CN102766791A - Quasicrystal-strengthened Mg-6Zn-3Y alloy with ultrafine solidification texture and preparation method thereof - Google Patents
Quasicrystal-strengthened Mg-6Zn-3Y alloy with ultrafine solidification texture and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a quasicrystal-strengthened Mg-6Zn-3Y alloy with an ultrafine solidification texture and a preparation method thereof. The quasicrystal-strengthened Mg-6Zn-3Y alloy consists of the following chemical components in percentage by weight: 87.0 to 93.0 percent of Mg, 3.0 to 10.0 percent of Zn and 0.5 to 3.0 percent of Y. The Mg-6Zn-3Y alloy with the ultrafine solidification texture, which contains nanoscale granular quasicrystals, is prepared from normal-pressure as-cast Mg-Zn-Y alloy material under GPa-level ultrahigh pressure as solidification pressure, temperature and solidification cooling rate are controlled. The as-cast texture is characterized in that: the granular quasicrystals are evenly and dispersely distributed on the ultrafine Alpha-Mg matrix, wherein the secondary dendrite arm spacing between Alpha-Mg dendrites is 7Mu m to 10Mu m, the diameter of the granular quasicrystal is 50nm to 100nm, and the volume of the granular quasicrystals accounts for 25 to 35 percent of the total volume of the alloy. The invention adopts a cubic press, solidification process parameters are controlled, i.e., the solidification pressure is 6GPa, the solidification temperature is 1300DEG C, and the solidification rate is 300K/S. Theultrafin quasicrystal-strengthened Mg-6Zn-3Y alloy has high mechanical properties and good thermal stability.
Description
Technical field
The present invention relates to a kind of spontaneous accurate brilliant Alloy And Preparation Method that strengthens of ultra-fine solidified structure, the specifically a kind of accurate brilliant Mg-6Zn-3Y of enhancing Alloy And Preparation Method with ultra-fine solidified structure.
Background technology
Magnesiumalloy has characteristics such as good electric conductivity, thermal conductivity, capability of electromagnetic shielding and high specific tenacity, specific rigidity, damping property; Be the lightest structural metallic materials of present practical application, have broad application prospects in industries such as aerospace, automobile and 3C (computingmachine, communicate by letter and consumption electronic product).Yet magnesiumalloy is because problems such as intensity is lower, poor toughness, the good high temperature creep property difference of plastic working difficulty have limited its further application in industry.Therefore, improve magnesium alloy mechanical property, enlarge the emphasis that the magnesiumalloy range of application is the research and development of magnesiumalloy technical field through various technologies of preparing.
From the Xie Qieman people such as (D.shechtman) of National Bureau of Standards (NBS) in 1984 finds accurate crystalline substance first in the Al-Mn of chilling alloy since, in aluminium base, magnesium base and other alloy, found a variety of accurate brilliant in succession.1993, the Luo Zhi equality people of China Beijing Inst. of Aeronautical Materials confirmed that at first the Mg3Zn6Y ternary phase in the Mg-Zn-Y alloy is an icosahedral quasicrystal, and was that accurate crystalline substance has carried out number of research projects to Mg-Zn-RE.Accurate crystalline phase makes it have excellent mechanical property and physicals because of having unique atomic arrangement structure, like HS, low-friction coefficient, lower thermal conductivity, low conductivity, anti-oxidant, corrosion-resistant etc.Research shows; Thinning microstructure is one of topmost enhancement method of magnesiumalloy; And as accurate crystalline form looks, size, quantity and the distribution of wild phase performance important influence to Magnuminium; The disperse granular accurate crystalline phase that distributes is expected to obtain high-performance quasicrystal particle reinforced magnesium matrix alloy material and matrix material on magnesium alloy substrate.
Find through retrieval, in disclosed technology, disclose magnesium base spherical quasi crystal master alloy and preparation method thereof like CN 101705405 A; Adopt the method for controlled chilling speed to prepare five yuan of magnesium bases of Mg-Zn-Y-Mn-Cu icosahedron spherical quasi crystal master alloy; Its chemical ingredients is (wt. %): Mg 55.0 ~ 65.0%, and Zn 30.0 ~ 40.0%, and Y 2.5 ~ 5.5%; Mn 0.10 ~ 1.50%, and Cu 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 2 ~ 7, and volume accounts for 35 ~ 45% of TV.
