CN105543603B - Low-rare-earth high-strength deforming magnesium alloy and preparation method thereof - Google Patents
Low-rare-earth high-strength deforming magnesium alloy and preparation method thereof Download PDFInfo
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- CN105543603B CN105543603B CN201610081996.2A CN201610081996A CN105543603B CN 105543603 B CN105543603 B CN 105543603B CN 201610081996 A CN201610081996 A CN 201610081996A CN 105543603 B CN105543603 B CN 105543603B
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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
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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 a low-rare-earth high-strength deforming magnesium alloy and a preparation method thereof. The low-rare-earth high-strength deforming magnesium alloy is composed of the following components in percentage by mass: 5.10-5.60 wt.% of Zn, 0.40-0.90 wt.% of Zr, 0.90-1.30 wt.% of Ce, 0.40-2.30 wt.% of Y, and the balance of Mg and inevitable impurities. A magnesium alloy cast ingot containing rare-earth cerium and yttrium is subjected to hot extrusion, so that the crystal grains are obviously refined, and the cerium, yttrium, magnesium and zinc form a fine dispersive strengthening phase capable of effectively preventing the recrystallized grains from growth and strengthening the matrix in the hot extrusion process, thereby obtaining the high tensile strength. The aging heat treatment is carried out after the hot extrusion so as to separate out more fine dispersive second phases capable of further enhancing the alloy strength, wherein the maximum yield strength can exceed 410 MPa which is obviously higher than that of the traditional commercial high-strength ZK60 deforming magnesium alloy. The alloy has the advantages of simple preparation method and lower cost, and has great application potential.
Description
Technical field
The present invention relates to a kind of magnesium alloy, more particularly to a kind of low rare earth high strength wrought magnesium alloy and preparation method.
Background technology
In recent years, with the anxiety of energy availability and demand, a large amount of consumption of non-renewable energy resources, energy crisis are gradually highlighted.For
Energy saving, various countries are more urgent to the demand of new material, especially light alloy material, such as magnesium and magnesium alloy materials.Magnesium alloy
Have the advantages that density is little, specific strength is high, superior shock-proof and damping performance, splendid capability of electromagnetic shielding, be that industry should at present
The most light structural metallic materials with.Meanwhile, plastics are compared, its recyclability is even better, non-environmental-pollution, is described as " 21 generation
The important green engineering structural metallic materials of discipline ".However, as the absolute intensity of magnesium alloy is relatively low, plastic deformation ability is poor,
Extensive application of the magnesium alloy on structural material is limited greatly, it is therefore necessary to develop high-strength magnesium alloy to expand magnesium alloy
Practical application.
In recent years, for development of high strength magnesium alloy, the heavy rare earth elements such as substantial amounts of Gd, Y are generally added in the magnesium alloy,
This can dramatically increase the intensity of magnesium alloy, and can further improve intensity by timeliness, have good precipitation strength to make
With.T. Homma et al. have studied As-extruded Mg-10Gd-5.7Y-1.6Zn-0.6Zr (wt.%) magnesium alloy, and its tensile strength can
542MPa is reached, yield strength is up to 473MPa.C. the Mg-8.2Gd-3.8Y-1.0Zn-0.4Zr that Xu et al. is studied
(wt.%) after extruding, rolling and timeliness, up to 505MPa, yield strength is 416MPa to tensile strength to alloy.Although this
A little magnesium alloys possess excellent intensity, but its high content of rare earth causes high preparation cost, it is difficult to fundamentally solve work
The application of demand in industry.Therefore, it is badly in need of the low rare earth of exploitation, the high-strength magnesium alloy of low cost, is existed with fundamentally expanding magnesium alloy
Application in industry.
Typical Representatives of the ZK60 as Mg-Zn-Zr series deformation magnesium alloys, with better intensity, plasticity and corrosion resistance,
Its specific strength can exceed some high-strength aluminum alloys.Y and Ce are more conventional alloying elements in ZK60 alloys.Y and Ce can
Significantly crystal grain thinning, can be improved intensity, and the addition of Y and Ce can form alloy phase, can be passed through by refined crystalline strengthening mode
Second-phase strength improving intensity, while content of rare earth can avoid the formation of the second thick phase less.It is certain due to containing in alloy
The Zn elements of amount, carry out simple low temperature aging heat treatment, can promote the Second Phase Precipitation of small and dispersed, effectively hinder basal plane position
Wrong motion, greatly improves the intensity of alloy.Therefore, the present invention intend add a small amount of Y and Ce on the basis of Mg-Zn-Zr alloys with
Develop a kind of lower-cost low rare earth high strength deformed magnesium alloy material.
