CN116814996B - A low temperature forming method for high rare earth content magnesium alloy - Google Patents

A low temperature forming method for high rare earth content magnesium alloy Download PDF

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CN116814996B
CN116814996B CN202310913199.6A CN202310913199A CN116814996B CN 116814996 B CN116814996 B CN 116814996B CN 202310913199 A CN202310913199 A CN 202310913199A CN 116814996 B CN116814996 B CN 116814996B
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magnesium
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rare earth
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CN116814996A (en
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邓坤坤
曹芳芳
王翠菊
聂凯波
史权新
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Taiyuan University of Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • 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
    • 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
    • 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

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Abstract

一种高稀土含量镁合金的低温成形方法，属于镁合金材料技术领域，解决稀土镁合金硬度高、难变形、成形所需温度高的技术问题，解决方案为：以Mg‑Gd‑Y‑Zn合金为基体，可变形Ti颗粒为增强相制备Tip/稀土镁基复合材料，通过对搅拌温度、搅拌速度以及搅拌时间进行调控，获得Ti颗粒分布均匀、基体表面无明显团聚的稀土镁基复合材料，在此基础上进一步通过挤压变形和退火工艺来实现稀土镁合金的低温成形。通过本发明制得的Tip/稀土镁基复合材料屈服强度为324.5MPa，抗拉强度为361.5MPa，伸长率为9.1%。

A low-temperature forming method for a magnesium alloy with a high rare earth content belongs to the technical field of magnesium alloy materials, solves the technical problems of high hardness, difficult deformation and high forming temperature required for rare earth magnesium alloys, and the solution is: using Mg-Gd-Y-Zn alloy as a matrix and deformable Ti particles as a reinforcing phase to prepare a Tip/rare earth magnesium-based composite material, by regulating the stirring temperature, stirring speed and stirring time, a rare earth magnesium-based composite material with uniform Ti particle distribution and no obvious agglomeration on the matrix surface is obtained, and on this basis, low-temperature forming of rare earth magnesium alloys is further realized by extrusion deformation and annealing processes. The Tip/rare earth magnesium-based composite material prepared by the present invention has a yield strength of 324.5MPa, a tensile strength of 361.5MPa, and an elongation of 9.1%.

Description

Low-temperature forming method of magnesium alloy with high rare earth content
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to a low-temperature forming method of a magnesium alloy with high rare earth content.
Background
The rare earth magnesium alloy has excellent room temperature and high temperature mechanical properties and good creep resistance, can be used for service tasks in high temperature and high stress environments, is applied in large scale in important industries such as aerospace, national defense, military industry and automobiles, and becomes the high-performance magnesium alloy with the highest potential in the new century, and is highly valued by scientific researchers, wherein the Mg-Gd-Y-Zn alloy has great development potential.
However, for rare earth magnesium alloys, the shapes are difficult to shape when the rare earth content exceeds 10 wt.%. In order to realize the forming, the forming temperature is generally higher than 450 ℃, on one hand, the higher the deformation temperature is, the larger the grain size is, the lower the mechanical property is, and on the other hand, the high-temperature forming has higher requirements on equipment and causes energy consumption, which is not beneficial to promoting the development of green low carbon. Therefore, lowering the forming temperature is an important direction for the development of high rare earth magnesium alloys in the future.
Disclosure of Invention
In order to overcome the defects in the prior art and solve the technical problems of high hardness, difficult deformation and high temperature required by forming of the rare earth magnesium alloy, the invention provides a low-temperature forming method of the magnesium alloy with high rare earth content.
The design concept of the invention is as follows:
On one hand, the invention prepares the rare earth magnesium-based composite material with uniformly dispersed Ti particles and no obvious agglomeration on the surface by adding the deformable Ti particles as reinforcement into the high rare earth magnesium alloy;
On the other hand, the mechanical property of the high-rare-earth magnesium-based composite material is improved by a process combining extrusion and annealing, extrusion is an effective deformation mode for improving the structure and the property of cast magnesium alloy, and because the material is subjected to strong three-way compressive stress during extrusion deformation, casting defects can be remarkably eliminated, the structure is thinned, and the plastic deformation of a blank is facilitated, so that the control of the extrusion forming process on the structure and the property of the magnesium alloy is very important;
In a word, the invention selects Mg-Gd-Y-Zn alloy as a matrix, deformable Ti particles are used as reinforcements, the grain diameter of the Ti particles is 20-30 um, the high rare earth magnesium-based composite material with uniform Ti particle distribution and no obvious agglomeration on the surface is prepared, the mechanical property of the high rare earth magnesium-based composite material is improved by the process of combining extrusion and annealing, and the low-temperature forming of the high rare earth magnesium alloy is realized.
