CN108707847B - Aging heat treatment process for low-rare earth nano heterogeneous magnesium alloy - Google Patents

Aging heat treatment process for low-rare earth nano heterogeneous magnesium alloy Download PDF

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CN108707847B
CN108707847B CN201810740418.4A CN201810740418A CN108707847B CN 108707847 B CN108707847 B CN 108707847B CN 201810740418 A CN201810740418 A CN 201810740418A CN 108707847 B CN108707847 B CN 108707847B
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magnesium alloy
nano heterogeneous
aging
treatment
rare earth
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CN108707847A (en
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万迎春
刘楚明
高永浩
蒋树农
余世伦
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Hunan Mayu Technology Co.,Ltd.
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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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention relates to an aging heat treatment process for a low rare earth nano heterogeneous magnesium alloy. The magnesium alloy comprises the following components in atomic percentage: mg-0.91-1.36 Gd-0.87-1.29Y-0.06-0.14 Zr, performing rotary swaging deformation on an extrusion bar, controlling the rotary swaging temperature to be 50-200 ℃, the pass deformation to be 10-20%, the total deformation to be 5-50%, and the feeding speed to be 2-4 mm/min to prepare the nano heterogeneous magnesium alloy, performing primary aging treatment on the obtained nano heterogeneous magnesium alloy at 100-130 ℃, wherein the treatment time is 5-20 h, performing secondary aging treatment on the alloy subjected to the primary aging treatment at 130-175 ℃, wherein the treatment time is 10-40 h, and the nano heterogeneous magnesium alloy subjected to the aging treatment is improved by 80-120 MPa in tensile strength compared with the unaged state and is improved by 80-120 MPa in yield strength.