The content of the invention
It is an object of the invention to provide a kind of low rare earth high strength wrought magnesium alloy and preparation method, the magnesium alloy passes through
After adding the cerium and yttrium of low content, hot extrusion and direct aging are carried out, high intensity can be obtained, while ensureing preferable
Plasticity.
The low rare earth high-strength wrought magnesium alloy that the present invention is provided, is made up of Mg, Zn, Zr, Ce, Y, the quality hundred of its each component
Point content is：Zn：5.10~5.60 wt.%；Zr：0.40~0.90 wt.%；Ce：0.90~1.30 wt.%；Y：0.40~2.30
wt.%；Remaining is Mg and inevitable impurity.Inevitably impurity of the invention is Fe, Si etc., and its total amount is less than 0.03
wt.%。
The preparation method of a kind of low rare earth high-strength wrought magnesium alloy of the present invention, it is characterised in that including following step
Suddenly：
A) alloy melting and casting：Formula is calculated by above-mentioned low rare earth high strength wrought magnesium alloy to get the raw materials ready, raw materials
In the middle of technical pure magnesium ingot, pure zinc ingot, Mg-28.54wt.%Zr intermediate alloys, Mg-30wt.%Ce intermediate alloys, Mg-30wt.%Y
Alloy.Pure magnesium and intermediate alloy are preheated to into 200 ~ 250 DEG C in an oven, 1 ~ 2h is incubated；In SF6+CO2Under gas shield, by magnesium
Ingot is put in crucible, heats melting；At a temperature of 720 ~ 740 DEG C, add in magnesium melt
Gold, should be pressed into below liquid level rapidly during addition, stir after thawing；When temperature rises to 690 ~ 720 DEG C, by the conjunction
Golden composition proportion amount adds pure zinc ingot, stirs after thawing；Magnesium melt temperature is risen to into 740 ~ 760 DEG C, in adding Mg-Zr
Between alloy, it is to be melted after stirring 2 ~ 5 minutes, make composition uniform；30 ~ 60 minutes are stood at 730 ~ 750 DEG C, after standing is finished, is beaten
Dross on surface of fusant is dragged for, when temperature drops to 690 ~ 710 DEG C, in SF6+CO2Under gas shield, enter in 200 ~ 300 DEG C of swage
Row casting；
B) machine：According to the size of extruder recipient by above-mentioned ingot casting sawing, railway carriage to suitable dimension；
C) homogenization：Homogenization Treatments are carried out under 390 ~ 420 DEG C of temperature conditionss, temperature retention time is 12 ~ 18h；
D) hot extrusion：The ingot casting and extrusion die after Homogenization Treatments is preheated 2 ~ 3 hours at 350 ~ 400 DEG C before extruding,
Extrusion temperature is 390 DEG C ~ 420 DEG C, and extrusion ratio is 26:1, extruding rate is 0.60 ~ 1.20m/min, obtains a diameter of 16 mm's
Magnesium alloy rod；
E) Ageing Treatment：The sample for having extruded is cut into sample, is put in oil bath furnace, temperature be 150 ~ 200 DEG C, the time be 10 ~
40h。
Compared to existing technology, the present invention has the advantages that：
1st, a small amount of Rare-Earth Ce added in the present invention and Y, are combined with Mg, Zn, form dystectic Mg-Zn-Ce and Mg-
Zn-Y ternary phases.During hot extrusion deformation, these are mutually broken into very tiny granule, and even dispersion is distributed in magnesio
In body, strengthen matrix, while dynamic recrystallization can be effectively promoted, hinder growing up for crystal grain, obtain tiny recrystal grain.
