CN102618766B - A kind of preparation method of quasicrystal reinforced high-strength Mg-Zn-Y alloy - Google Patents
A kind of preparation method of quasicrystal reinforced high-strength Mg-Zn-Y alloy Download PDFInfo
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- CN102618766B CN102618766B CN 201210119861 CN201210119861A CN102618766B CN 102618766 B CN102618766 B CN 102618766B CN 201210119861 CN201210119861 CN 201210119861 CN 201210119861 A CN201210119861 A CN 201210119861A CN 102618766 B CN102618766 B CN 102618766B
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- 229910000946 Y alloy Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000013079 quasicrystal Substances 0.000 title claims abstract description 7
- 239000000956 alloy Substances 0.000 claims abstract description 47
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 46
- 239000011777 magnesium Substances 0.000 claims abstract description 26
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 23
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 18
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 14
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 9
- 238000003723 Smelting Methods 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims 1
- 239000002893 slag Substances 0.000 claims 1
- 239000006104 solid solution Substances 0.000 abstract description 13
- 239000011159 matrix material Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 229910002058 ternary alloy Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010120 permanent mold casting Methods 0.000 description 1
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- Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
Abstract
本发明是一种高强度镁合金的制备方法，特别是一种通过固溶时效析出细小近球状准晶相增强高强度Mg-Zn-Y合金。本发明的合金中化学元素质量百分比：5.0-6.0%Zn，1.0%Y，余量为Mg，且Zn与Y质量比介于5~6之间。其中Zn以纯Zn加入，Y以Mg-25wt.%Y中间合金形式加入，Mg则采用工业纯镁。本发明镁合金经过预热、熔炼、精炼、金属型成型和热处理后得到的合金组织为α-Mg固溶体和二十面体准晶相，且准晶形态近似球状，尺寸细小。弥散析出的准晶颗粒依靠对位错的强钉扎和与基体形成牢固的界面，可显著增强镁合金。本发明的高强镁合金，其抗拉强度大于250MPa，延伸率大于5%。本发明可进一步推动高强镁合金在航空、航天、交通等众多领域的广泛应用。The invention relates to a preparation method of a high-strength magnesium alloy, in particular to a high-strength Mg-Zn-Y alloy reinforced by precipitation of fine near-spherical quasi-crystalline phases through solid solution aging. The mass percentage of chemical elements in the alloy of the present invention: 5.0-6.0% Zn, 1.0% Y, the balance is Mg, and the mass ratio of Zn and Y is between 5-6. Among them, Zn is added as pure Zn, Y is added as Mg-25wt.% Y master alloy, and Mg is industrially pure magnesium. The alloy microstructure obtained after preheating, smelting, refining, metal molding and heat treatment of the magnesium alloy of the present invention is α-Mg solid solution and icosahedral quasicrystal phase, and the quasicrystal shape is approximately spherical and small in size. Dispersed and precipitated quasicrystalline particles can significantly strengthen magnesium alloys by virtue of strong pinning of dislocations and formation of a firm interface with the matrix. The high-strength magnesium alloy of the present invention has a tensile strength greater than 250MPa and an elongation greater than 5%. The invention can further promote the wide application of the high-strength magnesium alloy in many fields such as aviation, spaceflight, and transportation.
Description
Technical field
The present invention relates to the preparation method of high-strength magnesium alloy material and technology of preparing, particularly a kind of quasicrystal reinforced magnesium alloy.
Technical background
Magnesium alloy is the lightest structural metallic materials during engineering is used, and is described as " 21st century green engineering structural metallic materials ".Along with the fast development in fields such as Aeronautics and Astronautics, traffic, the strong magnesium alloy of lightweight height ratio is had higher requirement in recent years, on alloy designs, advanced machining technology, seek new breakthrough thereby force people to have to try every means.The Mg-Zn-Y alloy is a kind of very promising high strength and low cost magnesium alloy, mainly is because this alloy just can obtain having the icosahedral quasicrystal phase (I-phase) of high powerful feature under the routine casting condition.The two-phase coexistent district that has accurate crystalline substance and α-Mg in the Mg-Zn-Y ternary alloy system, this contains accurate brilliant high-performance Mg-Zn-Y alloy to exploitation and has the important engineering meaning.Yet the accurate crystalline phase that is herring-bone form in the Mg-Zn-Y alloy that adopts the routine casting method to prepare is very thick, material mechanical performance is difficult to the contribution that provides useful.
Summary of the invention
The present invention mainly is at above deficiency, provides a kind of particle the accurate brilliant preparation method who strengthens high-strength magnesium alloy.Technical scheme of the present invention is:
(1) select the Mg-Zn-Y alloy, chemical element mass percent in this alloy: 5.0-6.0% Zn, 1.0% Y, surplus is Mg, and Zn and Y mass ratio can guarantee to obtain in the as-cast structure accurate brilliant and α-Mg two-phase like this between 5 ~ 6.
