CN111560550A - Homogenization heat treatment method for Mg-Gd-Y rare earth magnesium alloy ingot - Google Patents

Homogenization heat treatment method for Mg-Gd-Y rare earth magnesium alloy ingot Download PDF

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CN111560550A
CN111560550A CN202010452735.3A CN202010452735A CN111560550A CN 111560550 A CN111560550 A CN 111560550A CN 202010452735 A CN202010452735 A CN 202010452735A CN 111560550 A CN111560550 A CN 111560550A
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magnesium alloy
heat treatment
rare earth
earth magnesium
alloy ingot
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黄元春
雒晓宇
刘良春
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention discloses a homogenization heat treatment method of an Mg-Gd-Y rare earth magnesium alloy ingot, and particularly relates to the technical field of magnesium alloy material preparation, wherein the homogenization heat treatment process comprises the following steps: and (3) placing the magnesium alloy ingot in a homogenizing heat treatment furnace, heating to the temperature of 520-525 ℃, preserving the heat for at least 10-12h, performing air cooling at the speed of 60-80 ℃/h, and then cooling to the room temperature to obtain a finished product. The invention adopts a reasonable homogenization annealing system, thereby achieving the purposes of eliminating component segregation and eliminating internal stress of the Mg-Gd-Y rare earth magnesium alloy, and particularly effectively storing the growth of a strengthening phase LPSO phase in the Mg-Gd-Y alloy in a matrix and crystal grains, thereby effectively improving the alloy strength and the heat resistance, providing preparation for the subsequent plastic forming processing technology, and the technology is suitable for rare earth magnesium alloy castings with various sizes and improving the performance of rare earth magnesium alloy casting materials for aerospace and rail traffic.

Description

Homogenization heat treatment method for Mg-Gd-Y rare earth magnesium alloy ingot
Technical Field
The invention relates to the technical field of magnesium alloy material preparation, in particular to a heat treatment method for eliminating component segregation of Mg-Gd-Y rare earth magnesium alloy, eliminating casting stress, promoting the growth of a special strengthening phase LPSO phase and improving the uniformity and mechanical property of a structure.
Background
The magnesium alloy is a novel light alloy with light weight, high strength, high specific stiffness and specific strength, has the advantages of good electric conduction and heat conduction performance, good electromagnetic shielding performance, good damping and shock absorption effects, easy cutting and the like, is applied to the fields of aerospace, military industry, rail transit, automobiles and the like more and more widely at present, but the traditional deformed magnesium alloy can generate composition segregation and casting stress in the casting process, which can bring the problems of difficult deformation, easy cracking and the like to further plastic forming and processing of cast ingots, so that the homogenization heat treatment of the cast ingots with reasonable process is necessary before plastic deformation.
Due to the special physical and chemical characteristics of the rare earth elements, the addition of the rare earth elements in the magnesium alloy can generate a high-melting-point second phase or be dissolved in the magnesium alloy matrix in a solid solution manner, and the effects of grain refinement and second phase reinforcement are achieved, so that the magnesium alloy has good effects of improving the comprehensive mechanical property and the heat resistance. However, the addition of high rare earth elements causes large casting stress during casting. However, the traditional homogenization method for other rare earth element magnesium alloys cannot be applied to the Mg-Gd-Y rare earth magnesium alloy, and particularly, the special LPSO phase second phase strengthening effect is influenced, so that the advantages of the Mg-Gd-Y rare earth magnesium alloy cannot be fully exerted.
