CN113215461A - Magnesium alloy with high bulging property and high heat resistance and preparation method thereof - Google Patents
Magnesium alloy with high bulging property and high heat resistance and preparation method thereof Download PDFInfo
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- CN113215461A CN113215461A CN202110461311.8A CN202110461311A CN113215461A CN 113215461 A CN113215461 A CN 113215461A CN 202110461311 A CN202110461311 A CN 202110461311A CN 113215461 A CN113215461 A CN 113215461A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
The invention discloses a magnesium alloy with high bulging property and high heat resistance, which comprises 0.5-2.0% of X element by mass percent, wherein the X element is one or more of rare earth element and calcium element; and the ratio of the Schmid factor of non-basal-plane slip of at least one of the cylindrical surface slip and the conical surface slip of the magnesium alloy to the Schmid factor of basal-plane slip is 1.0-1.4. Also discloses a preparation method of the magnesium alloy. The magnesium alloy disclosed by the invention is simple in component and is in a low-alloying category, the ratio of Schmid factors of non-basal plane slippage and basal plane slippage is 1.0-1.4, the relative activity of the non-basal plane slippage and the basal plane slippage is effectively balanced, the requirement on high bulging property can be met, and the damage of the basal plane slippage to heat resistance can be avoided. The preparation method has the advantages of reasonable process design, simple equipment requirement, convenient operation, low cost and high efficiency, and can stably prepare the magnesium alloy with high bulging property and high heat resistance.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal materials and processing, relates to a magnesium alloy with high bulging property and high heat resistance and a preparation method thereof, and particularly relates to a magnesium alloy with high bulging property and high heat resistance and a preparation method thereof, wherein the Schmid factor ratio of non-basal surface slippage to basal surface slippage is 1.0-1.4.
Background
With the increasing severity of energy and environmental issues, the weight reduction of structural materials is becoming more and more important. Magnesium alloy has many advantages of high specific strength, good damping performance, easy recovery and the like as the lightest metal structural material at present, and attracts the attention of a plurality of high and new technology industries. But the further popularization and application of the material are always limited by the problems that the material has poor bulging capacity at room temperature and is easy to generate creep failure when being used at medium and high temperature.
In recent years, researchers at home and abroad adopt a plurality of strategies to improve the room temperature bulging property of magnesium alloy, and the aims are achieved by weakening texture and refining crystal grains by introducing shear deformation or adding a large amount of alloying elements and the like. The texture weakening can improve the basal plane slippage Schmid factor to be more than 0.4, which is beneficial to improving the bulging property; meanwhile, the fine grain size can increase the proportion of a grain boundary, help to coordinate plastic deformation and bring higher bulging property. Basal slip is, however, the most common cause of creep failure, with excessively high basal slip Schmid factors compromising heat resistance; meanwhile, the grain boundary strength of the alloy at medium and high temperature is low, when the grain size is reduced, the proportion of the grain boundary is increased, the contribution of grain boundary sliding to creep strain is also increased, and the heat resistance of the alloy is deteriorated.
On the other hand, when strong basal plane texture exists in the magnesium alloy, most crystal grains are in hard orientation, namely the basal plane slip Schmid factor is often less than 0.3, while the cylindrical surface slip Schmid factor and the conical surface slip Schmid factor are close to 0.5 at the same time, and the starting stress of the cylindrical surface slip and the conical surface slip is larger, so that the creep strain rate caused by dislocation slip at high temperature is reduced, and therefore, the strong basal plane texture is beneficial to improving the heat resistance of the material. However, strong basal texture can cause the Schmid factor of basal slippage to be obviously reduced, and the bulging performance is damaged. Moreover, the grain boundary slippage of coarse crystals is difficult, which is generally beneficial to heat resistance but not beneficial to room temperature bulging property, and the contradiction effect of fine crystals and coarse crystals on service performance is also one of the bottlenecks of magnesium alloy development.
In conclusion, how to solve the contradiction between the room temperature bulging property and the medium-high temperature heat resistance of the magnesium alloy and how to balance the relative activities of basal plane slippage, cylindrical surface slippage and conical surface slippage is always a difficult problem in preparing high-service magnesium alloy and developing the magnesium alloy industry, and a component design and tissue regulation and control process of the magnesium alloy with the room temperature bulging property, the medium-high temperature heat resistance and the high-high temperature heat resistance, which is simple, efficient and low in cost, is urgently needed to be provided, so that the requirements of the fields of transportation, aerospace, national defense war industry and the like on multi-temperature safe service magnesium alloy are met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a magnesium alloy with high bulging property and high heat resistance and a preparation method thereof. The magnesium alloy disclosed by the invention is simple in component and is in a low-alloying category, the ratio of Schmid factors of non-basal-plane slippage and basal-plane slippage of the magnesium alloy is 1.0-1.4, the relative activity of the non-basal-plane slippage and the basal-plane slippage is effectively balanced, the requirement of high bulging property on the basal-plane slippage Schmid factors can be met, and the damage of the basal-plane slippage on heat resistance can be avoided. The preparation method has the advantages of reasonable process design, simple equipment requirement, convenient operation, low cost and high efficiency, and can stably prepare the magnesium alloy with high bulging property and high heat resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the magnesium alloy with high bulging property and high heat resistance comprises 0.5-2.0% of X element in percentage by mass, wherein the X element is one or more of rare earth elements and calcium elements; and the ratio of the Schmid factor of non-basal plane slip of at least one of the cylindrical surface slip and the conical surface slip of the magnesium alloy to the Schmid factor of basal plane slip is 1.0-1.4.
