CN116024471A - High-strength plastic multi-water-soluble channel magnesium alloy and preparation method thereof - Google Patents
High-strength plastic multi-water-soluble channel magnesium alloy and preparation method thereof Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 180
- 238000002360 preparation method Methods 0.000 title abstract description 34
- 230000032683 aging Effects 0.000 claims abstract description 41
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- 239000011777 magnesium Substances 0.000 claims abstract description 22
- 238000005266 casting Methods 0.000 claims abstract description 20
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- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
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- 229910052802 copper Inorganic materials 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 105
- 238000001556 precipitation Methods 0.000 claims description 38
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- 230000008569 process Effects 0.000 abstract description 6
- 229910052718 tin Inorganic materials 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 21
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- 238000005260 corrosion Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000003723 Smelting Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 229910017706 MgZn Inorganic materials 0.000 description 5
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- 239000000243 solution Substances 0.000 description 4
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- 238000005728 strengthening Methods 0.000 description 3
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Abstract
The invention discloses a magnesium alloy with high strength and plastic and multiple water-soluble channels and a preparation method thereof, wherein the magnesium alloy comprises the following components in percentage by mass: the alloy comprises 1% -4% of X element, 0.1% -0.4% of Y element, 0% -2% of Z element, the balance of Mg element, at least one of Nd, sm and Zn, at least one of Cu, ni and Sr and at least one of Al and Sn. The preparation method comprises the following steps: and taking required raw materials, and sequentially carrying out uniform mixing, melting, refining, casting, homogenization treatment, high-temperature deformation, low-temperature deformation, aging treatment or creep aging treatment to obtain the magnesium alloy. The magnesium alloy has high plasticity and high dissolution rate, is a novel magnesium alloy with excellent performance, and the preparation method has the advantages of simple process, convenient operation, high production efficiency and the like, is suitable for large-scale preparation, and is convenient for industrial application.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal materials and processing, and relates to a magnesium alloy with high strength and plasticity and high dissolution rate and a preparation method thereof.
Background
Magnesium alloys have been gradually applied to the preparation of soluble products due to the characteristic of easy corrosion. In order to accelerate the dissolution rate of magnesium alloy, the means adopted at the present stage is to add transition group elements and Mg matrix forming compounds as the cathode of the micro-couple, and the Mg matrix is used as the anode of the micro-couple in turn. However, the solid solution limit of transition group elements in the Mg matrix is lower, and the formed micro-couple cathode often causes brittle failure of the magnesium alloy, has unsatisfactory strength and plasticity and increases the damage probability of products. Therefore, researchers adopt the idea of adding rare earth elements to enhance plasticization, and design a Mg-RE-TM system, however, due to the characteristic that rare earth elements are easy to diffuse, no precipitation zone is usually distributed along grain boundaries after aging treatment, and the alloy is difficult to weaken or eliminate through subsequent heat treatment. In addition, based on the prior research results of the inventor of the application, the following is found: the existing method for weakening or eliminating the grain boundary non-precipitation zone has the consequence that the content of the grain boundary compound which cannot be formed or formed is low, so that the corrosion channels in the magnesium alloy are low, and the defect of poor water solubility still exists. Therefore, how to effectively eliminate the precipitation zone of the grain boundary, obtain the magnesium alloy with high strength and plasticity and high dissolution rate and the preparation method matched with the magnesium alloy with simple process, convenient operation and high production efficiency, and have great significance for expanding the wide application of the magnesium alloy.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a magnesium alloy with high strength and plasticity and high dissolution rate and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the magnesium alloy with the high strength and the high plasticity and the multiple water-soluble channels comprises the following components in percentage by mass: 1 to 4 percent of X element, 0.1 to 0.4 percent of Y element, 0 to 2 percent of Z element and the balance of Mg element; the X element is at least one of Nd element, sm element and Zn element; the Y element is at least one of Cu element, ni element and Sr element, and the Z element is at least one of Al element and Sn element.
According to the magnesium alloy with the high-strength and high-plasticity multi-water-soluble channel, when the X element does not contain Zn element, the total content of the X element is 1% -3%, and the total content of the Z element is 1% -2%.
According to the magnesium alloy with the high-strength and high-plasticity multi-water-soluble channel, when the X element only comprises the Sm element, the content of the Sm element is 2% -3%, and the total content of the Z element is 1% -2%.
According to the magnesium alloy with the high-strength and high-plasticity multi-water-soluble channel, when the X element only contains the Zn element, the content of the Zn element is 2% -4%, and the total content of the Z element is 0% -1%.
According to the magnesium alloy with the high-strength and high-plasticity multi-water-soluble channel, when the Y element is any one of Cu, ni and Sr, the content of the Y element is 0.2-0.4%.
The magnesium alloy with the high strength and the high plasticity and multiple water-soluble channels is further improved, and the grain boundary of the magnesium alloy contains MgY phase consisting of Y element;
the magnesium alloy contains 40% or more of twin crystals in the interior of crystal grains.
According to the magnesium alloy with the high-strength and high-plasticity multi-water-soluble channel, more than 50% of grains in the magnesium alloy contain twin crystals, and more than 50% of twin crystals have twin crystal boundary non-precipitation zones.
