CN114703388A - Method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains - Google Patents
Method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains Download PDFInfo
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 33
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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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
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
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- 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
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Abstract
The invention relates to a method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains, belonging to the field of Mg-Zn-Al series cast magnesium alloy preparation. Preheating raw materials, placing metal Mg, metal Al, metal Zn, metal Cu and Mg-5 wt.% Mn intermediate alloy into a smelting furnace, introducing protective gas, smelting at the temperature of 720-760 ℃ until the metal is completely molten, and preserving heat for 10-15 min to obtain an alloy melt A; adding the dried magnesium carbonate powder into the alloy melt A, uniformly stirring, slagging, and standing for 10-20 min to obtain an alloy melt B with refined grains; purifying and refining the alloy melt B with refined grains by using an RJ-6 refining agent for 5-10 min, regulating the temperature of the melt to 720-740 ℃ after slagging-off treatment, and standing for 20-40 min to obtain a refined alloy melt C; pouring the refined alloy melt C into a preheating mould, demoulding, and cooling to room temperature in air to obtain an alloy ingot; and carrying out solid solution-two-stage aging treatment on the alloy ingot to obtain a magnesium alloy ingot. The magnesium alloy grain is refined and cast by magnesium carbonate, and the magnesium alloy grain has high yield strength and good plasticity after heat treatment.
Description
Technical Field
The invention relates to a method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains, belonging to the field of Mg-Zn-Al series cast magnesium alloy preparation.
Background
The magnesium alloy has a series of advantages of low density, high specific strength and specific rigidity, strong electromagnetic shielding capability, good damping performance, easy recovery and the like, and is the lightest metal engineering structural material in the current practical application. The magnesium alloy has obvious effects on realizing light weight, reducing energy consumption, reducing environmental pollution and the like.
Currently, magnesium alloys used in industry mainly include two types, cast and wrought magnesium alloys. The cast magnesium alloy accounts for 70 percent of the total consumption of the magnesium alloy product. However, the low yield strength and insufficient toughness of the traditional casting magnesium alloy such as AZ91D and AM60B still remain key problems limiting the wide range of applications of the magnesium alloy. Although the strength of the alloy can be increased by adding alloying elements such as Ca, Si, RE, this method generally reduces the elongation of the alloy. The yield strength is an important parameter to be considered when the alloy material is actually used, because irreversible plastic deformation occurs when the material is stressed to be greater than the yield strength, and permanent functional failure is often caused. Reducing the grain size of the metallic material is the only method to improve both the strength and the plasticity of the alloy. At present, the mainstream means for refining grains in the cast magnesium alloy comprises various grain refiners, external energy and energy input modes such as mechanical vibration, electromagnetic stirring, high-speed shearing, ultrasonic treatment and the like. The use of external energy requires special equipment and complicated process flow, and the time and money costs are high, which is not suitable for large-scale industrial production.
In the prior art, a magnesium alloy grain refining device consists of more than ten structural units, including a wire feeder, a froster and the like, has a complex structure, can only realize the step of gradually feeding wires (grain refiner strontium strips), and is not beneficial to large-scale industrial production. The grain refinement method for the large-size semi-continuous casting magnesium alloy ingot is also realized by feeding Mg-Ti-Zr grain refinement alloy wires to the middle part of the melt by a wire feeding method. The refined grain refining effect is good, but the grain refined alloy wire contains 0.5-15% of Ti and 10-25% of Zr, and the alloy contains Gd, Y, Nd and other precious rare earth elements, so that the production cost is further improved, and the application of the alloy is limited. The grain refining type cast magnesium alloy and the preparation method thereof have the advantages that the obtained alloy has obvious grain refining effect, higher tensile strength (more than or equal to 300MPa) and excellent high-temperature creep resistance, but the plasticity of the alloy is only 5 to 8 percent. In the smelting process, expensive ZrC and HfC are used as grain refiners, and vibration stirring and copper mold water cooling are needed to correspondingly increase the production cost. The magnesium alloy refiner containing graphene and the preparation method thereof are characterized in that the obtained refiner is added into a ZK60 alloy melt according to the mass fraction of 0.1 wt%, the grain size of the ZK60 alloy obtained after stirring and casting is reduced to about 40 mu m from the original 85 mu m, and the grain refining effect is remarkable. However, the preparation process of the refiner graphene in the method is complex, graphene oxide can be finally prepared only by the processes of high-temperature reduction, ultrasonic dispersion, mixing with metal powder, suction filtration, drying, powder pressing and the like, and large-scale production is difficult.