The invention is realized by the following technical scheme:
A low-temperature forming method of a magnesium alloy with high rare earth content comprises the following steps:
S1, ti powder pretreatment, namely firstly, wrapping Ti powder by adopting Zn foil, and respectively recording the weight of the Ti powder and the weight of the Zn foil, then, putting the Ti powder wrapped by the Zn foil into a container wrapped by adopting Al foil together, and putting the Ti powder into a drying furnace for preheating, wherein the preheating temperature is 140-180 ℃, and reserving for later use;
S2, selecting raw materials, namely firstly cutting magnesium blocks according to the size of a crucible, polishing the magnesium blocks, magnesium gadolinium intermediate alloy and magnesium yttrium intermediate alloy by an angle grinder, removing oxide skin on the surface, then weighing the magnesium blocks, zinc particles, magnesium gadolinium intermediate alloy and magnesium yttrium intermediate alloy, wherein the components of the raw materials and the mass percentage content thereof are 3wt.% of zinc, 5wt.% to 10wt.% of gadolinium, 2wt.% of yttrium and the balance of magnesium;
S3, placing the clean crucible into a smelting furnace for preheating, taking out the crucible after the clean crucible is preheated to 430-550 ℃, uniformly coating a coating agent on the inner wall of the crucible, and then placing the crucible into the smelting furnace;
s4, heating the smelting furnace to 740-760 ℃, and after the surface of the crucible turns yellow, putting the magnesium block weighed in the step S2 into the crucible for heating until the magnesium block is completely melted, and continuously introducing protective gas into the smelting furnace in the process of melting the magnesium block to prepare magnesium liquid;
s5, cooling the smelting furnace to 710-720 ℃, removing an oxide layer on the surface of the magnesium liquid, adding the zinc particles weighed in the step S2 into the magnesium liquid, stirring for 0.5-1.5 min, and then preserving heat for 10-20 min;
S6, after the heat preservation of the step S5 is finished, naturally cooling the alloy liquid to 600-640 ℃ along with a smelting furnace, taking the alloy liquid to be in a semi-solid state, removing an oxide layer on the surface of the semi-solid alloy melt, then placing the alloy liquid into a stirring paddle, starting a stirring device to mechanically stir, taking out Ti powder pretreated in the step S1 after the semi-solid alloy melt forms a stable vortex, adding the Ti powder and Zn foil into the semi-solid alloy melt, wherein the addition amount of the Ti powder accounts for 5-15% of the total volume fraction of the melt, and removing the stirring paddle after stirring for 10-20 min;
S7, mechanically stirring, namely raising the temperature of the smelting furnace to 700-740 ℃ again, removing an oxide layer on the surface of the alloy melt, then placing the magnesium-gadolinium intermediate alloy and the magnesium-yttrium intermediate alloy weighed in the step S2 into the alloy melt, placing the alloy into a stirring paddle again for mechanical stirring after the alloy is melted, and withdrawing the stirring paddle after the mechanical stirring is finished for 5-20 min;
S8, ultrasonic dispersion treatment, namely removing an oxide layer on the surface of the alloy liquid prepared in the step S7, extending an ultrasonic working rod which is preheated to 480-500 ℃ in advance into a position 20mm below the liquid surface of the alloy liquid, taking out the ultrasonic working rod after ultrasonic dispersion for 5-8 min, and standing for 3-5 min under heat preservation;
S9, casting, namely preheating a casting die to 400-500 ℃, removing an oxide layer on the surface of the alloy liquid after ultrasonic dispersion treatment in the step S8, casting the alloy liquid into the preheated casting die, and carrying out die casting by using a press, wherein the pressure is 400KN, the dwell time is 180-300S, taking out an ingot after die casting is completed, and naturally cooling to room temperature to obtain a Tip/rare earth magnesium-based composite ingot;
S10, extrusion forming and annealing treatment, namely firstly cutting the Tip/rare earth magnesium-based composite material cast ingot prepared in the step S9 into a plurality of extrusion blocks, polishing the surfaces of the extrusion blocks, then placing the extrusion blocks in an extrusion die, preheating the extrusion blocks to 360 ℃, carrying out hot extrusion forming on the extrusion blocks by using a press machine, wherein the extrusion rate is 0.1mm/S, the extrusion temperature is 360 ℃, the extrusion ratio is 16:1, and finally, placing the extrusion rod cooled to room temperature in a muffle furnace with the heating temperature of 360 ℃ for 30min, and rapidly taking out and quenching after the heat preservation is finished to prepare the Tip/rare earth magnesium-based composite material.
Further, in the step S2, the purity of the magnesium block is 99.9%, the purity of the zinc particles is 99.9%, the magnesium gadolinium intermediate alloy is Mg-30Gd, the purity of the magnesium gadolinium intermediate alloy is 99.9%, the magnesium yttrium intermediate alloy is Mg-30Y, and the purity of the magnesium yttrium intermediate alloy is 99.9%.
Further, in the step S3, the coating agent consists of talcum powder paint and zinc oxide paint, wherein the talcum powder paint comprises 80g of talcum powder, 20g of water glass and 250ml of water, and the zinc oxide paint comprises 45g of zinc oxide, 45g of water glass and 250ml of water.
Further, in the step S4, the shielding gas is a mixed gas formed by CO 2 and SF 6, and the volume ratio of CO 2 to SF 6 is 99:1.