As a general technical conception, the invention also provides a preparation method of the magnesium alloy with high strength and high plasticity and multiple water-soluble channels, which adopts any one of the following modes to prepare the magnesium alloy with high strength and high plasticity and multiple water-soluble channels;
the first mode comprises the following steps:
s1, weighing required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot;
s2, homogenizing the cast ingot; the homogenization treatment temperature is 400-490 ℃; the homogenization treatment time is 6-48 hours;
s3, carrying out high-temperature deformation on the homogenized material; the high-temperature deformation temperature is 300-450 ℃, and the true strain is 0.5-1.2;
s4, carrying out low-temperature deformation on the material subjected to the high-temperature deformation; the temperature of the low-temperature deformation is 20-150 ℃, and the true strain is 0.02-0.2;
s5, aging the material subjected to low-temperature deformation to obtain the high-strength plastic multi-water-soluble channel magnesium alloy; the temperature of the aging treatment is 150-220 ℃; the aging treatment time is 6-60 hours.
Mode two, including the following step:
(1) Weighing required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot;
(2) Homogenizing the cast ingot; the homogenization treatment temperature is 400-490 ℃; the homogenization treatment time is 6-48 hours;
(3) Carrying out high-temperature deformation on the homogenized material; the high-temperature deformation temperature is 300-450 ℃, and the true strain is 0.5-1.2;
(4) Carrying out low-temperature deformation on the material subjected to high-temperature deformation; the temperature of the low-temperature deformation is 20-150 ℃, and the true strain is 0.02-0.2;
(5) Creep aging treatment is carried out on the material after low-temperature deformation, and the magnesium alloy with high strength and high plasticity and multiple water-soluble channels is obtained; the temperature of the creep aging treatment is 150-220 ℃, and the true strain is 0.1-0.6.
When the method is further improved and the mode I is adopted to prepare the magnesium alloy with the high-strength and high-plasticity and high-water-solubility channels, when the element X does not contain the element Zn, the homogenization treatment temperature in the step S2 is 440-490 ℃, and the high-temperature deformation temperature in the step S3 is 390-450 ℃; when the element X contains only Zn, the homogenization treatment temperature in the step S2 is 400-440 ℃, and the high-temperature deformation temperature in the step S3 is 300-390 ℃.
The preparation method of the magnesium alloy with the high-strength and high-plasticity multi-water-solubility channel is further improved, when the magnesium alloy with the high-strength and high-plasticity multi-water-solubility channel is prepared in the mode II, when the element X does not contain the element Zn, (2) the homogenization treatment temperature in the step is 440-490 ℃, and (3) the high-temperature deformation temperature in the step is 390-450 ℃; when the element X contains only Zn, the temperature of the homogenization treatment in the step (2) is 400 to 440 ℃ and the temperature of the high-temperature deformation in the step (3) is 300 to 390 ℃.
Compared with the prior art, the invention has the advantages that:
(1) Aiming at the characteristics that no precipitation zone exists at the grain boundary and the plasticity of the magnesium alloy is damaged generally, and the defect that the existing magnesium alloy cannot have high plasticity and high dissolution rate simultaneously is overcome, the invention creatively provides the magnesium alloy with high-strength plastic multiple water-soluble channels, the dissolution rate of the magnesium alloy is improved by transferring the grain boundary no precipitation zone which is harmful to the magnesium alloy originally to the twin crystal boundary no precipitation zone, eliminating the grain boundary no precipitation zone, improving the magnesium alloy plasticity, simultaneously utilizing the twin grain boundary no precipitation zone and the grain boundary compound as corrosion channels, and particularly: according to the invention, by adding 1% -4% of X element (X element is at least one of Nd element, sm element and Zn element), on one hand, nd element and Sm element are light rare earth elements, and the solid solution limit of Nd element and Sm element in Mg matrix is not more than 6%, so that a cylindrical precipitated phase and a twin crystal boundary non-precipitated band can be formed by adding Nd element and Sm element with the total content of not more than 4%, and compared with heavy rare earth element, the development cost is greatly reduced, on the other hand, as non-rare earth element, zn element has lower price, and compared with other non-rare earth elements, zn atom has higher diffusion rate in Mg matrix, the twin crystal boundary non-precipitated band required by the invention is easier to obtain; in the invention, a large amount of transition group elements are not needed to be added, and only Y element (the Y element is at least one of Cu element, ni element and Sr element) with the total content of 0.1-0.4% is added, so that a grain boundary compound can be formed with a Mg matrix, and meanwhile, a twin grain boundary non-precipitation zone is used as a corrosion channel together, thereby realizing rapid reaction of magnesium alloy and water, avoiding damage to the strong plasticity of the magnesium alloy, saving the addition cost of the transition group elements, and enabling the magnesium alloy to have strong strength at the same timePlasticity and rapid water solubility; in the invention, Z element (Z element is at least one of Al element and Sn element) with the total content of 0-2% is also added, so that the twin crystal number of the magnesium alloy is further increased. Therefore, in the invention, by optimizing the types and the addition amounts of each additive element, the harmful grain boundary non-precipitation zone can be converted into the beneficial twin boundary non-precipitation zone, so that the twin boundary non-precipitation zone and the grain boundary compound are used as corrosion channels together, the strong plasticity of the magnesium alloy can be improved, the dissolution rate of the magnesium alloy in water can be improved, and meanwhile, the precipitated phases in the grains and the twin crystal can further improve the strength, thereby obtaining the magnesium alloy with the high plasticity and the high dissolution rate, wherein the tensile strength at room temperature is more than or equal to 220MPa, the yield strength is more than or equal to 120MPa, the elongation is more than or equal to 15%, and the dissolution rate in water at 50 ℃ is more than or equal to 15mg cm -2 ·h -1 Is a novel magnesium alloy with excellent performance.