Therefore, the mode of grain refinement by an external field needs to use complex instruments and equipment, and the production cost is increased; some methods of refining the crystal grains by adding an expensive grain refiner are not favorable for expanding the application range of the magnesium alloy.
Disclosure of Invention
Aiming at the problem that complex instruments and equipment are needed in the mode of grain refinement in the prior art, the production cost is increased; the invention provides a method for refining the crystal grains of the Mg-Zn-Al series casting magnesium alloy containing Mn, namely, magnesium carbonate powder is used as the crystal grain refiner to refine the crystal grains of the Mg-Zn-Al-Cu-Mn series casting magnesium alloy, so as to obtain the casting magnesium alloy product with yield strength higher than 220MPa and elongation higher than 10 percent.
A method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains comprises the following steps of taking the mass fraction of Mn-containing Mg-Zn-Al series cast magnesium alloy as 100%, Zn 7.2% -10.7%, Al 0.8% -2.4%, Mn 0.2% -0.5%, Cu 0.2% -0.7%, and the balance of Mg and inevitable impurities, wherein the total content of the impurities is not higher than 0.10%;
the method for grain refinement comprises the following specific steps:
(1) weighing raw materials: weighing metal Mg, metal Al, metal Zn, metal Cu and Mg-5 wt.% of Mn master alloy according to the mass percentage;
(2) preheating the raw materials in the step (1), placing metal Mg, metal Al, metal Zn, metal Cu and Mg-5 wt.% Mn intermediate alloy into a smelting furnace, introducing protective gas, smelting at the temperature of 720-760 ℃ until the metal is completely molten, and preserving heat for 10-15 min to obtain an alloy melt A;
(3) adding the dried magnesium carbonate powder into the alloy melt A, uniformly stirring, slagging, and standing for 10-20 min to obtain an alloy melt B with refined grains;
(4) purifying and refining the alloy melt B with refined grains by using an RJ-6 refining agent for 5-10 min, regulating the temperature of the melt to 720-740 ℃ after slagging-off treatment, and standing for 20-40 min to obtain a refined alloy melt C;
(5) pouring the refined alloy melt C into a preheating mould, demoulding, and cooling to room temperature in air to obtain an alloy ingot;
(6) and carrying out solid solution-two-stage aging treatment on the alloy ingot to obtain the magnesium alloy ingot.
The preheating temperature in the step (2) is 100-200 ℃.
The protective gas in the step (2) is CO2And SF6Mixed gas, CO in shielding gas2The volume fraction of (A) is 95-99%.
The adding amount of the magnesium carbonate powder in the step (3) is 0.2-2 wt% of the alloy melt A.
The RJ-6 refining agent in the step (4) is added in an amount of 1-2 wt.% of the alloy melt B
And (5) preheating the die at 200-220 ℃.
The concrete method of the solid solution-two-stage aging treatment in the step (6) is
1) Raising the temperature of the alloy ingot to 370-400 ℃ at a constant speed, carrying out solution treatment for 12-24 h, and then putting the alloy ingot into water at the temperature of 15-25 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60-100 ℃ at a constant speed, and carrying out primary aging treatment for 16-24 h; and then raising the temperature to 150-200 ℃ at a constant speed, carrying out secondary aging treatment for 2-8 h, and then putting the magnesium alloy ingot into water at the temperature of 15-25 ℃ for quenching treatment to obtain the magnesium alloy ingot.