Preferably, in the magnesium alloy, the volume fraction of crystal grains with the grain size less than or equal to 15 mu m is 40-80%. When the amount of the fine crystals is too low, the bulging property is reduced, when the amount of the fine crystals is too high, the heat resistance is reduced, and when the volume fraction of the crystal grains with the grain size of less than or equal to 15 mu m is 40-80%, the bulging property at room temperature and the heat resistance at medium and high temperatures can be better and synchronously improved.
Preferably, the ratio of the Schmid factor of the cylindrical surface slippage and the conical surface slippage of the magnesium alloy to the Schmid factor of the basal surface slippage is in the range of 1.0-1.4. The ratio of Schmid factors of the two non-basal plane slippage and the basal plane slippage is in the range of 1.0-1.4, so that the plastic deformation can be better coordinated, the strength and the plasticity of the magnesium alloy can be synchronously improved, and the combination of the room temperature bulging property and the medium-high temperature heat resistance can be better obtained.
Preferably, the magnesium alloy further contains a manganese element or a zirconium element, and the mass percentage of the manganese element or the zirconium element is 0-0.5%. The proper amount of manganese and zirconium can increase the metal surface fluidity of the coarse-grain magnesium alloy, is more favorable for bulging property, and does not damage heat resistance.
Preferably, the magnesium alloy further contains an indium element or a zinc element, and the mass percentage of the indium element or the zinc element is 0-0.5%. Proper amounts of indium and zinc can increase the atom clusters in the magnesium alloy fine crystal, enhance the heat resistance of the fine crystal and do not damage the bulging property.
As a general inventive concept, the present invention also provides a method for preparing a magnesium alloy having high bulging property and high heat resistance, comprising the steps of:
s1, preparing a magnesium alloy ingot according to alloy component requirements, carrying out homogenization treatment, and then carrying out thermal deformation for 1 pass or multiple passes at 400-500 ℃, wherein the deformation direction of the thermal deformation is fixed;
s2, performing thermal deformation on the magnesium alloy obtained in the step S1 at 450-520 ℃ for 1 or more passes, wherein the accumulated true strain of the thermal deformation is 0.4-0.8, and the deformation direction of the 1 st pass thermal deformation is perpendicular to the deformation direction of the thermal deformation in the step S1, so that the magnesium alloy with high bulging property and high heat resistance is obtained.
Preferably, the heat distortion temperature of step S2 is not lower than the heat distortion temperature of step S1. The heating thermal deformation in the step S2 can obtain a larger degree of crystal grain rotation, obtain a more appropriate Schmid factor ratio and fine crystal ratio, and is more beneficial to simultaneously improving the bulging property and the heat resistance.
Preferably, the annealing treatment is further included after the step S2, the temperature of the annealing treatment is 250 ℃ to 350 ℃, and the time of the annealing treatment is 10min to 120 min. The annealing process can induce the growth of fine crystal of the rigid core, promote dislocation in the coarse crystal to form a large-angle interface or new fine crystal, and further improve the bulging property and the heat resistance.
Preferably, in step S1, the cumulative true strain of the thermal deformation is 0.3 to 0.7.
Preferably, in step S1, the thermal deformation is performed in a plurality of passes. The multi-pass thermal deformation is easier to obtain a strong texture, which is helpful for improving the effect of the step S2, namely, the coarse crystals are broken into fine crystals to a greater extent in the step S2, the fine crystals grow into coarse crystals, and the Schmid factor ratio and the fine crystal ratio which are more beneficial for synchronously improving the bulging property and the heat resistance are obtained.
Preferably, in step S2, the thermal deformation is performed in 1 pass. The single-pass thermal deformation can reduce the dynamic recrystallization times to avoid excessive fine crystal quantity, and can better force the coarse crystal to deflect to weaken the texture, thereby obtaining the Schmid factor ratio and the fine crystal ratio which are more beneficial to synchronously improving the bulging property and the heat resistance.
Compared with the prior art, the invention has the advantages that:
1. the magnesium alloy disclosed by the invention is reasonably controlled to form, and meanwhile, the ratio of Schmid factors of non-basal-plane slippage and basal-plane slippage of the magnesium alloy is controlled to be 1.0-1.4, so that the relative activities of the non-basal-plane slippage and the basal-plane slippage are effectively balanced, the requirements of high bulging property on the basal-plane slippage Schmid factors can be met, the damage of the basal-plane slippage on heat resistance can be avoided, and the magnesium alloy has both high bulging property and high heat resistance; the magnesium alloy of the invention has the total content of the added elements of 0.5 to 3 percent, belongs to the category of low alloying components, avoids using expensive metals such as silver, nickel and the like, avoids excessively depending on rare earth resources, has low cost, is beneficial to protecting the environment and saving resources, and has wide application range;
the invention adds a proper amount of rare earth and calcium elements, can reduce dendrites in the cast ingot and increase equiaxed crystals, so that the size of initial crystal grains is less than or equal to 200 mu m, directly improves the plasticity of the cast ingot, is also beneficial to applying large strain thermal deformation to the magnesium alloy subsequently and improving the strength of the magnesium alloy, obtains excellent combination of plasticity and strength, and is beneficial to simultaneously obtaining high bulging property and high heat resistance; atomic clusters or fine compounds can be formed in the grain boundary to prevent the crystal fracture in the creep process, which is beneficial to improving the medium-high temperature heat resistance, and a proper amount of rare earth and calcium elements are beneficial to the grain deflection in the thermal deformation process, so that the relative activity of non-basal plane slip and basal plane slip can be balanced, and the ratio is beneficial to synchronously improving the room temperature bulging property and the medium-high temperature heat resistance; in addition, a proper amount of rare earth and calcium elements are added, so that large-scale recrystallization in the thermal deformation process can be hindered, enough number of coarse crystals can be reserved, newly formed fine crystal boundaries can be pinned, fine crystals can be prevented from rapidly growing to the coarse crystals, a structure containing various crystal grain sizes from submicron to 150 mu m can be obtained after thermal deformation, the volume fraction of the fine crystals with the crystal grain size of less than or equal to 15 mu m can be controlled within the range of 40-80%, the requirement of room-temperature bulging property on the number of the fine crystals can be further met, and the medium-high temperature heat resistance can be prevented from being damaged by excessive fine crystals.
