CN111945048A - Low-cost high-strength wrought magnesium alloy and preparation method thereof - Google Patents
Low-cost high-strength wrought magnesium alloy and preparation method thereof Download PDFInfo
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- CN111945048A CN111945048A CN202010627075.8A CN202010627075A CN111945048A CN 111945048 A CN111945048 A CN 111945048A CN 202010627075 A CN202010627075 A CN 202010627075A CN 111945048 A CN111945048 A CN 111945048A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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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 relates to a low-cost high-strength wrought magnesium alloy and a preparation method thereof, belonging to the technical field of metal materials. The magnesium alloy consists of Mg, Sm and Ca elements, and comprises the following components in percentage by mass: sm:4.8-5.6 wt.%; 0.8-1.0wt.% Ca; the balance of Mg and inevitable impurity elements. The invention solves the problems of overhigh cost of rare earth elements used in the existing magnesium alloy and the like, and the deformed Mg-Sm-Ca alloy obtained by carrying out high-pressure torsion and heat treatment after the solid solution of the Mg-Sm-Ca alloy has the advantages of light weight, high hardness, low cost, good heat resistance and the like and has wide application prospect.
Description
Technical Field
The invention relates to a low-cost high-strength wrought magnesium alloy and a preparation method thereof, belonging to the technical field of metal materials.
Background
The magnesium alloy is used as a novel structural material in the 21 st century, has the advantages of low density, low elastic modulus, high specific strength and specific stiffness, good electromagnetic shielding performance and the like, and has wide application prospects in the fields of traffic, communication, electrical appliances and aerospace. However, magnesium alloys have limited applications due to their relatively low strength and poor thermal stability.
The Mg rare earth alloy has excellent mechanical property, and the research on the Mg rare earth alloy is increasingly wide in recent years. The solid solubility of the rare earth element in magnesium is high, nano-scale precipitation can be formed, and the aging strengthening characteristic is obvious. However, rare earth elements are expensive. Sm has a unique orthorhombic structure with strengthening action slightly greater than Gd and much less expensive than Nd, Y and Gd. The maximum solid solubility of Sm in Mg at 530 ℃ is 5.7 wt.%, much higher than the solid solubility of Nd (3.6 wt.%). The cheap Ca is introduced as a grain refiner, and the research shows that the addition amount of the Ca is 1.0wt.% so that the magnesium grains can be obviously refined by forming a stable Mg2Ca phase. Therefore, the research and development of the low-cost high-strength magnesium alloy have certain development potential.
Disclosure of Invention
The invention aims to provide a low-cost high-strength wrought magnesium alloy and a preparation method thereof, wherein the wrought magnesium alloy has the advantages of light weight, high hardness, good heat resistance and the like, does not contain noble metal, and has good economic benefit and wide application prospect.
In order to achieve the purpose, the invention adopts the technical scheme that:
the low-cost high-strength wrought magnesium alloy is Mg-Sm-Ca alloy wrought magnesium alloy, and comprises the following raw material components in percentage by mass:
sm: 3.2-6.8 wt.%; 0.8-1.2 wt.% Ca; the balance being Mg and unavoidable impurity elements.
The technical scheme of the invention is further improved as follows: the magnesium alloy comprises the following components in percentage by mass:
sm: 4.8-5.2 wt.%; 0.9-1.1 wt.% Ca; the balance being Mg and unavoidable impurity elements.
The technical scheme of the invention is further improved as follows: the total content of impurity elements is less than 0.03 wt.%.
A preparation method of a low-cost high-strength wrought magnesium alloy comprises the following steps:
firstly, preparing a magnesium alloy ingot: raw material ingredients of magnesium ingots, samarium blocks and calcium particles are smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: carrying out solution treatment on the magnesium alloy ingot at 510-530 ℃ for 8-12 hours, carrying out water quenching, and processing into a high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 3-5 GPa, the number of torsion turns is 1-5 r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation;
fourthly, aging treatment: and (3) carrying out heat treatment on the high-pressure torsion sample at 125-200 ℃ for 0.5-30 hours, and carrying out air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy.
The technical scheme of the invention is further improved as follows: in the first step, the raw material is pure metal.
The technical scheme of the invention is further improved as follows: and isolating the magnesium alloy from air in the treatment processes of the second step and the fourth step.