As; CN 101705406 A disclose magnesium base spherical quasi crystal master alloy and preparation method thereof; Adopt the method for controlled chilling speed to prepare Mg-Zn-Y-C quaternary magnesium base icosahedron spherical quasi crystal master alloy, its chemical ingredients is (wt. %): Mg 55.0 ~ 65.0%, and Zn 30.0 ~ 40.0%; Y 2.5 ~ 5.5%, and C 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 2 ~ 7, and volume accounts for 40 ~ 48% of TV.
As; CN 101705407 A disclose magnesium base spherical quasi crystal master alloy and method for making thereof; Adopt the method for controlled chilling speed to prepare Mg-Zn-Y-Ti quaternary magnesium base icosahedron spherical quasi crystal master alloy, its chemical ingredients is (wt. %): Mg 55.0 ~ 65.0%, and Zn 30.0 ~ 40.0%; Y 2.5 ~ 5.5%, and Ti 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 6 ~ 10, and volume accounts for 30 ~ 40% of TV.
As; CN 102212727 A disclose a kind of spontaneous accurate brilliant Mg-Zn-Y alloy and melting method of strengthening; Be employed in the method that adds Al-Ti-C in the melt and prepared the spontaneous accurate brilliant Mg-Zn-Y of enhancing alloy; Its chemical ingredients is (wt. %): Zn 3.0 ~ 10.0%, and Y 0.5 ~ 3.0%, and Al-Ti-C 0.05 ~ 1.0%.
In sum; Above-mentioned disclosed patented technology content mainly be common solidify with the rapid solidification condition under the magnesium base spherical quasi crystal master alloy that makes; Its prepared icosahedral quasicrystal phase yardstick that goes out is level; And about accurate brilliant yardstick at other report of level seldom, especially have the accurate brilliant Mg-6Zn-3Y of the enhancing alloy of ultra-fine solidified structure for preparation under ultra-high voltage and do not see relevant report.
Summary of the invention
In view of above-mentioned present situation; The purpose of this invention is to provide a kind of accurate brilliant Mg-6Zn-3Y of enhancing magnesiumalloy with ultra-fine solidified structure, the prepared quasicrystal reinforced magnesium alloy with the accurate crystalline substance of spontaneous nanometer and ultra-fine solidified structure has higher mechanical property and thermostability.
Another object of the present invention has provided the preparation method of this Mg-6Zn-3Y alloy, under GPa level ultra-high voltage, has the quasicrystal reinforced magnesium alloy of ultra-fine solidified structure through the method preparation of control freezing pressure, Heating temperature and rate of cooling.
The technical scheme that technical solution problem of the present invention is taked is:
Have the accurate brilliant alloy that strengthens of ultra-fine solidified structure, its chemical ingredients is counted by mass percent wt%: Mg: 87.0 ~ 93.0%, Zn: 3.0 ~ 10.0%, Y: 1.0 ~ 3.0%.
The preparation method of the spontaneous quasicrystal reinforced magnesium alloy of said ultra-fine solidified structure comprises the steps:
1, as cast condition Mg-Zn-Y alloy material under the preparation normal pressure:
Getting and accounting for raw material total amount mass percent is 91.0% magnesium ingot, 6.0% zinc ingot metal, 3.0% pure yttrium, puts into baking oven and under 200 ℃, carries out preheating baking, and the Heating temperature of crucible electrical resistance furnace is set at 760 ~ 780 ℃; When crucible temperature rises to 350 ~ 400 ℃, in crucible, add magnesium ingot and zinc ingot metal earlier, begin to feed the CO2/SF6 mixed gas as protection gas; Continue to heat up, treat that magnesium ingot and zinc ingot metal in the crucible melts fully after, add pure yttrium again; Treat that pure yttrium melts the back fully and stirred 2 ~ 5 minutes; 760 ~ 780 ℃ of insulations 10 ~ 15 minutes, remove the solution surface scum silica frost, the Mg-Zn-Y alloy solution is cast in the metal pattern; Obtain Mg-6Zn-3Y cast alloy material, the cast alloy material is carried out abundant diffusion annealing;
2, control freezing pressure, Heating temperature and rate of cooling prepare the accurate brilliant Mg-6Zn-3Y of the enhancing alloy with ultra-fine solidified structure under GPa level ultra-high voltage:
The Mg-6Zn-3Y alloy material that step 1 is obtained carries out the line cutting, and the high pressure that is processed into Ф 4 х 5mm is used sample, and puts into graphite assembling cover; Graphite assembling cover is put into an actor's rendering of an operatic tune of CS-1B type high pressure six-plane piercer; The setting freezing pressure is 6GPa, and Heating temperature is 1300 ℃, is heated rapidly to preset Heating temperature; Make sample melt fully; And under this temperature heat-insulation pressure keeping 15min, to solidify rate of cooling be 300K/S in control, finally makes the accurate brilliant Mg-6Zn-3Y of the enhancing alloy of the ultra-fine solidified structure that contains the icosahedral quasicrystal phase.
