CN112048653A - Ultrafine-grained wrought magnesium alloy material and preparation method thereof - Google Patents
Ultrafine-grained wrought magnesium alloy material and preparation method thereof Download PDFInfo
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- CN112048653A CN112048653A CN202010873447.5A CN202010873447A CN112048653A CN 112048653 A CN112048653 A CN 112048653A CN 202010873447 A CN202010873447 A CN 202010873447A CN 112048653 A CN112048653 A CN 112048653A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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Abstract
The invention provides an ultrafine grained wrought magnesium alloy material and a preparation method thereof, wherein the magnesium alloy material contains at least one high solid solubility rare earth element and at least one low solid solubility rare earth element, the high solid solubility rare earth element is selected from at least one of gadolinium or yttrium, the low solid solubility rare earth element is selected from at least one of neodymium or samarium, the total mass content of the rare earth elements is more than 13%, the mass content of the high solid solubility rare earth element is 10-15%, and the mass content of the low solid solubility rare earth element is 2-5%; the balance being magnesium. The preparation method comprises the following steps: carrying out solution treatment, water quenching and cooling; preheating; and carrying out backward extrusion and cooling to prepare the ultrafine-grained wrought magnesium alloy material. The element proportion and the forming process of the magnesium alloy material can greatly reduce the size of magnesium alloy grains, the plasticity of the prepared magnesium alloy product is greatly improved, and the magnesium alloy product is suitable for superplastic forming processing.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to an ultrafine-grained wrought magnesium alloy material and a preparation method 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.
The magnesium alloy crystal is in a close-packed hexagonal structure, the slip system is less, the critical shear stress of the cylindrical surface and conical surface slip is much larger than that of the basal surface during plastic forming at room temperature or below 300 ℃, the c or < c + a > slip is difficult to start at low temperature, the low-temperature formability of the magnesium alloy is poor, and the processing and forming difficulty becomes the biggest obstacle of the industrial application of the magnesium alloy, so that the application amount of the deformed magnesium alloy is far behind that of steel and aluminum alloy. The high rare earth wrought magnesium alloy has the advantages of high mechanical strength, weak anisotropy and the like, has wide application prospect, but the addition of the rare earth element further improves the processing and forming difficulty of the magnesium alloy. The novel plastic processing method is developed, the plastic processing capacity of the magnesium alloy, particularly the high-rare earth magnesium alloy, is improved, and the method has great application value.
According to the current research situation, fine crystal grains can induce a deformation mechanism of grain boundary sliding and room temperature recrystallization while improving the yield strength, so that plastic deformation is a coordinated deformation mode, the plastic deformation processing capacity of the material is improved, and the plasticity of the material is greatly improved. Therefore, the material is required to have ultra-fine grains (less than or equal to 5 mu m), the finer the grains, the better the superplastic forming capability of the magnesium alloy is improved, and the application potential of the magnesium alloy plastic processing can be further expanded by searching the magnesium alloy superfine grain and superplastic forming mechanism. However, the preparation of the magnesium alloy ultrafine crystal still mainly adopts processes of severe deformation, such as an equal channel angular extrusion process, a high-pressure torsion process, a multidirectional forging technology and the like, and the processes have high requirements on equipment and complex processes. Further seeking an alloying method for enabling the magnesium alloy to have better superplasticity and a simpler deformation processing technology matched with the alloying method for preparing the ultrafine magnesium alloy material, better developing low-temperature superplastic forming and high-strain-rate superplastic forming technologies and improving the production efficiency of the large-plastic-deformation magnesium alloy.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor of the invention carries out intensive research, utilizes various recrystallization behaviors, and provides an ultrafine grained wrought magnesium alloy material and a preparation method thereof.
The technical scheme provided by the invention is as follows:
in a first aspect, an ultra-fine grained wrought magnesium alloy material comprises: the magnesium alloy comprises at least one high solid solubility rare earth element and at least one low solid solubility rare earth element, wherein the high solid solubility rare earth element is selected from at least one of gadolinium (Gd) or yttrium (Y), the low solid solubility rare earth element is selected from at least one of neodymium (Nd) or samarium (Sm), and the total mass content of the rare earth elements is more than 13%.
Furthermore, the magnesium alloy only contains one high-solid-solubility rare earth element and one low-solid-solubility rare earth element.
