CN114075637A - Mg-Mn-Er series wrought magnesium alloy and preparation method thereof - Google Patents

Mg-Mn-Er series wrought magnesium alloy and preparation method thereof Download PDF

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Publication number
CN114075637A
CN114075637A CN202111372813.XA CN202111372813A CN114075637A CN 114075637 A CN114075637 A CN 114075637A CN 202111372813 A CN202111372813 A CN 202111372813A CN 114075637 A CN114075637 A CN 114075637A
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magnesium
alloy
magnesium alloy
ingot
wrought
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潘复生
周世博
刘婷婷
汤爱涛
盛光敏
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Chongqing University
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Chongqing 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

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  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a Mg-Mn-Er wrought magnesium alloy and a preparation method thereof, wherein the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.3-1.5% of Mn, 1-3% of Er, and the balance of Mg and inevitable impurities. The preparation method comprises the following steps: s1, preparing raw materials, and weighing a pure magnesium ingot, a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy according to the component proportion of the Mg-Mn-Er series wrought magnesium alloy; s2, smelting, namely melting a pure magnesium ingot to obtain a magnesium melt, adding a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy into the magnesium melt, melting the magnesium-manganese intermediate alloy and the magnesium-erbium intermediate alloy, and cooling to obtain a magnesium alloy ingot; s3, carrying out solution treatment on the magnesium alloy ingot for 12-36 h at the temperature of 400-560 ℃, and cooling the magnesium alloy ingot to room temperature by water; s4, performing hot extrusion on the magnesium alloy ingot at the temperature of 250-350 ℃ to obtain a magnesium alloy rod, and obtaining the Mg-Mn-Er series wrought magnesium alloy. The preparation method has the advantages of high strength and plasticity, simple process flow, low requirement on equipment and suitability for large-scale industrial production.