The invention has the beneficial effects that:
(1) according to the invention, magnesium carbonate powder is used as a grain refiner to refine grains of the Mg-Zn-Al-Cu-Mn alloy, the grains of the alloy can be obviously refined by magnesium carbonate, the refined alloy is subjected to heat treatment (solid solution-double stage aging treatment), the mechanical property is obviously improved, a cast magnesium alloy product with yield strength higher than 220MPa and elongation higher than 10% is obtained, and the performance is obviously superior to that of common cast magnesium alloys such as AZ91D and AM 60B;
(2) the method for realizing the grain refinement of the magnesium alloy is simple and controllable, has extremely low cost and is easy for industrial application;
(3) according to the invention, through adding trace alloying elements Mn, Mn can be combined with impurity elements such as Fe in the alloy, the melt is purified, and the alloy casting quality and corrosion resistance are improved; mn is combined with O element introduced by magnesium carbonate and Al in the alloy to generate Mn-A with high melting pointl-O phase (spinel-structured MnAl)2O4) Can be used as a heterogeneous nucleation point of alpha-Mg in the alloy solidification process, and plays a role in refining alloy grains by compounding with magnesium carbonate;
(4) according to the invention, the melt is refined by the RJ-6 refining agent after being melted, and after the refining is finished, a standing impurity removal method is adopted, so that the impurities of the melt can be greatly reduced, the quality of the alloy is improved, and the mechanical property and the corrosion resistance of the alloy are ensured;
(5) aiming at the fact that the Mg-Zn-Al-Cu-Mn alloy has a remarkable aging strengthening effect, the solid solution-two-stage aging heat treatment process is carried out on the alloy, and the mechanical property of the alloy is remarkably improved by utilizing the precipitation strengthening effect of the MgZn phase; the benefits of the two-stage aging are: after the solution treatment, a low-temperature pre-aging (primary aging) stage is beneficial to the rapid formation of a large amount of Zn enrichment regions (G.P regions) with uniform distribution of the alloy, and the G.P regions can be used as heterogeneous nucleation points of a precipitation strengthening phase MgZn phase in a high-temperature aging (secondary aging) process, so that the MgZn phase is promoted to be more uniformly dispersed and precipitated, the precipitation strengthening effect is improved, and the strength of the alloy is further improved.
(6) According to the invention, the ductility of the alloy can be improved and the age hardening effect can be enhanced by adding trace alloy element Cu, and the Cu can improve the eutectic temperature of Mg-Zn alloy, so that the alloy can be subjected to solution treatment at a higher temperature, more Zn and Al elements are dissolved into a magnesium matrix in a solid solution manner, and the effects of solid solution strengthening and age hardening are improved.
Drawings
FIG. 1 shows the grain size statistics (electron back-scattered diffraction) of the alloy of comparative example and example 3 in the as-cast state;
FIG. 2 shows the grain size statistics (light microscopy) of the alloys of comparative example and example 3 in the aged state;
FIG. 3 is a high resolution TEM and plane scan image of the alloy of example 3 in solid solution state, (a) is the distribution of the second phase, (b) is an enlarged view of the graph (a) showing the interplanar spacing of α -Mg after solid solution, and (c) is α -Mg, MnAl2O4、MgZn2The phase relationship between them; (d) high angle annular dark field image (HAADF) of typical area, (e-i) isSurface distribution diagram of elements Mg, Zn, Al, Mn and Cu.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Comparative example: the high-strength Mg-Zn-Al-Mn-Cu cast magnesium alloy comprises the following components in percentage by weight: 10.0% of Zn, 1.0% of Al, 0.3% of Mn, 0.5% of Cu, and the balance of Mg and inevitable impurities in the smelting process, wherein the total content of the impurities is less than 0.1%; the element adding mode is as follows: mg, Zn, Al and Cu are added in pure Mg (99.97%) blocks, pure Zn (99.9%) blocks, pure Al (99.7% blocks) and pure Cu (99.9%) blocks, and Mn element is added in a mode of Mg-5 wt.% Mn master alloy;
(1) preparing materials: the raw materials are metal pure Mg, metal pure Zn, metal pure Al, metal pure Cu and Mg-5 wt.% Mn intermediate alloy, and are proportioned according to the weight percentage; before smelting, polishing and cleaning an oxide film on the surface of a raw material, considering the condition of element burning loss in the smelting process, and calculating the element burning loss rate according to the actual condition;
(2) smelting: preheating the raw materials in the step (1) at the temperature of 180-200 ℃, putting Mg blocks, Zn blocks, Al blocks, Mg-5 wt.% of Mn intermediate alloy and Cu blocks into a cleaned and dried stainless steel crucible, and putting the stainless steel crucible into a resistance furnace for smelting; the smelting temperature is controlled to be 750-760 ℃, and CO is used for smelting2And SF6The mixed gas is shielding gas, and CO in the shielding gas2The volume fraction of (A) is 95-99%; after the metal in the crucible is completely melted, preserving the heat for 15min to obtain an alloy melt A;
(3) refining: purifying and refining the alloy melt A by using an RJ-6 refining agent; the refining agent is 1.5 wt.% of the alloy melt A, drying treatment is carried out for 35min at the temperature of 230-250 ℃ before the refining agent is added, and the refining agent is uniformly stirred for 6min up and down, left and right by using a perforated ladle during refining to ensure that the refining agent is fully contacted with the melt; after refining, slagging off the alloy melt, adjusting the temperature to 720-740 ℃, and standing for 30min to obtain an alloy melt B;
(4) pouring: the method comprises the following steps of (1) preheating the mold for 60min at the temperature of 200-220 ℃ in order to improve the fluidity of a melt and ensure the mold filling capacity, demolding after the casting is finished for 10min, and cooling in the air to room temperature to obtain an alloy ingot;
(5) and (3) heat treatment: carrying out solid solution-two-stage aging treatment on the alloy ingot obtained in the step (4), wherein the specific method of the solid solution-two-stage aging treatment is
1) Raising the temperature of the alloy ingot to 370 ℃ at a constant speed, carrying out solution treatment for 24h, and then putting the alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60 ℃ at a constant speed, and carrying out primary aging treatment for 16 h; then raising the temperature to 175 ℃ at a constant speed, carrying out secondary aging treatment for 2h, and then putting the magnesium alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a magnesium alloy ingot;
the alloy obtained in this comparative example had an average grain size of 38.5 μm in the as-cast state, as shown in FIGS. 1 (a) and (b), and an average grain size of 56.8 μm in the aged state, as shown in FIGS. 2(a) and (b), and the Yield Strength (YS) and Elongation (EL) of the alloy in the aged state were 231.0MPa and 9.3%, respectively.