Further, the sum of the weight of the Zn foil in the step S1 and the weight of the zinc particles in the step S2 is the total content of Zn element in the Tip/rare earth magnesium-based composite material prepared in the step S10.
Further, in the steps S5 to S9, a slag ladle is adopted to remove an oxide layer on the surface of the semi-solid alloy melt or alloy liquid, and the surface of the slag ladle is coated with a coating agent.
The invention has the beneficial effects that:
The invention adds the deformable Ti particles as reinforcement into the rare earth magnesium alloy to prepare the rare earth magnesium-based composite material with even Ti particle distribution and no obvious agglomeration on the surface, and further improves the structure and mechanical properties of the rare earth magnesium-based composite material by the process of combining extrusion and annealing, thereby realizing the low-temperature forming of the high rare earth magnesium alloy. After extrusion and annealing treatment, the yield strength of the rare earth magnesium-based composite material is 324.5MPa, the tensile strength is 361.5MPa, and the elongation is 9.1%.
Drawings
FIG. 1 is a graph showing a heating mechanism of the Tip/Mg-10Gd-2Y-3Zn composite material prepared in example 1;
FIG. 2 is a microstructure morphology of the as-cast Tip/Mg-10Gd-2Y-3Zn composite material prepared in example 1;
FIG. 3 is a microstructure morphology of the extruded Tip/Mg-10Gd-2Y-3Zn composite material prepared in example 1;
FIG. 4 is a microstructure morphology of the annealed Tip/Mg-10Gd-2Y-3Zn composite material prepared in example 1;
FIG. 5 is a graph comparing stress-strain curves of as-cast and annealed Tip/Mg-10Gd-2Y-3Zn composites prepared in example 1.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
Example 1
The low-temperature forming method of the magnesium alloy with high rare earth content shown in fig. 1 comprises the following steps:
S1, ti powder pretreatment, namely firstly, wrapping Ti powder by adopting Zn foil, and respectively recording the weight of the Ti powder and the weight of the Zn foil, then, putting the Ti powder wrapped by the Zn foil into a container wrapped by adopting Al foil together, and putting the Ti powder into a drying furnace for preheating at the preheating temperature of 140 ℃ for later use;
S2, selecting raw materials, namely firstly cutting magnesium blocks according to the size of a crucible, polishing the magnesium blocks, magnesium gadolinium intermediate alloy and magnesium yttrium intermediate alloy by an angle grinder, removing oxide skin on the surface, wherein the purity of the magnesium blocks is 99.9%, the purity of zinc particles is 99.9%, the magnesium gadolinium intermediate alloy is Mg-30Gd, the purity of the magnesium gadolinium intermediate alloy is 99.9%, the magnesium yttrium intermediate alloy is Mg-30Y, the purity of the magnesium yttrium intermediate alloy is 99.9%, then weighing the magnesium blocks, the zinc particles, the magnesium gadolinium intermediate alloy and the magnesium yttrium intermediate alloy, so that the composition of each element in the raw materials and the mass percentage content thereof are 3wt.% zinc, 5wt.% yttrium and 2wt.% magnesium, and finally, wrapping the weighed raw materials by fresh-keeping films respectively for later use, wherein the sum of the weight of Zn foil in the step S1 and the weight of the zinc particles in the step S2 is the total content of Zn elements in the final Tip/rare earth magnesium matrix composite;
s3, placing the clean crucible into a smelting furnace for preheating, taking out the crucible after the clean crucible is preheated to 430 ℃, uniformly coating a coating agent on the inner wall of the crucible, and then placing the crucible into the smelting furnace, wherein the coating agent consists of talcum powder paint and zinc oxide paint, the talcum powder paint comprises 80g of talcum powder, 20g of water glass and 250ml of water, and the zinc oxide paint comprises 45g of zinc oxide, 45g of water glass and 250ml of water;
S4, heating a smelting furnace to 740 ℃, and after the surface of the crucible turns yellow, putting the magnesium blocks weighed in the step S2 into the crucible for heating until the magnesium blocks are completely melted, continuously introducing protective gas into the smelting furnace in the process of melting the magnesium blocks to prepare magnesium liquid, wherein the protective gas consists of mixed gas of CO 2 and SF 6, and the volume ratio of CO 2 to SF 6 is 99:1;
s5, cooling the smelting furnace to 710 ℃, removing an oxide layer on the surface of the magnesium liquid, adding the zinc particles weighed in the step S2 into the magnesium liquid, stirring for 0.5min, and then preserving heat for 10min;