Description

Mg-Mn-Er series wrought magnesium alloy and preparation method thereof
Technical Field
The invention relates to the technical field of magnesium alloy materials, in particular to an Mg-Mn-Er series wrought magnesium alloy and a preparation method thereof.
Background
Magnesium alloy is the lightest structural material of practical metals, 2/3 for aluminum and 1/4 for iron. In addition, the magnesium alloy has excellent performances of strong shock resistance, excellent wear resistance and thermal conductivity, easy recovery of waste materials and the like, and has been widely applied to the aerospace industry, the automobile industry, the electronic industry, the instrument industry and the like. The magnesium alloy can be divided into cast magnesium alloy and wrought magnesium alloy, compared with the cast magnesium alloy, the wrought magnesium alloy eliminates a series of casting defects such as macrosegregation, air holes and the like after deformation treatment, and has more excellent mechanical properties, so that the wrought magnesium alloy has more development potential than the cast magnesium alloy on a structural stress member.
Most magnesium alloys have a close-packed hexagonal structure, the magnesium alloys are subjected to extrusion or rolling treatment to form a typical basal plane texture, the mechanical properties of the magnesium alloys are obviously represented by tensile-compression yield asymmetry, and the tensile-compression yield asymmetry of the wrought magnesium alloys greatly limits the application range of the wrought magnesium alloys, so that the further improvement of the mechanical properties of the magnesium alloys and the improvement of the tensile-compression yield asymmetry of the magnesium alloys are always important research directions of magnesium alloy scientific research workers. According to the introduction of related documents, the refining of the crystal grains of the magnesium alloy can not only improve the strength and the plasticity of the magnesium alloy, but also improve the tension-compression yield asymmetry of the magnesium alloy.
The magnesium alloy with good performance can be prepared by large plastic deformation of the magnesium alloy, such as equal channel angular extrusion, high-pressure torsion and the like, but the requirement on equipment is high, and in addition, the magnesium alloy extruded at the equal channel angular has strong texture, is difficult to be twisted at high pressure, and is difficult to prepare a large sample. In the conventional extrusion, the finer grains can be obtained by reducing the extrusion temperature, but the magnesium alloy with the lower temperature has poor plastic deformation capability, and the deformation treatment is usually difficult due to the effects of precipitation and other factors. Therefore, an experimental method which has low requirements on equipment and is simple and easy to operate and a method for preparing the wrought magnesium alloy with good comprehensive performance are urgently needed.
Disclosure of Invention
The invention aims to provide a Mg-Mn-Er wrought magnesium alloy and a preparation method thereof, wherein the Mg-Mn-Er wrought magnesium alloy has high strength and plasticity, and the preparation method has the advantages of simple process flow, low requirement on equipment and suitability for large-scale industrial production.
The Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.3-1.5% of Mn, 1-3% of Er, and the balance of Mg and inevitable impurities.
Further, the paint comprises the following components in percentage by weight: 0.3-0.9% of Mn, 1-2% of Er, and the balance of Mg and inevitable impurities.
A preparation method of Mg-Mn-Er wrought magnesium alloy comprises the following steps:
s1, preparing raw materials, weighing a pure magnesium ingot, a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy according to the component proportion of the Mg-Mn-Er series wrought magnesium alloy in claim 1 or 2;
s2, smelting, namely melting a pure magnesium ingot to obtain a magnesium melt, adding a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy into the magnesium melt, melting the magnesium-manganese intermediate alloy and the magnesium-erbium intermediate alloy to obtain a magnesium alloy melt, and cooling to obtain a magnesium alloy ingot;
s3, carrying out solution treatment on the magnesium alloy ingot for 12-36 h at the temperature of 400-560 ℃, and cooling the magnesium alloy ingot to room temperature by water;
s4, performing hot extrusion on the magnesium alloy ingot at the temperature of 250-350 ℃ to obtain a magnesium alloy rod, and obtaining the Mg-Mn-Er series wrought magnesium alloy.
Further, the extrusion ratio of the hot extrusion in S4 is 10: 1-80: 1, the extrusion speed is 0.5-3 m/min.
Further, the extrusion ratio of the hot extrusion in S4 is 15: 1-30: 1, the extrusion speed is 0.5-1.5 m/min.
Further, before the S4 is subjected to hot extrusion, the magnesium alloy ingot is preheated for 0.5-3 hours at the temperature of 200-300 ℃.
Further, the weight percentage of Mn in the magnesium-manganese intermediate alloy is 3%, and the weight percentage of Er in the magnesium-erbium intermediate alloy is 20%.
Further, the cooling of S2 specifically includes: the crucible containing the magnesium alloy melt was cooled in saturated brine at a temperature of 60 ℃.
Compared with the prior art, the invention has the following beneficial effects.
1. According to the invention, the contents of Mn element and Er element are reasonably limited, so that Mn and Er can be completely dissolved in Mg matrix in a solid manner, the ingot with the microstructure of single-phase magnesium is obtained, the solid solution strengthening and plasticizing effects of the Mn and Er elements are utilized, the phenomenon that the deformation of the alloy in the extrusion process is hindered by a second phase generated by excessive addition of the elements is avoided, and finally, the high-strength tough magnesium alloy with fine and uniform alloy microstructure and excellent mechanical property is obtained.
