CN114635068B - High-strength and high-toughness cast magnesium rare earth alloy and preparation method thereof - Google Patents
High-strength and high-toughness cast magnesium rare earth alloy and preparation method thereof Download PDFInfo
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- CN114635068B CN114635068B CN202210242703.XA CN202210242703A CN114635068B CN 114635068 B CN114635068 B CN 114635068B CN 202210242703 A CN202210242703 A CN 202210242703A CN 114635068 B CN114635068 B CN 114635068B
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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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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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 discloses a high-strength and high-toughness cast magnesium-rare earth alloy and a preparation method thereof, wherein the magnesium alloy comprises the following components in percentage by mass: 2.6 to 3.0 percent of Nd,0.1 to 0.4 percent of Zn,0.1 to 0.4 percent of La,0.3 to 0.7 percent of Zr, less than 0.2 percent of total amount of impurity elements Si, fe, cu and Ni and the balance of Mg; the preparation method comprises the working procedures of material drying, magnesium melting, alloying element addition, refining, casting forming, heat treatment and the like. According to the invention, through microalloying of low-cost La element and optimization of a subsequent hot-treatment process, the room-temperature yield strength of the Mg-Nd series alloy is obviously improved, and meanwhile, the manufacturing cost of the alloy is not obviously increased, so that the popularization and application of the Mg-Nd series alloy are facilitated.
Description
Technical Field
The invention relates to a high-strength and high-toughness cast magnesium-rare earth alloy and a preparation method thereof, belonging to the technical field of metal structural materials.
Background
As the lightest metal structural material, the magnesium alloy has the advantages of high specific strength, high specific rigidity, good shock absorption and the like, and is widely applied to the fields of aerospace, rail transit, 3C and the like. The Mg-Nd system has good room temperature strength and casting performance, and has been widely applied in the aerospace field in recent years, such as EZ30Z cast magnesium rare earth alloy and ZM6 magnesium rare earth alloy in China in national standards of cast magnesium alloy ingot (GB/T19078-2016). Although the Mg-Nd series alloy has good casting performance, the room temperature yield strength of the alloy is lower, usually lower than 150MPa, and severely limits the application range of the Mg-Nd series alloy. How to further improve the strong plasticity of Mg-Nd series alloy becomes one of the hot research directions of casting magnesium rare earth alloy. Therefore, magnesium Elektron develops commercial high-strength magnesium rare earth alloy EV31 (Mg-Nd-Gd-Zn-Zr, elektron 21) on the basis of the existing Mg-Nd alloy, the room temperature strength of the alloy is further improved by adding 1.0-1.7 wt.% Gd element on the basis of the Mg-Nd alloy, the room temperature yield strength of the Mg-Nd alloy is improved from 140MPa of ZM6 and EZ30Z magnesium rare earth alloy to 170MPa of EV31 magnesium rare earth alloy, and the application of the Mg-Nd alloy is remarkably promoted. However, the Gd element has high cost, and the addition of 1.0-1.7wt% Gd element obviously increases the manufacturing cost of the alloy; meanwhile, the Gd element has relatively active chemical property, so that oxide scale defects are more easily introduced in the casting process, and the quality of castings is reduced. Therefore, how to improve the room temperature strength of mg—nd based alloys without significantly increasing the manufacturing cost of the alloys becomes an industrial problem in the design and development of magnesium rare earth alloys.
Disclosure of Invention
The invention aims to provide a high-strength and high-toughness cast magnesium rare earth alloy and a preparation method thereof, aiming at the defects existing in the prior art. According to the invention, a high-strength casting magnesium rare earth alloy is developed on the basis of the Mg-Nd series alloy by a microalloying method, the room temperature strength of the Mg-Nd series alloy is improved, the alloy manufacturing cost is not obviously improved, and the popularization and the application of the Mg-Nd series alloy are facilitated.
The invention aims at realizing the following technical scheme:
in a first aspect, the invention provides a high-strength and high-toughness cast magnesium rare earth alloy, which comprises the following components in percentage by weight:
Nd：2.6～3.0％，
Zn：0.1～0.4％，
La：0.1～0.4％，
Zr：0.3～0.7％，
the balance being magnesium and unavoidable impurities, the sum of the weight percentages of said impurities not exceeding 0.2%.