Example 1: the low-cost high-strength Mg-Zn-Al-Mn-Cu cast magnesium alloy is prepared by adding 0.2 mass percent of magnesium carbonate as a grain refiner in the smelting process, wherein the magnesium alloy comprises the following components in percentage by weight: 10.0% of Zn, 1.0% of Al, 0.3% of Mn, 0.5% of Cu, and the balance of Mg and inevitable impurities in the smelting process, wherein the total content of the impurities is less than 0.1%; the element adding mode is as follows: mg, Zn, Al and Cu are added in a pure Mg (99.97%) block, a pure Zn (99.9%) block, a pure Al (99.7% block) block and a pure Cu (99.9%) block, and the Mn element is added in a mode of Mg-5 wt.% of Mn master alloy;
(1) preparing materials: the raw materials are metal pure Mg, metal pure Zn, metal pure Al, metal pure Cu and Mg-5 wt.% Mn intermediate alloy, and are proportioned according to the weight percentage; before smelting, polishing and cleaning an oxide film on the surface of a raw material, considering the condition of element burning loss in the smelting process, and calculating the element burning loss rate according to the actual condition;
(2) smelting: preheating the raw materials in the step (1) at the temperature of 180-200 ℃, and then carrying outPutting Mg blocks, Zn blocks, Al blocks, Mg-5 wt.% of Mn intermediate alloy and Cu blocks into a stainless steel crucible which is cleaned and dried, and putting the stainless steel crucible into a resistance furnace for smelting; the smelting temperature is controlled to be 750-760 ℃, and CO is used for smelting2And SF6The mixed gas is shielding gas, and CO in the shielding gas2The volume fraction of (A) is 95-99%; after the metal in the crucible is completely melted, preserving the heat for 15min to obtain an alloy melt A;
(3) adding magnesium carbonate powder dried at 85 ℃ for 1.5h into the alloy melt A, stirring for 3min by using a strainer to uniformly distribute the magnesium carbonate powder into the melt A, slagging, and standing for 18min to obtain an alloy melt B with refined grains; wherein magnesium carbonate powder is added in an amount of 0.2 wt.% of alloy melt a;
(4) purifying and refining the alloy melt B by using an RJ-6 refining agent; the refining agent is 1.5 wt.% of the alloy melt A, drying treatment is carried out for 35min at the temperature of 230-250 ℃ before the refining agent is added, and the refining agent is uniformly stirred for 6min up and down, left and right by using a perforated ladle during refining to ensure that the refining agent is fully contacted with the melt; after refining, slagging off the alloy melt, adjusting the temperature to 720-740 ℃, and standing for 30min to obtain an alloy melt C;
(5) pouring: the method comprises the following steps of (1) preheating the mold for 60min at the temperature of 200-220 ℃ in order to improve the fluidity of a melt and ensure the mold filling capacity, demolding after the casting is finished for 10min, and cooling to room temperature in the air to obtain an alloy ingot;
(6) and (3) heat treatment: carrying out solid solution-two-stage aging treatment on the alloy ingot obtained in the step (5), wherein the specific method of the solid solution-two-stage aging treatment is
1) Raising the temperature of the alloy ingot to 370 ℃ at a constant speed, carrying out solution treatment for 24h, and then putting the alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60 ℃ at a constant speed, and carrying out primary aging treatment for 16 h; then raising the temperature to 175 ℃ at a constant speed, carrying out secondary aging treatment for 2h, and then putting the magnesium alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a magnesium alloy ingot;
the alloy obtained in this example had an as-cast average grain size of 35.6 μm, an aged average grain size of 54.5 μm, and an as-aged Yield Strength (YS) and Elongation (EL) of 230.8MPa and 10.2%, respectively; compared with the comparative example, the grain size of the alloy is slightly reduced after 0.2 mass percent of magnesium carbonate is added, the yield strength of the alloy is correspondingly improved, and the elongation is obviously improved.