(2) In the magnesium alloy, when the X element does not contain Zn element, the total content of the X element is optimized to be 1-3%, and the total content of the Z element is optimized to be 1-2%, so that the twin crystal quantity is increased by reducing the content of the rare earth element (X element) and improving the content of the Z element. When the X element only contains Sm element, the content of Sm element is optimized to be 2-3%, the total content of Z element is optimized to be 1-2%, the price of Sm is lower than that of Nd, the use cost of rare earth elements can be reduced by optimizing the contents of Sm element and Z element, the total content of Z element is promoted to be easier to induce twinning, and the quantity of twinning without precipitation bands are increased. When the X element only contains Zn element, the content of Zn element is optimized to be 2-4%, the total content of Z element is optimized to be 0-1%, and by taking Zn element as non-rare earth element and properly reducing the content of Z element, the variety of added elements can be reduced, and the texture strength of the basal plane can be reduced, thereby being beneficial to improving the strength and plasticity of the magnesium alloy. When the Y element is any one of Cu, ni and Sr, the content of the Y element is optimized to be 0.2-0.4%, which is beneficial to increasing the grain boundary compound and accelerating the dissolution rate of the magnesium alloy.
(3) In the magnesium alloy, more than 50% of grains contain twin crystals, and more than 50% of twin crystals have twin crystal boundary non-precipitation zones, so that the non-precipitation zones at the twin crystal boundary can increase corrosion channels, and the reaction rate of the magnesium alloy and water is accelerated.
(4) The invention also provides a preparation method of the magnesium alloy with the high strength plastic multiple water-soluble channels, which is characterized in that the magnesium alloy with high strength plastic and high dissolution rate can be prepared by weighing the required raw materials according to the mass percent of each component in the magnesium alloy, and sequentially carrying out uniform mixing, melting, refining, casting, homogenization treatment, high-temperature deformation, low-temperature deformation, aging treatment or creep aging treatment. In the preparation method, the deformation amount adopted by high-temperature deformation is smaller, so that the energy consumption can be saved, the processing efficiency can be improved, large-specification components can be conveniently prepared, meanwhile, the grain refinement is realized without adopting severe plastic deformation, on the contrary, the grain size is not required to be changed, the high-density twin crystal is generated by utilizing subsequent low-temperature deformation, the twin crystal is used as a strengthening mechanism, further, the precipitation strengthening effect is generated by utilizing aging (namely static aging) or creep aging (namely stress-induced dynamic aging), particularly, a precipitation phase is formed in the twin crystal, and the twin crystal boundary can be pinned, so that the twin crystal boundary can become a high-density interface to strongly plasticize the magnesium alloy and can be used as a corrosion channel to improve the water-soluble rate of the magnesium alloy. In addition, the preparation method has the advantages of simple process, convenient operation, high production efficiency and the like, is suitable for large-scale preparation, and is convenient for industrialized application.
(5) In the preparation method, when the element X does not contain Zn, the homogenization treatment temperature is 440-490 ℃, and the high-temperature deformation temperature is 390-450 ℃, so that the rare earth magnesium alloy strong plasticity is improved more favorably, because the rare earth magnesium alloy has high strength and is difficult to process, the homogenization and deformation temperature is increased, and the rare earth magnesium alloy strong plasticity is improved more favorably; when the X element only contains Zn element, the homogenization treatment temperature is 400-440 ℃, and the high-temperature deformation temperature is 300-390 ℃, which is more beneficial to improving the strong plasticity of the non-rare earth magnesium alloy because the non-rare earth magnesium alloy has low strength and the Zn-containing magnesium alloy has high-temperature brittleness, thereby being more beneficial to improving the strong plasticity of the non-rare earth magnesium alloy by reducing the homogenization and deformation temperature.
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
FIG. 1 is a schematic diagram of the microstructure of the high-strength multi-water-soluble channel magnesium alloy prepared in example 1 of the present invention.
Detailed Description
The invention is further described below in connection with the drawings and the specific preferred embodiments, but the scope of protection of the invention is not limited thereby.
In the following examples, materials and instruments used are commercially available unless otherwise specified. The process adopted is a conventional process, the equipment adopted is a conventional equipment, and the obtained data are all average values of more than three repeated experiments.
Example 1
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels comprises, by mass, 3% of Nd element, 0.3% of Ni element, 2% of Al element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy in the embodiment comprises the following steps:
s1, smelting and casting: weighing the required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot.