2. According to the invention, a small amount of manganese and zirconium elements are added, so that the method is beneficial to reducing dendrites in the cast ingot and enhancing the plasticity and metal fluidity of the magnesium alloy, and the heat resistance is not damaged; the invention can add a small amount of indium and zinc elements, is beneficial to solid solution strengthening of the magnesium alloy, has high solid solution limit of indium and zinc in the magnesium matrix, and cannot be used as simple substances to damage the bulging property.
3. The severe plastic deformation can obviously enhance the texture, and the magnesium alloy with high heat resistance is prepared, but the bulging property is reduced by an excessively low basal plane slip Schmid factor (<0.3) and an excessively high column/cone slip Schmid factor (> 0.45); texture can be weakened through complex processes such as equal channel angular extrusion, cross rolling and the like, and the magnesium alloy with high bulging property is prepared, but the heat resistance is reduced by an excessively high basal plane slip Schmid factor (>0.4) and an excessively low column/cone slip Schmid factor (< 0.35). According to the preparation method, through controlling process steps and parameters, the magnesium alloy with high texture strength is prepared by utilizing the thermal deformation of the step S1, the magnesium alloy is only beneficial to non-basal plane slippage but not beneficial to basal plane slippage, then the thermal deformation of the step S2 is utilized, the direction of the maximum positive stress of the magnesium alloy is rotated by 90 degrees, the orientation concentration degree of crystal grains, namely the texture strength, can be quickly weakened by 30-40 percent, the Schmid factor ratio of the non-basal plane slippage to the basal plane slippage is enabled to be in the range of 1.0-1.4, the relative activity of the non-basal plane slippage and the basal plane slippage is balanced, and therefore the high bulging property and the high heat resistance are simultaneously met, and the excellent combination of the bulging property and the heat resistance is obtained. The thermal deformation related to the preparation method can be finished by conventional forging, extruding, rolling and other processing modes, and the preparation method has the advantages of simple requirement on equipment, convenience in operation and high production efficiency.
4. The room temperature bulging capacity of the magnesium alloy prepared by the invention is more than 3 times of that of the prior commercial AZ31 magnesium alloy; meanwhile, the heat-resistant service temperature of the magnesium alloy prepared by the method can be raised to 200-250 ℃, is obviously higher than the heat-resistant service temperature of AZ31 magnesium alloy by 150 ℃, the heat-resistant service life of the magnesium alloy reaches more than 3 times of that of AZ31 magnesium alloy under the same heat-resistant service condition, and the high-bulging-property and high-heat-resistance magnesium alloy can be effectively and stably obtained.
Drawings
FIG. 1 is a Schmid factor histogram of Mg-0.8Y-0.2Ca-0.5Mn-0.1In alloy slip of example 1, where (a) is the Schmid factor histogram of basal plane slip, (b) is the Schmid factor histogram of cylindrical plane slip, and (c) is the Schmid factor histogram of cone slip.
FIG. 2 is a graph showing the grain size distribution of the Mg-0.8Y-0.2Ca-0.5Mn-0.1In alloy of example 1.
FIG. 3 is a Schmid factor histogram of Mg-8.0Y-1.0Ca-0.5Mn-0.1In alloy slip of comparative example 1, where (a) is a Schmid factor histogram of basal plane slip, (b) is a Schmid factor histogram of cylindrical plane slip, and (c) is a Schmid factor histogram of conical plane slip.
FIG. 4 is a graph showing the grain size distribution of the Mg-8.0Y-1.0Ca-0.5Mn-0.1In alloy of comparative example 1.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
Example 1
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 0.8% of Y, 0.2% of Ca, 0.5% of Mn, 0.1% of In, and the balance of Mg.
The Schmid factor ratio of cylindrical surface slip to basal plane slip of the high-bulging high-heat-resistance magnesium alloy of the embodiment is 1.19, the Schmid factor ratio of conical surface slip to basal plane slip is 1.22, the alloy has a mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size less than or equal to 15 μm is 60%.
A method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment comprises the following steps:
s1, carrying out homogenization treatment on the alloy, and then carrying out thermal deformation for 3 passes at 500 ℃, wherein the accumulated true strain is 0.7, and the deformation directions of all the passes are the same;
s2, carrying out thermal deformation on the magnesium alloy at 520 ℃ for 1 pass, wherein the accumulated true strain is 0.8, and the thermal deformation direction is vertical to that of the step S1 to obtain a finished product.
