CN107058924A - Regulate and control high-strength high-plastic heat resistance magnesium alloy of LPSO structures and nanoprecipitation phase and preparation method thereof - Google Patents
Regulate and control high-strength high-plastic heat resistance magnesium alloy of LPSO structures and nanoprecipitation phase and preparation method thereof Download PDFInfo
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- CN107058924A CN107058924A CN201710258417.1A CN201710258417A CN107058924A CN 107058924 A CN107058924 A CN 107058924A CN 201710258417 A CN201710258417 A CN 201710258417A CN 107058924 A CN107058924 A CN 107058924A
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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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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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
- C22C23/06—Alloys based on magnesium with a rare earth metal 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
- 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
The invention discloses a kind of regulation and control LPSO structures and the preparation method of the high-strength high-plastic heat resistance magnesium alloy of nanoprecipitation phase, its step includes：A, Mg Y Zn alloy cast ingots are cut, be placed in equal channel angular extrusion die and be incubated at 280~330 DEG C, ECAP processing then is carried out to ingot casting, obtain Ultra-fine Grained bulk；B, by above-mentioned Ultra-fine Grained bulk be placed in heat-treatment furnace 350~400 DEG C be incubated 2~8h, quenching；It is subsequently placed in vacuum drying oven and 22~30h is incubated at 200~225 DEG C, quenching obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The present invention processes the ultrafine grain rare earth magnesium alloy for obtaining the structure containing LPSO with high-ductility by ECAP, and then the LPSO structures in alloy are regulated and controled by dual heat treatment, and introduce nanoprecipitation phase, strengthened using refined crystalline strengthening, LPSO phases and nanoprecipitation mutually strengthens the combination of these three intensifiers and uniformly, acquisition is provided simultaneously with the heat resistance magnesium alloy of high intensity, high-ductility and high creep resistance energy.
Description
Technical field
The present invention relates to a kind of regulation and control LPSO structures and the high-strength high-plastic heat resistance magnesium alloy of nanoprecipitation phase and its preparation
Method, belongs to Alloy Processing field.
Background technology
As most light structural metallic materials, magnesium has broad application prospects in lightweight field.But, magnesium alloy
Absolute intensity is relatively low, temperature-room type plasticity is not enough and seriously limits it in the popularization in each field and uses the shortcomings of poor heat resistance.
Magnesium-rare earth (Mg-RE systems) is the Typical Representative of high-strength magnesium alloy in existing magnesium alloy system.Due to the unique property of RE elements
Can, Mg-RE systems alloy can obtain high-strength or even superelevation strong by approach such as solution strengthening, precipitation hardening and complex intensifyings
Degree.As a rule, the mechanical property of magnesium-rare earth and rare earth element content are closely related.When RE contents are less, in satiety
It is low even without structural hardening effect with having in solid solution ag(e)ing process, the intensity and heat resistance of alloy can be caused poor；
And with increase RE contents make magnesium-rare earth close to high strength alumin ium alloy strength level when, can cause the plasticity of magnesium alloy acute again
Strong to decline, room temperature elongation is substantially reduced (＜ 3%).Accordingly, it would be desirable on the premise of alloying element content is controlled, seek effectively
The phase of Strengthening and Toughening second and Strengthening and Toughening structure improve the comprehensive mechanical property of magnesium alloy.
It is enhanced that Japanese scholars Kawamura is prepared for LPSO phases first using the method for rapid solidification/powder metallurgy
Mg97Y2Zn1(at%) alloy (Y.Kawamura, et al.Materials Transactions, 42 (2001) 1172-
1176), its room-temperature yield strength reaches 610MPa, elongation percentage 5%, and has good high-temperature behavior, in magnesium matrix crystal grain
The LPSO structures of formation are the main causes that the alloy property is improved.In addition, Mg-Y-Zn alloy systems are with age-hardening phenomenon
Exemplary alloy, the precipitation sequence of precipitated phase is followed successively by SSSS (hcp) → β " (D0 in ag(e)ing process19)→β'(cbco)→β
(bcc), wherein peak value timeliness β ' coherent precipitates have along [0001]αThe convex lens shape of elongation, significantly can hinder dislocation to transport
Reciprocation occurs for dynamic and crystal boundary, so as to improve alloy strength.Such as document《Microstructure and mechanical
properties of a Mg94Zn2Y4extruded alloy with long period stacking ordered
structure》Described in (H.Liu, et al.Transactions of Nonferrous Metals Society of
China, 23 (2013) 3598-3603), after Ageing Treatment, by the efficient hardening of β ' precipitated phases, As-extruded Mg94Zn2Y4
Tensile strength, yield strength and the elongation percentage of alloy are respectively 410MPa, 272MPa and 2.8%.