S2, homogenizing: the ingot was subjected to homogenization treatment at 470 ℃ for 12 hours.
S3, high-temperature deformation: and carrying out high-temperature deformation on the homogenized material, wherein the high-temperature deformation temperature is 450 ℃, and the true strain is 1.2.
S4, low-temperature deformation: and (3) carrying out low-temperature deformation on the material subjected to high-temperature deformation, wherein the temperature of the low-temperature deformation is 20 ℃, and the true strain is 0.2.
S5, aging: and (3) aging the material subjected to low-temperature deformation, wherein the aging temperature is 220 ℃ and the aging time is 12 hours, so that the high-strength plastic multi-water-soluble channel magnesium alloy, called Mg-3Nd-0.3Ni-2Al alloy for short, is marked as sample No. 1.
FIG. 1 is a schematic diagram of the microstructure of the high-strength multi-water-soluble channel magnesium alloy prepared in example 1 of the present invention. As shown in fig. 1, mgNi phase exists at the grain boundary of the magnesium alloy, 60% (the percentage refers to the number percentage) of the grain interior contains twin crystals, and in these twin crystals, all twin grain boundaries exist without precipitation zones, and at the same time, mgNd phase is also contained in the grain interior and twin crystal interior.
Comparative example 1
The magnesium alloy comprises, by mass, 6% of Nd element, 0.3% of Ni element, 2% of Al element and the balance of Mg element.
The preparation method of the magnesium alloy is the same as in example 1.
The resulting Mg-6Nd-0.3Ni-2Al alloy was labeled sample No. 2.
Through tests, mgNi phases exist at the grain boundaries of the magnesium alloy, 20% of grains contain twin crystals, 30% of twin crystal boundaries in the twin crystals have no precipitation zone, and meanwhile, the MgNd phases are contained in the grains and the twin crystals.
Comparative example 2
The magnesium alloy comprises, by mass, 3% of Nd element, 0.3% of Ni element, 5% of Al element and the balance of Mg element.
The preparation method of the magnesium alloy is the same as in example 1.
The resulting Mg-3Nd-0.3Ni-5Al alloy was labeled as sample No. 3.
Through tests, mgNi and MgAl phases exist at the grain boundary of the magnesium alloy, 70% of grains contain twin crystals, no precipitation zone exists in all twin crystal boundaries in the twin crystals, and meanwhile MgNd and MgAl phases are contained in the grains and the twin crystals.
The 3 magnesium alloys obtained in example 1 and comparative examples 1 to 2 were subjected to unidirectional tensile test at room temperature and water-soluble test at 50℃and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the magnesium alloy (sample No. 1) with high strength and high plasticity and multiple water-soluble channels prepared in example 1 has both high strength and high dissolution rate. However, the magnesium alloy (sample No. 2) prepared in comparative example 1 has an excessively high Nd content, and thus has enhanced corrosion resistance, resulting in interruption of dissolution of the magnesium alloy in water; in addition, the magnesium alloy (sample No. 3) prepared in comparative example 2 has too high Al content, which results in excessive twin crystal number and formation of MgAl brittle phase, and also weakens the solid solution strengthening effect and deteriorates the strong plasticity of the magnesium alloy.
Example 2
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels contains, by mass, 4% of Zn element, 0.4% of Sr element, 0.4% of Sn element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy comprises the following steps:
s1, smelting and casting: weighing the required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot.
S2, homogenizing: the ingot was subjected to homogenization treatment at 400 ℃ for 6 hours.
S3, high-temperature deformation: and carrying out high-temperature deformation on the homogenized material, wherein the high-temperature deformation temperature is 300 ℃, and the true strain is 0.5.
S4, low-temperature deformation: and carrying out low-temperature deformation on the material subjected to high-temperature deformation, wherein the temperature of the low-temperature deformation is room temperature, and the true strain is 0.1.
S5, aging: and (3) aging the material subjected to low-temperature deformation, wherein the aging temperature is 150 ℃ and the aging time is 48 hours, so that the high-strength plastic multi-water-soluble channel magnesium alloy, called Mg-4Zn-0.4Sr-0.4Sn alloy for short, is marked as sample No. 2.
Through tests, mgSr phases exist at crystal boundaries of the magnesium alloy, 70% (the percentage refers to the number percentage) of crystal grains contain twin crystals, no precipitation zone exists at the twin crystal boundaries of 90% (the percentage refers to the number percentage) of the twin crystals, and MgZn phases exist in the crystal grains and the twin crystal grains.
Example 3
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels comprises, by mass, 4% of Zn element, 0.4% of Sr element, 1.4% of Sn element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy in the embodiment is the same as that in the embodiment 2.
The resulting Mg-4Zn-0.4Sr-1.4Sn alloy was labeled as sample No. 5.
Through tests, mgSr phases exist at the grain boundaries of the magnesium alloy, 95% of grain interiors contain twin crystals, no precipitation zones exist at 80% of the twin crystal boundaries in the twin crystals, and MgZn phases exist in the grain interiors and the twin crystal interiors.
Comparative example 3
The magnesium alloy contains, by mass, 0.4% of Zn element, 0.4% of Sr element, 0.4% of Sn element and the balance of Mg element.