2. The content of Mn is limited to be controlled to be 0.3-1.5%, the content of impurity elements can be reduced, and Mn in the content can play a role in strengthening the alloy. The content of Er is controlled to be 1-3%, and the solid solution strengthening plasticizing effect is realized by matching two alloy elements. Through multiple solid solution strengthening, the strength of the alloy is improved, and meanwhile, the plasticity of the alloy can be synchronously improved.
3. The invention can improve the alloy structure, refine the crystal grains and obtain the high-strength and high-toughness magnesium alloy material while optimizing the yield asymmetry of the wrought magnesium alloy by optimizing the design of the alloy components and improving the deformation process. The preparation method is simple and easy to operate, has low requirements on equipment, is low in cost, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is an X-ray diffraction spectrum of a product obtained in examples one to three of the present invention and comparative example one;
FIG. 2 is a graph showing mechanical property curves of alloys according to examples one to three and comparative example one of the present invention;
FIG. 3 is a graph showing mechanical property curves of alloys according to the fourth to sixth embodiments of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
In one embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.3% of Mn, 2% of Er, and the balance of Mg and inevitable impurities. The preparation method of the magnesium alloy comprises the following steps.
S1, preparing raw materials, and weighing a pure magnesium ingot, a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy according to the component proportion of the Mg-Mn-Er series wrought magnesium alloy. The weight percentage of Mn in the magnesium-manganese intermediate alloy is 3%, and the weight percentage of Er in the magnesium-erbium intermediate alloy is 20%.
S2, smelting, preheating a pure magnesium ingot for 30min at the temperature of 300 ℃, and then preheating the pure magnesium ingot at the temperature of 720-750 ℃ in the presence of SF6And CO2The magnesium alloy melt is completely melted under the protection of the mixed gas to obtain a magnesium melt, after the temperature of the magnesium melt is raised to 720 ℃ and stabilized, a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate earphone are added into the completely melted magnesium melt, the mixture is fully stirred for 5min to be uniformly mixed, when the temperature is raised to 700-750 ℃, the temperature is kept for 10-30 min, and then scum on the surface is removed to obtain a pure magnesium alloy melt. And (3) cooling the obtained crucible containing the magnesium alloy melt in saturated saline water at 60 ℃ to obtain a magnesium alloy ingot. And cutting and turning the obtained magnesium alloy ingot to a proper size for later use.
And S3, coating the magnesium alloy ingot with graphite powder, performing solution treatment for 18 hours at the temperature of 400-560 ℃, taking out, and immediately cooling to room temperature by water.
S4, removing oxide skin on the surface of the magnesium alloy ingot, preheating the magnesium alloy ingot for 2.0 hours at the temperature of 350 ℃, then coating a magnesium alloy lubricant on the surface of the magnesium alloy ingot, and performing hot extrusion on the magnesium alloy ingot at the temperature of 350 ℃ by using an extrusion die to obtain a magnesium alloy rod. The extrusion ratio in the hot extrusion is 20: 1, extruding at the speed of 1.0m/min to obtain the Mg-Mn-Er wrought magnesium alloy.
In the second embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.6% of Mn, 2% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
In the third embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.9% of Mn, 2% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
In the fourth embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.3% of Mn, 1% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
In the fifth embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.6% of Mn, 1% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
In the sixth embodiment, the Mg-Mn-Er wrought magnesium alloy comprises the following components in percentage by weight: 0.9% of Mn, 1% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
Comparative example one: comprises the following components in percentage by weight: 2% of Er, and the balance of Mg and inevitable impurities. The preparation method is the same as the first embodiment.
The X-ray diffraction analysis was performed on the products obtained in examples one to three and comparative example, respectively, and the results are shown in fig. 1. By reasonably limiting the addition amount of Mn and Er, the Mn and Er are ensured to be completely dissolved in the magnesium matrix, and the obtained product is in a single-phase state.
The products of examples one to six and comparative example one were tested using a tensile specimen designed according to the GB/T228.1: 2010 standard at a tensile rate of 1.5mm/s, the results being shown in FIG. 2, FIG. 3 and Table 1.
TABLE 1 mechanical Property test results for different materials
Mg(%) Er(%) Mn(%) Tensile strength/(MPa) Yield strength/(MPa) Elongation/percent
Example one 97.7 2 0.3 201 134 35.34
Example two 97.4 2 0.6 211 155 35.15
EXAMPLE III 97.1 2 0.9 237 200 34.01
Example four 98.7 1 0.3 200 146 32.01
EXAMPLE five 98.4 1 0.6 227 192 25.57
EXAMPLE six 98.1 1 0.9 242 212 24.22
Comparative example 1 98 2 0 100 171 27.35
As can be seen from table 1, examples one to six all had higher strength and plasticity. Although the elongation of the comparative example I is slightly higher than that of the examples five and six, the tensile strength and yield strength are lower, and the application range is limited.