S6, after the heat preservation of the step S5 is finished, naturally cooling the alloy liquid to 600 ℃ along with a smelting furnace, taking the alloy liquid to be in a semi-solid state, removing an oxide layer on the surface of the semi-solid alloy melt, then placing the alloy liquid into a stirring paddle, starting a stirring device to mechanically stir, taking out Ti powder pretreated in the step S1 after the semi-solid alloy melt forms a stable vortex, adding the Ti powder and Zn foil into the semi-solid alloy melt, wherein the addition amount of the Ti powder is 5% of the total melt volume percent, stirring for 10min, and then withdrawing from the stirring paddle;
s7, mechanically stirring, namely raising the temperature of the smelting furnace to 700 ℃ again, removing an oxide layer on the surface of the alloy melt, then placing the magnesium-gadolinium intermediate alloy and the magnesium-yttrium intermediate alloy weighed in the step S2 into the alloy melt, placing the alloy into a stirring paddle again for mechanical stirring after the alloy is melted, and withdrawing the stirring paddle after the mechanical stirring is finished;
s8, ultrasonic dispersion treatment, namely removing an oxide layer on the surface of the alloy liquid prepared in the step S7, extending an ultrasonic working rod which is preheated to 480 ℃ in advance to a position 20mm below the liquid surface of the alloy liquid, taking out the ultrasonic working rod after ultrasonic dispersion for 5min, and preserving heat and standing for 3min;
S9, casting, namely preheating a casting die to 400 ℃, removing an oxide layer on the surface of the alloy liquid after ultrasonic dispersion treatment in the step S8, casting the alloy liquid into the preheated casting die, and carrying out die casting by using a press, wherein the pressure is 400KN, the dwell time is 180S, taking out the cast ingot after die casting is completed, naturally cooling the cast ingot to room temperature, and obtaining a cast ingot of the Tip/rare earth magnesium-based composite material, wherein a microstructure morphology diagram of the cast Tip/Mg-7Gd-2Y-3Zn composite material is shown in FIG. 2, ti particles in the cast composite material are uniformly dispersed, obvious agglomeration and oxidation slag inclusion are not generated on the surface, and a second phase is distributed along a grain boundary in a discontinuous network form;
S10, extrusion forming and annealing treatment, namely firstly cutting the Tip/rare earth magnesium-based composite material cast ingot prepared in the step S9 into a plurality of extrusion blocks, polishing the surfaces of the extrusion blocks, then placing the extrusion blocks in an extrusion die, preheating the extrusion blocks to 360 ℃, carrying out hot extrusion forming on the extrusion blocks by using a press machine, wherein the extrusion rate is 0.1mm/S, the extrusion temperature is 360 ℃, the extrusion ratio is 16:1, and finally, placing the extrusion rod cooled to room temperature in a muffle furnace with the heating temperature of 360 ℃ for 30min, and rapidly taking out and quenching after the heat preservation is finished to prepare the Tip/rare earth magnesium-based composite material.
The microstructure morphology diagram of the extruded Tip/Mg-7Gd-2Y-3Zn composite material is shown in fig. 3, and the fact that the Ti particles are obviously elongated after extrusion is shown in fig. 3, obvious dynamic recrystallization occurs in a matrix, and the grain size is obviously thinned compared with that of an as-cast composite material.
The microstructure morphology diagram of the annealed Tip/Mg-7Gd-2Y-3Zn composite material is shown in FIG. 4, and the recrystallization rate of the extruded alloy after annealing treatment is improved and the grain size is increased according to the graph in FIG. 4.
As can be seen from FIG. 5, the as-cast composite material has a yield strength, a tensile strength and an elongation of 99.0MPa, 134.5MPa and 0.93%, respectively, and after annealing, the composite material has a yield strength of 324.5MPa, a tensile strength of 361.5MPa and an elongation of 9.1%.
Example 2
A low-temperature forming method of a magnesium alloy with high rare earth content comprises the following steps:
S1, ti powder pretreatment, namely firstly, wrapping Ti powder by adopting Zn foil, and respectively recording the weight of the Ti powder and the weight of the Zn foil, then, putting the Ti powder wrapped by the Zn foil into a container wrapped by adopting Al foil together, and putting the Ti powder into a drying furnace for preheating at 160 ℃ for later use;