Description

Aging heat treatment process for low-rare earth nano heterogeneous magnesium alloy
Technical Field
The invention relates to the field of nano metal material processing, in particular to an aging heat treatment process for a nano heterogeneous magnesium alloy.
Background
The nano-structure material has excellent physical property, chemical property and mechanical property, and has wide application prospect. However, the nano-structure material has low plasticity and is difficult to prepare, which seriously hinders the research and application process. Compared with the nano-structure material, the nano-heterogeneous material has the advantages of higher plasticity, easier preparation and the like, and has extremely high application and research values.
The magnesium alloy has the advantages of low density, high specific strength, high specific stiffness, high damping and the like, and has important significance for the fields of aerospace, transportation and the like due to the excellent weight reduction characteristic of the magnesium alloy as a new-generation light structural material. However, the existing magnesium alloy has low mechanical properties and is difficult to meet the requirements of the fields of aerospace and the like on high-performance materials. The preparation of the nano heterogeneous magnesium alloy and the research on the time-effect heat treatment process of the nano heterogeneous magnesium alloy have important significance for preparing high-strength and even ultrahigh-strength magnesium alloys.
Disclosure of Invention
The invention aims to provide an aging heat treatment process for a low-rare earth nano heterogeneous magnesium alloy, which comprises the following components in atomic percentage: mg-0.91-1.36 Gd-0.87-1.29Y-0.06-0.14 Zr, comprising the following steps:
a. carrying out rotary swaging deformation on the extruded bar, controlling the rotary swaging temperature to be 50-200 ℃, controlling the pass deformation to be 10-20%, controlling the total deformation to be 5-50%, and controlling the feeding speed to be 2-4 mm/min to prepare the nano heterogeneous magnesium alloy;
b. carrying out primary aging treatment on the nano heterogeneous magnesium alloy prepared by rotary swaging deformation at the temperature of 100-130 ℃, wherein the treatment time is 5-20 h;
c. and carrying out secondary aging treatment on the alloy subjected to primary aging at 130-175 ℃, wherein the treatment time is 10-40 h.
The nanometer heterogeneous magnesium alloy is prepared by rotary swaging deformation.
The primary aging treatment is to treat the nano heterogeneous magnesium alloy prepared by rotary swaging deformation for 10-15 hours at 110-130 ℃.
And the secondary aging treatment is to treat the alloy subjected to the primary aging treatment at 130-160 ℃ for 10-40 h.
The aging heat treatment difficulty of the low rare earth nanometer isomeric magnesium alloy related by the invention is that the nanometer isomeric magnesium alloy has unevenness in several aspects:
1. the grain size is not uniform, and the grain size of the nano heterogeneous magnesium alloy prepared by the rotary swaging method is not uniform;
2. the internal stress is distributed unevenly, the stress in the nanocrystalline area where recrystallization has occurred is smaller, and the internal stress in the ultrafine grain area where recrystallization has not occurred is very large;
3. the micro-region has uneven components, and the deformed nano heterogeneous magnesium alloy has uneven components in the micro-region within the range of dozens of nanometers due to the segregation of crystal boundary atoms and the formed intra-crystal atom clusters during the rotary swaging process.
The inhomogeneous structure and composition of the nano-isomeric magnesium alloy determine that the nano-isomeric magnesium alloy is easy to have the following problems in the aging heat treatment process:
1. in the nano heterogeneous magnesium alloy, the thermal stability of regions with different crystal grain sizes is different, and the smaller the crystal grain is, the worse the thermal stability is. The grain growth must not happen in the aging treatment process, so the highest aging temperature bearable by the nano-crystalline area and the ultra-fine crystalline area is different;
2. compared with a rare earth element depletion region, the rare earth element enrichment region is easier to generate desolventization of the rare earth element, so that the aging decomposition behaviors of the two regions are asynchronous;
3. the rare earth enrichment zone has higher second phase nucleation and growth power, and is easy to form a coarse massive stable phase which can severely reduce the mechanical property of the alloy;
4. the internal stress has the function of inducing nucleation and growth of the second phase, and compared with the low stress area, the high stress area has higher nucleation and growth power of the second phase, so that a coarse block stable phase is easily formed in the high stress area, and the mechanical property of the alloy is severely reduced due to the formation of the block stable phase.
The invention has the advantages that:
1. the invention provides a two-stage aging heat treatment process. During the first stage aging process, most internal stress generated by rotary swaging deformation is eliminated, and the generation of coarse massive stable phases is easily caused by the excessive internal stress, so that the first stage aging is indispensable. In order to ensure that crystal grains do not grow in the aging process, the first-stage aging temperature should be as low as possible, but the internal stress cannot be eliminated easily at too low temperature, the method combines theoretical analysis and a large number of tests, finally verifies that the temperature of 100-130 ℃ is the optimal first-stage aging treatment temperature of the nano heterogeneous magnesium alloy, and explores the appropriate aging treatment time of 5-20 h, so that most of the internal stress can be eliminated, and the crystal grains do not grow.
2. In the second stage of aging treatment, solid solution decomposition, second phase nucleation and growth mainly occur. If the aging temperature is too high and the aging time is too long, massive rare earth-rich phases are easily generated, but if the aging temperature is too low and the aging time is too short, the aging strengthening effect cannot be achieved. The method combines theoretical analysis and a large number of tests, finally determines that the aging is carried out for 10-40 h at 130-175 ℃, can ensure that a nanocrystalline area and an ultra-fine crystalline area reach a peak aging state, and does not generate a coarse blocky stable phase.
Detailed Description
Example 1
The magnesium alloy comprises the following components in atomic percentage: mg-1.36Gd-1.03Y-0.13Zr, and the extrusion bar is subject to rotary swaging deformation at 100 ℃, the pass deformation is controlled to be 15 percent, 15 percent and 10 percent, the total deformation is controlled to be 35 percent, the feeding speed is controlled to be 3mm/min, and the nano isomeric magnesium alloy is prepared.
And carrying out primary aging treatment on the obtained nano heterogeneous magnesium alloy at 130 ℃ for 15h, and then carrying out secondary aging treatment at 175 ℃ for 20 h. According to GB/T228-2002, mechanical property test is carried out on the aged alloy, and the aged alloy is compared with the alloy before aging, and the result shows that compared with the non-aged nano heterogeneous magnesium alloy, the aged alloy has the tensile strength improved by 85MPa and the yield strength improved by 100 MPa.
Example 2
The magnesium alloy comprises the following components in atomic percentage: mg-1.36Gd-1.03Y-0.13Zr, and the extrusion bar is subject to rotary swaging deformation at 100 ℃, the pass deformation is controlled to be 15 percent, 10 percent and 10 percent, the total deformation is 31 percent, the feeding speed is controlled to be 3mm/min, and the nano isomeric magnesium alloy is prepared.
And carrying out primary aging treatment on the obtained nano heterogeneous magnesium alloy at 110 ℃ for 15h, and then carrying out secondary aging treatment at 150 ℃ for 40 h. According to GB/T228-2002, mechanical property test is carried out on the aged magnesium alloy, and the aged magnesium alloy is compared with the alloy before aging, and the result shows that compared with the non-aged nano heterogeneous magnesium alloy, the aged magnesium alloy has the advantages that the tensile strength is improved by 90MPa, and the yield strength is improved by 110 MPa.
Example 3
The magnesium alloy comprises the following components in atomic percentage: mg-1.09Gd-0.69Y-0.14Zr, performing rotary swaging deformation on the extrusion bar at 200 ℃, controlling the pass deformation of 15 percent, 15 percent and the total deformation of 48 percent, and controlling the feeding speed of 2mm/min to prepare the nano isomeric magnesium alloy.
And carrying out primary aging treatment on the obtained nano heterogeneous magnesium alloy at 130 ℃ for 10h, and then carrying out secondary aging treatment at 175 ℃ for 25 h. The mechanical property of the aged magnesium alloy is tested according to GB/T228-2002 and compared with the alloy before aging, and the result shows that compared with the non-aged nano heterogeneous magnesium alloy, the tensile strength of the aged alloy is improved by 100MPa, and the yield strength of the aged alloy is improved by 115 MPa.

Claims (3)

1. An aging heat treatment process for a low-rare earth nano heterogeneous magnesium alloy, which comprises the following components in percentage by atom of the magnesium alloy, Mg-0.91-1.36 Gd-0.87-1.29Y-0.06-0.14 Zr, and is characterized by comprising the following steps: the method comprises the steps of carrying out rotary swaging deformation on an extrusion bar, controlling rotary swaging temperature to be 50-200 ℃, controlling pass deformation to be 10-20%, controlling total deformation to be 5-50%, controlling feeding speed to be 2-4 mm/min, preparing a nano heterogeneous magnesium alloy, carrying out primary aging treatment on the obtained nano heterogeneous magnesium alloy at 100-130 ℃, wherein the treatment time is 10-20 h, and carrying out secondary aging treatment on the alloy subjected to primary aging treatment at 130-175 ℃, wherein the treatment time is 25-40 h.
2. The aging heat treatment process of the low rare earth nano heterogeneous magnesium alloy according to claim 1, characterized in that: the primary aging treatment is to treat the nano heterogeneous magnesium alloy prepared by rotary swaging deformation for 10-15 hours at 110-130 ℃.
3. The aging heat treatment process of the low rare earth nano heterogeneous magnesium alloy according to claim 1, characterized in that: and the secondary aging treatment is to treat the alloy subjected to the primary aging treatment at 130-160 ℃ for 25-40 h.
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