CN114293079B - Ultrahigh-plasticity rare earth wrought magnesium alloy and preparation method of extruded sheet thereof - Google Patents
Ultrahigh-plasticity rare earth wrought magnesium alloy and preparation method of extruded sheet thereof Download PDFInfo
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Abstract
The invention provides an ultrahigh-plasticity rare earth wrought magnesium alloy and a preparation method of an extruded sheet thereof, belonging to the technical field of magnesium alloy materials and forming, wherein the magnesium alloy comprises the following components in percentage by mass: 0 to 4 percent of Gd, 0 to 4 percent of Er, 0.1 to 0.6 percent of Zr and the balance of Mg, wherein the total rare earth content is 1 to 4 percent, and the ultrahigh plasticity rare earth magnesium alloy material is upset and is asymmetrically extruded by an extrusion die. The invention has two advantages: 1. in the aspect of the forming process, the die is used for upsetting, so that different areas of the extruded plate are fully deformed, grains are further refined, and the defect of strong basal plane texture of the extruded plate in the traditional deformation process can be greatly weakened by non-uniform extrusion; 2. in the aspect of material design, the ultrahigh-plasticity magnesium alloy plate is obtained by the action of activating a non-crystal face sliding system by using rare earth elements, and the elongation of the plate after fracture is more than or equal to 35%. The wrought magnesium alloy plate provided by the invention has the characteristics of ultrahigh plasticity and weak texture at room temperature, can be subjected to large-strain room-temperature forming and processing, and has a wide application prospect.
Description
Technical Field
The invention belongs to the technical field of alloy materials, and particularly relates to a super-high-plasticity rare earth wrought magnesium alloy and a preparation method of an extruded sheet thereof.
Background
The magnesium alloy is used as the lightest metal material for the structure, has the advantages of high specific strength, high specific stiffness, excellent shock absorption and noise reduction performance, good electromagnetic shielding performance, excellent machining performance, easy recovery and the like, can replace the traditional steel and aluminum alloy, and has wide application prospect in the fields of aviation, aerospace, automobiles, electronics and the like. However, the magnesium alloy crystal is in a close-packed hexagonal structure, the slip system is less, the critical shear stress of cylindrical surface and conical slip is much larger than that of basal plane slip during plastic forming at room temperature, c or < c + a > slip is difficult to start at room temperature, and meanwhile, the traditional deformed magnesium alloy material generally has the characteristic of strong texture, so that the magnesium alloy product has the problems of poor room temperature formability and difficult processing forming, which also becomes the biggest obstacle of industrial application of the magnesium alloy, and the application amount of the magnesium alloy is far behind that of steel and aluminum alloy.
The definition of high plasticity of magnesium alloy in the industry at present is that the magnesium alloy material is generally regarded as an ultrahigh plasticity magnesium alloy material when the elongation after fracture exceeds 30% in tensile deformation at room temperature. The magnesium alloy plate with ultrahigh plasticity and weak texture at normal temperature is developed, has excellent secondary forming processability and has great significance for popularizing the development of the magnesium alloy industry.
Disclosure of Invention
The invention aims to solve the problems of low room temperature plasticity and difficult forming of the existing magnesium alloy plate, and provides an ultrahigh-plasticity rare earth deformation magnesium alloy and a preparation method of an extrusion plate thereof.
The technical scheme provided by the invention is as follows:
in a first aspect, the magnesium alloy comprises the following components in percentage by mass: 0 to 4 percent of Gd, 0 to 4 percent of Er, 0.1 to 0.6 percent of Zr, the balance of Mg, the total content of rare earth: 1 to 4 percent.
Further, the magnesium alloy comprises the following components in percentage by mass: 1.5 to 2.0 percent of Gd, 0.1 to 0.6 percent of Zr and the balance of Mg.
Further, the magnesium alloy comprises the following components in percentage by mass: 1.5 to 3.0 percent of Er, 0.1 to 0.6 percent of Zr and the balance of Mg.