It can be seen that, using LPSO structures and nano beta ' precipitated phase can effectively improve the intensity of alloy, but the plasticity of alloy
It can be remarkably decreased, and as LPSO phases in alloy or β ' precipitate the increase of phase volume fraction, elongation percentage, which drastically declines, (to be less than
3%).Therefore, how on the basis of LPSO structures and β ' precipitated phase efficient hardenings, further improve the plasticity of magnesium alloy, be
Solve the key issue of such magnesium-rare earth application bottleneck.
The content of the invention
It is an object of the invention to provide a kind of high-strength high-plastic heat-resisting magnesium alloy preparation method.
The technical solution adopted by the present invention is：The high-strength high-plastic heat resistant magnesium of a kind of regulation and control LPSO structures and nanoprecipitation phase is closed
The preparation method of gold, its step includes：
A, Mg-Y-Zn alloy cast ingots are cut, be placed in equal channel angular extrusion die in 280~330 DEG C of progress
Insulation, then carries out the continuous Equal-channel Angular Pressing of 12~20 passages (ECAP) to ingot casting, obtains Ultra-fine Grained bulk；
B, by above-mentioned Ultra-fine Grained bulk be placed in heat-treatment furnace 350~400 DEG C be incubated 2~8h, be immediately placed in after taking-up
Quenched in water；It is subsequently placed in vacuum drying oven and is incubated 22~30h at 200~225 DEG C, is immediately placed in water and carries out after taking-up
Quenching, obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase；
Wherein Y in Mg-Y-Zn alloys：10~13wt%, Zn：3.32~5.31wt%, Y:Zn atomic ratios are more than or equal to 1.8
Less than or equal to 2.2, surplus is Mg.
It is preferred that, soaking time is 30min in step A.
It is preferred that, hardening heat is 25 DEG C in step B.
The invention also discloses above-mentioned method prepare it is high-strength high-plastic containing LPSO structures and nanoprecipitation phase
Heat resistance magnesium alloy.
When keeping Y/Zn atomic ratios close to 2 in Mg-Y-Zn alloys, 18R-LPSO/ α-Mg two-phase magnesium alloys can be obtained；And
With the increase of content of solute in alloy, the volume fraction of 18R-LPSO phases is continuously increased in alloy, therefore, alloy of the present invention
Composition range be：Y：10~13wt%, Zn：Zn：3.32~5.31wt%, Y:Zn atomic ratios are less than or equal to more than or equal to 1.8
2.2, surplus is Mg, it is ensured that alloy is 18R-LPSO/ α-Mg two-phase magnesium alloys；And the volume fraction of 18R-LPSO phases is moderate,
For 35~54%, can both avoid 18R-LPSO phase contents it is too low caused by enhancing effect it is not good, also inhibits 18R-LPSO phases and contain
Measure the too high obvious weakening to alloy plasticity；Meanwhile, the alloying component also assures that alloy has strong age-hardening feature.
When the temperature of heat treatment or thermoplasticity processing is higher than 350 DEG C, the 18R-LPSO in Mg-Y-Zn alloys meets gradually
Dissolving, while the transgranular 14H-LPSO phases for separating out lamellar.ECAP of the present invention processing temperature is 280~330 DEG C, can effectively be pressed down
Make the Dynamic Precipitation of the 14H-LPSO phases under thermal-stress coupling effect when ECAP is processed, it is ensured that after being processed through ECAP in alloy
The still all 18R structures of LPSO phases, are easy to follow-up dual two kinds of LPSO structures of heat treatment accuracy controlling.In addition, 18R-LPSO phases
Kinking can occur after being processed through traditional plastic, the formation of kind band can reduce alloy plasticity while alloy strength is improved.This
Invention, can effectively crystal grain thinning, the uniformity of raising ultrafine-grained (UFG) microstructure, and make using the processing of 12~20 multi-pass continuous ECAPs
18R-LPSO phases are broken at kinking, and the graininess for being refined as 0.5~2 μm is distributed in grain boundaries.Connect by multi-pass of the present invention
After continuous ECAP processing, the microscopic structure of the magnesium alloy of acquisition is ultra-fine α-Mg crystal grain+crystal boundary 18R-LPSO particles, with moderate
Intensity, tensile strength ＞ 350MPa, and excellent plasticity, elongation percentage ＞ 20%.