Example 2: the low-cost high-strength Mg-Zn-Al-Mn-Cu cast magnesium alloy is prepared by adding 0.5 mass percent of magnesium carbonate as a grain refiner in the smelting process, wherein the magnesium alloy comprises the following components in percentage by weight: 10.0% of Zn, 1.0% of Al, 0.3% of Mn, 0.5% of Cu, and the balance of Mg and inevitable impurities in the smelting process, wherein the total content of the impurities is less than 0.1%; the element adding mode is as follows: mg, Zn, Al and Cu are added in a pure Mg (99.97%) block, a pure Zn (99.9%) block, a pure Al (99.7% block) block and a pure Cu (99.9%) block, and the Mn element is added in a mode of Mg-5 wt.% of Mn master alloy;
(1) preparing materials: the raw materials are metal pure Mg, metal pure Zn, metal pure Al, metal pure Cu and Mg-5 wt.% Mn intermediate alloy, and are proportioned according to the weight percentage; before smelting, polishing and cleaning an oxide film on the surface of a raw material, considering the condition of element burning loss in the smelting process, and calculating the element burning loss rate according to the actual condition;
(2) smelting: preheating the raw materials in the step (1) at the temperature of 180-200 ℃, putting Mg blocks, Zn blocks, Al blocks, Mg-5 wt.% of Mn intermediate alloy and Cu blocks into a cleaned and dried stainless steel crucible, and putting the stainless steel crucible into a resistance furnace for smelting; the smelting temperature is controlled to be 750-760 ℃, and CO is used for smelting2And SF6The mixed gas is shielding gas, and CO in the shielding gas2The volume fraction of (A) is 95-99%; after the metal in the crucible is completely melted, preserving the heat for 15min to obtain an alloy melt A;
(3) adding magnesium carbonate powder dried at 85 ℃ for 1.5h into the alloy melt A, stirring for 3min by using a strainer to uniformly distribute the magnesium carbonate powder into the melt A, slagging, and standing for 18min to obtain an alloy melt B with refined grains; wherein magnesium carbonate powder is added in an amount of 0.5 wt.% of alloy melt a;
(4) purifying and refining the alloy melt B by using an RJ-6 refining agent; the refining agent is 1.5 wt.% of the alloy melt A, drying treatment is carried out for 35min at the temperature of 230-250 ℃ before the refining agent is added, and the refining agent is uniformly stirred for 6min up and down, left and right by using a perforated ladle during refining to ensure that the refining agent is fully contacted with the melt; after refining, slagging off the alloy melt, adjusting the temperature to 720-740 ℃, and standing for 30min to obtain an alloy melt C;
(5) pouring: the method comprises the following steps of (1) preheating the mold for 60min at the temperature of 200-220 ℃ in order to improve the fluidity of a melt and ensure the mold filling capacity, demolding after the casting is finished for 10min, and cooling in the air to room temperature to obtain an alloy ingot;
(6) and (3) heat treatment: adopting solid solution-two-stage aging treatment on the alloy ingot obtained in the step (5), wherein the specific method of the solid solution-two-stage aging treatment is
1) Raising the temperature of the alloy ingot to 370 ℃ at a constant speed, carrying out solution treatment for 24h, and then putting the alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60 ℃ at a constant speed, and carrying out primary aging treatment for 16 h; then raising the temperature to 175 ℃ at a constant speed, carrying out secondary aging treatment for 2h, and then putting the magnesium alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a magnesium alloy ingot;
the alloy obtained in this example had an as-cast average grain size of 28.7 μm, an aged average grain size of 45.6 μm, and an aged Yield Strength (YS) and Elongation (EL) of 236.2MPa and 14.5%, respectively; compared with the comparative example, the grain size of the alloy is reduced by about 10 μm after 0.5 mass percent of magnesium carbonate is added, the yield strength of the alloy is correspondingly improved, and the elongation is obviously improved.