The invention adopts Nd (neodymium) as a first component: the prior study shows that the solid solubility of Nd in Mg solid solution is almost zero at 200 ℃, and the solid solubility at the eutectic temperature of 552 ℃ is 3.6wt%, so that the aging precipitation strengthening and solid solution strengthening effects are good only by adding a small amount of Nd element alloy. The study shows that when Nd content is more than 3.0wt.%, the Mg12Nd phase generated in the casting process is difficult to be completely dissolved in a short time when the solution treatment is carried out at high temperature; when Nd content is less than 2.6 wt%, alloy strengthening effect is low in subsequent aging treatment, and mechanical properties of castings are difficult to guarantee. In the invention, the components of Nd element are as follows: 2.6 to 3.0wt.%.
The invention adopts Zn (zinc) as a second component: the existing research shows that when trace Zn elements are added into an Mg-Nd alloy system, zn exists in a solid solution atom form in a magnesium matrix and a precipitated phase, so that a non-basal plane sliding system is activated when the magnesium alloy is subjected to room temperature plastic deformation, and the room temperature plasticity of the alloy is obviously improved; in the system of the present invention, when the Zn content is >0.4wt.%, zn element reacts with Zr element during the solution treatment to form more acicular Zn2Zr3 phase, which has a negative effect on the plasticity of the alloy, although having a certain strengthening effect. In the invention, the Zn comprises the following components in percentage by weight: 0.1 to 0.40wt.%.
La (lanthanum) is adopted as a third component: the prior study shows that La has almost no solid solubility in magnesium alloy, and La and Mg form Mg at 610 DEG C 12 La eutectic phase; the study shows that Mg 12 La phase can well pin grain boundary during high-temperature solution treatment of alloy at 540-550 ℃, effectively inhibit coarsening of magnesium alloy grains, and meanwhile, trace La element dissolved into a magnesium matrix can improve the number density of Mg-Nd precipitated phase and enhance the strengthening effect of aging precipitated phase. When La content is>0.4wt.% Mg in the alloy 12 La phase particles coarsen, and alloy plasticity is obviously reduced. In the invention, the La comprises the following components: 0.10 to 0.40wt.%. In addition, la can play a role of inhibiting coarsening of crystal grains even in low-temperature solution treatment, but in low-temperature solution treatment, mgNd eutectic phases formed in the casting process cannot be completely dissolved into a magnesium alloy matrix, and the precipitation phase strengthening effect in subsequent aging is weakened. On the other hand, when the solution treatment temperature is higher than 550 ℃, the La element can effectively inhibit coarsening of the crystal grain size, but the inhibition effect is weaker than 545 to 555 ℃, the average crystal grain size is significantly increased, and meanwhile, overburning (local melting) is liable to occur. If the temperature is 580 ℃, local melting (overburning) is generated in the alloy, and cracks are generated in the casting/alloy during quenching.
The Zr (zirconium) is adopted as a fourth component, and similar to the conventional Zr-containing magnesium alloy, the effect of Zr in the Mg-Nd-Zn-La alloy is mainly grain refinement, and the content of Zr element is 0.3 to 0.7 weight percent.
Preferably, the impurity element contains at least one of silicon, iron, copper and nickel, and the content of silicon element is not more than 0.01%, the content of iron element is not more than 0.01%, the content of copper element is not more than 0.03% and the content of nickel element is not more than 0.005%.
In a second aspect, the invention also provides a preparation method of the high-strength and high-toughness cast magnesium rare earth alloy, which comprises the following steps:
and (3) baking: preheating pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr intermediate alloy respectively;
melting magnesium: melting the dried pure magnesium in a protective atmosphere environment;
adding alloy elements: when the temperature of the magnesium solution reaches 700-720 ℃, directly adding pure zinc, mg-Nd and Mg-La intermediate alloy into the magnesium solution; after all the intermediate alloy is melted, adding the Mg-Zr intermediate alloy when the temperature of the melt is raised to 760-780 ℃, and skimming the surface scum after the Mg-Zr intermediate alloy is melted;
refining: after Zr element is added, when the temperature of the melt is reduced to 750-760 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780-790 ℃ and the melt is kept stand;
casting and forming: standing the magnesium liquid to 690-740 ℃, skimming surface scum, and carrying out metal gravity casting to obtain Mg-Nd-Zn-La-Zr magnesium rare earth alloy sheet ingots;
and (3) heat treatment: and carrying out high-temperature solid solution treatment on the magnesium rare earth alloy sheet ingot, then quenching in water, and finally carrying out single-stage aging treatment to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
As one embodiment of the present invention, the high temperature solution treatment means solution treatment at 545 to 555 ℃ for 4 to 8 hours.