The technical scheme of the invention is further improved as follows: step two and step four are isolated from air by covering and compacting the magnesium alloy with magnesium oxide powder in the crucible.
Due to the adoption of the technical scheme, the invention has the following technical effects:
the invention firstly provides a low-cost high-strength heat-resistant magnesium alloy, which comprises the components of Mg-Sm-Ca, wherein Sm is an inexpensive rare earth element, the maximum solid solubility of Sm in Mg at 530 ℃ is 5.7 wt.%, and the alloy has good solid solution strengthening and precipitation strengthening effects. After a proper amount of cheap Ca is added, stable Mg2Ca phase can be formed to obviously refine magnesium grains. In addition, the Ca segregation capacity is strong, the diffusion of other elements is inhibited, the heterogeneous nucleation effect is achieved, and the growth of crystal grains is hindered. After high-pressure twisting, a large number of crystal defects (grain boundaries, dislocations, vacancies, and the like) are generated, the deformation resistance is increased, and work hardening occurs. The interaction between dislocations in the alloy contributes to the strength of the alloy. The crystal defects caused by pre-deformation can provide more precipitation phase nucleation sites, increase the precipitation number density in the subsequent aging treatment process and have good aging hardening effect. In addition, the pinning of the nanoscale precipitates at the grain boundary after the aging treatment effectively reduces the grain boundary mobility and the grain growth driving force, and the alloy shows good recovery resistance to dislocation rearrangement, has high thermal stability and further improves the strength. The low-cost high-strength wrought magnesium alloy has excellent mechanical properties.
The invention also provides a preparation method of the low-cost high-strength heat-resistant magnesium alloy, which has the following advantages:
1. the process is simple and controllable, the deformation degree is large, and the grain refining effect is obvious.
2. The alloy has low cost. Most magnesium rare earth alloys are relatively expensive, while Sm is much cheaper than Nd, Y and Gd. In the alloy, the consumption of Sm and Ca is less, the impurity content is less, and the material cost is greatly reduced.
3. Compared with the traditional magnesium alloy, the Mg-Sm-Ca alloy has obvious aging strengthening characteristic, can cause crystal defects by combining the most effective high-pressure torsion in a severe plastic deformation method, effectively increases precipitation nuclei, can form compact nano precipitates at a relatively low aging temperature, improves the alloy hardness through solid solution strengthening, grain boundary strengthening, precipitation strengthening and the like, and has certain economic benefit and development potential.
Drawings
FIG. 1 is a scanning electron micrograph of the aged microstructure of the magnesium alloy with a modified morphology according to example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of a morphotropic magnesium alloy microstructure in example 2 of the present invention;
FIG. 3 is a selected electron diffraction pattern corresponding to the microstructure of the morphotropic magnesium alloy of example 2;
FIG. 4 is a transmission electron micrograph of the aged microstructure of the magnesium alloy with a modified morphology according to example 3 of the present invention and a corresponding selected electron diffraction pattern;
FIG. 5 is a graph of the HAADF microstructure of the aged wrought magnesium alloy of example 3 of the present invention;
FIG. 6 shows the result of XRD analysis of the microstructure of the wrought magnesium alloy of example 3 of the present invention after aging.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments:
the invention discloses a low-cost high-strength wrought magnesium alloy, which is prepared from Sm 3.2-6.8 wt% of raw materials; 0.8-1.2 wt.% Ca; the balance being Mg and unavoidable impurity elements. Preferred is Sm: 4.8-5.2 wt.%; 0.9-1.1 wt.% Ca; the balance of Mg and inevitable impurity elements, and the total content of the impurity elements is controlled below 0.03 wt.%.
The invention also provides a preparation method of the low-cost high-strength wrought magnesium alloy, which is prepared by smelting and casting, solid solution treatment, high-pressure torsion and timely treatment of pure magnesium, pure samarium and pure calcium as raw materials, and comprises the following steps:
firstly, preparing a magnesium alloy ingot: raw material ingredients of pure magnesium, pure samarium and pure calcium are smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: covering the magnesium alloy ingot in a crucible with magnesium oxide powder and compacting the magnesium alloy to isolate air, carrying out solution treatment on the magnesium alloy ingot at 510-530 ℃ for 8-12 hours, carrying out water quenching, and processing the magnesium alloy ingot into a high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 3-5 GPa, the number of torsion turns is 1-5 r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation;
fourthly, aging treatment: and covering and compacting the high-pressure torsion sample by using magnesium oxide powder in a crucible to isolate air, then carrying out heat treatment at 125-200 ℃ for 0.5-30 hours, and carrying out air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy.