First time heat treatment condition of the invention be 350~400 DEG C be incubated 2~8h, can be achieved alloy in 18R and 14H this
The Effective Regulation of two kinds of LPSO phases.From heat treatment temperature at 350~400 DEG C, it can both ensure 14H-LPSO precipitation, also can
Suppress growing up for ultra-fine grain.By controlling heat treatment temperature and time, the shape of both LPSO phases of 18R and 14H can be regulated and controled
State, volume fraction and Spatial Distribution Pattern.Second of heat treatment condition of the present invention is to be incubated 22~30h at 200~225 DEG C, can
Realize effective precipitation of peak timeliness nanoprecipitation phase.Meanwhile, the heat treatment temperature is relatively low, will not be to LPSO phases and Ultra-fine Grained
Grain produces influence.After dual heat treatment, polynary LPSO structures can be obtained the ultra-fine of complex intensifying is mutually cooperateed with nanoprecipitation
Brilliant high-strength high-plastic heat resistance magnesium alloy.
The present invention processes to obtain by the continuous Equal-channel Angular Pressing of multi-pass (ECAP) contains LPSO knots with high-ductility
The ultrafine grain rare earth magnesium alloy of structure, and then the LPSO structures in alloy are regulated and controled by dual heat treatment, and introduce nanometer
Precipitated phase, strengthened using refined crystalline strengthening, LPSO phases and nanoprecipitation mutually strengthen the combinations of these three intensifiers with uniformly,
The magnesium alloy of acquisition has following characteristic：
(1) the brilliant crystallite dimension of homogenous superfine is 0.5~1.5 μm, and the volume fraction of LPSO phases is moderate (32~54%), is closed
Gold utensil has good plasticity.
(2), can be real on the premise of ultra-fine grain is not grown up by controlling the temperature and time of dual heat treatment
Now to the Effective Regulation of the form, volume fraction and spatial distribution of both LPSO structures of 18R in ultra-fine grain and 14H, and analyse
Go out the nanoprecipitation phase of Dispersed precipitate.
(3) refined crystalline strengthening, LPSO phases strengthen and precipitation strength combination with uniformly, can make alloy obtain high intensity；
Meanwhile, crystal boundary 18R-LPSO particles+transgranular 14H-LPSO synusia+transgranular nanoprecipitation mutually cooperates with the heat endurance of composite reinforcement
It is good, at high temperature can effectively pin crystal boundary, suppress crystal grain and grow up, make alloy that there is good mechanical behavior under high temperature.
(4) magnesium alloy obtained has good comprehensive mechanical property, and room temperature tensile intensity is more than 400MPa, yield strength
More than 300MPa, elongation percentage is more than 15%, and the secondary creep rates under 250 DEG C/80MPa creep conditions are less than 5 X 10-8s-1。
Brief description of the drawings
Fig. 1 is that 14H-LPSO phases in ultra-fine grain in obtained high-strength high-plastic heat resistance magnesium alloy in embodiment 1 and nanometer are heavy
The TEM photos of shallow lake phase
Embodiment
Technical scheme is further described below by way of specific embodiment, but the present invention be not limited to
Lower specific embodiment.
Embodiment 1
It is Mg-10wt%Y-3.32wt%Zn, Y by composition:Zn atomic ratios are cut for 2.2 alloy cast ingot, are placed in
Insulation 30min is carried out at 280 DEG C in equal channel angular extrusion die, then carrying out the continuous equal channel angular of 12 passages to ingot casting squeezes
Pressure, obtains Ultra-fine Grained bulk；Above-mentioned Ultra-fine Grained bulk is placed in heat-treatment furnace and is incubated 2h at 350 DEG C, is immediately placed in after taking-up
Quenched in 25 DEG C of water；It is subsequently placed in vacuum drying oven and is incubated 30h at 225 DEG C, is immediately placed in 25 DEG C of water and carries out after taking-up
Quenching, obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The average diameter of ultra-fine grain is about in alloy
1.3 μm, the volume fraction of LPSO phases is 32%.Fig. 1 shines for the 14H-LPSO phases and the TEM of nanoprecipitation phase in ultra-fine grain
Piece, the width of the 14H synusia of transgranular precipitation is about 60nm, and length of the precipitated phase along long axis direction is 30~50nm, and 14H-
The long axis direction of LPSO and β ' precipitated phases is orthogonal, the two all in α-Mg be in symbiosis and epibiosis, the specific position to structure more
Be conducive to hindering transgranular dislocation motion and suppress crystal boundary migration, so that alloy obtains excellent comprehensive mechanical property.Table 1 is arranged
The mechanical property of alloy is gone out, it is seen that the alloy has high intensity, high-ductility and excellent high-temperature creep resistance.
