%; Zr: 0.4wt.%; the balance is Mg.

[0094] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Zr, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0095] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 3 Between Pa.

[0096] (4) Turn on the melting function, increase the working current to 200 A to achieve alloy pre-melting, and then increase the working current to 350 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0097] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated twice to obtain a uniform alloy ingot through multiple melting and mixing.

[0098] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 850°C, apply electromagnetic stirring with a stirring current of 20A, and hold for 30s. Then reduce the working current to maintain the melt temperature at 550°C, continue applying electromagnetic stirring with a stirring current of 5A, and hold for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0099] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 540°C, the heating rate is 10°C / min, and the temperature is held for 12 hours. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0100] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 270°C, the heating rate is 10°C / min, the holding time is 30h, and then it is air cooled.

[0101] In a seventh exemplary embodiment, the method for preparing a soluble magnesium alloy may include the following steps: (1) The alloy composition includes: Fe: 0.1-0.15 wt.%; Al: 3-3.2 wt.%; Zn: 1.5-1.8 wt.%; Gd: 6.0-7.0 wt.%; Y: 2.2-2.6 wt.%; Ni: 0.85-1.1 wt.%; Zr: 0.38-0.42 wt.%; the balance is Mg.

[0102] (2) Place the Mg particles, Al particles, Zn particles, Al-Fe, Zr, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-up order.

[0103] (3) Turn on the electric arc melting equipment, start the mechanical pump, pump the gas pressure in the cavity to below 10 Pa, and fill it with high-purity argon gas to 1×10 Pa. 4 The above process is repeated 3 times to finally stabilize the working pressure inside the cavity at 1×10 Pa. 2 Between Pa.

[0104] (4) Turn on the melting function, increase the working current to 100 A to achieve alloy pre-melting, and then increase the working current to 250 A. After the alloy is completely melted, cool it to obtain alloy ingot.

[0105] (5) Flip the alloy ingot and repeat steps (3)-(4). This process is repeated 3 times, with the aim of obtaining a uniform alloy ingot through multiple melting and mixing.

[0106] (6) During the final melting of the alloy ingot, after the magnesium alloy ingot has completely melted, maintain the melt temperature at 680°C, apply electromagnetic stirring with a stirring current of 10A for 30s. Then reduce the working current to maintain the melt temperature at 630°C, continue applying electromagnetic stirring with a stirring current of 10A for 20s. Then remove the electromagnetic stirring, cool, and obtain the magnesium alloy ingot.

[0107] (7) The as-cast alloy is subjected to solution treatment, wherein the heating temperature is raised to 520°C, the heating rate is 10°C / min, and the temperature is held for 10h. Then, it is quenched in water to room temperature to fully dissolve the coarse eutectic phase and eliminate compositional segregation.

[0108] (8) The alloy from step (7) is subjected to aging treatment, wherein the heating temperature is raised to 250°C, the heating rate is 10°C / min, the temperature is held for 24 hours, and then air-cooled.

[0109] The present invention provides a method for preparing soluble magnesium alloys. This method utilizes arc melting and electromagnetic stirring techniques to prepare as-cast magnesium alloys, allowing precipitates to be dispersed in the matrix at the micro- and nano-scale. This provides an ideal microstructure basis for achieving uniform and rapid corrosion of the magnesium alloy. Simultaneously, by employing solution treatment followed by aging to prepare the soluble magnesium alloy, coarse primary precipitates are reduced, while fine precipitates are generated and dispersed, promoting uniform and rapid corrosion, maximizing the galvanic corrosion effect, and avoiding the formation of localized corrosion pits.

[0110] The method of this invention, when the small-particle cathode phase is dispersedly distributed, can form a large number of micro-couple pairs in the alloy, promoting uniform and rapid corrosion, maximizing the galvanic corrosion effect, and effectively avoiding the formation of localized corrosion pits. It also significantly improves the strength and toughness of the alloy. In the process of preparing soluble magnesium alloys by arc melting, applying electromagnetic stirring to the melt can generate forced convection, breaking up local component segregation, uniformly dispersing solute atoms, increasing heterogeneous nucleation sites, and simultaneously breaking down coarse primary phases and inhibiting the subsequent aggregation and growth of precipitates. Ultimately, this achieves significant refinement and uniform dispersion of the precipitates, thereby synergistically optimizing the dissolution rate and mechanical properties, providing a feasible path for the on-demand design of material functional properties.