In a second aspect, a method for preparing an ultrahigh-plasticity rare earth wrought magnesium alloy extruded plate comprises the following steps:
s1, alloy smelting: pure Mg ingot, mg-Gd intermediate alloy, mg-Er intermediate alloy and Mg-Zr intermediate alloy are used as raw materials, the raw materials are proportioned according to the proportion of 0-4% of Gd, 0-4% of Er, 0.1-0.6% of Zr and the balance of Mg, the content of rare earth does not exceed 4%, and the magnesium alloy ingot is cast by semi-continuous casting after the alloy batching is melted. Semi-continuous casting process: preheating alloy raw materials to 40-80 ℃, adding the alloy raw materials into a crucible, spraying a covering agent, heating to 700-750 ℃, and smelting under the protection of SF6 and CO2 atmosphere; after all the materials are melted, removing slag and refining for 10-20 min; after refining is finished, removing slag, and keeping the temperature and standing for at least 30min; sampling and analyzing the components, and if the components are qualified, cooling to 680-690 ℃ for semi-continuous casting.
S2, heat treatment: and (3) carrying out solid solution treatment on the magnesium alloy ingot prepared by the step (S1) and air cooling, wherein the solid solution temperature is 360-450 ℃, and the solid solution time is 4-16 h.
S3, forging and pressing treatment: preheating the magnesium alloy ingot prepared in the step S2 to a forging temperature, and carrying out forging treatment, wherein the forging temperature is 300-400 ℃, the pressure maintaining time is not less than 5min, the billet is ensured to be filled in the cavity, the diameter of the forged billet is 8-10% larger than that of the extruded billet, and the forging strain is not less than 10%.
S4, machining: and (4) machining the magnesium alloy ingot prepared in the step (S3) into an extrusion blank with a required size.
S5, upsetting: and (3) preheating the extrusion blank obtained in the step (S4) to the extrusion temperature, and upsetting the extrusion blank in an extruder by using a solid steel die, wherein the upsetting ratio is 1.1-2, and the extrusion temperature is 300-450 ℃.
S6, extrusion forming: and (4) carrying out extrusion forming on the upset extrusion billet of the S5 by adopting an asymmetric extrusion die to prepare the magnesium alloy extrusion plate. The asymmetric die consists of an upper extrusion die cavity and a lower forming channel hole, wherein the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, the lower forming channel hole is in a rectangle shape as shown in figure 1, wherein the slope angle alpha = 30-80 degrees, the slope angle beta = 45-90 degrees, the angle beta > -alpha is provided, the extrusion ratio is 5-45, and the extrusion speed is 0.4-3.0 m/s.
The preparation method of the ultrahigh-plasticity rare earth wrought magnesium alloy and the extruded sheet thereof provided by the invention has the following beneficial effects:
(1) Compared with the prior art, the method adopts low-content Gd, er and Zr as alloying elements, and the Gd element is dissolved in the matrix in a solid solution manner, so that the solid solution strengthening effect can be achieved, and the basal plane slippage and the start of the stretching twin crystal in the room-temperature deformation process are facilitated; compared with Gd element, the Er element has more obvious effect of weakening the extrusion texture and can effectively reduce the anisotropy of the mechanical property of the material; zr element can obviously refine the as-cast crystal grains of the alloy, realizes the improvement of the strength and the room temperature plasticity of the magnesium alloy, and the element proportion is coordinated with the upsetting and the asymmetric extrusion process, thereby having more excellent texture weakening effect.
(2) The invention adopts the methods of forging and upsetting in advance, plays a role of refining the grain size in advance, promotes the generation and accumulation of twin crystals and dislocation, promotes the dynamic recrystallization process in the subsequent extrusion process, is favorable for improving the plasticity and reducing the anisotropy of the mechanical property of the material.
(3) The asymmetric extrusion method adopted by the invention changes the flow speed difference generated in the extrusion process of the inner cavity structure of the extrusion die, generates shear deformation, improves the plate texture, has obvious refined crystal grains, reduces the anisotropy of the mechanical property of the material and obviously improves the room temperature formability.
(4) The invention can be quickly formed by conventional deformation equipment, is easy to control and is beneficial to popularization and application.