Embodiment 2
It is Mg-11wt%Y-4wt%Zn, Y by composition:Zn atomic ratios are cut for 2 alloy cast ingot, the passage such as are placed in
Insulation 30min is carried out at 300 DEG C in angular extrusion die, the continuous Equal-channel Angular Pressing of 16 passages then is carried out to ingot casting, obtained
Obtain Ultra-fine Grained bulk；Above-mentioned Ultra-fine Grained bulk is placed in heat-treatment furnace and is incubated 4h at 360 DEG C, 25 DEG C of water are immediately placed in after taking-up
It is middle to be quenched；It is subsequently placed in vacuum drying oven and is incubated 28h at 220 DEG C, is immediately placed in 25 DEG C of water and is quenched after taking-up, obtained
To the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The average diameter of ultra-fine grain is about 1.1 μm in alloy,
The volume fraction of LPSO phases is 38%, and the mechanical property of alloy is shown in Table 1.
Embodiment 3
It is Mg-12wt%Y-4wt%Zn, Y by composition:Zn atomic ratios are cut for 2.2 alloy cast ingot, are placed in etc. and to be led to
Insulation 30min is carried out at 310 DEG C in road angular extrusion die, the continuous Equal-channel Angular Pressing of 16 passages then is carried out to ingot casting,
Obtain Ultra-fine Grained bulk；Above-mentioned Ultra-fine Grained bulk is placed in heat-treatment furnace and is incubated 5h at 370 DEG C, 25 DEG C are immediately placed in after taking-up
Quenched in water；It is subsequently placed in vacuum drying oven and is incubated 25h at 210 DEG C, is immediately placed in 25 DEG C of water and is quenched after taking-up,
Obtain the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The average diameter of ultra-fine grain is about 1.0 μm in alloy,
The volume fraction of LPSO phases is 44%, and the mechanical property of alloy is shown in Table 1.
Embodiment 4
It is Mg-12wt%Y-4.5wt%Zn, Y by composition:Zn atomic ratios are cut for 1.96 alloy cast ingot, are placed in
Insulation 30min is carried out at 320 DEG C in equal channel angular extrusion die, then carrying out the continuous equal channel angular of 18 passages to ingot casting squeezes
Pressure, obtains Ultra-fine Grained bulk；Above-mentioned Ultra-fine Grained bulk is placed in heat-treatment furnace and is incubated 6h at 390 DEG C, is immediately placed in after taking-up
Quenched in 25 DEG C of water；It is subsequently placed in vacuum drying oven and is incubated 24h at 200 DEG C, is immediately placed in 25 DEG C of water and carries out after taking-up
Quenching, obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The average diameter of ultra-fine grain is about in alloy
0.8 μm, the volume fraction of LPSO phases is 46%, and the mechanical property of alloy is shown in Table 1.
Embodiment 5
It is Mg-13wt%Y-5.31wt%Zn, Y by composition:Zn atomic ratios are cut for 1.8 alloy cast ingot, are placed in
Insulation 30min is carried out at 330 DEG C in equal channel angular extrusion die, then carrying out the continuous equal channel angular of 20 passages to ingot casting squeezes
Pressure, obtains Ultra-fine Grained bulk；Above-mentioned Ultra-fine Grained bulk is placed in heat-treatment furnace and is incubated 8h at 400 DEG C, is immediately placed in after taking-up
Quenched in 25 DEG C of water；It is subsequently placed in vacuum drying oven and is incubated 22h at 200 DEG C, is immediately placed in 25 DEG C of water and carries out after taking-up
Quenching, obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase.The average diameter of ultra-fine grain is about in alloy
0.6 μm, the volume fraction of LPSO phases is 54%, and the mechanical property of alloy is shown in Table 1.