Subsequent low temperature aging, can promote the Second Phase Precipitation of small and dispersed, be advantageous to strengthen matrix, after Jing timeliness, surrender
Intensity reaches as high as 412MPa, and tensile strength reaches as high as 421MPa, hence it is evident that higher than conventional commercial high-strength deforming magnesium alloy ZK60
Yield strength, while keeping certain elongation percentage, this has fully excavated the use potentiality of magnesium alloy materials.
2nd, present invention process is simple, easily operation and regulation and control, the equipment for being adopted such as smelting furnace, heat extruder, oil bath furnace
Be conventional common apparatus, with it is portable strong the characteristics of.
Description of the drawings
Fig. 1 commercialization ZK60 magnesium alloy extrusion state microstructure scanned photographs (do not contain cerium and yttrium)；
1 magnesium alloy extrusion state microstructure scanned photograph of Fig. 2 embodiments；
2 magnesium alloy extrusion state microstructure scanned photograph of Fig. 3 embodiments；
3 magnesium alloy extrusion state microstructure scanned photograph of Fig. 4 embodiments.
Specific embodiment
The present invention is described in further detail in conjunction with specific embodiments with reference to the accompanying drawings, it should be noted that these
Embodiment is that, for illustrating the present invention, rather than limitation of the present invention, protection scope of the present invention is not limited to following enforcement
Example.Embodiment 1：The low magnesium-rare earth of the present embodiment includes following component by weight percentage：Zn 5.19wt.%, Zr 0.66
1.18 wt.% of wt.%, Ce, Y 0.49 wt.%, balance of Mg.
Prepare by said ratio and in the following manner, can just obtain the magnesium alloy of the present embodiment：
A) alloy smelting and casting：Raw materials be technical pure magnesium ingot, pure zinc ingot, Mg-28.54%Zr intermediate alloys,
Mg-30%Ce intermediate alloys, Mg-30%Y intermediate alloys.Pure magnesium and intermediate alloy are preheated to into 200 DEG C (or 250 in an oven
DEG C), it is incubated 2h；In SF6+CO2Under gas shield, magnesium ingot is put in crucible, heats melting；720 DEG C (or 730 DEG C, 740
DEG C) at a temperature of, Mg-Y the and Mg-Ce intermediate alloys of drying are added in magnesium melt, liquid level should be pressed into rapidly during addition with
Under, stir after thawing；When treating that temperature rises to 690 DEG C (or 700 DEG C, 720 DEG C), add by the alloying component proportional quantity
Pure zinc ingot, stirs after thawing；Magnesium melt temperature is risen to into 740 DEG C（Or 750 DEG C, 760 DEG C）Add
Gold, rear stirring to be melted 5 minutes, makes composition uniform；45 minutes are stood at 730 DEG C (or 750 DEG C), after standing is finished, is salvaged
Dross on surface of fusant, treats that temperature drops to 690 DEG C (or 710 DEG C), in SF6+CO2Under gas shield, at 200 DEG C (or 300 DEG C)
Cast in swage.
B) machine：According to the size of extruder recipient by above-mentioned ingot casting sawing, railway carriage to suitable dimension；
C) homogenization：Homogenization Treatments are carried out under 400 DEG C of (or 390 DEG C, 420 DEG C) temperature conditionss, temperature retention time is
12h (or 18h)；
D) hot extrusion：By the ingot casting and extrusion die after Homogenization Treatments at 370 DEG C (or 350 DEG C, 400 DEG C) before extruding
Preheating 2.5h (2h, 3h), extrusion temperature are 400 DEG C (or 390 DEG C, 420 DEG C), and extrusion ratio is 26:1, extruding rate is 0.60
(or 1.20m/min), obtains the magnesium alloy rod of a diameter of 16 mm；
E) Ageing Treatment：The sample for having extruded is cut into sample, is put in oil bath furnace, temperature be 180 DEG C (or 150 DEG C, 200
DEG C), the time is 15h（Or 40h, 10h）.
Embodiment 2：The low magnesium-rare earth of the present embodiment includes following component by weight percentage：Zn 5.34wt.%, Zr
1.05 wt.% of 0.71 wt.%, Ce, Y 1.04 wt.%, balance of Mg.Obtain alloy smelting and the casting of the present embodiment magnesium alloy
Make-machine-homogenization-hot extrusion-aging treatment method is same as Example 1.