The preparation method of the magnesium alloy is the same as in example 2.
The resulting Mg-0.4Zn-0.4Sr-0.4Sn alloy, labeled sample No. 6.
Through tests, mgSr phases exist at crystal boundaries of the magnesium alloy, 60% of crystal grains contain twin crystals, and all twin crystal boundaries do not contain precipitation-free bands in the twin crystals.
Comparative example 4
The magnesium alloy contains, by mass, 0.4% of Zn element, 0.04% of Sr element, 0.4% of Sn element and the balance of Mg element.
The preparation method of the magnesium alloy is the same as in example 2.
The resulting Mg-4Zn-0.04Sr-0.4Sn alloy was designated sample No. 7.
Through tests, mgSr phases are not present at the grain boundaries of the magnesium alloy, 80% of grain interiors contain twin crystals, no precipitation zones are present at 90% of the twin crystal boundaries in the twin crystals, and MgZn phases are present in both the grain interiors and the twin crystal interiors.
The results of unidirectional tensile test at room temperature and water-soluble test at 50℃were carried out on the 4 magnesium alloys obtained in examples 2 to 3 and comparative examples 3 to 4, and are shown in Table 2.
TABLE 2
As can be seen from table 2, the magnesium alloy (sample No. 4) with high strength and high plasticity and multiple water-soluble channels prepared in example 2 has both high strength and high dissolution rate; the magnesium alloy (sample No. 5) with high strength and high plasticity and multiple water-soluble channels prepared in example 3 has increased Sn content to form a larger number of twin crystals, but Sn element is not easy to diffuse, so that the diffusion of Zn element is weakened, the number of precipitation zones of MgZn phase and twin crystal boundary is synchronously reduced, and the strong plasticity and dissolution rate are synchronously reduced. The magnesium alloy (sample No. 6) prepared in comparative example 3, due to insufficient Zn element content, did not form a precipitate-free zone at the twin grain boundary, and the dissolution rate was reduced; the magnesium alloy (sample No. 7) prepared in comparative example 4 had insufficient Sr element content, resulting in no MgSr phase formed at the grain boundary and a decrease in dissolution rate.
Example 4
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels comprises, by mass, 2% of Sm element, 0.2% of Cu element, 1% of Al element, 0.2% of Sn element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy comprises the following steps:
s1, smelting and casting: weighing the required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot.
S2, homogenizing: the ingot was subjected to homogenization treatment at 490 c for 24 hours.
S3, high-temperature deformation: the homogenized material was subjected to high temperature deformation at 420 ℃ with a true strain of 0.8.
S4, low-temperature deformation: and (3) carrying out low-temperature deformation on the material subjected to high-temperature deformation, wherein the temperature of the low-temperature deformation is 120 ℃, and the true strain is 0.05.
S5, aging: and (3) carrying out creep aging treatment on the material subjected to low-temperature deformation, wherein the temperature of the creep aging treatment is 200 ℃, the true strain is 0.2, and the magnesium alloy with high strength and multiple water-soluble channels, called Mg-2Sm-0.2Cu-1Al-0.2Sn alloy for short, is marked as sample No. 8.
Through tests, mgCu phases exist at the grain boundaries of the magnesium alloy, 60% of grains contain twin crystals, no precipitation zone exists at 70% of twin crystal boundaries in the twin crystals, and MgSm phases exist in the grains and the twin crystals.
Example 5
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels contains 1% of Sm element, 0.2% of Cu element and the balance of Mg element by mass percent.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy in the embodiment is the same as that in the embodiment 4.
The resulting Mg-1Sm-0.2Cu alloy was labeled as sample No. 9.
Through tests, mgCu phases exist at the grain boundaries of the magnesium alloy, 70% of grains contain twin crystals, no precipitation zone exists at 20% of twin crystal boundaries in the twin crystals, and MgSm phases exist in the grains and the twin crystals.
Example 6
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels comprises, by mass, 2% of Sm element, 0.1% of Cu element, 0.1% of Ni element, 1% of Al element, 0.2% of Sn element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy in the embodiment is the same as that in the embodiment 4.
The resulting Mg-2Sm-0.1Cu-0.1Ni-1Al-0.2Sn alloy was labeled sample No. 10.
Through tests, mgCu and MgNi phases exist at the grain boundary of the magnesium alloy, 40% of grains contain twin crystals, no precipitation zone exists at 70% of twin crystal boundaries in the twin crystals, and meanwhile, mgSm phases exist in the grains and the twin crystals.
Comparative example 5
The magnesium alloy comprises, by mass, 2% of Sm element, 0.2% of Cu element, 0.2% of Ni element, 0.2% of Sr element, 1% of Al element, 0.2% of Sn element and the balance of Mg element.
The preparation method of the magnesium alloy is the same as in example 4.
The resulting Mg-2Sm-0.2Cu-0.2Ni-0.2Sr-1Al-0.2Sn alloy was designated sample No. 11.
Through tests, mgCu, mgNi and MgSr phases exist at the grain boundary of the magnesium alloy, 30% of grains contain twin crystals, 70% of twin crystal boundaries exist in the twin crystals, and MgSm phases exist in the grains and the twin crystals.