Disclosure of Invention
In view of the above, in order to solve the problems in the prior art, an object of the present invention is to improve the defects of the conventional magnesium alloy homogenization heat treatment method, and an embodiment of the present invention provides a Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method, which adopts a reasonable homogenization annealing schedule, i.e., 520 ℃ ×. 10-12h, to achieve the purposes of eliminating component segregation and internal stress of the Mg-Gd-Y rare earth magnesium alloy, and in particular, effectively storing the growth of a reinforcement LPSO phase in the Mg-Gd-Y alloy in a matrix and grains, thereby achieving the purposes of improving the comprehensive mechanical properties and preparing for further forming and processing, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method specifically comprises the following operation steps:
the method comprises the following steps: according to the set component requirement of the magnesium alloy, adding pure metal and intermediate metal containing different elements into a smelting furnace, starting a resistance heating device of the smelting furnace, and preserving heat until alloy components are melted into uniform metal melt with set components for casting;
step two: heating and preheating the heat treatment furnace;
step three: casting and molding the metal melt in the step one into a magnesium alloy blank, rapidly cooling, and then rapidly transferring into a preheated heat treatment furnace;
step four: carrying out heat preservation treatment on the magnesium alloy blank transferred into the preheated heat treatment furnace;
step five: after completion, the heat-treated magnesium alloy ingot was taken out and cooled to room temperature.
In a preferred embodiment, after the pure metal containing different elements and the intermediate metal are added into the smelting furnace in the step one, the components are melted into a uniform metal melt by heating to 760 ℃.
In a preferred embodiment, the heat treatment furnace in the second step is preheated to 500-520 ℃ at a heating rate of 100 ℃/h.
In a preferred embodiment, the cooling operation described in step three is a rapid cooling to 200 ℃ by means of forced air cooling.
In a preferred embodiment, the heat-preservation treatment operation in the fourth step is heat preservation in a heat treatment furnace at the temperature of 520 ℃ and 525 ℃ for 10-12 h.
In a preferred embodiment, after the magnesium alloy blank in the fifth step is taken out, the magnesium alloy blank is subjected to blast cooling, and the cooling speed is controlled to be 60-80 ℃/h.
The invention also provides an Mg-Gd-Y rare earth magnesium alloy ingot, the tensile strength at room temperature is more than or equal to 245MPa, and the elongation is more than or equal to 7%.
In a preferred embodiment, the Mg-Gd-Y rare earth magnesium alloy has a composition in mass percent of Gd: 8-11%, Y: 2-4%, Zn: 1-3%, Zr: 0.2-0.6%, and the balance of Mg and non-removable impurity elements.
The invention has the technical effects and advantages that:
1. the homogenization heat treatment method of the rare earth magnesium alloy provided by the invention can adopt a reasonable homogenization annealing system, namely, the temperature is increased by 525 ℃ for 10-12h aiming at the cast ingot of the Mg-Gd-Y rare earth magnesium alloy, thereby achieving the purposes of eliminating component segregation and internal stress of the Mg-Gd-Y rare earth magnesium alloy, particularly effectively storing the growth of a strengthening phase LPSO phase in the Mg-Gd-Y alloy in a matrix and crystal grains, and further achieving the purposes of improving comprehensive mechanical properties and preparing for further forming and processing;
2. the invention not only puts forward requirements for the homogenization heat treatment process, but also gives clear instructions for the temperature rise and the temperature drop rate in the heat treatment process, because not only are temperature and time process parameters in the homogenization process, but also the temperature gradients of heating and air cooling have obvious influence on the homogenized microstructure and the ingot casting performance, the invention also gives accurate requirements for the two process parameters, thereby further ensuring the homogenized effect and finally improving the product quality;
3. the method has simple and clear process and accurate requirement, is suitable for factory mass production under the engineering condition, simultaneously has shorter heating time for Mg-Gd-Y alloy compared with the traditional rare earth magnesium alloy homogenization treatment method, can greatly and effectively save electric energy and production cost for mass production enterprises, and has very important significance for improving the economic benefit of the enterprises and optimizing the product structure.
Drawings
FIG. 1 is a schematic diagram showing the size and distribution of the as-cast second phase after the homogenization heat treatment by the method of the present invention.