The following are specific examples of the present invention:
example 1
Firstly, preparing a magnesium alloy ingot: sm is the following components in percentage by mass: 6.8 wt.%; 1.2wt.% Ca; the balance of Mg and inevitable impurity elements, the total content of the impurity elements is below 0.03wt.%, and the mixture is smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: the magnesium alloy ingot is subjected to solution treatment at 530 ℃ for 8 hours, and during the treatment, the magnesium alloy ingot is covered by magnesium oxide powder in a crucible and compacted. Water quenching and processing into high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 5GPa, the number of torsion turns is 4r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation;
fourthly, aging treatment: the high-pressure twisted sample was heat-treated at 150 ℃ for 8 hours, during which it was covered with magnesium oxide powder in a crucible and compacted. Air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy.
The microstructure of the low-cost high-strength wrought magnesium alloy prepared in this example is shown in FIG. 1, and the Vickers hardness thereof is 135 HV.
Example 2
The mass percentage of the low-cost high-strength wrought magnesium alloy is Sm: 5.0 wt.%; ca:0.8 wt.%; the balance being Mg and unavoidable impurity elements.
The preparation of the low-cost high-strength wrought magnesium alloy comprises the following steps:
firstly, preparing a magnesium alloy ingot: sm is the following components in percentage by mass: 5.0 wt.%; ca:0.8 wt.%; the balance of Mg and inevitable impurity elements, the total content of the impurity elements is below 0.03wt.%, and the mixture is smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: the magnesium alloy ingot is subjected to solution treatment at 530 ℃ for 8 hours, and during the treatment, the magnesium alloy ingot is covered by magnesium oxide powder in a crucible and compacted. Water quenching and processing into high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 5GPa, the number of torsion turns is 1r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation; the microstructure of the deformed magnesium alloy is shown in figure 2, the size of a sub-crystal is 108nm, and the existence of a nano-crystal is confirmed by selecting an electron diffraction pattern close to a continuous ring structure. The uneven contrast inside the crystal grains is caused by the distortion of crystal lattices after high-pressure torsion;
fourthly, aging treatment: the high-pressure twisted samples were heat treated at 175 ℃ for 1, 2, 3, 8, 17, 30 hours, during which they were covered with magnesium oxide powder in a crucible and compacted. Air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy.
The mechanical properties of the low-cost high-strength wrought magnesium alloy prepared in this example are shown in the following table:
| aging time (hours) | 1 | 2 | 3 | 8 | 17 | 30 |
| Vickers Hardness (HV) | 131 | 130 | 119 | 116 | 115 | 116 |
Example 3
The mass percentage of the low-cost high-strength wrought magnesium alloy is Sm: 5.2 wt.%; 0.9 wt.% Ca; the balance being Mg and unavoidable impurity elements.
The preparation of the low-cost high-strength wrought magnesium alloy comprises the following steps:
firstly, preparing a magnesium alloy ingot: sm is the following components in percentage by mass: 5.2 wt.%; 0.9 wt.% Ca; the balance of Mg and inevitable impurity elements, the total content of the impurity elements is below 0.03wt.%, and the mixture is smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: the magnesium alloy ingot is subjected to solution treatment at 530 ℃ for 8 hours, and during the treatment, the magnesium alloy ingot is covered by magnesium oxide powder in a crucible and compacted. Water quenching and processing into high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 5GPa, the number of torsion turns is 4r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation;
fourthly, aging treatment: the high-pressure twisted samples were aged at 125 deg.C, 150 deg.C and 175 deg.C for 1, 3, 5, 8, 17, 23, 30 hours, covered with magnesium oxide powder in a crucible and compacted during the process. Air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy. The microstructure aged for 8 hours at 125 ℃ is shown in fig. 4, dislocation entanglement is serious in some sub-grains, complex structures such as dislocation walls, dislocation cells and the like are formed, due to the fact that large stress and strain are generated in the high-pressure twisting process, crystal lattices are distorted, high-density dislocations are formed in crystals, and the dislocation strengthening effect is achieved. The presence of nanocrystals with high angle grain boundaries was confirmed by the selection of a continuous ring structure whose electron diffraction pattern comprises multiple point reflections. As shown in FIG. 5, the high defect density (e.g., dislocations, grain boundaries, and vacancies) introduced by HPT deformation provides nucleation sites, enhances precipitates, and Mg after aging41Sm5The phase precipitation is shown in figure 6 and is distributed in a dispersed manner, so that dislocation slippage can be effectively hindered, and the alloy strength is favorably improved.
