KR101680046B1 - Method for manufacturing high-strength wrought magnesium alloy by conducting aging treatment prior to plastic working and high-strength wrought magnesium alloy manufactured thereby - Google Patents
Method for manufacturing high-strength wrought magnesium alloy by conducting aging treatment prior to plastic working and high-strength wrought magnesium alloy manufactured thereby Download PDFInfo
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- KR101680046B1 KR101680046B1 KR1020150009455A KR20150009455A KR101680046B1 KR 101680046 B1 KR101680046 B1 KR 101680046B1 KR 1020150009455 A KR1020150009455 A KR 1020150009455A KR 20150009455 A KR20150009455 A KR 20150009455A KR 101680046 B1 KR101680046 B1 KR 101680046B1
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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
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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
Abstract
(A) preparing a magnesium alloy billet; (b) homogenizing heat treatment of the magnesium alloy billet; (c) aging the homogenized heat treated magnesium alloy billet; And (d) subjecting the aged magnesium alloy billet to hot or warm working. According to the present invention, there is provided a method for producing a magnesium alloy material, comprising the steps of: pre-aging (before homogenizing heat treatment, The precipitation hardening is caused by inhibiting the crystal growth of the dynamic recrystallized grains formed at the time of plastic working, and the precipitation hardening is suppressed by the precipitation hardening, Magnesium alloy processing material of high strength can be manufactured through the improvement of the strength due to grain refinement and the effect.
Description
The present invention relates to a method for manufacturing a high strength magnesium alloy processing material and a high strength magnesium alloy processing material produced thereby.
Magnesium alloys not only have extremely low densities as compared with other metal materials but also are attracting attention as very attractive materials in automobile, railway and aviation industries because of their excellent non-strength, dimensional stability, electromagnetic shielding ability and heat dissipation.
The magnesium alloy material made of such a magnesium alloy is largely divided into cast magnesium alloys and wrought Mg alloys. Among them, the cast material is superior in moldability, but its surface is very rough, There is a problem that it is not suitable for manufacturing a high quality magnesium alloy product requiring a high strength because a large amount of time and cost is required for the surface treatment of the surface and internal defects such as shrinkage porosity are generated.
Therefore, studies have been made to achieve excellent mechanical properties of magnesium alloy processing materials which do not have the above-mentioned problems. As a result of these efforts, relatively low prices such as AZ80 (Mg-8.0Al-0.5Zn, wt.%) , High strength magnesium alloy extruded material having suitable strength and ductility, and excellent corrosion resistance have been commercialized and widely used [Non-Patent
Nevertheless, magnesium alloy processing materials are still limited in applications and components due to their low strength compared to commercial aluminum alloys (Al alloys) or steel, and the development of magnesium alloy processing materials with improved strength This is an urgent situation.
The present invention can increase the fraction of the secondary phase produced after hot working and reduce the average grain size of the crystal grains, thereby making it possible to produce a magnesium alloy processing material having excellent strength in a conventional magnesium alloy material including a commercial magnesium alloy material And to provide a high-strength magnesium alloy processing material produced thereby.
According to an aspect of the present invention, there is provided a method for manufacturing a magnesium alloy billet comprising the steps of: (a) preparing a magnesium alloy billet; (b) homogenizing heat treatment of the magnesium alloy billet; (c) Aging the magnesium alloy billet, and (d) hot or hot working the aged magnesium alloy billet.
In addition, the step (a) is characterized by comprising the following steps:
(i) preparing a melt containing magnesium and an alloy element; And
(ii) injecting the melt into a mold at a temperature of 650 to 750 DEG C to form a billet.
Also, in the step (b), a homogenization heat treatment is performed at 350 to 550 ° C for 0.5 to 96 hours, thereby producing a magnesium alloy processing material.
Also, in the step (b), the magnesium alloy billet is pre-heated at a temperature of 250 to 350 ° C., and then subjected to homogenization heat treatment.
Further, the step (b) further comprises a step of cooling the magnesium alloy billet after the homogenization heat treatment, and then cooling the magnesium alloy billet.
In the step (c), the aging treatment is performed at a temperature of 100 to 500 ° C for 1 to 300 hours.
Also, in the step (d), the hot or hot working is carried out by using at least one method selected from rolling, extrusion or forging.