Embodiment 3：The low magnesium-rare earth of the present embodiment includes following component by weight percentage：Zn 5.26wt.%, Zr
1.12 wt.% of 0.59 wt.%, Ce, Y 2.29 wt.%, balance of Mg.Obtain alloy smelting and the casting of the present embodiment magnesium alloy
Make-machine-homogenization-hot extrusion-aging treatment method is same as Example 2, difference is that aging time is
35h。
Taking 1,2 and 3 magnesium alloy rod of above-described embodiment carries out room temperature tensile test experiments, and the performance measured is shown in Table 1.In order to
It is easy to compare, in table 1, gives the mechanical performance data of general commercial ZK60 extruded barses simultaneously.
The room-temperature mechanical property of 1 low rare earth high strength magnesium alloy of the present invention of table
| Alloy | Yield strength σ0.2/MPa | Tensile strength sigmab/MPa | Elongation percentage δ/% |
| Commercial ZK60 | 250-270 | 320-340 | 10-15 |
| Embodiment 1 | 407 | 421 | 7.1 |
| Embodiment 2 | 380 | 387 | 9.8 |
| Embodiment 3 | 412 | 419 | 4.5 |
From table 1, the alloy (embodiment 1,2 and 3) of the present invention is with than commercial high-strength deforming magnesium alloy ZK60（When
Effect state）Higher intensity, particularly yield strength, are significantly higher than ZK60 magnesium alloys.The maximum tensile strength is more than 420MPa, maximum
Anti- yield strength can meet the fields such as Aero-Space, defence and military, track traffic to magnesium alloy bearing capacity more than 410MPa
Requirement.From scanning electron microscope displaing micro tissue topography（Fig. 1-4）As can be seen that after hot extrusion, even dispersion in magnesium matrix
Be dispersed with tiny Second Phase Particle, energy spectrum analysiss show these granules be Ce, Y and Mg, Zn combine to form Mg-Zn-Ce,
Mg-Zn-Y ternary phases and MgZn2Phase.The precipitation of these compounds, can be effectively promoted dynamic recrystallization, hinder recrystal grain
Grow up, obtain quite tiny recrystal grain（About 1 μm or so of the average grain size of embodiment 1-2 magnesium alloy）, reinforcing
Phase Mg-Zn-Ce and Mg-Zn-Y can effectively hinder dislocation movement by slip, strengthen matrix.During subsequent direct aging is processed, in magnesium alloy
The very tiny MgZn of many nano-grade sizes can be separated out2Phase, MgZn2Orientation relationship with matrix is symbiosis and epibiosis, and this
The MgZn separated out in alloy2It is mutually rod-short, this can effectively hinder the sliding of basal plane dislocation, and then significantly improve alloy
Intensity.Therefore, the high intensity of wrought magnesium alloy of the present invention is mainly derived from the contribution of refined crystalline strengthening and precipitation strength.
Finally illustrate, above example is only unrestricted to illustrate technical scheme, although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the present invention's
Technical scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, which all should be covered
In the middle of scope of the presently claimed invention.