S2, selecting raw materials, namely firstly cutting magnesium blocks according to the size of a crucible, polishing the magnesium blocks, magnesium gadolinium intermediate alloy and magnesium yttrium intermediate alloy by an angle grinder, removing oxide skin on the surface, wherein the purity of the magnesium blocks is 99.9%, the purity of zinc particles is 99.9%, the magnesium gadolinium intermediate alloy is Mg-30Gd, the purity of the magnesium gadolinium intermediate alloy is 99.9%, the magnesium yttrium intermediate alloy is Mg-30Y, the purity of the magnesium yttrium intermediate alloy is 99.9%, then weighing the magnesium blocks, the zinc particles, the magnesium gadolinium intermediate alloy and the magnesium yttrium intermediate alloy, so that the composition of each element in the raw materials and the mass percentage content thereof are 3wt.% zinc, 7wt.% yttrium and 2wt.% magnesium, and finally, wrapping the weighed raw materials by fresh-keeping films respectively for later use, wherein the sum of the weight of Zn foil in the step S1 and the weight of the zinc particles in the step S2 is the total content of Zn elements in the final Tip/rare earth magnesium matrix composite;
S3, placing the clean crucible into a smelting furnace for preheating, taking out the crucible after the clean crucible is preheated to 500 ℃, uniformly coating a coating agent on the inner wall of the crucible, and then placing the crucible into the smelting furnace, wherein the coating agent consists of talcum powder paint and zinc oxide paint, the talcum powder paint comprises 80g of talcum powder, 20g of water glass and 250ml of water, and the zinc oxide paint comprises 45g of zinc oxide, 45g of water glass and 250ml of water;
S4, heating a smelting furnace to 750 ℃, and after the surface of the crucible turns yellow, putting the magnesium blocks weighed in the step S2 into the crucible for heating until the magnesium blocks are completely melted, continuously introducing protective gas into the smelting furnace in the process of melting the magnesium blocks to prepare magnesium liquid, wherein the protective gas consists of mixed gas of CO 2 and SF 6, and the volume ratio of CO 2 to SF 6 is 99:1;
S5, cooling the smelting furnace to 715 ℃, removing an oxide layer on the surface of the magnesium liquid, adding the zinc particles weighed in the step S2 into the magnesium liquid, stirring for 1min, and then preserving heat for 15min;
S6, after the heat preservation in the step S5 is finished, naturally cooling the alloy liquid to 620 ℃ along with a smelting furnace, taking the alloy liquid to be in a semi-solid state, removing an oxide layer on the surface of the semi-solid alloy melt, then placing the alloy liquid into a stirring paddle, starting a stirring device to mechanically stir, taking out Ti powder pretreated in the step S1 after the semi-solid alloy melt forms a stable vortex, adding the Ti powder and Zn foil into the semi-solid alloy melt, wherein the addition amount of the Ti powder is 10% of the total melt volume fraction, stirring for 15min, and then withdrawing from the stirring paddle;
S7, mechanically stirring, namely heating the smelting furnace to 720 ℃ again, removing an oxide layer on the surface of the alloy melt, then placing the magnesium-gadolinium intermediate alloy and the magnesium-yttrium intermediate alloy weighed in the step S2 into the alloy melt, placing the alloy into a stirring paddle again for mechanical stirring after the alloy is melted, and removing the stirring paddle after the mechanical stirring is finished;
S8, ultrasonic dispersion treatment, namely removing an oxide layer on the surface of the alloy liquid prepared in the step S7, extending an ultrasonic working rod which is preheated to 490 ℃ in advance to a position 20mm below the liquid surface of the alloy liquid, taking out the ultrasonic working rod after ultrasonic dispersion for 7min, and keeping the temperature and standing for 4min;
s9, casting, namely preheating a casting mould to 450 ℃, removing an oxide layer on the surface of the alloy liquid after ultrasonic dispersion treatment in the step S8, casting the alloy liquid into the preheated casting mould, and carrying out die casting by using a press under the pressure of 400KN for 240S, taking out the cast ingot after die casting, and naturally cooling to room temperature to obtain a Tip/rare earth magnesium-based composite cast ingot, wherein in the steps S5 to S9, a slag ladle is adopted to remove the oxide layer on the surface of the semi-solid alloy melt or the alloy liquid, and the surface of the slag ladle is coated with a coating agent;
S10, extrusion forming and annealing treatment, namely firstly cutting the Tip/rare earth magnesium-based composite material cast ingot prepared in the step S9 into a plurality of extrusion blocks, polishing the surfaces of the extrusion blocks, then placing the extrusion blocks in an extrusion die, preheating the extrusion blocks to 360 ℃, carrying out hot extrusion forming on the extrusion blocks by using a press machine, wherein the extrusion rate is 0.1mm/S, the extrusion temperature is 360 ℃, the extrusion ratio is 16:1, and finally taking out the extrusion plate prepared by extrusion forming, placing the extrusion plate in a muffle furnace with the heating temperature of 360 ℃ for heat preservation for 30min, and rapidly taking out and quenching after the heat preservation is finished to prepare the Tip/rare earth magnesium-based composite material.