In addition, the step (d) further comprises a step of subjecting the magnesium alloy billet to hot or hot working and then aging the magnesium alloy billet.
The aging treatment after the hot or hot working is performed at 150 to 250 ° C for 1 to 360 hours.
In addition, the present invention proposes a magnesium alloy processing material produced by the above manufacturing method in another aspect of the invention.
According to the method of manufacturing a high strength magnesium alloy processing material according to the present invention, by performing the pre-aging treatment (the aging treatment carried out after the homogenization heat treatment and before the plastic working), the fine secondary phase precipitates are treated with the magnesium alloy crystal system and the matrix And this precipitate interferes with the crystal growth of the dynamic recrystallized grains formed during the plastic working by the grain boundary pinning effect, thereby improving the strength due to grain refinement and increasing the strength by precipitation hardening. A magnesium alloy material having a high strength can be produced.
FIG. 1 is a flow chart showing each step of a method for manufacturing a magnesium alloy material according to the present invention.
2 is an electron microscope (SEM or TEM) photograph showing the difference in the microstructure of the magnesium alloy according to the presence or absence of the aging treatment after the homogenization treatment in Example 1 of the present application.
3 is a scanning electron microscope (SEM) image showing the difference in the microstructure of the magnesium alloy according to the conditions of the aging treatment after the homogenization treatment in Examples 2-1 to 2-3 of the present application.
FIGS. 4 (a) and 4 (b) are scanning electron microscope (SEM) and electron backscattering diffraction (EBSD) images showing the microstructure of the magnesium alloy workpiece prepared in Comparative Example 1 and Example 1, respectively.
5 is a stress-strain graph according to a room temperature tensile test (crosshead speed: 1.5 mm / min) for the magnesium alloy material prepared in Example 1 and Comparative Example 1 of the present application.
In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
Embodiments in accordance with the concepts of the present invention can make various changes and have various forms, so that specific embodiments are illustrated in the drawings and described in detail in this specification or application. It should be understood, however, that it is not intended to limit the embodiments according to the concepts of the present invention to the particular forms of disclosure, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises ",or" having ", or the like, specify that there is a stated feature, number, step, operation, , Steps, operations, components, parts, or combinations thereof, as a matter of principle.
Hereinafter, the present invention will be described in detail.
FIG. 1 is a process diagram showing a process of manufacturing a magnesium alloy material according to the present invention.
As shown in FIG. 1, a method for manufacturing a magnesium alloy processing material according to the present invention comprises the steps of: (a) preparing a magnesium alloy billet; (b) homogenizing heat treatment of the magnesium alloy billet; (c) aging the homogenized heat treated magnesium alloy billet; And (d) hot or hot working the aged magnesium alloy billet.
The step (a) is a method of producing a magnesium alloy billet by melting a raw material containing magnesium to prepare a magnesium alloy melt, and then injecting the molten magnesium alloy into a mold. More specifically, the step (a) Preparing a molten metal containing an element; And injecting the molten metal into a mold to form a billet.
The temperature for carrying out the casting process is not particularly limited, but it is preferable that the casting can be performed at a temperature of 650 to 750 ° C, because when the casting is performed at a temperature lower than 650 ° C, the fluidity of the magnesium alloy melt can be lowered If casting is performed at a temperature exceeding 750 캜, the magnesium alloy molten metal may be rapidly oxidized and impurities may be mixed during casting, resulting in a problem that the purity of the produced magnesium alloy billet is lowered It is because.
The magnesium alloy molten metal can be produced by melting a magnesium alloy raw material. The magnesium alloy molten metal may be produced by gravity casting, continuous casting, sand casting or casting, as long as it is a method commonly used in the art. A casting method such as a pressure casting may be a typical example.
The step (b) is a step of homogenizing the magnesium alloy billet produced in the step (a), and the homogeneous heat treatment is performed to remove the uneven structure due to the segregation of the alloy element during the casting of the magnesium alloy melt And the high-temperature processability and mechanical properties of the magnesium alloy can be improved.
When the homogenization heat treatment is performed at a temperature of less than 350 ° C, the content of the alloying element dissolved in the magnesium matrix is small, so that the dynamic precipitation during hot or hot working, which will be described later, the effect of strengthening the alloy by dynamic precipitation is not significant. When the homogenization heat treatment is carried out at a temperature higher than 550 ° C., the homogeneous heat treatment temperature of the magnesium alloy is high, so that local dissolution of the magnesium alloy billet occurs, This is because there is a problem.