The results of unidirectional tensile test at room temperature and water-soluble test at 50℃were carried out on the 4 magnesium alloys obtained in examples 4 to 6 and comparative example 5, and are shown in Table 3.
TABLE 3 Table 3
As can be seen from table 3, the magnesium alloy (sample No. 8) with high strength and high plasticity and multiple water-soluble channels prepared in example 4 has both high strength and high dissolution rate; the magnesium alloy (sample No. 9) with high strength and high plasticity and multiple water-soluble channels prepared in the embodiment 5 has reduced MgSm phase due to reduced Sm element content, so that the number of precipitation-free bands of twin crystal boundaries is reduced, and the dissolution rate is greatly reduced; the magnesium alloy (sample No. 10) with high strength and high plasticity and multiple water-soluble channels prepared in the example 5 contains Cu and Ni elements at the same time, so that the twin crystal number is reduced, the corrosion channels are reduced, and the dissolution rate is reduced; the magnesium alloy (sample No. 11) prepared in comparative example 5 had no high strength due to brittle fracture of the magnesium alloy caused by an increase in the number of grain boundary compounds due to an excessively high total content of Cu, ni and Sr.
Example 7
The magnesium alloy with high strength and high plasticity and multiple water-soluble channels comprises, by mass, 0.5% of Nd element, 3% of Sm element, 0.4% of Ni element, 1% of Al element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy comprises the following steps:
s1, smelting and casting: weighing required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot;
s2, homogenizing: homogenizing the cast ingot, wherein the temperature of the homogenizing treatment is 450 ℃ and the time is 36 hours;
s3, high-temperature deformation: carrying out high-temperature deformation on the homogenized material, wherein the high-temperature deformation temperature is 400 ℃, and the true strain is 0.5;
s4, low-temperature deformation: carrying out low-temperature deformation on the material subjected to high-temperature deformation, wherein the temperature of the low-temperature deformation is 150 ℃, and the true strain is 0.08;
s5, aging: and (3) carrying out creep aging treatment on the material subjected to low-temperature deformation, wherein the temperature of the creep aging treatment is 180 ℃, the true strain is 0.6, and the magnesium alloy with high strength and multiple water-soluble channels, called Mg-0.5Nd-3Sm-0.4Ni-1Al alloy for short, is marked as a sample No. 12.
Through tests, mgNi phases exist at the grain boundaries of the magnesium alloy, 60% of grains contain twin crystals, no precipitation zone exists at 80% of twin crystal boundaries in the twin crystals, and MgSm phases exist in the grains and the twin crystals.
Example 8
A magnesium alloy with high strength and multiple water-soluble channels has the same composition as in example 7.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy comprises the following steps:
s1, smelting and casting: the same as in example 7.
S2, homogenizing: the temperature was 420℃and the time was 48 hours.
S3, high-temperature deformation: the temperature was 300℃and the true strain was 0.5.
S4, low-temperature deformation: the same as in example 7.
S5, creep aging: the same as in example 7.
The resulting Mg-0.5Nd-3Sm-0.4Ni-1Al alloy was labeled as sample No. 13.
Through tests, mgNi phases exist at the grain boundaries of the magnesium alloy, 50% of grains contain twin crystals, most of the twin crystals are mutually intersected twin crystals, no precipitation zone exists at only 20% of twin crystal boundaries, and meanwhile, mgSm phases exist in the grains and the twin crystals.
Comparative example 6
A magnesium alloy having the same composition as in example 7.
The preparation method of the magnesium alloy comprises the following steps:
s1, smelting and casting: the same as in example 7;
s2, homogenizing: the same as in example 7;
s3, high-temperature deformation: the temperature is 490 ℃, and the true strain is 0.5;
s4, low-temperature deformation: the same as in example 7;
s5, creep aging: the same as in example 7.
The resulting Mg-0.5Nd-3Sm-0.4Ni-1Al alloy was labeled as sample No. 14.
Through tests, mgNi phases exist at the grain boundaries of the magnesium alloy, 20% of grains contain twin crystals, no precipitation-free bands exist at the twin crystal boundaries in the twin crystals, and meanwhile MgSm phases exist in the grains and the twin crystals.
The 3 magnesium alloys obtained in examples 7 to 8 and comparative example 6 were subjected to unidirectional tensile test at room temperature and water-soluble test at 50℃and the results are shown in Table 4.
TABLE 4 Table 4
As can be seen from table 4, the magnesium alloy (sample No. 12) with high strength and high plasticity and multiple water-soluble channels prepared in example 7 has both high strength and high dissolution rate; the magnesium alloy (sample No. 13) with high strength and multiple water-soluble channels prepared in example 8, because of the decrease of the homogenization temperature and the high temperature deformation temperature, leads twin crystals to be arranged in the grains not in parallel but to be intersected with each other, so that the number of non-precipitated bands is reduced, and the strong plasticity and the dissolution rate are synchronously reduced; the magnesium alloy (sample No. 14) prepared in comparative example 2 has excessively high deformation temperature and excessively high degree of grain refinement, so that twin crystals and twin crystal boundaries have no precipitation zone, and the dissolution rate is greatly reduced.