The resulting Mg-0.8Y-0.2Ca-0.5Mn-0.1In alloy was labeled sample No. 1, as shown In FIG. 1, with a ratio of cylindrical slip Schmid factor (0.433) to basal slip Schmid factor (0.364) of 1.19 and a ratio of conical slip Schmid factor (0.444) to basal slip Schmid factor (0.364) of 1.22, while, as shown In FIG. 2, the alloy had a mixed grain size with a grain volume fraction of 60% with a grain size of 15 μm or less.
Comparative example 1
A magnesium alloy contains, by mass%, 8.0% Y, 1.0% Ca, 0.5% Mn and 0.1% In, with the balance being Mg.
The preparation method of the magnesium alloy is different from that of the embodiment 1 only In that the raw material composition is Mg-8.0Y-1.0Ca-0.5Mn-0.1 In.
The resulting Mg-8.0Y-1.0Ca-0.5Mn-0.1In alloy was labeled sample No. 2, and as shown In FIG. 3, the ratio of the cylindrical surface slip Schmid factor (0.460) to the basal surface slip Schmid factor (0.260) was 1.77, and the ratio of the conical surface slip Schmid factor (0.476) to the basal surface slip Schmid factor (0.260) was 1.83, while, as shown In FIG. 4, the alloy had a mixed grain size with a 30 volume fraction of grains having a grain size of 15 μm or less.
Comparative example 2
A magnesium alloy contains, by mass%, 0.2% Ca, 0.5% Mn and 0.1% In, with the balance being Mg.
The magnesium alloy was prepared In a manner different from that of example 1 only In that the raw material composition was Mg-0.2Ca-0.5Mn-0.1 In.
The resulting Mg-0.2Ca-0.5Mn-0.1In alloy was labeled sample No. 3, and had a ratio of cylindrical slip Schmid factor (0.316) to basal slip Schmid factor (0.411) of 0.77, a ratio of conical slip Schmid factor (0.341) to basal slip Schmid factor (0.411) of 0.83, and the alloy had a mixed grain size with a grain size of 15 μm or less In a volume fraction of 90%.
The obtained 3 magnesium alloys and the existing commercial AZ31 magnesium alloy were loaded at room temperature at a rate of 1 × 10-5s-1The results of the tensile creep test at 250 ℃ and 80MPa are shown in Table 1, in which the bulging property is represented by the ratio of the thickness after bulging to the thickness before bulging, and the heat resistance is represented by the creep life.
TABLE 1
| Sample number | Bulging ability | Creep life (hours) | |
| 1 | Example 1 | 4.9 | ≥100 |
| 2 | Comparative example 1 | 1.5 | 80 |
| 3 | Comparative example 2 | 3.2 | 18 |
| AZ31 | 1.6 | 20 |
As can be seen from Table 1, sample No. 1 has balanced relative activities of non-basal plane slip and basal plane slip, and the volume percentage of fine crystals is reasonable, compared with AZ31 magnesium alloy, sample No. 1 obtains high bulging property and high heat resistance at the same time; in contrast, sample 2 had inferior bulging properties to those of AZ31 magnesium alloy due to too high non-basal plane slip Schmid factor and too low basal plane slip Schmid factor, and sample 3 had inferior heat resistance to AZ31 magnesium alloy due to too low non-basal plane slip Schmid factor and too high integral number of fine crystals.
Example 2
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 2.0% of Gd, 0.2% of Zr, 0.5% of Zn, and the balance of Mg.
The Schmid factor ratio of cylindrical surface slip to basal plane slip of the high-bulging high-heat-resistance magnesium alloy of the embodiment is 1.27, the Schmid factor ratio of conical surface slip to basal plane slip is 1.36, the alloy has a mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size less than or equal to 15 μm is 50%.
A method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment comprises the following steps:
s1, carrying out homogenization treatment on the alloy, and then carrying out thermal deformation for 2 passes at 400 ℃, wherein the accumulated true strain is 0.3, and the deformation directions of all the passes are the same;
s2, carrying out thermal deformation on the magnesium alloy at 450 ℃ for 1 pass, wherein the accumulated true strain is 0.4, and the thermal deformation direction is vertical to that of the step S1;
and S3, annealing the magnesium alloy at 250 ℃ for 120min to obtain a finished product.
The resulting Mg-2.0Gd-0.2Zr-0.5Zn alloy was labeled sample No. 4, with a ratio of cylindrical slip Schmid factor (0.416) to basal slip Schmid factor (0.328) of 1.27, a ratio of conical slip Schmid factor (0.447) to basal slip Schmid factor (0.328) of 1.36, and the alloy had a mixed grain size with a 50 volume fraction of grains having a grain size of 15 μm or less.
Example 3
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 2.0% of Gd and 0.5% of Zn, and the balance of Mg.
The method for producing the magnesium alloy having high bulging properties and high heat resistance of this example is different from example 2 only in that the raw material composition is Mg-2.0Gd-0.5 Zn.
The resulting Mg-2.0Gd-0.5Zn alloy was labeled sample No. 5, with a ratio of cylindrical slip Schmid factor (0.428) to basal slip Schmid factor (0.315) of 1.36, a ratio of conical slip Schmid factor (0.482) to basal slip Schmid factor (0.315) of 1.53, and the alloy had a mixed grain size with a 45 volume fraction of grains having a grain size of 15 μm or less.