In addition, it is preferable that the homogenization heat treatment is performed for 0.5 to 96 hours. If the homogenization heat treatment is performed for less than 0.5 hour, diffusion of the alloying element does not sufficiently occur and the effect of the homogenization heat treatment is not exhibited. It is not economical because the increase in effect is not large compared with the execution time.
Further, it is preferable to pre-heat the magnesium alloy billet at 250 to 350 ° C prior to the homogenization heat treatment so as to prevent cracking and deformation due to the rapid heat treatment of the magnesium alloy billet.
Further, it is preferable to further include a step of cooling the magnesium alloy billet after the homogenization heat treatment and cooling. A specific method for performing the cooling step is not particularly limited, but magnesium (Mg), which is composed of supersaturated solid solution Water quenching is more preferable than air cooling in that the alloy billet can be obtained to further increase the dynamic precipitation on the secondary phase in hot or hot working to be described later.
Next, in the step (c), the magnesium alloy billet subjected to the homogenization heat treatment in the step (b) is aged.
As in this step, when aging prior to plastic working is performed prior to the aging treatment, that is, a large amount of fine secondary phase precipitates are formed, and such precipitates are formed in a dynamic The crystal growth of the recrystallized grains is prevented by the grain boundary pinning effect, whereby the strength according to grain refinement and the strength due to precipitation hardening can be achieved at the same time.
The aging treatment of the magnesium alloy billet in this step is preferably carried out at a temperature of 100 to 500 ° C. This is because when the aging treatment is carried out at a temperature lower than 100 ° C., the precipitate formation rate becomes slow and a long time heat treatment is required If the aging treatment is carried out at a temperature of 500 ° C or more, the size of the precipitate to be formed becomes large and it may be difficult to obtain the expected effect.
It is preferable that the aging treatment is performed by heat treatment for 1 to 300 hours. If the aging treatment is performed for less than 1 hour, the amount of precipitate formed is not so small, and the effect of the aging treatment is less than expected. There is a problem that the effect of the aging treatment is not further improved and the further heat treatment is ineffective.
Next, the step (d) is a step of hot-working or hot-working the aged magnesium alloy billet in the step (c).
In this step, the magnesium alloy billet is subjected to hot or warm working using at least one known plastic working method selected from rolling, extrusion, forging, and the like. The magnesium alloy billet is not limited to the method of plastic working by rolling, extruding or forging, and is not limited to a method commonly used in the art.
In this step, after the magnesium alloy billet is hot-worked or hot-worked, the magnesium alloy processing material is aged again to further improve the mechanical properties of the magnesium alloy processing material. The aging treatment may be performed at a temperature of 150 to 250 ° C For 1 to 360 hours.
According to the process for producing a high strength magnesium alloy material according to the present invention as described above in detail, the fine secondary phase precipitate is converted into magnesium (Mg) by carrying out a pre-aging treatment (aging treatment after homogenization heat treatment and before plastic working) Alloys are formed in a large amount in the grain boundaries and the matrix, and these precipitates interfere with the crystal growth of the dynamic recrystallized grains formed during the calcining process through the grain boundary pinning effect, thereby improving the strength due to grain refinement and precipitating hardening It is possible to manufacture a high-strength magnesium alloy processing material.
Hereinafter, a method of manufacturing a magnesium alloy material according to the present invention will be described in more detail with reference to the preferred embodiments. The embodiments shown are merely technical examples for explaining the present invention in more detail and are not intended to limit the scope of the present invention.
≪ Example 1 >
First, a cast billet made of a magnesium alloy (AZ80) having the composition shown in Table 1 was prepared.
[Table 1]
The magnesium alloy billet was homogenized at 400 ° C for 15 hours, water quenched, and processed into cylindrical specimens (diameter: 80 mm,
Figure 2 is an electron micrograph showing the difference between the magnesium alloy microstructures with and without after homogenizing treatment aging treatment, the microstructure of the previous sample being an aging treatment performed from Figure 2 the secondary by the homogenization heat treatment (Mg 17 Al 12 ) were completely dissolved in the magnesium matrix and no secondary phase particles were observed (see FIG. 2 (a)). In the microstructure of the specimen subjected to aging treatment after the homogenization heat treatment, however, many Mg 17 Al 12 grains (See Fig. 2 (b)), it can be seen that plate-like Mg 17 Al 12 precipitates exist in the crystal grains with a specific orientation with respect to the magnesium matrix (see Fig. 2 (c)) .