Furthermore, the mass content of the high solid solubility rare earth element is 10-15%, and the mass content of the low solid solubility rare earth element is 2-5%; the balance being magnesium.
In a second aspect, a method for preparing an ultrafine grained wrought magnesium alloy material comprises the following steps:
step 1, carrying out solution treatment on a prepared billet according to the proportion of elements in a magnesium alloy material, and carrying out water quenching and cooling;
step 2, heating the ingot after the solution treatment in an electromagnetic induction heating furnace or an atmosphere circulating heat treatment furnace to a specified temperature;
and 3, carrying out backward extrusion on the heated pretreated sample, and cooling to prepare the superfine-grained wrought magnesium alloy material.
According to the ultrafine-grained wrought magnesium alloy material and the preparation method thereof provided by the invention, the ultrafine-grained wrought magnesium alloy material has the following beneficial effects:
the rare earth magnesium alloy material has superfine crystal grains different from other magnesium alloys, and the size of the magnesium alloy crystal grains is greatly reduced by adding at least two rare earth elements with different solid solubility and carrying out a backward extrusion process plastic forming process.
Drawings
FIG. 1 shows the optical structure of a Mg-10Gd-5Nd rare earth magnesium alloy after solution treatment in example 2 of the present invention;
FIG. 2 is a comparison of the grain sizes of the magnesium alloys of examples 1, 2, 3, 4, 5 of the present invention and comparative 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.
According to a first aspect of the present invention, an ultrafine grained wrought magnesium alloy material is provided, the magnesium alloy composition comprising at least one high solid solubility rare earth element and at least one low solid solubility rare earth element, wherein the high solid solubility rare earth element is selected from gadolinium (Gd) or yttrium (Y) or a combination thereof, the low solid solubility rare earth element is selected from neodymium (Nd) or samarium (Sm) or a combination thereof, and the total mass content of the rare earth elements is > 13%.
Furthermore, the high solid solubility rare earth element is selected from one of gadolinium (Gd) or yttrium (Y), and the low solid solubility rare earth element is selected from one of neodymium (Nd) or samarium (Sm).
Furthermore, the magnesium alloy only contains one high-solid-solubility rare earth element and one low-solid-solubility rare earth element.
Through a large amount of researches and experiments, the inventor finds that the high-solid-solubility rare earth element can induce the nucleation of a crystal boundary of the alloy in the hot extrusion process, promote the recrystallization nucleation and obviously refine the grain size of the extruded magnesium alloy; meanwhile, the low solid solubility rare earth provides ultrafine particles with particle-stimulated nucleation, the growth of recrystallized grains in the hot extrusion process is effectively inhibited, and the ultrafine-grained high-rare earth wrought magnesium alloy material can be finally obtained through the coupling effect of the low solid solubility rare earth and the recrystallized grains.
Furthermore, in the magnesium alloy material, the mass content of the high solid solubility rare earth element is 10-15%, and the mass content of the low solid solubility rare earth element is 2-5%; the balance being magnesium (Mg).
Through a large amount of researches and experiments, the inventor finds that for the rare earth elements with high solid solubility, in the solubility range, the more the rare earth elements are added, the more the refining effect of extruded crystal grains is obvious, and when the mass content of the elements is between 10 and 15 percent, the refining effect of the crystal grains of the rare earth elements with high solid solubility is optimal; for the rare earth elements with low solid solubility, the refining effect is not obvious when the adding amount is low, the solid solution effect of the rare earth elements with high solid solubility can be influenced when the adding amount is too high, and the grain refining effect is finally influenced, so that when the mass content of the elements is between 2 and 5 percent, the comprehensive grain refining effect of the rare earth elements with low solid solubility is optimal.
According to a second aspect of the present invention, there is provided a method for preparing an ultra-fine grained wrought magnesium alloy material, comprising the steps of:
step 1, carrying out solution treatment on a prepared billet according to the proportion of elements in a magnesium alloy material, and carrying out water quenching and cooling;
step 2, heating the ingot after the solution treatment in an electromagnetic induction heating furnace or an atmosphere circulating heat treatment furnace to a specified temperature;
and 3, carrying out backward extrusion on the heated pretreated sample, and cooling to prepare the superfine-grained wrought magnesium alloy material.
In the step 1, the solution treatment temperature is 500-550 ℃, and the time is 16-24 hours.
In step 2, the heating to the designated temperature is performed until the temperature is 400-460 ℃.