Example 4
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 2.0% of Gd and 0.2% of Zr, with the balance being Mg.
The magnesium alloy of the present example having high bulging properties and high heat resistance was prepared in the same manner as in example 2 except that the raw material composition was Mg-2.0Gd-0.2 Zr.
The resulting Mg-2.0Gd-0.2Zr alloy was labeled sample No. 6, and had a ratio of cylindrical surface slip Schmid factor (0.342) to basal surface slip Schmid factor (0.364) of 0.94, a ratio of conical surface slip Schmid factor (0.386) to basal surface slip Schmid factor (0.364) of 1.06, and at the same time, the alloy had a mixed grain size with a grain volume fraction of 40% for grains having a grain size of 15 μm or less.
Comparative example 3
A magnesium alloy contains, by mass%, 2.0% Gd, 2.0% Zr, and 5.0% Zn, with the balance being Mg.
The preparation method of the magnesium alloy is different from that of the embodiment 2 only in that the raw material composition is Mg-2.0Gd-2.0Zr-5.0 Zn.
The resulting Mg-2.0Gd-2.0Zr-5.0Zn alloy was labeled sample No. 7, and had a ratio of cylindrical slip Schmid factor (0.465) to basal slip Schmid factor (0.272) of 1.71, a ratio of conical slip Schmid factor (0.482) to basal slip Schmid factor (0.272) of 1.77, and at the same time, the alloy had a mixed grain size with a 30 volume fraction of grains having a grain size of 15 μm or less.
The obtained 4 magnesium alloys and the existing commercial AZ31 magnesium alloy were loaded at room temperature at a rate of 1 × 10-4s-1The results of the tensile creep test at 200 ℃ and 100MPa are shown in Table 2, in which the bulging property is represented by the ratio of the thickness after bulging to the thickness before bulging, and the heat resistance is represented by the creep life.
TABLE 2
| Sample number | Bulging ability | Creep life (hours) | |
| 4 | Example 2 | 4.7 | ≥100 |
| 5 | Example 3 | 4.3 | ≥100 |
| 6 | Example 4 | 4.5 | 90 |
| 7 | Comparative example 3 | 1.3 | 70 |
| AZ31 | 1.4 | 25 |
As can be seen from Table 2, the samples No. 4, No. 5 and No. 6 have balanced relative activities of non-basal plane slippage and basal plane slippage, and the percentage of fine crystal volume is reasonable, compared with AZ31 magnesium alloy, the samples No. 3 simultaneously obtain high bulging property and high heat resistance, especially the sample No. 4, and the bulging property and the heat resistance are further improved by simultaneously adding 0.2% of Zr and 0.5% of Zn; in contrast, samples 7 all had inferior bulging properties to AZ31 magnesium alloy due to too high a non-basal-slip Schmid factor and too low a basal-slip Schmid factor.
Example 5
The magnesium alloy with high bulging property and high heat resistance of the invention comprises 1.0% of Ca and 0.4% of Zn by mass percent, and the balance of Mg.
The Schmid factor ratio of cylindrical surface slip to basal plane slip of the high-bulging high-heat-resistance magnesium alloy of the embodiment is 1.26, the Schmid factor ratio of conical surface slip to basal plane slip is 1.26, the alloy has a mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size less than or equal to 15 μm is 70%.
A method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment comprises the following steps:
s1, carrying out homogenization treatment on the alloy, and then carrying out thermal deformation for 5 passes at 480 ℃, wherein the accumulated true strain is 0.6, and the deformation directions of all the passes are the same;
s2, carrying out thermal deformation on the magnesium alloy at 500 ℃ for 1 pass, wherein the accumulated true strain is 0.5, and the thermal deformation direction is vertical to that of the step S1;
s3, annealing the magnesium alloy at 350 ℃ for 10min to obtain a finished product.
The resulting Mg-1.0Ca-0.4Zn alloy was labeled sample No. 8, and had a ratio of cylindrical surface slip Schmid factor (0.437) to basal surface slip Schmid factor (0.347) of 1.26 and a ratio of conical surface slip Schmid factor (0.437) to basal surface slip Schmid factor (0.347) of 1.26, while the alloy had a mixed grain size with a grain size of 15 μm or less in a fraction of 70% by volume of grains.
Example 6
The magnesium alloy with high bulging property and high heat resistance of the invention comprises 1.0% of Ca and 0.4% of Zn by mass percent, and the balance of Mg.
The method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment is different from the embodiment 5 only in that the finished product is obtained after the step of S2, and the step of S3 is not performed.
The resulting Mg-1.0Ca-0.4Zn alloy was labeled sample No. 9, and had a ratio of cylindrical slip Schmid factor (0.441) to basal slip Schmid factor (0.324) of 1.36, a ratio of conical slip Schmid factor (0.476) to basal slip Schmid factor (0.324) of 1.47, and a mixed grain size with a grain size of 15 μm or less in a fraction of 50% by volume.
Example 7
The magnesium alloy with high bulging property and high heat resistance of the invention comprises 1.0% of Ca and 0.4% of Zn by mass percent, and the balance of Mg.
A method for preparing the magnesium alloy having high bulging property and high heat resistance according to the present example is different from example 5 only in that the heat distortion temperature of the step S2 is 460 ℃.