Next, the aged specimen was opened at 250 ° C., and then extruded at 250 ° C. (ram speed: 1 mm / sec, extrusion ratio: 25) and air-cooled to prepare a magnesium alloy processing material.
≪ Examples 2-1 to 2-3 >
First, a cast billet made of a magnesium alloy (TAZ711) having the composition shown in Table 2 below was prepared. Specifically, a magnesium alloy melt obtained by dissolving a raw metal such as magnesium in an inert atmosphere containing carbon dioxide (CO 2 ) and sulfur hexafluoride (SF 6 ) and at a temperature of 800 ° C was poured into a steel mold preheated to 210 ° C, Alloy billets were prepared.
[Table 2]
The magnesium alloy billet was subjected to homogenization heat treatment at 500 ° C for 12 hours, followed by water quenching, and then worked into a cylindrical specimen (diameter: 80 mm,
FIG. 3 is a scanning electron microscope (SEM) photograph showing the difference in the microstructure of the magnesium alloy according to the conditions of the aging treatment after the homogenization treatment. As shown in FIG. 3, the fine Mg 2 Sn precipitates are agglomerated by the grain boundaries of the magnesium alloy And it is confirmed that the particle size of the precipitate increases as the heat treatment temperature or time is increased.
Next, the aged specimens were extruded under different extrusion conditions (1)
≪ Comparative Example 1 &
A magnesium alloy processing material was prepared in the same manner as in Example 1, except that the extrusion process was immediately performed without aging after the homogenization heat treatment.
≪ Comparative Example 2 &
A magnesium alloy processing material was prepared in the same manner as in Example 2-1, except that the aging treatment was not performed before the extrusion step.
<Experimental Example>
FIGS. 4 (a) and 4 (b) are scanning electron microscope (SEM) and electron backscattering diffraction (EBSD) images showing the microstructure of the magnesium alloy workpiece prepared in Comparative Example 1 and Example 1, respectively.
Referring to FIGS. 4 (a) and 4 (b), it can be seen that the magnesium alloy processing materials of Comparative Example 1 and Example 1 have a similar microstructure despite the difference in presence or absence of the pre-aging treatment. Specifically, in both of the microstructures of the magnesium alloy processed materials of Comparative Example 1 and Example 1, the secondary overt precipitate particles were not observed in the coarse dynamic recrystallization region (coarse DRX region) having a relatively large grain size, In the fine DRX region with a fine grain size, many spherical Mg 17 Al 12 grains are distributed in the grain boundaries and serve to suppress the crystal growth of the dynamic recrystallized grains due to the grain boundary pinning effect. In addition, It can be confirmed that a small amount of band-type Mg 17 Al 12 particles having a width of 1 to 5 μm is distributed.
However, the magnesium alloy processing material of Example 1 is 57% more than the magnesium alloy processing material of Comparative Example 1, which has a fraction of a fine DRX region of 49%, and thus the pre-aging process results in an average grain size The magnesium alloy processing material of Example 1 has a fraction of band-shaped Mg 17 Al 12 particles which adversely affects mechanical properties as compared with the magnesium alloy processing material of Comparative Example 1 It was confirmed that it decreased from 2.3% to 0.5%, and this result led to the improvement of the strength of the magnesium alloy processing material as shown below.
5 and Table 3 show the results of a tensile test at room temperature (1.5 mm / min) for the magnesium alloy material prepared in Example 1 and Comparative Example 1, respectively. The stress- strain graphs and key figures.
[Table 3]
5 and Table 3 show that when the aging treatment is carried out before the sintering process as in the first embodiment of the present invention, the magnesium alloy crystal grains become finer and the precipitation hardening effect is enhanced, and both the yield strength and the tensile strength of the magnesium alloy processing material are increased .