[0111] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A soluble magnesium alloy material, characterized in that, Soluble magnesium alloy material is Mg a Al b Zn c Fe d Gd e Y f Ni g alloy; Wherein, a+b+c+d+e+f+g=100%; 0.5wt.%<b<5wt.%, 0.2wt.%<c<4.5wt.%, 0.1wt.%<d<1.2wt.%, 3.0wt.%<e<10.0wt.%, 1.0wt.%<f<5.0wt.%, 0.1wt.%<g<1.5wt.%, with the balance being a.

2. The soluble magnesium alloy material according to claim 1, characterized in that, Soluble magnesium alloy material is Mg a Al b Zn c Fe d Gd e Y f Ni g Zr h alloy; Wherein, 0.2wt.%<h<0.5wt.%.

3. A method for preparing soluble magnesium alloy materials based on electromagnetic stirring synergistic heat treatment, characterized in that, Comprising: 1) Weigh magnesium-gadolinium master alloy, magnesium-yttrium master alloy, magnesium-nickel master alloy, Mg particles, Al particles, Zn particles, and aluminum-iron alloy by mass; place the Mg particles, Al particles, Zn particles, Al-Fe alloy, Mg-Ni, Mg-Gd and Mg-Y master alloys in a copper crucible in a bottom-to-top order; 2) Fill the electric arc melting equipment with protective gas and control the pressure inside the chamber to stabilize at 1×10⁻⁶. 2 Pa ~ 1×10 3 Pa; 3) Melt the materials until completely molten to obtain a molten liquid; then perform cooling treatment to obtain an alloy ingot; 4) Melt the alloy ingot until completely molten, and apply multi-stage electromagnetic stirring to the molten liquid; then stop the electromagnetic stirring and perform cooling treatment to obtain a magnesium alloy ingot; 5) Perform solution treatment on the magnesium alloy ingot to eliminate component segregation; 6) Perform aging treatment on the alloy material after the solution treatment; A soluble magnesium alloy material is obtained.

4. The preparation method according to claim 3, characterized in that, A protective gas is introduced into the electric arc melting equipment, and the pressure inside the chamber is controlled to be stable at 1×10⁻⁶. 2 Pa ~ 1×10 3 Pa, including: The mechanical pump was used to evacuate the gas pressure inside the arc melting equipment chamber to below 10 Pa, and then high-purity argon gas was introduced to a pressure of 1×10 Pa. 4 Pa; repeat the above process 3 times to stabilize the working pressure inside the cavity at 1×10 Pa. 2 Pa ~ 1×10 3 Between Pa.

5. The preparation method according to claim 3, characterized in that, Melt the materials until completely molten to obtain a molten liquid; Then perform cooling treatment to obtain an alloy ingot, comprising: Raise the working current of the arc melting equipment to a working current of 100 A-200 A to realize pre-melting of the alloy; Raise the working current to 250 A-350 A, and after the alloy is completely molten, perform cooling to obtain an alloy ingot; Turn over the alloy ingot, repeat the above process 2-3 times to obtain an alloy ingot with uniform components.

6. The preparation method according to claim 3, characterized in that, Applying multi-stage electromagnetic stirring to the molten liquid, comprising: In the first stage, maintain the melt temperature at 680°C-850°C and apply electromagnetic stirring; wherein the stirring current is 10-20A, and the duration is 30s; In the second stage, maintain the melt temperature at 550°C-630°C and apply electromagnetic stirring; wherein the stirring current is 5-10A, and the holding time is 20s.

7. The preparation method according to claim 3, characterized in that, Performing solution treatment on the magnesium alloy ingot, comprising: Perform solution treatment on the magnesium alloy ingot, control the heating temperature to rise to 450-540°C at a heating rate of 10°C / min, and hold for 6-12h; then perform water quenching to room temperature.

8. The preparation method according to claim 3, characterized in that, Performing aging treatment on the alloy material after the solution treatment, comprising: Perform aging treatment on the alloy material, control the heating temperature to rise to 180-270°C at a heating rate of 10°C / min, and hold for 15-30h; then perform air cooling to room temperature.

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