As one embodiment of the invention, the quenching medium in the water quenching process is water and the water temperature is 25-80 ℃.
As one embodiment of the invention, the single-stage aging treatment refers to aging treatment at 200-225 ℃ for 16-64 hours.
As one embodiment of the invention, the transfer time of the ingot in the in-water quenching process is <20 seconds.
As one embodiment of the invention, the protective atmosphere is SF 6 And CO 2 Is a mixed gas of (a) and (b).
As one embodiment of the present invention, the preheating is at 200 ℃ for more than 3 hours. Preferably at 200-250 deg.c for 3-8 hr.
In one embodiment of the present invention, in the step of adding the alloying element, the surface dross is skimmed off and stirred for 2 to 3 minutes.
As one embodiment of the present invention, the standing time in the refining step is 15 to 30 minutes.
Compared with the prior art, the invention has the following beneficial effects:
1) Compared with the existing high-strength cast magnesium rare earth alloys EZ30Z and ZM6, the invention can obviously improve the room temperature yield strength of the alloy from 140MPa of EZ30Z and ZM6 to 170MPa of the Mg-Nd-Zn-La-Zr alloy by adding a small amount of La element while not obviously improving the manufacturing cost of the alloy, and is more beneficial to popularization and application of the Mg-Nd alloy.
2) Compared with the existing high-strength cast magnesium rare earth alloy EV31, the Mg-Nd-Zn-La-Zr alloy developed by the invention has quite strong plasticity, but the manufacturing cost of the alloy is obviously reduced: according to the invention, a small amount of low-cost La element is used for replacing high-content high-cost Gd element, so that the manufacturing cost of the alloy is remarkably reduced.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 shows the effect of trace La elements on the grain size distribution of the alloy after solution treatment: (a) The microstructure of the Mg-2.8Nd-0.2Zn-0.4Zr magnesium rare earth alloy in comparative example 1 after solution treatment has an average grain size of 124+/-15 mu m; (b) In example 2, the microstructure of Mg-2.8Nd-0.2Zn-0.2La-0.4Zr magnesium rare earth alloy after solution treatment had an average grain size of 59.+ -. 12. Mu.m.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.8wt.% Nd, 0.2wt.% Zn,0.1 wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is increased to 770 ℃, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 2 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 750 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780 ℃ and the standing time is 20 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 700 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.2Zn-0.1La-0.4Zr prepared in the embodiment are as follows: the yield strength is 168+/-5 MPa, the tensile strength is 294+/-8 MPa, and the elongation is 12.4+/-1.0%.
Example 2
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.8wt.% Nd, 0.2wt.% Zn, 0.2wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is increased to 770 ℃, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 2 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 750 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780 ℃ and the standing time is 20 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 700 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.2Zn-0.2La-0.4Zr prepared in the embodiment are as follows: yield strength 174+ -6 MPa, tensile strength 306+ -7 MPa, elongation 11.6+ -0.8%.
In the present invention, la element has three roles in the alloy, (1) Mg 12 La phase in alloy<The grain boundary can be well pinned during high-temperature solution treatment at 555 ℃, and the coarsening of magnesium alloy grains can be effectively inhibited; (2) The trace La element dissolved in the magnesium matrix can improve the number density of the Mg-Nd precipitated phase in the subsequent aging heat treatment, and the strengthening effect of the aging precipitated phase is improved; (3) Mg of 12 La phase dispersion strengthening effect. The comprehensive effect of the three functions obviously improves the strong plasticity of the alloy. If Ce element is used as the material for preventing coarsening of grains in the solid solution treatment process of the magnesium alloy: ce can also prevent coarsening of crystal grains in the solution treatment process of magnesium alloy, but cannot improve the alloy strength and plasticity, and the inherent reason is that Ce element has negative influence on the strengthening effect of magnesium rare earth alloy precipitated phases in the subsequent aging treatment, and the strength and plasticity of the alloy are reduced.