In the step 3, the extrusion speed in the back extrusion process is 0.1-1.0 m/s, preferably 0.1-0.6 m/s; the extrusion ratio is 1: 30-90, preferably 1: 50-70; the extrusion temperature is 400-440 ℃.
In step 3, the cooling is carried out by natural cooling in air.
Examples
Example 1
The ultrafine-grained wrought magnesium alloy material comprises the following components in percentage by mass: y: 10%, Sm: 4 percent; the balance being Mg.
A preparation method of an ultrafine grained wrought magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 16 hours at 530 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an electromagnetic induction heating furnace, wherein the electromagnetic induction heating temperature is 400 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 430 ℃, the extrusion rate of 0.6m/s and the extrusion ratio of 1:70, and naturally cooling in the air to obtain the ultrafine grained wrought magnesium alloy material Mg-10Y-4 Sm.
As shown in FIG. 2, the grain size of the extruded magnesium alloy was 6.1. mu.m, and the grains of the magnesium alloy were extremely fine. The extrusion tensile strength is 354MPa, the elongation is 15 percent, and is higher than the extrusion elongation of the magnesium alloy with high rare earth content mentioned in most reports at present (the extrusion elongation of the Mg-10Gd-2Y alloy is reported to be 6.7 percent).
Example 2
The ultrafine-grained wrought magnesium alloy material comprises the following components in percentage by mass: 10% of Gd, 5% of Nd and the balance of Mg.
A preparation method of an ultrafine grained wrought magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 16 hours at 530 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an electromagnetic induction heating furnace, wherein the electromagnetic induction heating temperature is 450 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 420 ℃, at the extrusion speed of 0.3m/s and at the extrusion ratio of 1:52, and naturally cooling in air to obtain the ultrafine-grained deformed magnesium alloy material Mg-10Gd-5 Nd.
As shown in FIGS. 1 and 2, the grain size of the magnesium alloy after extrusion was 5.5. mu.m, and the grains of the magnesium alloy were extremely refined. The tensile strength in an extrusion state is 389MPa, the elongation is 20 percent, and the comprehensive mechanical property is further improved.
Example 3
The ultrafine-grained wrought magnesium alloy material comprises the following components in percentage by mass: 10% of Gd, 5% of Sm and the balance of Mg.
A preparation method of an ultrafine grained wrought magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 18 hours at 530 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an electromagnetic induction heating furnace, wherein the electromagnetic induction heating temperature is 450 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 420 ℃, the extrusion rate of 0.6m/s and the extrusion ratio of 1:70, and naturally cooling in air to obtain the ultrafine-grained wrought magnesium alloy material Mg-10Gd-5 Sm.
As shown in FIG. 2, the grains of the extruded magnesium alloy are refined by 5.2 μm, and the grains of the magnesium alloy are greatly refined. The tensile strength in the extruded state was 382MPa, and the elongation was 20%.
Example 4
The ultrafine-grained wrought magnesium alloy material comprises the following components in percentage by mass: 15% of Y, 2% of Nd and the balance of Mg.
A preparation method of an ultrafine grained wrought magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 24 hours at 520 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an electromagnetic induction heating furnace, wherein the electromagnetic induction heating temperature is 450 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 430 ℃, the extrusion rate of 0.1m/s and the extrusion ratio of 1:52, and naturally cooling in the air to obtain the ultrafine-grained wrought magnesium alloy material Mg-15Y-2 Nd.
As shown in FIG. 2, the grain size of the extruded magnesium alloy was 4.8. mu.m, and the grains of the magnesium alloy were extremely fine. The tensile strength in an extrusion state is 406MPa, the elongation is 17 percent, and the mechanical property is further improved along with the reduction of the grain size.
Example 5
The ultrafine-grained wrought magnesium alloy material comprises the following components in percentage by mass: 15% of Gd, 5% of Nd and the balance of Mg.
A preparation method of an ultrafine grained wrought magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 24 hours at 550 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an atmosphere cyclic heat treatment furnace, wherein the heating temperature of the atmosphere cyclic heat treatment is 450 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 420 ℃, at the extrusion speed of 0.3m/s and at the extrusion ratio of 1:30, and naturally cooling in air to obtain the ultrafine-grained wrought magnesium alloy material Mg-15Gd-5 Nd.