FIG. 2 is a schematic representation of the size and distribution of the as-cast second phase prior to the homogenization heat treatment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a homogenizing heat treatment method for an Mg-Gd-Y rare earth magnesium alloy ingot, which specifically comprises the following operation steps:
the method comprises the following steps: adding pure metals and intermediate metals containing different elements into a smelting furnace according to the set component requirements of the magnesium alloy, starting a resistance heating device of the smelting furnace to heat to 760 ℃, melting all components into uniform metal melt, and preserving heat until the alloy components are melted into uniform metal melt with set components to cast;
step two: preheating the heat treatment furnace to 500-520 ℃ at the heating rate of 100 ℃/h;
step three: casting and molding the metal melt in the step one into a magnesium alloy blank, rapidly cooling to 200 ℃ in a blast cooling mode, and then rapidly transferring to a preheated heat treatment furnace;
step four: preserving the heat of the magnesium alloy blank transferred into the preheated heat treatment furnace in the heat treatment furnace at the temperature lower than 520 ℃, wherein the heat preservation time is less than 10 hours;
step five: and after the completion, taking out the magnesium alloy blank subjected to the heat treatment, carrying out air blast cooling, cooling at the cooling rate of 60-80 ℃/h, and cooling to room temperature.
The invention also provides an Mg-Gd-Y rare earth magnesium alloy ingot, the tensile strength at room temperature is more than or equal to 245MPa, the elongation is more than or equal to 7 percent, and the Mg-Gd-Y rare earth magnesium alloy comprises the following components in percentage by mass: 8-11%, Y: 2-4%, Zn: 1-3%, Zr: 0.2-0.6%, and the balance of Mg and non-removable impurity elements.
Example 2:
the invention provides a homogenizing heat treatment method for an Mg-Gd-Y rare earth magnesium alloy ingot, which specifically comprises the following operation steps:
the method comprises the following steps: adding pure metals and intermediate metals containing different elements into a smelting furnace according to the set component requirements of the magnesium alloy, starting a resistance heating device of the smelting furnace to heat to 760 ℃, melting all components into uniform metal melt, and preserving heat until the alloy components are melted into uniform metal melt with set components to cast;
step two: preheating the heat treatment furnace to 500-520 ℃ at the heating rate of 100 ℃/h;
step three: casting and molding the metal melt in the step one into a magnesium alloy blank, rapidly cooling to 200 ℃ in a blast cooling mode, and then rapidly transferring to a preheated heat treatment furnace;
step four: preserving the heat of the magnesium alloy blank transferred into the preheated heat treatment furnace for 10-12h in the heat treatment furnace at the temperature of 520-525 ℃;
step five: and after the completion, taking out the magnesium alloy blank subjected to the heat treatment, carrying out air blast cooling, cooling at the cooling rate of 60-80 ℃/h, and cooling to room temperature.
The invention also provides an Mg-Gd-Y rare earth magnesium alloy ingot, the tensile strength at room temperature is more than or equal to 245MPa, the elongation is more than or equal to 7 percent, and the Mg-Gd-Y rare earth magnesium alloy comprises the following components in percentage by mass: 8-11%, Y: 2-4%, Zn: 1-3%, Zr: 0.2-0.6%, and the balance of Mg and non-removable impurity elements.
Example 3:
the invention provides a homogenizing heat treatment method for an Mg-Gd-Y rare earth magnesium alloy ingot, which specifically comprises the following operation steps:
the method comprises the following steps: adding pure metals and intermediate metals containing different elements into a smelting furnace according to the set component requirements of the magnesium alloy, starting a resistance heating device of the smelting furnace to heat to 760 ℃, melting all components into uniform metal melt, and preserving heat until the alloy components are melted into uniform metal melt with set components to cast;
step two: preheating the heat treatment furnace to 500-520 ℃ at the heating rate of 100 ℃/h;
step three: casting and molding the metal melt in the step one into a magnesium alloy blank, rapidly cooling to 200 ℃ in a blast cooling mode, and then rapidly transferring to a preheated heat treatment furnace;
step four: preserving the heat of the magnesium alloy blank transferred into the preheated heat treatment furnace in the heat treatment furnace at the temperature of more than 525 ℃, wherein the heat preservation time is more than 12 hours;
step five: and after the completion, taking out the magnesium alloy blank subjected to the heat treatment, carrying out air blast cooling, cooling at the cooling rate of 60-80 ℃/h, and cooling to room temperature.