Claims (1)
1. a kind of low rare earth high strength wrought magnesium alloy, it is characterised in that the magnesium alloy is made up of Mg, Zn, Zr, Ce, Y,
Zn：5.26~5.60 wt.%；Zr：0.59~0.71 wt.%；Ce：0.90~1.30 wt.%；Y：0.40~2.30 wt.%；Remaining is
Mg and inevitable impurity, total impurities are less than 0.03 wt.%；
The preparation method of the magnesium alloy, comprises the steps：
A) alloy melting and casting：Get the raw materials ready by low rare earth high strength wrought magnesium alloy formula, raw materials are pure magnesium
Ingot, pure zinc ingot, Mg-28.54wt.%Zr intermediate alloys, Mg-30wt.%Ce intermediate alloys, Mg-30wt.%Y intermediate alloys；Will be pure
Magnesium and intermediate alloy are preheated to 200 ~ 250 DEG C in an oven, are incubated 1 ~ 2h；In SF6+CO2Under gas shield, magnesium ingot is put into into earthenware
In crucible, melting is heated；Mg-Y the and Mg-Ce intermediate alloys of drying at a temperature of 720 ~ 740 DEG C, are added in magnesium melt, is added
When should be pressed into below liquid level rapidly, stir after fusing；When temperature rises to 690 ~ 720 DEG C, by the alloying component
Proportional quantity adds pure zinc ingot, stirs after fusing；Magnesium melt temperature is risen to into 740 ~ 760 DEG C, Mg-Zr intermediate alloys are added,
After to be melted, stirring 2 ~ 5 minutes, make composition uniform；30 ~ 60 minutes are stood at 730 ~ 750 DEG C, after standing is finished, melt table is salvaged
Edema over the face slag, when temperature drops to 690 ~ 710 DEG C, under SF6+CO2 gas shields, is cast in 200 ~ 300 DEG C of swage；
B) machine：According to the size of extruder recipient by the ingot casting sawing of cast molding, railway carriage to suitable dimension；
C) homogenization：Homogenization Treatments are carried out under 390 ~ 420 DEG C of temperature conditionss, temperature retention time is 12 ~ 18h；
D) hot extrusion：The ingot casting and extrusion die after Homogenization Treatments is preheated 2 ~ 3 hours at 350 ~ 400 DEG C before extruding, extruding
Temperature is 390 DEG C ~ 420 DEG C, and extrusion ratio is 26:1, extruding rate is 0.60 ~ 1.20m/min, and the magnesium for obtaining a diameter of 16 mm is closed
Golden bar；
E) Ageing Treatment：The sample for having extruded is cut into sample, is put in oil bath furnace, temperature is 150 ~ 200 DEG C, the time is 10 ~ 40h.
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| KR101858856B1 (en) * | 2016-12-21 | 2018-05-17 | 주식회사 포스코 | High strength magnesium alloy having excellent fire-retardant, and method for manufacturing the same |
| CN108311652B (en) * | 2018-02-06 | 2019-12-17 | 洛阳晟雅镁合金科技有限公司 | Preparation process of ME20M magnesium alloy slab ingot |
| CN108342630B (en) * | 2018-05-18 | 2020-03-31 | 句容百利镁合金材料科技有限公司 | Magnesium alloy, preparation method of magnesium alloy section bar and preparation method of magnesium alloy rim |
| CN108950337B (en) * | 2018-08-07 | 2020-06-23 | 重庆大学 | Low-cost high-strength Mg-Zn-Y-Ce-Ca magnesium alloy and preparation method thereof |
| CN109022984B (en) * | 2018-09-25 | 2021-01-19 | 中国科学院海洋研究所 | Zn-containing corrosion-resistant rare earth magnesium alloy and preparation method thereof |
| CN109825751A (en) * | 2019-04-02 | 2019-05-31 | 北京工业大学 | A kind of high thermal conductivity strong mechanical performance magnesium alloy materials and preparation method thereof |
| CN112458349A (en) * | 2020-11-06 | 2021-03-09 | 重庆大学 | Low-rare earth high-strength wrought magnesium alloy containing neodymium and yttrium and preparation method thereof |
| CN113528913A (en) * | 2021-08-02 | 2021-10-22 | 西安四方超轻材料有限公司 | High-thermal-conductivity wrought magnesium alloy material and preparation method thereof |
| CN115233010A (en) * | 2022-06-24 | 2022-10-25 | 重庆大学 | Method for efficiently preparing high-strength magnesium alloy |
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| CN102978498A (en) * | 2012-12-18 | 2013-03-20 | 中国科学院长春应用化学研究所 | Rare-earth magnesium alloy and preparation method thereof |
| CN103952613A (en) * | 2014-05-19 | 2014-07-30 | 重庆大学 | Wrought magnesium alloy containing rare earth cerium and yttrium and having high yield ratio |
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| JP5035717B2 (en) * | 2005-06-24 | 2012-09-26 | 独立行政法人産業技術総合研究所 | Superplastic magnesium alloy manufacturing method from grain boundary precipitation type magnesium alloy scrap |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978498A (en) * | 2012-12-18 | 2013-03-20 | 中国科学院长春应用化学研究所 | Rare-earth magnesium alloy and preparation method thereof |
| CN103952613A (en) * | 2014-05-19 | 2014-07-30 | 重庆大学 | Wrought magnesium alloy containing rare earth cerium and yttrium and having high yield ratio |
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