Drawings
FIG. 1 is a schematic structural view of an asymmetric mold, the left view is a sectional view, and the right view is a rear view;
FIG. 2 is a room temperature tensile stress strain curve of the magnesium alloy sheet material in example 1;
FIG. 3 is a metallographic microstructure of an extruded magnesium alloy according to example 1.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
Example 1
S1, alloy smelting: pure Mg ingot, mg-20Er intermediate alloy and Mg-Zr intermediate alloy are used as raw materials, the raw materials are mixed according to the proportion of 3.0 percent of Er, 0.6 percent of Zr and the balance of Mg, and the magnesium alloy ingot is cast by semi-continuous casting after the alloy mixture is melted. Semi-continuous casting process: preheating alloy raw materials to 80 ℃, adding the alloy raw materials into a crucible, spraying a covering agent, heating to 700 ℃, and smelting under the protection of SF6 and CO2 atmosphere; after all the materials are melted, removing slag and refining for 15min; after refining is finished, removing slag, and keeping the temperature and standing for 30min; sampling and analyzing the components, and if the components are qualified, cooling to 690 ℃ for semi-continuous casting.
S2, heat treatment: and (3) carrying out solid solution treatment on the magnesium alloy ingot prepared by the step (S1) and air cooling, wherein the solid solution temperature is 450 ℃, and the solid solution time is 12h.
S3, forging and pressing treatment: and (3) preheating the magnesium alloy ingot prepared in the step (S2) to a forging temperature, carrying out forging treatment, wherein the forging temperature is 400 ℃, the pressure maintaining time is 5min, the billet is ensured to be full of the cavity, the diameter of the forged billet is 8% larger than that of the extruded billet, and the forging strain is 10%.
S4, machining: and machining the magnesium alloy ingot prepared in the step S3 into an extrusion blank with a required size.
S5, upsetting: and (5) preheating the extrusion blank obtained in the step (S4) to the extrusion temperature, and upsetting the extrusion blank in an extruder by using a solid steel die, wherein the upsetting ratio is 1.5, and the extrusion temperature is 400 ℃.
S6, extrusion molding: and (4) carrying out extrusion forming on the upset extrusion billet of the S5 by adopting an asymmetric extrusion die to prepare the magnesium alloy extrusion plate. The asymmetric die consists of an upper extrusion die cavity and a lower forming channel hole, wherein the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, the lower forming channel hole is in a shape of a rectangle, the slope angle alpha =45 degrees, the slope angle beta =60 degrees, the extrusion ratio is 25, and the extrusion speed is 0.4m/s.
Table 1 shows the results of the mechanical property measurements of example 1, and fig. 2 is a stress-strain graph thereof. FIG. 3 is a metallographic microstructure of an extruded alloy according to example 1 of the present invention, and it can be seen from the analysis that the alloy of the present invention has a grain size of about 12 μm and a fine grain size after one-time rapid hot extrusion.
TABLE 1 mechanical Properties of the examples
Example 2
S1, alloy smelting: pure Mg ingot, mg-20Gd intermediate alloy and Mg-Zr intermediate alloy are used as raw materials, the raw materials are mixed according to the proportion of Gd being 2.0 percent, zr being 0.6 percent and the balance being Mg, and the magnesium alloy ingot is cast by semi-continuous casting after the alloy mixture is melted. Semi-continuous casting process: preheating alloy raw materials to 80 ℃, adding the alloy raw materials into a crucible, spraying a covering agent, heating to 700 ℃, and smelting under the protection of SF6 and CO2 atmosphere; after all the materials are melted, removing slag and refining for 15min; after refining is finished, removing slag, and keeping the temperature and standing for 30min; sampling and analyzing the components, and if the components are qualified, cooling to 690 ℃ for semi-continuous casting.
S2, heat treatment: and (3) carrying out solid solution treatment on the magnesium alloy ingot prepared by the step (S1) and air cooling, wherein the solid solution temperature is 450 ℃, and the solid solution time is 12h.
S3, forging and pressing treatment: preheating the magnesium alloy ingot prepared in the step S2 to a forging temperature, and carrying out forging treatment, wherein the forging is carried out in a single-pass die forging mode, the forging temperature is 400 ℃, the pressure maintaining time is 5min, the billet is ensured to be filled in a cavity, the diameter of the forged billet is 8% larger than that of the extruded billet, and the forging strain is 10%.
S4, machining: and (4) machining the magnesium alloy ingot prepared in the step (S3) into an extrusion blank with a required size.
S5, upsetting: and (3) preheating the extrusion blank obtained in the step (S4) to the extrusion temperature, and upsetting the extrusion blank in an extruder by using a solid steel die, wherein the upsetting ratio is 1.5, and the extrusion temperature is 400 ℃.