Example 3
A low-temperature forming method of a magnesium alloy with high rare earth content comprises the following steps:
S1, ti powder pretreatment, namely firstly, wrapping Ti powder by adopting Zn foil, and respectively recording the weight of the Ti powder and the weight of the Zn foil, then, putting the Ti powder wrapped by the Zn foil into a container wrapped by adopting Al foil together, and putting the Ti powder into a drying furnace for preheating at 180 ℃ for later use;
S2, selecting raw materials, namely firstly cutting magnesium blocks according to the size of a crucible, polishing the magnesium blocks, magnesium gadolinium intermediate alloy and magnesium yttrium intermediate alloy by an angle grinder, removing oxide skin on the surface, wherein the purity of the magnesium blocks is 99.9%, the purity of zinc particles is 99.9%, the magnesium gadolinium intermediate alloy is Mg-30Gd, the purity of the magnesium gadolinium intermediate alloy is 99.9%, the magnesium yttrium intermediate alloy is Mg-30Y, the purity of the magnesium yttrium intermediate alloy is 99.9%, then weighing the magnesium blocks, the zinc particles, the magnesium gadolinium intermediate alloy and the magnesium yttrium intermediate alloy, so that the composition of each element in the raw materials and the mass percentage content thereof are 3wt.% zinc, 10wt.% gadolinium and 2wt.% yttrium, and the balance magnesium, and finally, wrapping the weighed raw materials by fresh-keeping films respectively for later use, wherein the sum of the weight of Zn foil in the step S1 and the weight of the zinc particles in the step S2 is the total content of Zn elements in the final Tip/rare earth magnesium matrix composite;
S3, placing the clean crucible into a smelting furnace for preheating, taking out the crucible after the clean crucible is preheated to 550 ℃, uniformly coating a coating agent on the inner wall of the crucible, and then placing the crucible into the smelting furnace, wherein the coating agent consists of talcum powder paint and zinc oxide paint, the talcum powder paint comprises 80g of talcum powder, 20g of water glass and 250ml of water, and the zinc oxide paint comprises 45g of zinc oxide, 45g of water glass and 250ml of water;
S4, heating a smelting furnace to 760 ℃, and after the surface of the crucible turns yellow, putting the magnesium block weighed in the step S2 into the crucible for heating until the magnesium block is completely melted, and continuously introducing a protective gas into the smelting furnace in the process of melting the magnesium block to prepare magnesium liquid, wherein the protective gas consists of CO 2 and SF 6 to form a mixed gas, and the volume ratio of CO 2 to SF 6 is 99:1;
s5, cooling the smelting furnace to 720 ℃, removing an oxide layer on the surface of the magnesium liquid, adding the zinc particles weighed in the step S2 into the magnesium liquid, stirring for 1.5min, and then preserving heat for 20min;
S6, after the heat preservation of the step S5 is finished, naturally cooling the alloy liquid to 640 ℃ along with a smelting furnace, taking the alloy liquid to be in a semi-solid state, removing an oxide layer on the surface of the semi-solid alloy melt, then placing the alloy liquid into a stirring paddle, starting a stirring device to mechanically stir, taking out Ti powder pretreated in the step S1 after the semi-solid alloy melt forms a stable vortex, adding the Ti powder and Zn foil into the semi-solid alloy melt, wherein the addition amount of the Ti powder is 15% of the total melt volume percent, stirring for 20min, and then withdrawing from the stirring paddle;
S7, mechanically stirring, namely heating the smelting furnace to 740 ℃ again, removing an oxide layer on the surface of the alloy melt, then placing the magnesium-gadolinium intermediate alloy and the magnesium-yttrium intermediate alloy weighed in the step S2 into the alloy melt, placing the alloy into a stirring paddle again for mechanically stirring after the alloy is melted, and withdrawing the stirring paddle after the mechanical stirring is finished;
S8, ultrasonic dispersion treatment, namely removing an oxide layer on the surface of the alloy liquid prepared in the step S7, extending an ultrasonic working rod which is preheated to 500 ℃ in advance into a position 20mm below the liquid surface of the alloy liquid, taking out the ultrasonic working rod after ultrasonic dispersion for 8min, and keeping the temperature and standing for 5min;
S9, casting, namely preheating a casting mould to 500 ℃, removing an oxide layer on the surface of the alloy liquid after ultrasonic dispersion treatment in the step S8, casting the alloy liquid into the preheated casting mould, and carrying out die casting by using a press under the pressure of 400KN for 300S, taking out the cast ingot after die casting, and naturally cooling to room temperature to obtain a Tip/rare earth magnesium-based composite cast ingot;