As shown in FIG. 2, the grain size of the extruded magnesium alloy was 4.3 μm, and the grains of the magnesium alloy were extremely fine. The extrusion tensile strength is 411MPa, the elongation is 15%, and the comprehensive mechanical property is excellent due to fine crystal grains and high rare earth content.
Comparative example 1
A magnesium alloy material comprises the following components in percentage by mass: gd: 10%, Nd: 2 percent; the balance being Mg.
A preparation method of a magnesium alloy material comprises the following steps:
(1) carrying out solution treatment on the prepared original billet for 16 hours at 530 ℃, and carrying out water quenching;
(2) heating the billet subjected to the solution treatment in an electromagnetic induction heating furnace, wherein the electromagnetic induction heating temperature is 400 ℃;
(3) and (3) carrying out backward extrusion on the pretreated billet at the extrusion temperature of 430 ℃, the extrusion rate of 0.6m/s and the extrusion ratio of 1:70, and naturally cooling in air to obtain the magnesium alloy material Mg-10Gd-2 Nd.
As shown in FIG. 2, the grain size of the extruded magnesium alloy is 25 μm, the grain size of the magnesium alloy is large, the tensile strength in the extruded state is 340MPa, and the elongation is 16%.
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 well known in the art.
Claims (8)
1. The ultrafine-grained wrought magnesium alloy material is characterized in that the magnesium alloy contains at least one high-solid-solubility rare earth element and at least one low-solid-solubility rare earth element, wherein the high-solid-solubility rare earth element is selected from at least one of gadolinium and yttrium, the low-solid-solubility rare earth element is selected from at least one of neodymium and samarium, and the total mass content of the rare earth elements is more than 13%.
2. The ultra-fine grained wrought magnesium alloy material according to claim 1, wherein the magnesium alloy composition comprises only one high solid solubility rare earth element and only one low solid solubility rare earth element.
3. The ultrafine grained wrought magnesium alloy material according to claim 1, wherein the mass content of the high solid solubility rare earth element is 10% to 15%, and the mass content of the low solid solubility rare earth element is 2% to 5%; the balance being magnesium.
4. The preparation method of the ultrafine-grained wrought magnesium alloy material is characterized by comprising the following steps of:
step 1, carrying out solution treatment on a prepared billet according to the proportion of elements in a magnesium alloy material, and carrying out water quenching and cooling;
step 2, heating the ingot after the solution treatment in an electromagnetic induction heating furnace or an atmosphere circulating heat treatment furnace to a specified temperature;
and 3, carrying out backward extrusion on the heated pretreated sample, and cooling to prepare the superfine-grained wrought magnesium alloy material.
5. The method according to claim 4, wherein the solution treatment temperature in step 1 is 500 to 550 ℃ and the time is 16 to 24 hours.
6. The method according to claim 4, wherein the heating to the predetermined temperature in the step 2 is heating to a temperature of 400 to 460 ℃.
7. The method according to claim 4, wherein in the step 3, the extrusion speed in the backward extrusion process is 0.1 to 1.0m/s, and the extrusion ratio is 1: 30-90 ℃, and the extrusion temperature is 400-440 ℃.
8. The method according to claim 4, wherein in the step 3, the cooling is performed by natural cooling in air.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114252466A (en) * | 2021-12-16 | 2022-03-29 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method of solid solubility in alloy crystal and comparison method of alloying element content in alloy |
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2020
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| US4401621A (en) * | 1981-03-25 | 1983-08-30 | Magnesium Elektron Limited | Magnesium alloys |
| CN101760710A (en) * | 2008-12-24 | 2010-06-30 | 中国科学院金属研究所 | Preparation method of fine crystalline superplastic heat-resistance magnesium alloy |
| CN103667755A (en) * | 2012-09-21 | 2014-03-26 | 上海航天精密机械研究所 | Rare earth-magnesium alloy smelting and purifying method |
| CN110923534A (en) * | 2019-11-13 | 2020-03-27 | 上海航天精密机械研究所 | Magnesium alloy with special extrusion bar texture and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114252466A (en) * | 2021-12-16 | 2022-03-29 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method of solid solubility in alloy crystal and comparison method of alloying element content in alloy |
| CN114252466B (en) * | 2021-12-16 | 2024-01-12 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method and comparison method for intra-crystal solid solubility of alloy |
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Application publication date: 20201208 |