Table 1 shows the heat treatment process and mechanical properties of the high strength and toughness cast magnesium rare earth alloy of the invention and the comparison table of ZM6, EZ30Z and EV31 of the existing high strength cast magnesium rare earth alloy. The mechanical property data of ZM6, EZ30Z and EV31 are self-test data and are superior to the national standard cast magnesium alloy ingot (GB/T19078-2016). FIG. 1 shows the effect of trace La elements on the grain size distribution of the alloy after solution treatment.
FIG. 1 illustrates that trace La elements can significantly inhibit coarsening of crystal grains in solid solution treatment of magnesium-rare earth alloy; table 1 shows that the high strength and toughness cast magnesium rare earth alloy of the invention has better strength and plasticity than ZM6 and EZ 30Z; compared with EV31, the high-strength and high-toughness cast magnesium rare earth alloy has equivalent yield strength, better tensile strength and plasticity.
TABLE 1
Example 3
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.8wt.% Nd, 0.2wt.% Zn, 0.4wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is increased to 770 ℃, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 2 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 750 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780 ℃ and the standing time is 20 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 700 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.2Zn-0.4La-0.4Zr prepared in the embodiment are as follows: the yield strength is 178+/-6 MPa, the tensile strength is 302+/-9 MPa, and the elongation is 8.2+/-0.6%.
Example 4
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.6wt.% Nd, 0.2wt.% Zn, 0.2wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is raised to 780 ℃, skimming surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 2 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 760 ℃, refining is carried out without power off, the temperature is increased to 780 ℃ after refining, and the standing time is 15 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 740 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.6Nd-0.2Zn-0.2La-0.4Zr prepared in the embodiment are as follows: the yield strength is 165+/-5 MPa, the tensile strength is 292+/-8 MPa, and the elongation is 12.6+/-0.7%.
Example 5
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 3.0wt.% Nd, 0.2wt.% Zn, 0.2wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is raised to 780 ℃, skimming surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 2 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 760 ℃, refining is carried out without power off, the temperature is increased to 780 ℃ after refining, and the standing time is 15 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 740 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-3.0Nd-0.2Zn-0.2La-0.4Zr prepared in the embodiment are as follows: the yield strength is 176+/-5 MPa, the tensile strength is 304+/-6 MPa, and the elongation is 10.4+/-0.8%.
Example 6
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.8wt.% Nd,0.1 wt.% Zn, 0.2wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is raised to 760 ℃, skimming surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 3 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 750 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780 ℃ and the standing time is 30 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 690 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.1Zn-0.2La-0.4Zr prepared in the embodiment are as follows: yield strength 177+ -5 MPa, tensile strength 302+ -5 MPa, elongation 11.5+ -0.7%.
Example 7
The embodiment relates to a high-strength and high-toughness cast magnesium-rare earth alloy, which comprises the following components in percentage by mass: 2.8wt.% Nd, 0.4wt.% Zn, 0.2wt.% La, 0.4wt.% Zr, the total content of impurity elements Si, fe, cu and Ni being less than 0.2wt.%, the balance Mg (wt.% means the percentage of components to the total mass of the magnesium alloy produced, the total mass being the sum of the mass of Mg, zn and various intermediate alloys).
The embodiment relates to a preparation method of the high-strength and high-toughness cast magnesium-rare earth alloy, wherein the casting process is carried out in SF 6 And CO 2 The method is carried out under the protection of the mixed gas, and comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr for more than 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure zinc, mg-30wt.% of Nd intermediate alloy and Mg-20wt.% of La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, adding Mg-30wt.% of Zr intermediate alloy when the temperature of the melt is raised to 760 ℃, skimming surface scum after the Mg-Zr intermediate alloy is melted, and stirring for 3 minutes. When Nd, la and Zr are added, the added intermediate alloy is supplemented in proper amount according to the actual yield of the elements.
(4) Refining: after Zr element is added, when the temperature of the melt is reduced to 750 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780 ℃ and the standing time is 30 minutes.