The invention also provides an Mg-Gd-Y rare earth magnesium alloy ingot, the tensile strength at room temperature is more than or equal to 245MPa, the elongation is more than or equal to 7 percent, and the Mg-Gd-Y rare earth magnesium alloy comprises the following components in percentage by mass: 8-11%, Y: 2-4%, Zn: 1-3%, Zr: 0.2-0.6%, and the balance of Mg and non-removable impurity elements.
The second-phase LPSO phase strengthening phase specific to the Mg-Gd-Y rare earth magnesium alloy ingot prepared in the example 1-3 is observed by metallographic observation and a scanning electron microscope SEM, and the observation result is as follows:
Figure BDA0002508228630000061
the mechanical properties and elongation of the Mg-Gd-Y rare earth magnesium alloy ingots prepared in examples 1 to 3 and the original ingots were determined, it was found that the Mg-Gd-Y rare earth magnesium alloy ingots prepared by the method of the present invention can eliminate component segregation and casting stress, promote growth of a specific strengthening phase LPSO phase, improve structural uniformity and mechanical properties, and at the same time, the size and distribution of the second phase of the Mg-Gd-Y rare earth magnesium alloy ingots prepared by the present invention and the original ingots and the size and distribution of the second phase before the homogenization heat treatment were observed by metallographic observation and scanning electron microscope SEM, and the accompanying drawings 1 and 2 of the description can be obtained, and it can be clearly observed by combining the accompanying drawings 1 and 2 of the description, that the brittle as-cast eutectic second phase in the original ingots almost decreased and disappeared, and the special second-phase LPSO phase strengthening phase in the Mg-Gd-Y series alloy is converted, grows into the crystal to a certain extent, and effectively achieves the effects of strengthening the alloy and improving the comprehensive mechanical property.
The implementation mode is specifically as follows: adding pure magnesium, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, pure zinc and pure zirconium into a smelting furnace according to the component requirements of a magnesium alloy product, sequentially adding the pure magnesium, the Mg-Gd intermediate alloy, the Mg-Y intermediate alloy, the pure zinc and the pure zirconium into the smelting furnace, starting a resistance heating device of the smelting furnace, heating to 760 ℃ to melt alloy components into a uniform Mg-Gd-Y-Zn-Zr intermediate magnesium alloy metal melt, preserving heat, removing slag, standing for 30min, casting into an ingot, heating the homogenizing heat treatment furnace to 500 ℃ at 100 ℃/h, carrying out blast cooling on the ingot to about 200 ℃, rapidly transferring into the preheating homogenizing heat treatment furnace, carrying out homogenizing heat treatment at 525 ℃ at 520 ℃ for 10-12h, taking out, carrying out blast cooling, cooling the ingot to room temperature at a cooling rate of 60-80 ℃/h, sawing an ingot sample, after being ground and polished by 2000-mesh metallographic abrasive paper, the alloy is corroded by 4% picric acid solution, and then is observed by metallographic observation and a scanning electron microscope SEM, the observation results are shown in figures 1 and 2, and comparison shows that the Mg-Gd-Y alloy treated by the homogenization heat treatment method provided by the invention is obviously reduced compared with an as-cast brittle second phase, an LPSO phase is fully generated, meanwhile, the mechanical property of the as-cast Mg-Gd-Y alloy ingot is 191MPa, the elongation is 5.4%, and the mechanical property of the ingot after homogenization heat treatment is 247MPa, the elongation is 7.7%, so that the effect of homogenizing and improving the comprehensive mechanical property of the ingot is realized.
Finally, it should be noted that: the previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (8)

1. A Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method is characterized in that: the method specifically comprises the following operation steps:
the method comprises the following steps: according to the set component requirement of the magnesium alloy, adding pure metal and intermediate metal containing different elements into a smelting furnace, starting a resistance heating device of the smelting furnace, and preserving heat until alloy components are melted into uniform metal melt with set components for casting;
step two: heating and preheating the heat treatment furnace;
step three: casting and molding the metal melt in the step one into a magnesium alloy blank, rapidly cooling, and then rapidly transferring into a preheated heat treatment furnace;
step four: carrying out heat preservation treatment on the magnesium alloy blank transferred into the preheated heat treatment furnace;
step five: after completion, the heat-treated magnesium alloy ingot was taken out and cooled to room temperature.