(2) crucible is preheating to 200 ℃, brushes general magnesium alloy smelting crucible coating.Crucible is heated to 500 ℃, joins technical pure Mg in the crucible and begin to feed the CO2+0.5vol%SF6 mixed gas and protect.Continue to be warmed up to 720 ℃ treat that pure magnesium melts fully after, add pure Zn, the Mg-25wt.%Y master alloy; Mg-25wt.%Y master alloy adding mode is for to be pressed in the alloy melt with iron bell jar, and slightly to around move about, prevent the poly-partially of rare earth, rare earth is diffused in the liquation rapidly equably.Pure Zn just can take out bell jar after being pressed into the alloy melt bottom with bell jar.Be warmed up to 750 ℃ and be incubated 20 ~ 30 minutes, treat that master alloy, pure Zn melt fully, carry out the melt refining treatment with C2Cl6, slagging-off and cool the temperature to 700 ℃ after the refining pours into the moulding of air cooling metal mold.The whole smelting and pouring process of alloy is all carried out under CO2+0.5vol%SF6 is mixed gas protected.
(3) heat-treat.Alloy is at first 450 ℃ of following solid solutions 16 hours, then 500 ℃ of solid solutions 20 hours.After treating solution treatment, the artificial aging that sample carried out under 360 ℃ 24 hours is handled.Adopting the reason of segmentation solid solution is to make the abundant solid solution of accurate crystalline phase of difficult solid solution enter matrix.Obtain the accurate brilliant of approximate spherical fine size after the timeliness, can play obvious strengthening effect.
The high-strength magnesium alloy of the present invention's preparation, its benefit is: strength of alloy is greater than 250MPa, and unit elongation is greater than 5%.
In the Mg-Zn-Y ternary alloy system, there is the two-phase coexistent district of accurate crystalline substance and α-Mg, this contains accurate brilliant high-performance Mg-Zn-Y to exploitation and has the important engineering meaning.The accurate brilliant enhancing high-performance Mg-Zn-Y series magnesium alloy crystal grain of routine casting is generally comparatively thick, isolates matrix easily, causes alloy mechanical property on the low side.In order to improve accurate brilliant thick problem, the present invention at first controls as cast condition accurate brilliant form and distribution by permanent mold casting, because the chilling action of metal mold, the alloy rate of cooling is very big, limited growing up of accurate crystalline substance, to a certain extent refinement accurate crystalline substance and it is disperseed preferably.Secondly, prepare to contain by heat treating method again and separate out accurate brilliant enhanced Mg-Zn-Y alloy.In heat treatment process, we have adopted the segmentation solid solution treatment process, make the accurate crystalline substance of as cast condition to greatest extent solid solution enter behind the matrix again timeliness and separate out, the accurate crystalline phase of separating out has tiny, the approximate globular feature of size can significantly improve alloy strength.
The high strength that accurate brilliant enhancing Mg-Zn-Y is an alloy is mainly derived from the strengthening effect of quasicrystal particle, and is accurate brilliant in forming stable accurate crystalline substance/magnesium matrix interface and the strong pinning of dislocation being realized alloy strengthening.
Embodiment
Embodiment 1
Present embodiment is a kind of high-strength Mg-Zn-Y alloy, and its composition is Mg-5wt.%Zn-1wt.%Y, and Zn and Y mass ratio are 5, and wherein Zn adds with industrial Zn, and Y adds with the Mg-25wt.%Y master alloy, and Mg then adopts pure magnesium.
The preparation method of present embodiment is:
The first step is preheating to 200 ℃ with crucible, brushes general magnesium alloy smelting crucible coating;
Second step was heated to 500 ℃ with crucible, joined technical pure Mg in the crucible and began to feed the CO2+0.5vol%SF6 mixed gas and protect;
In the 3rd step, after continuing to be warmed up to pure magnesium and melting fully, add Zn, Mg-25wt.%Y master alloy at 720 ℃.Mg-25wt.%Y master alloy adding mode is for to be pressed in the alloy melt with iron bell jar, and slightly to around move about, prevent the poly-partially of rare earth, rare earth is diffused in the liquation rapidly equably.Pure Zn just can take out bell jar after being pressed into the alloy melt bottom with bell jar.
The 4th step was warmed up to 750 ℃ and be incubated 20 ~ 30 minutes, treated that master alloy, pure Zn melt fully;
The 5th the step, carry out the melt refining treatment with C2Cl6, after the refining slagging-off and cool the temperature to 700 ℃, pour into the moulding of air cooling metal mold; The whole smelting and pouring process of alloy is all carried out under CO2+0.5vol%SF6 is mixed gas protected.
In the 6th step, heat-treat.Alloy at first, is followed 500 ℃ of solid solutions 20 hours after 16 hours 450 ℃ of following solid solutions.After treating solution treatment, the artificial aging that sample carried out under 360 ℃ 24 hours is handled.Timeliness is organized as α-Mg sosoloid, and its inside tiny I-phase that distributing, and accurate crystalline form attitude is approximate spherical.