The tensile strength, yield strength and elongation of the Mg — Mn — Er system wrought magnesium alloys prepared in examples one through three all increased with increasing Mn content. Examples four to six the amount of Er used was reduced from 2% to 1%, and the elongation, i.e. plasticity, was reduced although the tensile strength and yield strength increased with increasing Mn content. In general, the mechanical properties of the Mg-Mn-Er wrought magnesium alloys of examples one to three increased with increasing Mn, and the ductility of the alloys was higher than those of examples four to six, so Mg-2Er-XMn was the most suitable alloy from the composition point of view. In addition, the magnesium alloy ingot with a single-phase microstructure is obtained by reasonably controlling the composition components and the use amount of each component of the magnesium alloy, the solid solution strengthening effect of various elements is utilized, the plasticity reduction caused by the generation of a second phase due to excessive addition of the elements is avoided, a small amount of precipitated phase Mn is precipitated in the extrusion process, the junction boundary is pinned, the growth of the junction boundary is hindered, so that smaller crystal grains are formed, on the other hand, the solid-dissolved atoms can hinder the dislocation movement, the dislocation accumulation and the entanglement are facilitated to form a high-angle grain boundary segmentation matrix, and finally, the high-strength ductile magnesium alloy with a fine and uniform microstructure is obtained. The method can well improve the strength of the magnesium alloy material and simultaneously maintain the higher elongation.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. The Mg-Mn-Er wrought magnesium alloy is characterized by comprising the following components in percentage by weight: 0.3-1.5% of Mn, 1-3% of Er, and the balance of Mg and inevitable impurities.
2. The Mg-Mn-Er wrought magnesium alloy according to claim 1, wherein: comprises the following components in percentage by weight: 0.3-0.9% of Mn, 2-3% of Er, and the balance of Mg and inevitable impurities.
3. A preparation method of Mg-Mn-Er wrought magnesium alloy is characterized by comprising the following steps:
s1, preparing raw materials, weighing a pure magnesium ingot, a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy according to the component proportion of the Mg-Mn-Er series wrought magnesium alloy in claim 1 or 2;
s2, smelting, namely melting a pure magnesium ingot to obtain a magnesium melt, adding a magnesium-manganese intermediate alloy and a magnesium-erbium intermediate alloy into the magnesium melt, melting the magnesium-manganese intermediate alloy and the magnesium-erbium intermediate alloy to obtain a magnesium alloy melt, and cooling to obtain a magnesium alloy ingot;
s3, carrying out solution treatment on the magnesium alloy ingot for 12-36 h at the temperature of 400-560 ℃, and cooling the magnesium alloy ingot to room temperature by water;
s4, performing hot extrusion on the magnesium alloy ingot at the temperature of 250-350 ℃ to obtain a magnesium alloy rod, and obtaining the Mg-Mn-Er series wrought magnesium alloy.
4. The method for producing a Mg-Mn-Er wrought magnesium alloy according to claim 3, wherein: the extrusion ratio of the hot extrusion in S4 was 10: 1-80: 1, the extrusion speed is 0.5-3 m/min.
5. The method for producing a Mg-Mn-Er wrought magnesium alloy according to claim 4, wherein: the extrusion ratio of the hot extrusion in S4 was 15: 1-30: 1, the extrusion speed is 0.5-1.5 m/min.
6. The method for producing a Mg-Mn-Er wrought magnesium alloy according to claim 3, wherein: and preheating the magnesium alloy ingot for 0.5-3 hours at the temperature of 200-300 ℃ before hot extrusion of S4.
7. The method for producing a Mg-Mn-Er wrought magnesium alloy according to claim 3, wherein: the weight percentage of Mn in the magnesium-manganese intermediate alloy is 3%, and the weight percentage of Er in the magnesium-erbium intermediate alloy is 20%.
8. The method for producing a Mg-Mn-Er wrought magnesium alloy according to claim 3, wherein: the cooling of the S2 is specifically: the crucible containing the magnesium alloy melt was cooled in saturated brine at a temperature of 60 ℃.
CN202111372813.XA 2021-11-18 2021-11-18 Mg-Mn-Er series wrought magnesium alloy and preparation method thereof Pending CN114075637A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101787473A (en) * 2010-03-22 2010-07-28 北京工业大学 Tough antiflaming magnesium alloy and preparation method thereof
JP2011042847A (en) * 2009-08-24 2011-03-03 Peter Stolfig Magnesium alloy
KR20130012662A (en) * 2011-07-26 2013-02-05 한국기계연구원 High-strength high-ductility ignition-proof magnesium alloy
CN103233152A (en) * 2013-04-28 2013-08-07 重庆大学 Magnesium, manganese and yttrium alloy material suitable for battery cathode and preparation method thereof
CN103667838A (en) * 2014-01-03 2014-03-26 重庆大学 Mg-Sn-Mn system wrought magnesium alloy and preparation method thereof
CN110616356A (en) * 2019-10-15 2019-12-27 哈尔滨工程大学 Er-containing magnesium alloy and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011042847A (en) * 2009-08-24 2011-03-03 Peter Stolfig Magnesium alloy
CN101787473A (en) * 2010-03-22 2010-07-28 北京工业大学 Tough antiflaming magnesium alloy and preparation method thereof
KR20130012662A (en) * 2011-07-26 2013-02-05 한국기계연구원 High-strength high-ductility ignition-proof magnesium alloy
CN103233152A (en) * 2013-04-28 2013-08-07 重庆大学 Magnesium, manganese and yttrium alloy material suitable for battery cathode and preparation method thereof
CN103667838A (en) * 2014-01-03 2014-03-26 重庆大学 Mg-Sn-Mn system wrought magnesium alloy and preparation method thereof
CN110616356A (en) * 2019-10-15 2019-12-27 哈尔滨工程大学 Er-containing magnesium alloy and preparation method thereof

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Title
JINGZHANG等: "Microstructure and mechanical properties of Mg–1.8%Mn alloy modified by single Er and composite Er/Al microalloying", 《MATERIALS SCIENCE AND ENGINEERING: A》 *
宋鹏飞等: "高强变形镁合金的研究现状及展望", 《兵器材料科学与工程》 *

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