The comprehensive mechanical property of magnesium alloy made from the embodiment 1-5 of table 1 and its with WE54 heat resistance magnesium alloys and other
The performance comparison of the magnesium alloy of structure containing LPSO
[1] solid solution+Ageing Treatment, accounts for bright etc., casting, 60 (2011) 126-128.
[2] hot extrusion state, Zhen Rui, Ph.D. Dissertation, Southeast China University, 2015.
[3] prepared by rapid solidification/powder metallurgic method, Y.Kawamura, et al.Materials Transactions, and 42
(2001)1172-1176。
[4]+4 passage ECAP, J.S.Zhang, et al.Materials Science and Engineering are cast
A,559(2013)416-420。
[5] prepared by rapid solidification/powder metallurgic method, J.Zhu, et al.Journal of Alloys and
Compounds,703(2017)508-516.
[6] hot extrusion+Ageing Treatment, C.Xu, et al.Scientific Report, 7 (2017) 43391.
Claims (4)
1. a kind of preparation method of the high-strength high-plastic heat resistance magnesium alloy of regulation and control LPSO structures and nanoprecipitation phase, its step includes：
A, Mg-Y-Zn alloy cast ingots are cut, are placed in equal channel angular extrusion die and are incubated at 280~330 DEG C,
Then the continuous Equal-channel Angular Pressing of 12~20 passages is carried out to ingot casting, obtains Ultra-fine Grained bulk；
B, by above-mentioned Ultra-fine Grained bulk be placed in heat-treatment furnace 350~400 DEG C be incubated 2~8h, be immediately placed in after taking-up in water
Quenched；It is subsequently placed in vacuum drying oven and is incubated 22~30h at 200~225 DEG C, is immediately placed in water and is quenched after taking-up
Fire, obtains the ultra-fine grained magnesium alloy containing LPSO structures and nanoprecipitation phase；
Wherein Y in Mg-Y-Zn alloys：10~13wt%, Zn：3.32~5.31wt%, Y:Zn atomic ratios are less than more than or equal to 1.8
Equal to 2.2, surplus is Mg.
2. the preparation side of the high-strength high-plastic heat resistance magnesium alloy of regulation and control LPSO structures according to claim 1 and nanoprecipitation phase
Method, it is characterised in that：Soaking time is 30min in step A.
3. the preparation side of the high-strength high-plastic heat resistance magnesium alloy of regulation and control LPSO structures according to claim 1 and nanoprecipitation phase
Method, it is characterised in that：Hardening heat is 25 DEG C in step B.
4. the high-strength height containing LPSO structures and nanoprecipitation phase that the method any one of claim 1-3 is prepared
Mould heat resistance magnesium alloy.
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Cited By (6)
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|---|---|---|---|---|
| CN111101041A (en) * | 2020-01-13 | 2020-05-05 | 长沙理工大学 | Magnesium-yttrium-zinc hydrogen storage magnesium alloy and preparation method thereof |
| CN111334694A (en) * | 2020-04-14 | 2020-06-26 | 燕山大学 | Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase |
| CN111961937A (en) * | 2020-09-11 | 2020-11-20 | 河海大学 | Magnesium-based alloy wire with controllable degradation and preparation method thereof |
| CN112080675A (en) * | 2020-09-11 | 2020-12-15 | 河海大学 | High-strength and high-toughness magnesium/magnesium composite material with gradient interface and preparation method thereof |
| CN112359255A (en) * | 2020-11-11 | 2021-02-12 | 沈阳工业大学 | High-strength low-heat-cracking magnesium alloy |
| CN115418584A (en) * | 2022-08-26 | 2022-12-02 | 昆明理工大学 | Method for improving thermal stability of two-dimensional nano magnesium alloy material |
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| CN112080675A (en) * | 2020-09-11 | 2020-12-15 | 河海大学 | High-strength and high-toughness magnesium/magnesium composite material with gradient interface and preparation method thereof |
| CN112080675B (en) * | 2020-09-11 | 2021-09-07 | 河海大学 | High-strength and high-toughness magnesium/magnesium composite material with gradient interface and preparation method thereof |
| CN112359255A (en) * | 2020-11-11 | 2021-02-12 | 沈阳工业大学 | High-strength low-heat-cracking magnesium alloy |
| CN115418584A (en) * | 2022-08-26 | 2022-12-02 | 昆明理工大学 | Method for improving thermal stability of two-dimensional nano magnesium alloy material |
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