S6, extrusion molding: and (5) extruding and forming the upset extrusion billet of the S5 by adopting an asymmetric extrusion die to obtain the magnesium alloy extrusion plate. The asymmetric die consists of an upper extrusion die cavity and a lower forming channel hole, the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, and the lower forming channel hole is in a rectangular shape, wherein the slope angle alpha =45 degrees, the slope angle beta =60 degrees, the extrusion ratio is 25, and the extrusion speed is 0.4m/s.
After detection, table 1 shows the mechanical property detection results of example 2.
Example 3
S1, alloy smelting: pure Mg ingot, mg-20Gd intermediate alloy, mg-20Er intermediate alloy and Mg-Zr intermediate alloy are used as raw materials, 1.5 percent of Gd, 1.5 percent of Er, 0.6 percent of Zr and the balance of Mg are used as ingredients, and the magnesium alloy ingot is cast by semi-continuous casting after the ingredients of the alloy are melted. Semi-continuous casting process: preheating alloy raw materials to 80 ℃, adding the alloy raw materials into a crucible, spraying a covering agent, heating to 700 ℃, and smelting under the protection of SF6 and CO2 atmosphere; after all the materials are melted, removing slag and refining for 15min; after refining, removing slag, and standing for 30min at a constant temperature; sampling and analyzing the components, and if the components are qualified, cooling to 690 ℃ for semi-continuous casting.
S2, heat treatment: and (3) carrying out solid solution treatment on the magnesium alloy ingot prepared by the step (S1) and air cooling, wherein the solid solution temperature is 450 ℃, and the solid solution time is 12h.
S3, forging and pressing treatment: and (3) preheating the magnesium alloy ingot prepared in the step (S2) to a forging temperature, carrying out forging treatment, wherein the forging temperature is 400 ℃, the pressure maintaining time is 5min, the billet is ensured to be full of the cavity, the diameter of the forged billet is 8% larger than that of the extruded billet, and the forging strain is 10%.
S4, machining: and machining the magnesium alloy ingot prepared in the step S3 into an extrusion blank with a required size.
S5, upsetting: and (3) preheating the extrusion blank obtained in the step (S4) to the extrusion temperature, and upsetting the extrusion blank in an extruder by using a solid steel die, wherein the upsetting ratio is 1.5, and the extrusion temperature is 400 ℃.
S6, extrusion molding: and (4) carrying out extrusion forming on the upset extrusion billet of the S5 by adopting an asymmetric extrusion die to prepare the magnesium alloy extrusion plate. The asymmetric die consists of an upper extrusion die cavity and a lower forming channel hole, the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, and the lower forming channel hole is in a rectangular shape, wherein the slope angle alpha =45 degrees, the slope angle beta =60 degrees, the extrusion ratio is 25, and the extrusion speed is 0.4m/s.
Through detection, the detection results of the mechanical properties of example 2 are shown in table 1.
Comparative example 1
AZ31 magnesium alloy which is directly purchased in the market is processed into a cylinder with the diameter of 80mm and the length of 300mm, and the cylinder is extruded and formed by a hot extrusion process at one time, wherein the extrusion temperature is 420 ℃, the extrusion ratio is 25, and the extrusion speed is 1mm/s.
The mechanical properties of the AZ31 magnesium alloy deformed material are shown in Table 1.
The comparison shows that after the Er element, the Gd element and the Zr element are added, the room-temperature elongation of the magnesium alloy wrought material is obviously improved, and the positive effect of the Er element and the Zr element on the room-temperature plasticity of the magnesium alloy through the method of weakening the texture and refining the crystal grains is reflected.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are not particularly limited to the specific examples described herein.