S10, extrusion forming and annealing treatment, namely firstly cutting the Tip/rare earth magnesium-based composite material cast ingot prepared in the step S9 into a plurality of extrusion blocks, polishing the surfaces of the extrusion blocks, then placing the extrusion blocks in an extrusion die, preheating the extrusion blocks to 360 ℃, carrying out hot extrusion forming on the extrusion blocks by using a press machine, wherein the extrusion rate is 0.1mm/S, the extrusion temperature is 360 ℃, the extrusion ratio is 16:1, and finally, placing the extrusion rod cooled to room temperature in a muffle furnace with the heating temperature of 360 ℃ for 30min, and rapidly taking out and quenching after the heat preservation is finished to prepare the Tip/rare earth magnesium-based composite material.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (6)

1.一种高稀土含量镁合金的低温成形方法，其特征在于，包括以下步骤：1. A low temperature forming method for a magnesium alloy with a high rare earth content, characterized in that it comprises the following steps: S1、Ti粉预处理：首先，采用Zn箔包裹Ti粉，并分别记录Ti粉的重量和Zn箔的重量；然后，将Zn箔包裹的Ti粉一同放入采用Al箔包裹的容器中，并放入烘干炉中预热，预热温度为140℃~180℃，留待后步使用；S1. Pretreatment of Ti powder: First, wrap Ti powder with Zn foil, and record the weight of Ti powder and the weight of Zn foil respectively; then, put Ti powder wrapped with Zn foil into a container wrapped with Al foil, and put it into a drying furnace for preheating at a temperature of 140°C to 180°C, and reserve it for use in the next step; S2、原料选取：首先，根据坩埚尺寸切取镁块，将镁块、镁钆中间合金和镁钇中间合金用角磨机打磨，去除表面的氧化皮；然后，称取镁块、锌粒、镁钆中间合金和镁钇中间合金，使原料中各元素的组成及其质量百分比含量为：锌：3wt.%，钆：5wt.%~10wt.%，钇：2wt.%，其余为镁；最后，将称取的原料分别用保鲜膜包裹，留待后步使用；S2. Raw material selection: First, cut a magnesium block according to the size of the crucible, grind the magnesium block, magnesium-gadolinium master alloy and magnesium-yttrium master alloy with an angle grinder to remove the oxide scale on the surface; then, weigh the magnesium block, zinc particles, magnesium-gadolinium master alloy and magnesium-yttrium master alloy, so that the composition and mass percentage content of each element in the raw materials are: zinc: 3wt.%, gadolinium: 5wt.%~10wt.%, yttrium: 2wt.%, and the rest is magnesium; finally, wrap the weighed raw materials with plastic wrap respectively and keep them for use in the next step; S3、将洁净的坩埚放入熔炼炉中预热，待洁净的坩埚预热至430℃~550℃后取出，向坩埚的内壁上均匀地涂刷涂覆剂，然后再放入熔炼炉中；S3, placing a clean crucible into a melting furnace for preheating, taking out the clean crucible after it is preheated to 430°C-550°C, evenly applying a coating agent on the inner wall of the crucible, and then placing it into the melting furnace; S4、将熔炼炉升温至740℃~760℃，待坩埚的表面泛黄后，将步骤S2称取的镁块放入坩埚中加热直至镁块完全熔化，镁块熔化过程中熔炼炉内持续通入保护气，制得镁液；S4, heating the smelting furnace to 740°C-760°C, and after the surface of the crucible turns yellow, placing the magnesium block weighed in step S2 into the crucible and heating until the magnesium block is completely melted, and continuously introducing protective gas into the smelting furnace during the melting process of the magnesium block to obtain magnesium liquid; S5、熔炼炉降温至710℃~720℃，扒除镁液表面的氧化层，将步骤S2称取的锌粒加入镁液中并搅拌0.5min~1.5min，然后保温10min~20min；S5, the smelting furnace is cooled to 710°C-720°C, the oxide layer on the surface of the magnesium liquid is removed, the zinc particles weighed in step S2 are added to the magnesium liquid and stirred for 0.5min-1.5min, and then kept warm for 10min-20min; S6、待步骤S5保温结束后，合金液随熔炼炉自然冷却至600℃~640℃，此时合金液呈半固态状态，扒除半固态合金熔体表面的氧化层后置入搅拌桨，启动搅拌装置进行机械搅拌，待半固态合金熔体形成稳定的涡流后，取出步骤S1预处理后的Ti粉，Ti粉连同Zn箔一起加入半固态合金熔体中，其中Ti粉的添加量占总熔体的体积分数为5%~15%，搅拌10min~20min后撤离搅拌桨；S6, after the heat preservation of step S5 is completed, the alloy liquid is naturally cooled to 600°C~640°C with the smelting furnace, and the alloy liquid is in a semi-solid state. After the oxide layer on the surface of the semi-solid alloy melt is removed, a stirring paddle is placed, and the stirring device is started for mechanical stirring. After the semi-solid alloy melt forms a stable vortex, the Ti powder pretreated in step S1 is taken out, and the Ti powder is added to the semi-solid alloy melt together with the Zn foil, wherein the added amount of Ti powder accounts for 5%~15% of the volume fraction of the total melt, and the stirring paddle is removed after stirring for 10min~20min; S7、机械搅拌：熔炼炉再次升温至700℃~740℃，扒除合金熔体表面的氧化层，然后将步骤S2称取的镁钆中间合金和镁钇中间合金放入合金熔体中，待合金熔化后再次置入搅拌桨进行机械搅拌，搅拌时间5min~20min，机械搅拌结束后撤离搅拌桨；S7, mechanical stirring: the melting furnace is heated to 700°C-740°C again, the oxide layer on the surface of the alloy melt is removed, and then