Example 3: the high-strength Mg-Zn-Al-Mn-Cu cast magnesium alloy comprises the following components in percentage by weight: 10.0% of Zn, 1.0% of Al, 0.3% of Mn, 0.5% of Cu, and the balance of Mg and inevitable impurities in the smelting process, wherein the total content of the impurities is less than 0.1%; the element adding mode is as follows: mg, Zn, Al and Cu are added in pure Mg (99.97%) blocks, pure Zn (99.9%) blocks, pure Al (99.7% blocks) and pure Cu (99.9%) blocks, and Mn element is added in a mode of Mg-5 wt.% Mn master alloy;
(1) preparing materials: the raw materials are metal pure Mg, metal pure Zn, metal pure Al, metal pure Cu and Mg-5 wt.% Mn intermediate alloy, and are proportioned according to the weight percentage; polishing and cleaning an oxide film on the surface of a raw material before smelting, considering the condition of element burning loss in the smelting process, and calculating the element burning loss rate according to the actual condition;
(2) smelting: preheating the raw materials in the step (1) at the temperature of 180-200 ℃, putting Mg blocks, Zn blocks, Al blocks, Mg-5 wt.% of Mn intermediate alloy and Cu blocks into a cleaned and dried stainless steel crucible, and putting the stainless steel crucible into a resistance furnace for smelting; the smelting temperature is controlled to be 750-760 ℃, and CO is used for smelting2And SF6The mixed gas is shielding gas, and CO in the shielding gas2The volume fraction of (A) is 95-99%; after the metal in the crucible is completely melted, preserving the heat for 15min to obtain an alloy melt A;
(3) adding magnesium carbonate powder dried at 85 ℃ for 1.5h into the alloy melt A, stirring for 3min by using a strainer to uniformly distribute the magnesium carbonate powder into the melt A, slagging, and standing for 18min to obtain an alloy melt B with refined grains; wherein magnesium carbonate powder is added in an amount of 1 wt.% of alloy melt a;
(4) refining: purifying and refining the alloy melt B by using an RJ-6 refining agent; the refining agent is 1.5 wt.% of the alloy melt A, drying treatment is carried out for 35min at the temperature of 230-250 ℃ before the refining agent is added, and the refining agent is uniformly stirred for 6min up and down, left and right by using a perforated ladle during refining to ensure that the refining agent is fully contacted with the melt; after refining, slagging off the alloy melt, adjusting the temperature to 720-740 ℃, and standing for 30min to obtain an alloy melt C;
(5) pouring: the method comprises the following steps of (1) preheating the mold for 60min at the temperature of 200-220 ℃ in order to improve the fluidity of a melt and ensure the mold filling capacity, demolding after the casting is finished for 10min, and cooling in the air to room temperature to obtain an alloy ingot;
(6) and (3) heat treatment: adopting solid solution-two-stage aging treatment on the alloy ingot obtained in the step (5), wherein the specific method of the solid solution-two-stage aging treatment is
1) Raising the temperature of the alloy ingot to 370 ℃ at a constant speed, carrying out solution treatment for 24h, and then putting the alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60 ℃ at a constant speed, and carrying out primary aging treatment for 16 h; then raising the temperature to 175 ℃ at a constant speed, carrying out secondary aging treatment for 2h, and then putting the magnesium alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a magnesium alloy ingot;
the alloy obtained in this example had an as-cast average grain size of 22.5 μm, see (c) and (d) of FIG. 1, and an aged average grain size of 39.5 μm, see (c) and (d) of FIG. 2, and the Yield Strength (YS) and Elongation (EL) values of the alloy in the aged state were 240.0MPa and 16.1%, respectively;
comparison of comparative example (without magnesium carbonate) and example 3 (with 1% magnesium carbonate) the room temperature tensile Yield Strength (YS) and Elongation (EL) in the as-cast and aged state are shown in Table 1,
TABLE 1 comparison of tensile yield strength and elongation at room temperature for the as-cast and aged state of the comparative and present examples
Compared with a comparative example, the alloy grain is obviously refined after 1% of magnesium carbonate is added, the grain size is reduced by about 16 mu m, the mechanical property of the alloy is obviously improved, the yield strength is improved by about 10MPa, and particularly the elongation is obviously improved;