The obtained Mg-1.0Ca-0.4Zn alloy is marked as sample No. 10, the ratio of cylindrical surface slippage Schmid factor (0.289) to basal surface slippage Schmid factor (0.349) is 0.83, the ratio of conical surface slippage Schmid factor (0.373) to basal surface slippage Schmid factor (0.349) is 1.07, meanwhile, the alloy has mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size less than or equal to 15 mu m is 50%.
Comparative example 4
A magnesium alloy contains, by mass%, 1.0% of Ca and 0.4% of Zn, with the balance being Mg.
The magnesium alloy was prepared in a method different from example 5 only in that the heat distortion temperature of the S2 step was 420 ℃.
The resulting Mg-1.0Ca-0.4Zn alloy was labeled sample No. 11, and had a ratio of the cylindrical surface slip Schmid factor (0.326) to the basal surface slip Schmid factor (0.413) of 0.79 and a ratio of the conical surface slip Schmid factor (0.359) to the basal surface slip Schmid factor (0.413) of 0.87, while the alloy had a mixed grain size with a grain volume fraction of 30% for grains having a grain size of 15 μm or less.
Comparative example 5
A magnesium alloy contains, by mass%, 1.0% of Ca and 0.4% of Zn, with the balance being Mg.
The magnesium alloy was prepared in a manner different from that of example 5 only in that the cumulative true strain at the step of S2 was 0.3.
The resulting Mg-1.0Ca-0.4Zn alloy was labeled sample No. 12, and had a ratio of the cylindrical surface slip Schmid factor (0.320) to the basal surface slip Schmid factor (0.416) of 0.77 and a ratio of the conical surface slip Schmid factor (0.345) to the basal surface slip Schmid factor (0.416) of 0.83, and at the same time, the alloy had a mixed grain size with a grain volume fraction of 25% for grains having a grain size of 15 μm or less.
The obtained 5 magnesium alloys and the existing commercial AZ31 magnesium alloy were loaded at room temperature at a rate of 1 × 10-3s-1The results of the tensile creep test at 200 ℃ and 100MPa are shown in Table 3, in which the bulging property is represented by the ratio of the thickness after bulging to the thickness before bulging, and the heat resistance is represented by the creep life.
TABLE 3
| Sample number | Bulging ability | Creep life (hours) | |
| 8 | Example 5 | 4.5 | ≥100 |
| 9 | Example 6 | 4.1 | 90 |
| 10 | Example 7 | 4.2 | 85 |
| 11 | Comparative example 4 | 3.4 | 25 |
| 12 | Comparative example 5 | 2.9 | 20 |
| AZ31 | 1.3 | 25 |
As can be seen from table 3, samples No. 8, 9 and 10 have balanced relative activities of non-basal-plane slip and basal-plane slip, and the percentage of fine crystal volume is reasonable, and compared with AZ31 magnesium alloy, these 3 samples simultaneously achieve high bulging property and high heat resistance, especially sample No. 8, and the heat distortion temperature of step S2 is higher than that of step S1, and the annealing treatment of step S3 is performed, which further enhances bulging property and heat resistance; in contrast, samples 11 and 12 both had inferior heat resistance to AZ31 magnesium alloy due to too low non-basal slip Schmid factor and too high basal slip Schmid factor.
Example 8
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 1.5% of Nd, 0.2% of Mn and the balance of Mg.
The Schmid factor ratio of cylindrical surface slip to basal plane slip of the magnesium alloy with high bulging property and high heat resistance of the embodiment is 1.23, the Schmid factor ratio of conical surface slip to basal plane slip is 1.31, and meanwhile, the magnesium alloy has a mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size of less than or equal to 15 mu m is 60%.
A method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment comprises the following steps:
s1, carrying out homogenization treatment on the alloy, and then carrying out thermal deformation of 3 passes at 430 ℃, wherein the accumulated true strain is 0.3, and the thermal deformation directions of all the passes are the same;
s2, carrying out thermal deformation on the magnesium alloy at 480 ℃ for 1 pass, wherein the accumulated true strain is 0.6, and the thermal deformation direction is vertical to that of the step S1;
and S3, annealing the magnesium alloy at 300 ℃ for 50min to obtain a finished product.
The resulting Mg-1.5Nd-0.2Mn alloy was labeled sample No. 13, and had a ratio of cylindrical surface slip Schmid factor (0.407) to basal surface slip Schmid factor (0.331) of 1.23, a ratio of conical surface slip Schmid factor (0.434) to basal surface slip Schmid factor (0.331) of 1.31, and had a mixed crystal grain size with a crystal grain volume fraction of 60% having a crystal grain size of 15 μm or less.
Example 9
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 1.5% of Nd, 0.2% of Mn and the balance of Mg.
The method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment is different from the method of the embodiment 8 only in that the thermal deformation of the step S2 is performed by 3 passes, wherein the thermal deformation direction of the 1 st pass is perpendicular to the thermal deformation direction of the step S1, the thermal deformation direction of the 2 nd pass is perpendicular to the thermal deformation direction of the 1 st pass and the thermal deformation direction of the step S1, and the thermal deformation direction of the 3 rd pass is the same as the thermal deformation direction of the step S1.