Example 9
The magnesium alloy with the high-strength plastic multi-water-soluble channel comprises, by mass, 0.5% of Nd element, 0.5% of Sm element, 1.5% of Zn element, 0.1% of Cu element, 0.1% of Ni element, 0.1% of Sr element, 0.5% of Al element, 0.5% of Sn element and the balance of Mg element.
The preparation method of the high-strength plastic multi-water-soluble channel magnesium alloy comprises the following steps:
s1, smelting and casting: weighing the required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot.
S2, homogenizing: the ingot was subjected to homogenization treatment at 410 ℃ for 36 hours.
S3, high-temperature deformation: and carrying out high-temperature deformation on the homogenized material, wherein the high-temperature deformation temperature is 340 ℃, and the true strain is 1.
S4, low-temperature deformation: and (3) carrying out low-temperature deformation on the material subjected to high-temperature deformation, wherein the temperature of the low-temperature deformation is 20 ℃, and the true strain is 0.03.
S5, aging: and (3) carrying out creep aging treatment on the material subjected to low-temperature deformation, wherein the temperature of the creep aging treatment is 150 ℃, the true strain is 0.4, and the magnesium alloy with high strength and multiple water-soluble channels, namely Mg-0.5Nd-0.5Sm-1.5Zn-0.1Cu-0.1Ni-0.1Sr-0.5Al-0.5Sn alloy, is marked as sample No. 15.
Through tests, mgCu, mgNi and MgSr phases exist at the grain boundary of the magnesium alloy, 50% of the grain interiors contain twin crystals, no precipitation zone exists at 60% of the twin crystal boundaries in the twin crystals, and simultaneously, mgZn phases exist in the grain interiors and the twin crystal interiors.
Comparative example 7
A magnesium alloy having the same composition as in example 9.
The preparation method of the magnesium alloy comprises the following steps:
s1, smelting and casting: the same as in example 9;
s2, homogenizing: the same as in example 9;
s3, high-temperature deformation: the same as in example 9;
s4, low-temperature deformation: the temperature is room temperature, and the true strain is 0.01;
s5, creep aging: the same as in example 9.
The resulting Mg-0.5Nd-0.5Sm-1.5Zn-0.1Cu-0.1Ni-0.1Sr-0.5Al-0.5Sn alloy was labeled as sample No. 16.
Through tests, mgCu, mgNi and MgSr phases exist at the grain boundary of the magnesium alloy, 10% of grain interiors contain twin crystals in the twin crystals, no precipitation zones exist at all twin grain boundaries, and MgZn phases exist in the grain interiors and the twin crystal interiors.
Comparative example 8
A magnesium alloy having the same composition as in example 9.
The preparation method of the magnesium alloy comprises the following steps:
s1, smelting and casting: the same as in example 9;
s2, homogenizing: the same as in example 9;
s3, high-temperature deformation: the same as in example 9;
s4, low-temperature deformation: the same as in example 9;
s5, creep aging: the temperature was 150℃and the true strain was 0.8.
The resulting Mg-0.5Nd-0.5Sm-1.5Zn-0.1Cu-0.1Ni-0.1Sr-0.5Al-0.5Sn alloy was labeled as sample No. 17.
Through tests, mgCu, mgNi and MgSr phases exist at the grain boundary of the magnesium alloy, 50% of the grain interiors contain twin crystals and grain boundary non-precipitation zones, only 30% of the twin crystals exist at the twin crystal boundaries in the twin crystals, and meanwhile, mgZn phases exist in the grain interiors and the twin crystal interiors.
The 3 magnesium alloys obtained in example 9 and comparative examples 7 to 8 were subjected to unidirectional tensile test at room temperature and water-soluble test at 50℃and the results are shown in Table 5.
TABLE 5
As can be seen from table 5, the magnesium alloy (sample No. 15) with high strength and high plasticity and multiple water-soluble channels prepared in example 2 has both high strength and high dissolution rate; the magnesium alloy (sample No. 16) prepared in comparative example 7 has insufficient twin crystal number and too few corrosion channels due to too low true strain of low-temperature deformation, so that the reaction quantity of the magnesium alloy and water is obviously reduced; the magnesium alloy (sample No. 17) prepared in comparative example 7 also had no band precipitated at the grain boundary due to excessive true strain in creep aging, severely impairing the strength of the magnesium alloy.
From the above results, in the invention, by optimizing the types and the addition amounts of the additive elements, the harmful grain boundary non-precipitation zone can be converted into the beneficial twin boundary non-precipitation zone, so that the twin boundary non-precipitation zone and the grain boundary compound are used as corrosion channels together, the strong plasticity of the magnesium alloy can be improved, the dissolution rate of the magnesium alloy in water can be improved, and meanwhile, the precipitated phases in the grains and the twin can further improve the strength, thereby obtaining the magnesium alloy with both the high plasticity and the high dissolution rate, wherein the tensile strength at room temperature is more than or equal to 220MPa, the yield strength is more than or equal to 120MPa, the elongation is more than or equal to 15%, and the dissolution rate in water at 50 ℃ is more than or equal to 15mg cm -2 ·h -1 Is a novel magnesium alloy with excellent performance.