As shown in Example 1, when the aging treatment is carried out before the calcining process, the elongation is also increased. This result shows that (i) band-shaped Mg 17 Al 12 particles (Ii) the tensile stress was applied, the magnesium alloy working material produced in Example 1 had a higher magnesium content than the magnesium alloy processed material prepared in Comparative Example 1, Since the content of the Al solute dissolved in the substrate is reduced by the pre-aging treatment, serrated tensile flow, which is known to cause ductility deterioration unlike the processing material of Comparative Example 1, does not occur.
Table 4 below shows the results of a room temperature tensile test (crosshead speed: 1.5 mm / min) for the magnesium alloy material prepared in Examples 2-1 to 2-3 and Comparative Example 2 herein.
According to Table 4, the magnesium alloy processing materials manufactured in Examples 2-1 to 2-3 were compared with the magnesium alloy processing materials of Comparative Example 2 in which the pre-aging processing was not performed, 2 Sn) precipitation particles have an improved strength due to grain refinement effect and grain precipitation hardening effect through grain boundary pinning effect.
[Table 4]
Claims (10)
(b) homogenizing heat treatment of the magnesium alloy billet;
(c) aging and cooling the homogenized heat-treated magnesium alloy billet; And
(d) pre-heating the aged magnesium alloy billet and then hot or hot working the magnesium alloy billet.
Wherein the step (a) comprises the steps of:
(i) preparing a melt containing magnesium and an alloy element; And
(ii) injecting the melt into a mold at a temperature of 650 to 750 DEG C to form a billet.
Wherein the homogenization heat treatment is performed at 350 to 550 ° C for 0.5 to 96 hours in the step (b).
Wherein the magnesium alloy billet is pre-heated at a temperature of 250 to 350 DEG C in the step (b), and then subjected to homogenization heat treatment.
Wherein the step (b) further comprises cooling the magnesium alloy billet after the homogenization heat treatment.
Wherein the aging treatment is performed at a temperature of 100 to 500 DEG C for 1 to 300 hours in the step (c).
Wherein the hot or hot working in step (d) is carried out using at least one method selected from rolling, extruding or forging.
Wherein the step (d) further comprises aging the magnesium alloy billet after hot or hot working.
Wherein the aging treatment after hot or hot working is carried out at 150 to 250 DEG C for 1 to 360 hours.
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| KR1020150009455A KR101680046B1 (en) | 2015-01-20 | 2015-01-20 | Method for manufacturing high-strength wrought magnesium alloy by conducting aging treatment prior to plastic working and high-strength wrought magnesium alloy manufactured thereby |
| PCT/KR2015/005017 WO2016117768A1 (en) | 2015-01-20 | 2015-05-19 | Method for manufacturing magnesium alloy billet for plastic processing and high-strength wrought magnesium alloy manufacturing method including the same |
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| CN107557706A (en) * | 2017-09-04 | 2018-01-09 | 河北工业大学 | A kind of processing method for improving magnesium alloy strength |
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| KR102469771B1 (en) | 2020-04-22 | 2022-11-23 | 경북대학교 산학협력단 | METHOD FOR MANUFACTURING HIGH-STRENGTH PRECIPITATION HARDENING WROUGHT Mg-Al MAGNESIUM ALLOY INCLUDING PROCESS FOR SHORTENING AGING TREATMENT TIME |
| CN115874126A (en) * | 2022-12-09 | 2023-03-31 | 哈尔滨工业大学（威海） | Aging strengthening magnesium alloy strengthening and toughening treatment and preparation process |
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| KR100360994B1 (en) * | 1998-02-27 | 2003-02-25 | 신광선 | Method for improving corrosion resistance of magnesium alloy bearing aluminum |
| JP2006176873A (en) * | 2004-11-26 | 2006-07-06 | Aisin Seiki Co Ltd | Magnesium alloy and method for manufacturing magnesium alloy member |
| KR100994812B1 (en) * | 2010-04-05 | 2010-11-16 | 한국기계연구원 | High-strength high-ductility magnesium alloy extrudate and manufacturing method thereof |
| KR101277297B1 (en) * | 2011-02-18 | 2013-06-20 | 한국기계연구원 | High-strength high-ductility magnesium alloy extrusions with low anisotropy and manufacturing method thereof |
| KR101400140B1 (en) * | 2013-07-16 | 2014-05-30 | 한국기계연구원 | Preparing method for magnesium alloy extrudate and the magnesium alloy extrudate thereby |
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