The resulting Mg-1.5Nd-0.2Mn alloy, labeled sample No. 14, had a ratio of cylindrical slip Schmid factor (0.343) to basal slip Schmid factor (0.364) of 0.94 and a ratio of conical slip Schmid factor (0.389) to basal slip Schmid factor (0.364) of 1.07, while the alloy had a mixed grain size with a grain size ≦ 15 μm in a volume fraction of 70%.
Example 10
The magnesium alloy with high bulging property and high heat resistance comprises, by mass, 1.5% of Nd, 0.2% of Mn and the balance of Mg.
The method for manufacturing the magnesium alloy with high bulging property and high heat resistance of the present example is different from example 8 only in that the thermal deformation of step S1 is 1 pass.
The resulting Mg-1.5Nd-0.2Mn alloy was labeled sample No. 15, and had a ratio of cylindrical slip Schmid factor (0.427) to basal slip Schmid factor (0.312) of 1.37 and a ratio of conical slip Schmid factor (0.456) to basal slip Schmid factor (0.312) of 1.46, while the alloy had a mixed grain size with a grain volume fraction of 80% for grain sizes of 15 μm or less.
Comparative example 6
A magnesium alloy contains, by mass%, 1.5% Nd and 0.2% Mn, with the balance being Mg.
The magnesium alloy was prepared in a manner different from that of example 8 only in that the directions of hot deformation in the 3 passes of step S1 were perpendicular to each other.
The obtained Mg-1.5Nd-0.2Mn alloy is marked as sample No. 16, the ratio of cylindrical surface slippage Schmid factor (0.321) to basal surface slippage Schmid factor (0.387) is 0.83, the ratio of conical surface slippage Schmid factor (0.321) to basal surface slippage Schmid factor (0.387) is 0.83, and meanwhile, the alloy has mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size less than or equal to 15 mu m is 90%.
Comparative example 7
A magnesium alloy contains, by mass%, 1.5% Nd and 0.2% Mn, with the balance being Mg.
The magnesium alloy was prepared in the same manner as in example 8 except that the hot deformation direction in step S2 was the same as that in step S1.
The resulting Mg-1.5Nd-0.2Mn alloy was labeled sample No. 17, and had a ratio of cylinder slip Schmid factor (0.459) to basal slip Schmid factor (0.261) of 1.76 and a ratio of cone slip Schmid factor (0.473) to basal slip Schmid factor (0.261) of 1.81, while the alloy had a mixed grain size with a grain volume fraction of 30% for grain sizes of 15 μm or less.
The obtained 5 magnesium alloys and the existing commercial AZ31 magnesium alloy were loaded at room temperature at a rate of 1 × 10-3s-1The results of the tensile creep test at 200 ℃ and 100MPa are shown in Table 4, in which the bulging property is represented by the ratio of the thickness after bulging to the thickness before bulging, and the heat resistance is represented by the creep life.
TABLE 4
| Sample number | Bulging ability | Creep life (hours) | |
| 13 | Example 8 | 4.6 | ≥100 |
| 14 | Example 9 | 4.3 | 85 |
| 15 | Example 10 | 4.1 | ≥100 |
| 16 | Comparative example 6 | 3.3 | 15 |
| 17 | Comparative example 7 | 1.2 | 70 |
| AZ31 | 1.3 | 25 |
As can be seen from table 4, samples No. 13, 14 and 15 have balanced relative activities of non-basal slip and basal slip, and reasonable percent of fine crystal volume, and compared with AZ31 magnesium alloy, the 3 samples simultaneously obtain high bulging property and high heat resistance, especially sample No. 13, and the thermal deformation of step S2 has only 1 pass, while the thermal deformation of step S1 has multiple passes, which further enhances the bulging property and heat resistance; in contrast, sample 16 had too low a non-basal plane slip Schmid factor and too high a basal plane slip Schmid factor, resulting in inferior heat resistance to AZ31 magnesium alloy, and sample 17 had too high a non-basal plane slip Schmid factor and too low a basal plane slip Schmid factor, resulting in inferior bulging to AZ31 magnesium alloy.
Example 11
The magnesium alloy with high bulging property and high heat resistance of the invention comprises 0.8% of Ca and 0.1% of In by mass percent, and the balance of Mg.
The Schmid factor ratio of cylindrical surface slip to basal plane slip of the magnesium alloy with high bulging property and high heat resistance of the embodiment is 1.33, the Schmid factor ratio of conical surface slip to basal plane slip is 1.40, and meanwhile, the magnesium alloy has mixed crystal grain size, and the volume fraction of crystal grains with the crystal grain size of less than or equal to 15 mu m is 70%.
A method for preparing the magnesium alloy with high bulging property and high heat resistance of the embodiment comprises the following steps:
s1, carrying out homogenization treatment on the alloy, and then carrying out thermal deformation on the alloy for 4 passes at 470 ℃, wherein the accumulated true strain is 0.6, and the thermal deformation directions of all the passes are the same;
s2, carrying out thermal deformation on the magnesium alloy at 510 ℃ for 2 passes, wherein the accumulated true strain is 0.6, the thermal deformation direction of the 1 st pass is vertical to the thermal deformation direction of the step S1, and the thermal deformation direction of the 2 nd pass is the same as the thermal deformation direction of the step S1, so as to obtain a finished product.