(5) Casting and forming: standing the magnesium liquid, cooling to 690 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel die is 30mm, the preheating temperature is 200 ℃, and the Mg-Nd-Zn-La-Zr cast magnesium rare earth alloy sheet ingot with the wall thickness of 30mm is obtained.
(6) And (3) heat treatment: and carrying out high-temperature solid solution treatment for 540 ℃ for 8 hours on the magnesium rare earth alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment for 200 ℃ for 32 hours to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.4Zn-0.2La-0.4Zr prepared in the embodiment are as follows: the yield strength is 178+/-6 MPa, the tensile strength is 296+/-6 MPa, and the elongation is 9.2+/-1.2%.
Comparative example 1
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: la element is not added in the comparative example, and Mg-2.8Nd-0.2Zn-0.4Zr cast magnesium rare earth alloy tablet ingot is obtained.
The room-temperature mechanical properties of the cast magnesium rare earth alloy T6 state of Mg-2.8Nd-0.2Zn-0.4Zr prepared in the comparative example are as follows: the yield strength is 144+/-6 MPa, the tensile strength is 282+/-12 MPa, and the elongation is 12.8+/-1.6%. As shown in FIG. 1 (a), the microstructure of the Mg-2.8Nd-0.2Zn-0.4Zr alloy obtained in this comparative example was such that the average grain size of the T6-state alloy was 124.+ -. 15. Mu.m, and the grain size was significantly coarsened as compared with that of example 2 (FIG. 1 (b), in which the average grain size was 59.+ -. 12. Mu.m). Therefore, in the alloy system, trace La element can obviously inhibit coarsening of crystal grains in solid solution treatment of the magnesium-rare earth alloy.
Comparative example 2
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: the La element content in this comparative example was 0.6wt%, and Mg-2.8Nd-0.2Zn-0.6La-0.4Zr cast magnesium rare earth alloy ingots were obtained.
The Mg-2.8Nd-0.2Zn-0.6La-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast state (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 180+/-7 MPa, the tensile strength is 288+/-14 MPa, and the elongation is 4.7+/-0.6%. The room temperature plasticity of the alloy is significantly reduced compared to example 2.
Comparative example 3
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: la element is not added in the comparative example, and 0.2wt.% of Ce is added to obtain Mg-2.8Nd-0.2Zn-0.2Ce-0.4Zr cast magnesium rare earth alloy cast ingot.
The Mg-2.8Nd-0.2Zn-0.2Ce-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and the crystal grains are obviously coarsened compared with the original cast state (as-cast) alloy. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 136+/-8 MPa, the tensile strength is 276+/-10 MPa, and the elongation is 6.8+/-0.6%. The room temperature yield strength of the alloy is significantly reduced compared to example 2, as well as the tensile strength and room temperature plasticity are significantly reduced.
Comparative example 4
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: la element is not added in the comparative example, and 0.6wt.% of Ce is added to obtain Mg-2.8Nd-0.2Zn-0.6Ce-0.4Zr cast magnesium rare earth alloy cast ingot.
The Mg-2.8Nd-0.2Zn-0.6Ce-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 145+/-7 MPa, the tensile strength is 272+/-7 MPa, and the elongation is 5.4+/-0.5%. The room temperature yield strength and plasticity of the alloy are significantly reduced, as compared to example 2, while the tensile strength is also significantly reduced.
Comparative example 5
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: la element is not added in the comparative example, and 0.2wt.% Ca is added to obtain Mg-2.8Nd-0.2Zn-0.2Ca-0.4Zr cast magnesium rare earth alloy cast ingot.
The Mg-2.8Nd-0.2Zn-0.2Ca-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and the crystal grains are obviously coarsened compared with the original cast state (as-cast) alloy. The room temperature mechanical properties of the T6 state are as follows: yield strength 142+/-8 MPa, tensile strength 278+/-12 MPa and elongation 8.6+/-1.2%. The room temperature yield strength of the alloy is significantly reduced compared to example 2, with a relatively significant reduction in tensile strength and room temperature plasticity.