2. The Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method according to claim 1, characterized in that: and (2) adding pure metal and intermediate metal containing different elements into the smelting furnace in the step one, and heating to 760 ℃ to melt all the components into uniform metal melt.
3. The Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method according to claim 1, characterized in that: in the second step, the heat treatment furnace is preheated to 500-520 ℃ at a heating rate of 100 ℃/h.
4. The Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method according to claim 1, characterized in that: the cooling operation described in step three was carried out by rapidly cooling to 200 ℃ by means of forced air cooling.
5. The Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method according to claim 1, characterized in that: the heat preservation treatment operation in the fourth step is to preserve heat for 10-12h in a heat treatment furnace with the temperature of 520-525 ℃.
6. The Mg-Gd-Y rare earth magnesium alloy ingot homogenization heat treatment method according to claim 1, characterized in that: and taking out the magnesium alloy blank in the fifth step, and carrying out blast cooling, wherein the cooling speed is controlled to be 60-80 ℃/h.
7. An Mg-Gd-Y rare earth magnesium alloy ingot is characterized in that: the tensile strength at room temperature is more than or equal to 245MPa, and the elongation is more than or equal to 7 percent.
8. The Mg-Gd-Y rare earth magnesium alloy ingot according to claim 7, wherein: the Mg-Gd-Y rare earth magnesium alloy comprises the following components in percentage by mass: 8-11%, Y: 2-4%, Zn: 1-3%, Zr: 0.2-0.6%, and the balance of Mg and non-removable impurity elements.
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CN112251621A (en) * 2020-09-28 2021-01-22 湖南大学 Hydrogenation heat treatment method for improving corrosion resistance of LPSO (Long period molten oxide) enhanced magnesium alloy and alloy
CN113373329A (en) * 2021-05-17 2021-09-10 华北理工大学 Preparation method of nano gradient magnesium alloy
CN113444946A (en) * 2021-05-17 2021-09-28 中北大学 High-strength and high-toughness rare earth magnesium alloy and treatment method thereof
CN115233010A (en) * 2022-06-24 2022-10-25 重庆大学 Method for efficiently preparing high-strength magnesium alloy
CN115261694A (en) * 2022-04-20 2022-11-01 上海交通大学 Rare earth magnesium alloy suitable for electric arc additive manufacturing
CN115786828A (en) * 2022-11-09 2023-03-14 上海交通大学 Interlayer spacing regulation and control method and induced recrystallization method for magnesium alloy layer sheet-shaped LPSO structure

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112251621A (en) * 2020-09-28 2021-01-22 湖南大学 Hydrogenation heat treatment method for improving corrosion resistance of LPSO (Long period molten oxide) enhanced magnesium alloy and alloy
CN113373329A (en) * 2021-05-17 2021-09-10 华北理工大学 Preparation method of nano gradient magnesium alloy
CN113444946A (en) * 2021-05-17 2021-09-28 中北大学 High-strength and high-toughness rare earth magnesium alloy and treatment method thereof
CN113444946B (en) * 2021-05-17 2022-02-11 中北大学 High-strength and high-toughness rare earth magnesium alloy and treatment method thereof
CN115261694A (en) * 2022-04-20 2022-11-01 上海交通大学 Rare earth magnesium alloy suitable for electric arc additive manufacturing
CN115233010A (en) * 2022-06-24 2022-10-25 重庆大学 Method for efficiently preparing high-strength magnesium alloy
CN115786828A (en) * 2022-11-09 2023-03-14 上海交通大学 Interlayer spacing regulation and control method and induced recrystallization method for magnesium alloy layer sheet-shaped LPSO structure
CN115786828B (en) * 2022-11-09 2023-11-28 上海交通大学 Interlayer spacing regulating and controlling method and induced recrystallization method for sheet LPSO structure of magnesium alloy layer

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Application publication date: 20200821