Claims (7)
1. The ultrahigh-plasticity rare earth wrought magnesium alloy is characterized by comprising the following components in percentage by mass: 1.5 to 3.0 percent of Er, 0.1 to 0.6 percent of Zr and the balance of Mg;
the ultrahigh-plasticity rare earth wrought magnesium alloy is prepared by the preparation method comprising the following steps of:
s1, alloy smelting: taking a pure Mg ingot, an Mg-Er intermediate alloy and an Mg-Zr intermediate alloy as raw materials, mixing the raw materials according to the components and the mass percentage of the magnesium alloy, melting the alloy mixture, and casting the alloy mixture into a magnesium alloy ingot;
s2, heat treatment: carrying out solution treatment on the magnesium alloy ingot prepared by the S1 and air cooling;
s3, forging and pressing treatment: preheating the magnesium alloy ingot prepared in the step S2 to a forging temperature, and carrying out forging treatment, wherein the diameter of the forged billet needs to be 8-10% larger than that of the extruded billet, and the forging strain is not less than 10%;
s4, machining: machining the magnesium alloy ingot prepared in the step S3 into an extrusion blank with a required size;
s5, upsetting: preheating the extrusion blank obtained in the step S4 to an extrusion temperature, and upsetting in an extruder by using a solid die, wherein the upsetting ratio is 1.1-2;
s6, extrusion molding: extruding and forming the upset extrusion billet of the S5 by adopting an asymmetric extrusion die to prepare a magnesium alloy extrusion plate; the asymmetric extrusion die comprises an upper extrusion die cavity and a lower forming channel hole, wherein the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, and the lower forming channel hole is in a shape of a rectangle, wherein the slope angle & lt alpha = 30-80 DEG, the slope angle & lt beta = 45-90 DEG, and & lt beta & gt & lt alpha.
2. The method for preparing the ultrahigh-plasticity rare earth wrought magnesium alloy extruded sheet material of claim 1, comprising the following steps:
s1, alloy smelting: taking a pure Mg ingot, an Mg-Er intermediate alloy and an Mg-Zr intermediate alloy as raw materials, mixing the raw materials according to the components and the mass percentage of the magnesium alloy, melting the alloy mixture, and casting the alloy mixture into a magnesium alloy ingot;
s2, heat treatment: carrying out solution treatment on the magnesium alloy ingot prepared by the S1 and air cooling;
s3, forging and pressing treatment: preheating the magnesium alloy ingot prepared in the step S2 to a forging temperature, and carrying out forging treatment, wherein the diameter of the forged billet needs to be 8-10% larger than that of the extruded billet, and the forging strain is not less than 10%;
s4, machining: machining the magnesium alloy ingot prepared in the step S3 into an extrusion blank with a required size;
s5, upsetting: preheating the extrusion blank obtained in the step S4 to an extrusion temperature, and upsetting in an extruder by using a solid die, wherein the upsetting ratio is 1.1 to 2;
s6, extrusion forming: extruding and forming the extruded billet subjected to the upsetting in the S5 by adopting an asymmetric extrusion die to obtain a magnesium alloy extruded sheet; the asymmetric extrusion die comprises an upper extrusion die cavity and a lower forming channel hole, wherein the section of a strain section of the upper extrusion die cavity is in a shape of a non-isosceles triangle, and the lower forming channel hole is in a shape of a rectangle, wherein the slope angle & lt alpha = 30-80 DEG, the slope angle & lt beta = 45-90 DEG, and & lt beta & gt & lt alpha.
3. The method for preparing the ultrahigh-plasticity rare earth wrought magnesium alloy extruded plate according to claim 2, wherein the magnesium alloy ingot is prepared by a semi-continuous casting method in the step S1.
4. The method for preparing the ultra-high plasticity rare earth wrought magnesium alloy extruded plate of claim 2, wherein the solution treatment process in the step S2 comprises: solid solution temperature: 360 to 450 ℃, solid solution time: and air cooling to room temperature for 4-16 h.
5. The method for preparing the ultra-high plasticity rare earth deformation magnesium alloy extruded plate material of claim 2, wherein in the step S3, the forging and pressing are performed by single-pass die forging, the forging and pressing temperature is 300-400 ℃, the pressure maintaining time is not less than 5min, and the billet is ensured to be filled in the cavity.
6. The method for preparing the ultrahigh-plasticity rare earth wrought magnesium alloy extruded plate of claim 2, wherein in the step S5, the extrusion temperature is 300-450 ℃.
7. The method for preparing the ultrahigh-plasticity rare earth deformation magnesium alloy extruded sheet material disclosed by claim 2 is characterized in that in the step S6, the extrusion ratio is 5-45, and the extrusion speed is 0.4-3.0 m/S.
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