the high resolution transmission electron microscope and energy spectrum scanning image of the alloy of this example in solid solution state is shown in fig. 3, wherein (a) and (b) are HRTEM images of nanoscale phases, one is a relatively slender rod-shaped phase, i.e. 1 in (b), and the other is perpendicular to the former thicker and shorter rod-shaped phase, i.e. 2 in (b), and according to the HAADF-STEM image and the corresponding EDS surface scanning result, the nanoscale phases mainly consist of Mg, Al, Mn and Zn elements; performing fast Fourier transform on the whole area of the (b) to obtain (c), and judging the slender rod according to the calibration result of the diffraction spotThe phase is MnAl with a spinel structure2O4The phase relation with the magnesium matrix is [ 100 ]]Mg||[1 0 0]MnAl2O4(ii) a The thicker and shorter rod-shaped phase is MgZn2The phase relation with the magnesium matrix is [ 100 ]]Mg||[0 0 1]MgZn2(ii) a Through the characterization of the transmission electron microscope, the fact that MgCO with the mass fraction of 1 percent is added into the Mg-10Zn-1Al-0.5Cu-0.3Mn alloy can be confirmed3Then high melting point MnAl is generated in the melt2O4The fine high melting point phase can be used as a heterogeneous nucleation point of alpha-Mg to improve the nucleation rate and further has the effect of refining crystal grains, and can also be used as a precipitation strengthening phase MgZn2Promoting the precipitation of the precipitate; on the other hand, according to an Orowan strengthening mechanism, the hard fine phase is dispersed and distributed in the magnesium matrix, and the strength of the alloy can be effectively improved.
Example 4: the low-cost high-strength Mg-Zn-Al-Mn-Cu cast magnesium alloy is prepared by adding 2.0 mass percent of magnesium carbonate as a grain refiner in the smelting process, wherein the magnesium alloy comprises the following components in percentage by weight: 10.0% of Zn, 1.0% of Al, 0.3% of Mn, 0.5% of Cu, and the balance of Mg and inevitable impurities in the smelting process, wherein the total content of the impurities is less than 0.1%; the element adding mode is as follows: mg, Zn, Al and Cu are added in a pure Mg (99.97%) block, a pure Zn (99.9%) block, a pure Al (99.7% block) block and a pure Cu (99.9%) block, and the Mn element is added in a mode of Mg-5 wt.% of Mn master alloy;
(1) preparing materials: the raw materials are metal pure Mg, metal pure Zn, metal pure Al, metal pure Cu and Mg-5 wt.% Mn intermediate alloy, and are proportioned according to the weight percentage; before smelting, polishing and cleaning an oxide film on the surface of a raw material, considering the condition of element burning loss in the smelting process, and calculating the element burning loss rate according to the actual condition;
(2) smelting: preheating the raw materials in the step (1) at the temperature of 180-200 ℃, putting Mg blocks, Zn blocks, Al blocks, Mg-5 wt.% of Mn intermediate alloy and Cu blocks into a cleaned and dried stainless steel crucible, and putting the stainless steel crucible into a resistance furnace for smelting; the smelting temperature is controlled to be 750-760 ℃, and CO is used for smelting2And SF6The mixed gas is shielding gas, and CO in the shielding gas2The volume fraction of (A) is 95-99%; after the metal in the crucible is completely melted, preserving the heat for 15min to obtain an alloy melt A;
(3) adding magnesium carbonate powder dried at 85 ℃ for 1.5h into the alloy melt A, stirring for 3min by using a strainer to uniformly distribute the magnesium carbonate powder into the melt A, slagging, and standing for 18min to obtain an alloy melt B with refined grains; wherein magnesium carbonate powder is added in an amount of 2 wt.% of alloy melt a;
(4) refining: purifying and refining the alloy melt B by using an RJ-6 refining agent; the amount of the refining agent is 1.5 wt.% of the alloy melt A, the refining agent is dried for 35min at 230-250 ℃ before being added, and the refining agent is stirred for 6min at uniform speed up, down, left and right by using a strainer during refining to ensure that the refining agent is fully contacted with the melt; after refining, slagging off the alloy melt, adjusting the temperature to 720-740 ℃, and standing for 30min to obtain an alloy melt C;
(5) pouring: the method comprises the following steps of (1) preheating the mold for 60min at the temperature of 200-220 ℃ in order to improve the fluidity of a melt and ensure the mold filling capacity, demolding after the casting is finished for 10min, and cooling in the air to room temperature to obtain an alloy ingot;
(6) and (3) heat treatment: carrying out solid solution-two-stage aging treatment on the alloy ingot obtained in the step (5), wherein the specific method of the solid solution-two-stage aging treatment is