Alloy sample is carried out mechanics property analysis, and the result shows that the maximum tensile strength of this alloy room temperature is 246MPa, and yield strength is 60MPa, and unit elongation is 7.4%.
Embodiment 2
Present embodiment is a kind of high-strength Mg-Zn-Y alloy, and it becomes and is Mg-6wt.%Zn-1wt.%Y, and Zn and Y mass ratio are 6, and wherein Zn adds with industrial Zn, and Y adds with the Mg-25wt.%Y master alloy, and Mg then adopts pure magnesium.
The preparation method of present embodiment is:
The first step is preheating to 200 ℃ with crucible, brushes general magnesium alloy smelting crucible coating;
Second step was heated to 500 ℃ with crucible, joined technical pure Mg in the crucible and began to feed the CO2+0.5vol%SF6 mixed gas and protect;
In the 3rd step, after continuing to be warmed up to pure magnesium and melting fully, add Zn, Mg-25wt.%Y master alloy at 720 ℃.Mg-25wt.%Y master alloy adding mode is for to be pressed in the alloy melt with iron bell jar, and slightly to around move about, prevent the poly-partially of rare earth, rare earth is diffused in the liquation rapidly equably.Pure Zn just can take out bell jar after being pressed into the alloy melt bottom with bell jar;
The 4th step was warmed up to 750 ℃ and be incubated 20 ~ 30min, treated that master alloy, pure Zn melt fully;
The 5th the step, carry out the melt refining treatment with C2Cl6, after the refining slagging-off and cool the temperature to 700 ℃, pour into the moulding of air cooling metal mold.The whole smelting and pouring process of alloy is all carried out under CO2+0.5vol%SF6 is mixed gas protected;
In the 6th step, heat-treat.Alloy at first, is followed 500 ℃ of solid solutions 20 hours after 16 hours 450 ℃ of following solid solutions.After treating solution treatment, the artificial aging that sample carried out under 360 ℃ 24 hours is handled.
The alloy aging tissue is similarly α-Mg sosoloid, its inside tiny I-phase that distributing, and accurate crystalline form attitude is approximate spherical.Alloy sample is carried out mechanics property analysis, and the result shows that the maximum tensile strength of this alloy room temperature is 266MPa, and yield strength is 62MPa, and unit elongation is 7%.
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| CN103320663B (en) * | 2013-05-31 | 2015-06-24 | 中国科学院金属研究所 | Quasicrystal-containing magnesium alloy with high corrosion resistance and preparation method and application thereof |
| CN103993213B (en) * | 2014-05-27 | 2017-11-14 | 华东交通大学 | A kind of preparation method of double special construction phase composite strengthening Mg Zn y alloys |
| CN105714132B (en) * | 2014-12-03 | 2018-10-23 | 华东交通大学 | A kind of preparation method of high damping material while containing quasi-crystalline substance and long-periodic structure phase |
| CN105316550B (en) * | 2015-03-12 | 2019-01-25 | 华东交通大学 | A kind of high damping magnesium alloy containing long period structure phase and preparation method thereof |
| JP6594663B2 (en) * | 2015-05-27 | 2019-10-23 | 本田技研工業株式会社 | Heat-resistant magnesium casting alloy and its manufacturing method |
| CN104894445B (en) * | 2015-06-29 | 2017-04-12 | 西南交通大学 | Production method of ultrahigh-ductility Mg-Zn-Y alloy |
| CN105274412B (en) * | 2015-10-16 | 2017-05-17 | 东北大学 | Mg-Zn-Y directional solidification alloy and preparing method thereof |
| CN105256262B (en) * | 2015-10-29 | 2017-08-11 | 东北大学 | The method that Mg Zn y alloy aging hardening effects are improved by preset twin |
| CN108467962B (en) * | 2018-04-13 | 2019-12-17 | 中北大学 | A preparation method of magnesium zinc yttrium quasicrystal and boron carbide mixed reinforced magnesium matrix composite material |
| CN109763009A (en) * | 2019-03-07 | 2019-05-17 | 济南大学 | A kind of method of electric current processing Mg-Zn-Gd quasicrystalline alloy |
| CN110004343B (en) * | 2019-03-29 | 2021-07-13 | 上海交通大学 | High-strength, toughness and heat-resistant Mg-Gd-Er alloy suitable for gravity casting and preparation method thereof |
| CN109852857B (en) * | 2019-03-29 | 2021-08-06 | 上海交通大学 | High-strength, toughness and heat-resistant Mg-Y alloy suitable for gravity casting and preparation method thereof |
| CN109868402B (en) * | 2019-03-29 | 2021-08-17 | 上海交通大学 | High strength, toughness and heat resistance die-casting Mg-Y alloy and preparation method thereof |
| CN111621726A (en) * | 2020-05-22 | 2020-09-04 | 华东交通大学 | Preparation method of high-damping Mg-Zn-Y-based composite material |
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| CN100497697C (en) * | 2006-12-20 | 2009-06-10 | 太原理工大学 | Pseudo-crystal reinforced high zinc magnesium alloy and method for manufacturing same |
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