Comparative example 6
In this comparative example, 0.2wt.% La element was added to a conventional commercial magnesium alloy AZ91D (Mg-9.0 Al-0.6Zn-0.3mn, wt.%) to give an AZ91D-0.2La alloy. The preparation method comprises the following steps:
(1) And (3) baking: preheating the intermediate alloy of pure magnesium, pure aluminum, pure zinc, al-Mn and Mg-La for 3 hours at 200 ℃.
(2) Melting magnesium: placing the dried pure magnesium into SF 6 /CO 2 Melting in a gas-shielded crucible resistance furnace.
(3) Adding alloy elements: when the temperature of the magnesium solution reaches 720 ℃, directly adding pure aluminum, pure zinc, al-10wt.% Mn and Mg-20wt.% La intermediate alloy into the magnesium solution; after the intermediate alloy is completely melted, skimming the surface scum when the temperature of the melt is raised to 750 ℃, and stirring for 2.5min.
(4) Refining: and (3) keeping the temperature of the melt at 750 ℃, refining without power off, and raising the temperature of the refined melt to 760 ℃ and standing for 20min.
(5) Casting and forming: standing the magnesium liquid, cooling to 700 ℃, skimming surface scum, and carrying out metal gravity casting, wherein the wall thickness of the steel mould is 30mm, the preheating temperature is 200 ℃, and the cast magnesium alloy sheet ingot with the wall thickness of 30mm, mg-9.0Al-0.6Zn-0.3Mn-0.2La (AZ 91D-La) is obtained.
(6) And (3) heat treatment: and carrying out rapid high-temperature solution treatment at 430 ℃ for 60min on the AZ91D-La cast magnesium alloy sheet ingot, then quenching in water at 80 ℃, and finally carrying out single-stage aging treatment at 175 ℃ for 16h to obtain the T6-state AZ91D-0.2La cast magnesium alloy.
Compared with the AZ91D alloy, the average grain size of the AZ91D-0.2La alloy after solution treatment is larger, namely the grain size of the alloy after solution treatment cannot be thinned by adding a small amount of La element in the AZ91D magnesium alloy. After the conventional T6 treatment, the strong plasticity of the AZ91D-0.2La alloy is equivalent to that of the AZ91D magnesium alloy, and the improvement effect is avoided.
Comparative example 7
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: the content of Nd element in the comparative example is 2.0wt.%, and Mg-2.0Nd-0.2Zn-0.2La-0.4Zr cast magnesium rare earth alloy cast ingot is obtained.
The Mg-2.0Nd-0.2Zn-0.2La-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast state (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: yield strength 142+ -4 MPa, tensile strength 256+ -8 MPa, and elongation 12.8+ -1.2%. The room temperature yield strength and tensile strength of the alloy were significantly reduced compared to example 2.
Comparative example 8
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: the content of Nd element in the comparative example is 3.4wt.%, and Mg-3.4Nd-0.2Zn-0.2La-0.4Zr cast magnesium rare earth alloy cast ingot is obtained.
The Mg-3.4Nd-0.2Zn-0.2La-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast state (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 182+/-8 MPa, the tensile strength is 295+/-8 MPa, and the elongation is 4.4+/-0.6%. The room temperature plasticity of the alloy is significantly reduced compared to example 2.
Comparative example 9
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: zn is not added in the comparative example, and the Mg-2.8Nd-0.2La-0.4Zr cast magnesium rare earth alloy cast ingot is obtained.
The Mg-2.8Nd-0.2La-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast state (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 164+/-4 MPa, the tensile strength is 273+/-7 MPa, and the elongation is 5.4+/-0.8%. The room temperature plasticity of the alloy is significantly reduced and the tensile strength is also significantly reduced compared to example 2.
Comparative example 10
The preparation method adopted in this comparative example is substantially the same as that adopted in example 2, except that: the content of Zn element in the comparative example is 0.8wt.%, and Mg-2.8Nd-0.8Zn-0.2La-0.4Zr cast magnesium rare earth alloy cast ingot is obtained.
The Mg-2.8Nd-0.8Zn-0.2La-0.4Zr cast magnesium rare earth alloy prepared in the comparative example is subjected to high-temperature solution treatment, and compared with the original cast state (as-cast) alloy, the coarsening degree of the crystal grains is equivalent to that of the example 2. The room temperature mechanical properties of the T6 state are as follows: the yield strength is 172+/-5 MPa, the tensile strength is 284+/-6 MPa, and the elongation is 4.7+/-0.5%. The room temperature plasticity of the alloy is significantly reduced compared to example 2.