1) Raising the temperature of the alloy ingot to 370 ℃ at a constant speed, carrying out solution treatment for 24h, and then putting the alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60 ℃ at a constant speed, and carrying out primary aging treatment for 16 h; then raising the temperature to 175 ℃ at a constant speed, carrying out secondary aging treatment for 2h, and then putting the magnesium alloy ingot into water at the temperature of 20 ℃ for quenching treatment to obtain a magnesium alloy ingot;
the alloy obtained in this example had an as-cast average grain size of 20.2 μm, an aged average grain size of 35.4 μm, and Yield Strength (YS) and Elongation (EL) values of 198.6MPa and 6.8%, respectively, for the alloy in the as-cast state; compared with the comparative example, the alloy grain is obviously refined after 2.0 mass percent of magnesium carbonate is added, but the yield strength and plasticity of the alloy are obviously reduced, excessive magnesium carbonate is decomposed in a melt to form more MgO particles, the particles are agglomerated to form oxide inclusions, and cracks are easy to initiate and expand at the inclusions in the stretching process due to stress concentration, so that the alloy performance is deteriorated.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (7)
1. A method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains is characterized in that, by taking the mass fraction of Mn-containing Mg-Zn-Al series cast magnesium alloy as 100%, Zn is 7.2-10.7%, Al is 0.8-2.4%, Mn is 0.2-0.5%, Cu is 0.2-0.7%, and the balance is Mg and inevitable impurities, wherein the total content of the impurities is not higher than 0.10%;
the method for refining the crystal grains comprises the following specific steps:
(1) weighing raw materials: weighing metal Mg, metal Al, metal Zn, metal Cu and Mg-5 wt.% Mn intermediate alloy according to the mass percentage;
(2) preheating the raw materials in the step (1), putting metal Mg, metal Al, metal Zn, metal Cu and Mg-5 wt.% of Mn intermediate alloy into a smelting furnace, introducing protective gas, smelting at the temperature of 720-760 ℃ until the metal is completely molten, and preserving heat for 10-15 min to obtain an alloy melt A;
(3) adding the dried magnesium carbonate powder into the alloy melt A, uniformly stirring, slagging, and standing for 10-20 min to obtain an alloy melt B with refined grains;
(4) purifying and refining the alloy melt B with refined grains by using an RJ-6 refining agent for 5-10 min, regulating the temperature of the melt to 720-740 ℃ after slagging-off treatment, and standing for 20-40 min to obtain a refined alloy melt C;
(5) pouring the refined alloy melt C into a preheating mould, demoulding, and cooling to room temperature in air to obtain an alloy ingot;
(6) and carrying out solid solution-two-stage aging treatment on the alloy ingot to obtain a magnesium alloy ingot.
2. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: the preheating temperature in the step (2) is 100-200 ℃.
3. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: the protective gas in the step (2) is CO2And SF6Mixed gas, CO in shielding gas2The volume fraction of (A) is 95-99%.
4. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: and (3) adding the magnesium carbonate powder in an amount of 0.2-2 wt% of the alloy melt A.
5. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: and (4) adding the RJ-6 refining agent in the step (4) in an amount of 1-2 wt.% of the alloy melt B.
6. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: and (5) preheating the die at 200-220 ℃.
7. The method for grain refinement of a Mn-containing Mg-Zn-Al series cast magnesium alloy according to claim 1, characterized in that: the concrete method of the solid solution-two-stage aging treatment in the step (6) is
1) Raising the temperature of the alloy ingot to 370-400 ℃ at a constant speed, carrying out solution treatment for 12-24 h, and then putting the alloy ingot into water at the temperature of 15-25 ℃ for quenching treatment to obtain a solid solution alloy ingot;
2) raising the temperature of the solid solution alloy cast ingot to 60-100 ℃ at a constant speed, and carrying out primary aging treatment for 16-24 h; and then raising the temperature to 150-200 ℃ at a constant speed, carrying out secondary aging treatment for 2-8 h, and then placing the magnesium alloy ingot in water at the temperature of 15-25 ℃ for quenching treatment to obtain the magnesium alloy ingot.
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| CN115652155A (en) * | 2022-10-31 | 2023-01-31 | 上海航天精密机械研究所 | Efficient grain refiner for rare earth magnesium alloy, preparation method and use method thereof |
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