The mechanical properties of the low-cost high-strength wrought magnesium alloy prepared in this example are shown in the following table:
the above table shows that the wrought magnesium alloy has high strength after high-pressure torsion and aging, has less and cheap Sm and Ca consumption, and lower cost, and has certain economic benefit and development potential.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape, principle and the like of the invention are covered by the protection scope of the invention.
Claims (7)
1. A low-cost high-strength wrought magnesium alloy is characterized in that: the alloy is Mg-Sm-Ca alloy wrought magnesium alloy, and comprises the following raw material components in percentage by mass:
sm: 3.2-6.8 wt.%; 0.8-1.2 wt.% Ca; the balance being Mg and unavoidable impurity elements.
2. The low-cost high-strength wrought magnesium alloy according to claim 1, wherein: the magnesium alloy comprises the following components in percentage by mass:
sm: 4.8-5.2 wt.%; 0.9-1.1 wt.% Ca; the balance being Mg and unavoidable impurity elements.
3. A low cost high strength wrought magnesium alloy according to claim 1 or 2, wherein: the total content of impurity elements is less than 0.03 wt.%.
4. A preparation method of low-cost high-strength wrought magnesium alloy is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing a magnesium alloy ingot: raw material ingredients of magnesium ingots, samarium blocks and calcium particles are smelted and cast into magnesium alloy ingots;
secondly, preparing a high-pressure torsion material: carrying out solution treatment on the magnesium alloy ingot at 510-530 ℃ for 8-12 hours, carrying out water quenching, and processing into a high-pressure torsion material;
thirdly, preparing a high-pressure torsion sample: performing high-pressure torsion treatment at room temperature, wherein the torsion pressure is 3-5 GPa, the number of torsion turns is 1-5 r, the torsion speed is 1r/min, and preparing a high-pressure torsion sample through plastic deformation;
fourthly, aging treatment: and (3) carrying out heat treatment on the high-pressure torsion sample at 125-200 ℃ for 0.5-30 hours, and carrying out air cooling to room temperature to obtain the low-cost high-strength wrought magnesium alloy.
5. The low-cost high-strength wrought magnesium alloy according to claim 4, wherein: in the first step, the raw material is pure metal.
6. The low-cost high-strength wrought magnesium alloy according to claim 4, wherein: and isolating the magnesium alloy from air in the treatment processes of the second step and the fourth step.
7. The low-cost high-strength wrought magnesium alloy according to claim 6, wherein: step two and step four are isolated from air by covering and compacting the magnesium alloy with magnesium oxide powder in the crucible.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1965099A (en) * | 2004-06-15 | 2007-05-16 | 株式会社东京大学Tlo | High toughness magnesium-base alloy, drive component using same, and method for producing high toughness magnesium-base alloy material |
| CN109680195A (en) * | 2019-02-19 | 2019-04-26 | 北京大学 | A kind of Mg-RE system magnesium alloy and the preparation method and application thereof |
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- 2020-07-01 CN CN202010627075.8A patent/CN111945048A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1965099A (en) * | 2004-06-15 | 2007-05-16 | 株式会社东京大学Tlo | High toughness magnesium-base alloy, drive component using same, and method for producing high toughness magnesium-base alloy material |
| CN109680195A (en) * | 2019-02-19 | 2019-04-26 | 北京大学 | A kind of Mg-RE system magnesium alloy and the preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| CHAI YUESHENG ET AL.: "Microstructure and Mechanical Properties of Extruded Mg-Sm-Ca Alloys", 《RARE METAL MATERIALS AND ENGINEERING》 * |
| YANSHENG LI ET AL.: "Exceptional aging hardening behaviour of nanocrystalline Mg-Y-Nd-Gd-Zr alloy prepared by high pressure torsion", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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