In summary, through the above examples and comparative examples, it can be found that the room temperature yield strength of Mg-Nd alloy is significantly improved through microalloying of low-cost La element and optimization of subsequent heat treatment process, the strength of Mg-Nd-Zn-La-Zr alloy obtained through microalloying of La element reaches the level of EV31 magnesium rare earth alloy, and the plasticity is better than EV31, i.e., the technical scheme of the invention, while the room temperature strength of Mg-Nd alloy is improved, the manufacturing cost of alloy is not significantly increased, and the popularization and application of Mg-Nd alloy are more facilitated.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (9)
1. The high-strength and high-toughness cast magnesium rare earth alloy is characterized by comprising the following components in percentage by weight:
Nd：2.6～3.0％，
Zn：0.1～0.4％，
La：0.1～0.4％，
Zr：0.3～0.7％，
the balance being magnesium and unavoidable impurities, the sum of the weight percentages of said impurities not exceeding 0.2%;
the impurity element contains at least one of silicon, iron, copper and nickel, and the content of the silicon element is not more than 0.01%, the content of the iron element is not more than 0.01%, the content of the copper element is not more than 0.03%, and the content of the nickel element is not more than 0.005%.
2. A method of preparing a high strength and toughness cast magnesium rare earth alloy according to claim 1, said method comprising the steps of:
and (3) baking: preheating pure magnesium, pure zinc, mg-Nd, mg-La and Mg-Zr intermediate alloy respectively;
melting magnesium: melting the dried pure magnesium in a protective atmosphere environment;
adding alloy elements: when the temperature of the magnesium solution reaches 700-720 ℃, directly adding pure zinc, mg-Nd and Mg-La intermediate alloy into the magnesium solution; after all the intermediate alloy is melted, adding the Mg-Zr intermediate alloy when the temperature of the melt is raised to 760-780 ℃, and skimming the surface scum after the Mg-Zr intermediate alloy is melted;
refining: after Zr element is added, when the temperature of the melt is reduced to 750-760 ℃, refining is carried out without power off, and after refining, the temperature is increased to 780-790 ℃ and the melt is kept stand;
casting and forming: standing the magnesium liquid to 690-740 ℃, skimming surface scum, and carrying out metal gravity casting to obtain Mg-Nd-Zn-La-Zr magnesium rare earth alloy sheet ingots;
and (3) heat treatment: and carrying out high-temperature solid solution treatment on the magnesium rare earth alloy sheet ingot, then quenching in water, and finally carrying out single-stage aging treatment to obtain the high-strength and high-toughness cast magnesium rare earth alloy.
3. The method for producing a high strength and toughness cast magnesium rare earth alloy according to claim 2, wherein the high temperature solution treatment means solution treatment at 545 to 555 ℃ for 4 to 8 hours.
4. The method for producing a high strength and toughness cast magnesium rare earth alloy according to claim 2, wherein the single-stage aging treatment means aging treatment at 200 to 225 ℃ for 16 to 64 hours.
5. The method for producing a high strength and toughness cast magnesium rare earth alloy according to claim 2, wherein the quenching medium in the water quenching process is water and the water temperature is 25-80 ℃.
6. The method of producing a high strength and toughness cast magnesium rare earth alloy according to claim 2 or 5, wherein the transfer time of the ingot in the in-water quenching process is <20 seconds.
7. The method for preparing a high strength and toughness cast magnesium rare earth alloy according to claim 2, wherein the protective atmosphere is SF 6 And CO 2 Is a mixed gas of (a) and (b).
8. The method for producing a high strength and toughness cast magnesium rare earth alloy according to claim 2, wherein the preheating is performed at 200 to 250 ℃ for 3 to 8 hours.
9. The method for producing a high-strength and high-toughness cast magnesium rare earth alloy according to claim 2, wherein in the step of adding an alloying element, the surface dross is skimmed and stirred for 2 to 3 minutes; the standing time in the refining step is 15-30 minutes.
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