the magnesium-gadolinium master alloy and the magnesium-yttrium master alloy weighed in step S2 are placed into the alloy melt. After the alloy is melted, a stirring paddle is placed again for mechanical stirring for 5min-20min. After the mechanical stirring is completed, the stirring paddle is removed; S8、超声波分散处理：扒除步骤S7制得的合金液表面的氧化层，将预先已经预热到480℃~500℃的超声波工作杆伸入合金液液面下20mm处，超声波分散5min~8min后取出超声波工作杆，保温静置3min~5min；S8, ultrasonic dispersion treatment: remove the oxide layer on the surface of the alloy liquid obtained in step S7, insert the ultrasonic working rod preheated to 480°C to 500°C into the alloy liquid 20mm below the liquid surface, perform ultrasonic dispersion for 5min to 8min, then take out the ultrasonic working rod, keep it warm and let it stand for 3min to 5min; S9、浇铸：将浇铸模具预热至400℃~500℃，扒除步骤S8超声波分散处理后合金液表面的氧化层，然后将合金液浇铸至预热后的浇铸模具中，并用压力机进行压铸，压力为400kN，保压时间为180s~300s，压铸完成后取出铸锭自然冷却至室温，制得Tip/稀土镁基复合材料铸锭；S9, casting: preheat the casting mold to 400°C~500°C, remove the oxide layer on the surface of the alloy liquid after the ultrasonic dispersion treatment in step S8, then cast the alloy liquid into the preheated casting mold, and use a press to perform die casting, the pressure is 400kN, the holding time is 180s~300s, after the die casting is completed, take out the ingot and cool it naturally to room temperature to obtain a Tip/rare earth magnesium-based composite material ingot; S10、挤压成形及退火处理：首先，将步骤S9制得的Tip/稀土镁基复合材料铸锭切分成若干挤压块，并将挤压块表面打磨干净；然后，将挤压块放置于挤压模具中预热至360℃，使用压力机对挤压块进行热挤压成形，挤出速率为0.1mm/s，挤出温度为360℃，挤压比为16:1；最后，将冷却到室温的挤压棒放入加热温度为360℃的马弗炉中保温30min，保温结束后快速取出并淬火，制得Tip/稀土镁基复合材料。S10, extrusion forming and annealing treatment: First, the Tip/rare earth magnesium-based composite material ingot obtained in step S9 is cut into several extrusion blocks, and the surface of the extrusion blocks is polished clean; then, the extrusion blocks are placed in an extrusion mold and preheated to 360°C, and a press is used to hot extrude the extrusion blocks, with an extrusion rate of 0.1 mm/s, an extrusion temperature of 360°C, and an extrusion ratio of 16:1; finally, the extruded rod cooled to room temperature is placed in a muffle furnace with a heating temperature of 360°C and kept warm for 30 minutes. After the insulation is completed, it is quickly taken out and quenched to obtain the Tip/rare earth magnesium-based composite material. 2.根据权利要求1所述的一种高稀土含量镁合金的低温成形方法，其特征在于：在所述步骤S2中，所述镁块的纯度为99.9%，锌粒的纯度为99.9%；所述镁钆中间合金为Mg-30Gd，镁钆中间合金的纯度为99.9%；所述镁钇中间合金为Mg-30Y，镁钇中间合金的纯度为99.9%。2. The low-temperature forming method of a magnesium alloy with a high rare earth content according to claim 1, characterized in that: in the step S2, the purity of the magnesium block is 99.9%, the purity of the zinc particles is 99.9%; the magnesium-gadolinium master alloy is Mg-30Gd, and the purity of the magnesium-gadolinium master alloy is 99.9%; the magnesium-yttrium master alloy is Mg-30Y, and the purity of the magnesium-yttrium master alloy is 99.9%. 3.根据权利要求1所述的一种高稀土含量镁合金的低温成形方法，其特征在于：在所述步骤S3中，所述涂覆剂由滑石粉涂料和氧化锌涂料组成，所述滑石粉涂料的配比为：滑石粉80g、水玻璃20g和水250ml；所述氧化锌涂料的配比为：氧化锌45g、水玻璃45g和水250ml。3. The low-temperature forming method of a magnesium alloy with a high rare earth content according to claim 1 is characterized in that: in the step S3, the coating agent is composed of talcum powder coating and zinc oxide coating, and the ratio of the talcum powder coating is: 80g of talcum powder, 20g of water glass and 250ml of water; the ratio of the zinc oxide coating is: 45g of zinc oxide, 45g of water glass and 250ml of water. 4.根据权利要求1所述的一种高稀土含量镁合金的低温成形方法，其特征在于：在所述步骤S4中，所述保护气由CO2和SF6组成混合气体，CO2和SF6的体积比为99:1。4. The low-temperature forming method of a magnesium alloy with a high rare earth content according to claim 1, characterized in that: in the step S4, the shielding gas is a mixed gas composed of CO2 and SF6 , and the volume ratio of CO2 to SF6 is 99:1. 5.根据权利要求1所述的一种高稀土含量镁合金的低温成形方法，其特征在于：所述步骤S1中Zn箔的重量以及步骤S2中锌粒的重量之和为步骤S10制得的Tip/稀土镁基复合材料中Zn元素的总含量。5. The low-temperature forming method of a magnesium alloy with a high rare earth content according to claim 1, characterized in that the sum of the weight of the Zn foil in step S1 and the weight of the zinc particles in step S2 is the total content of the Zn element in the Tip/rare earth magnesium-based composite material obtained in step S10. 6.根据权利要求1所述的一种高稀土含量镁合金的低温成形方法，其特征在于：在所述步骤S5至步骤S9中，采用扒渣勺扒除半固态合金熔体或者合金液表面的氧化层，所述扒渣勺表面涂覆涂覆剂。6. A low-temperature forming method for a magnesium alloy with a high rare earth content according to claim 1, characterized in that: in the steps S5 to S9, a slag scoop is used to scrape off the oxide layer on the surface of the semi-solid alloy melt or the alloy liquid, and the surface of the slag scoop is coated with a coating agent.
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