The present invention is disclosed in the preferred embodiments, but is not limited thereto. Many variations and modifications of the present invention will be apparent to those skilled in the art, using the methods and techniques disclosed above. Therefore, any simple modification of the above embodiments according to the technical substance of the present invention is still within the scope of the technical solution of the present invention, without departing from the technical solution of the present invention.
Claims (10)
1. The magnesium alloy with the high-strength plastic multi-water-soluble channel is characterized by comprising the following components in percentage by mass: 1 to 4 percent of X element, 0.1 to 0.4 percent of Y element, 0 to 2 percent of Z element and the balance of Mg element; the X element is at least one of Nd element, sm element and Zn element; the Y element is at least one of Cu element, ni element and Sr element, and the Z element is at least one of Al element and Sn element.
2. The high-strength multi-water-soluble channel magnesium alloy according to claim 1, wherein when the element X does not contain Zn, the total content of the element X is 1% to 3%, and the total content of the element Z is 1% to 2%.
3. The high-strength multi-water-soluble channel magnesium alloy according to claim 1, wherein when the element X only comprises the element Sm, the content of the element Sm is 2% -3%, and the total content of the element Z is 1% -2%.
4. The high-strength multi-water-soluble channel magnesium alloy according to claim 1, wherein when the element X only contains the element Zn, the content of the element Zn is 2% -4%, and the total content of the element Z is 0-1%.
5. The high-strength multi-water-soluble channel magnesium alloy according to claim 1, wherein when the element Y is any one of Cu, ni and Sr, the content of the element Y is 0.2-0.4%.
6. The high-strength multi-aqueous channel magnesium alloy according to any one of claims 1 to 5, wherein grain boundaries of the magnesium alloy contain MgY phase composed of Y element;
the magnesium alloy contains 40% or more of twin crystals in the interior of crystal grains.
7. The high-strength multi-water-soluble channel magnesium alloy according to claim 6, wherein 50% or more of grains in the magnesium alloy contain twin crystals, and 50% or more of twin crystals have twin-crystal-boundary non-precipitation zones.
8. A method for preparing the magnesium alloy with high strength and high plasticity and multiple water-soluble channels according to any one of claims 1 to 7, wherein the magnesium alloy with high strength and high plasticity and multiple water-soluble channels is prepared by adopting any one of the following modes;
the first mode comprises the following steps:
s1, weighing required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot;
s2, homogenizing the cast ingot; the homogenization treatment temperature is 400-490 ℃; the homogenization treatment time is 6-48 hours;
s3, carrying out high-temperature deformation on the homogenized material; the high-temperature deformation temperature is 300-450 ℃, and the true strain is 0.5-1.2;
s4, carrying out low-temperature deformation on the material subjected to the high-temperature deformation; the temperature of the low-temperature deformation is 20-150 ℃, and the true strain is 0.02-0.2;
s5, aging the material subjected to low-temperature deformation to obtain the high-strength plastic multi-water-soluble channel magnesium alloy; the temperature of the aging treatment is 150-220 ℃; the time of the aging treatment is 6-60 hours;
mode two, including the following step:
(1) Weighing required raw materials according to the mass percentage of each component in the magnesium alloy, uniformly mixing, melting, refining and casting to obtain an ingot;
(2) Homogenizing the cast ingot; the homogenization treatment temperature is 400-490 ℃; the homogenization treatment time is 6-48 hours;
(3) Carrying out high-temperature deformation on the homogenized material; the high-temperature deformation temperature is 300-450 ℃, and the true strain is 0.5-1.2;
(4) Carrying out low-temperature deformation on the material subjected to high-temperature deformation; the temperature of the low-temperature deformation is 20-150 ℃, and the true strain is 0.02-0.2;
(5) Creep aging treatment is carried out on the material after low-temperature deformation, and the magnesium alloy with high strength and high plasticity and multiple water-soluble channels is obtained; the temperature of the creep aging treatment is 150-220 ℃, and the true strain is 0.1-0.6.
9. The method for preparing a magnesium alloy with high strength and multiple water-soluble channels according to claim 8, wherein when the magnesium alloy with high strength and multiple water-soluble channels is prepared in the first mode, when the element X does not contain the element Zn, the homogenization treatment temperature in the step S2 is 440-490 ℃, and the high-temperature deformation temperature in the step S3 is 390-450 ℃; when the element X contains only Zn, the homogenization treatment temperature in the step S2 is 400-440 ℃, and the high-temperature deformation temperature in the step S3 is 300-390 ℃.
10. The method for producing a high-strength, high-plasticity, multi-water-soluble channel magnesium alloy according to claim 8, wherein when the high-strength, high-plasticity, multi-water-soluble channel magnesium alloy is produced in mode two, when the element X does not contain the element Zn, the temperature of the homogenization treatment in step (2) is 440 ℃ to 490 ℃, and the temperature of the high-temperature deformation in step (3) is 390 ℃ to 450 ℃; when the element X contains only Zn, the temperature of the homogenization treatment in the step (2) is 400 to 440 ℃ and the temperature of the high-temperature deformation in the step (3) is 300 to 390 ℃.
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