The resulting Mg-0.8Ca-0.1In alloy was labeled sample No. 18, and had a ratio of cylindrical slip Schmid factor (0.415) to basal slip Schmid factor (0.312) of 1.33, a ratio of conical slip Schmid factor (0.438) to basal slip Schmid factor (0.312) of 1.40, and a mixed grain size with a grain size of 15 μm or less In a fraction of 70% by volume of grains.
Example 12
The magnesium alloy with high bulging property and high heat resistance of the invention contains 0.8% of Ca and the balance of Mg by mass%.
The method for producing the magnesium alloy having high bulging properties and high heat resistance of this example is different from example 11 only in that the raw material composition is Mg-0.8 Ca.
The resulting Mg-0.8Ca alloy was labeled sample No. 19, and had a ratio of cylinder slip Schmid factor (0.431) to basal slip Schmid factor (0.317) of 1.36 and a ratio of cone slip Schmid factor (0.466) to basal slip Schmid factor (0.317) of 1.47, while the alloy had a mixed grain size with a 75% volume fraction of grains having a grain size of 15 μm or less.
Comparative example 8
A magnesium alloy contains, by mass%, 0.8% Ca and 0.1% In, with the balance being Mg.
The magnesium alloy was prepared in a manner different from that of example 11 only in that the heat distortion temperature of step S1 was 510 ℃.
The resulting Mg-0.8Ca-0.1In alloy was labeled sample No. 20, and had a ratio of cylindrical slip Schmid factor (0.474) to basal slip Schmid factor (0.304) of 1.56, a ratio of conical slip Schmid factor (0.487) to basal slip Schmid factor (0.304) of 1.60, and a mixed grain size with a grain size of 15 μm or less In a 30 volume fraction of grains.
The obtained 3 magnesium alloys and the existing commercial AZ31 magnesium alloy were loaded at room temperature at a rate of 1 × 10-2s-1The results of the tensile creep test at 220 ℃ and 90MPa are shown in Table 5, in which the bulging property is represented by the ratio of the thickness after bulging to the thickness before bulging, and the heat resistance is represented by the creep life.
TABLE 5
| Sample number | Bulging ability | Creep life (hours) | |
| 18 | Example 11 | 3.9 | ≥100 |
| 19 | Example 12 | 3.8 | 90 |
| 20 | Comparative example 8 | 1.1 | 65 |
| AZ31 | 1.2 | 25 |
As can be seen from Table 5, samples No. 18 and 19 have balanced relative activities of non-basal plane slip and basal plane slip, and the percentage of fine crystal volume is reasonable, compared with AZ31 magnesium alloy, the samples have high bulging property and high heat resistance, especially sample No. 18, and the added In further enhances the heat resistance; in contrast, sample 20 had inferior bulging properties to those of the AZ31 magnesium alloy due to the excessively high non-basal-plane slip Schmid factor and the excessively low basal-plane slip Schmid factor.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. The magnesium alloy with high bulging property and high heat resistance is characterized by comprising 0.5-2.0% of X element by mass percent, wherein the X element is one or more of rare earth elements and calcium elements; and the ratio of the Schmid factor of non-basal plane slip of at least one of the cylindrical surface slip and the conical surface slip of the magnesium alloy to the Schmid factor of basal plane slip is 1.0-1.4.
2. The magnesium alloy according to claim 1, wherein the volume fraction of crystal grains having a grain size of 15 μm or less is 40 to 80%.
3. The magnesium alloy with high bulging property and high heat resistance according to claim 1 or 2, wherein the Schmid factor ratio of the cylindrical surface slippage and the conical surface slippage to the basal surface slippage of the magnesium alloy is in a range of 1.0-1.4.
4. The magnesium alloy according to claim 1 or 2, further comprising 0 to 0.5% by mass of a manganese element or a zirconium element.
5. The magnesium alloy according to claim 1 or 2, further comprising an indium element or a zinc element, wherein the indium element or the zinc element is contained in an amount of 0 to 0.5% by mass.
6. The method for producing a magnesium alloy having high bulging property and high heat resistance according to any one of claims 1 to 5, comprising the steps of:
s1, preparing a magnesium alloy ingot according to alloy component requirements, and carrying out thermal deformation on the magnesium alloy ingot at 400-500 ℃ in 1 pass or multiple passes with the same deformation direction after homogenization treatment;
s2, performing thermal deformation on the magnesium alloy obtained in the step S1 at 450-520 ℃ for 1 or more passes, wherein the accumulated true strain of the thermal deformation is 0.4-0.8, and the deformation direction of the 1 st pass thermal deformation is perpendicular to the deformation direction of the thermal deformation in the step S1, so that the magnesium alloy with high bulging property and high heat resistance is obtained.
7. The method of producing a magnesium alloy having high heat resistance and high expandability according to claim 6, wherein the heat distortion temperature in step S2 is not lower than the heat distortion temperature in step S1.
8. The method for producing a magnesium alloy having high bulging property and high heat resistance according to claim 6 or 7, further comprising an annealing treatment after step S2; the temperature of the annealing treatment is 250-350 ℃, and the time of the annealing treatment is 10-120 min.
9. The method of producing a magnesium alloy having high bulging property and high heat resistance according to claim 6 or 7, wherein the hot deformation is performed by 1-pass working in step S2.
10. The method for producing a magnesium alloy having high bulging property and high heat resistance according to claim 6 or 7, wherein in step S1, the hot deformation is performed by a plurality of passes;
the cumulative true strain of the thermal deformation is 0.3-0.7.
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