In the present invention; Quasicrystal reinforced magnesium alloy with ultra-fine solidified structure, its Characteristics of As-cast Structure is made up of granular accurate crystalline substance, α-Mg matrix and Mg-Zn-Y ternary phase, in as-cast structure; The secondary dendrite arm spacing of α-Mg dendrite is 7-10 μ m; Granular accurate crystalline phase is the I-Mg3Zn6Y phase with icosahedral structure of virus, and its diameter is 50-100 μ m, and granular accurate brilliant volume accounts for 25 ~ 35% of this alloy TV.
In the present invention, related graphite assembling cover comprises the boron nitride crucible, plumbago crucible, the WC supercharging post that set gradually in the agalmatolite, and six of said graphite assembling cover is faced should have the hammer of pressure, and the Mg-6Zn-3Y alloy sample is placed in the boron nitride crucible.
The invention has the beneficial effects as follows:
One, to have one of the innovative point of the accurate brilliant Mg-6Zn-3Y of the enhancing alloy preparation method of ultra-fine solidified structure be under GPa level superelevation in the present invention, through control freezing pressure, Heating temperature with solidify rate of cooling and obtain required alloy material.
1, freezing pressure has great influence to the acquisition of ultra-fine dendritic structure: when under GPa level high pressure, solidifying; It is little that the solute spread coefficient can be the index demultiplication; Then in matrix, form the solute atoms enrichment region easily, the existence that has heterogeneous forming core particle at crystals has increased the crystal nucleation rate greatly, and the crystalline speed of growth also can be suppressed simultaneously; So under hyperpressure, solidify, the dendritic structure of alloy obtains remarkable refinement.
2, Heating temperature also has considerable influence to solidified structure, and too high Heating temperature not only can make solidified structure generation alligatoring, and makes dendritic growth turn to column crystal by equiax crystal.
3, there is the rate of cooling of solidifying an of the best in the formation of accurate crystalline phase, and rate of cooling is crossed to hang down and can be caused growing up of accurate crystalline phase, influences the performance of alloy, but too high rate of cooling can suppress accurate brilliant forming core again, even can't obtain accurate crystalline phase.
Two, accurate brilliant the strengthen Mg-6Zn-3Y alloy of the present invention with ultra-fine solidified structure has higher performance and thermostability preferably.
1, the secondary dendrite arm spacing of α-Mg dendrite is reduced to 7-10 μ m by the 40-50 μ m under the normal pressure on the one hand, and dendritic structure obtains significant refinement; On the other hand, being distributed on α-Mg matrix of the brilliant even dispersion of a large amount of, tiny granular standard causes the microhardness of this alloy can reach HV89 (normal pressure is HV68 down), than having improved 31% under the normal pressure; Young's modulus is reduced to 62GPa by the 68GPa under the normal pressure, shows that this what gold utensil has intensity and good plasticity preferably.
2, the accurate brilliant alloy that strengthens with ultra-fine solidified structure that obtains under the high pressure is carried out long-time ageing treatment at 200 ℃, experimental result shows that this alloy structure has thermostability preferably.The DSC check and analysis show that also the accurate brilliant beginning solvent temperature that obtains under the high pressure is than high about 5 ℃ under the normal pressure, and the heat enthalpy value increase, and this shows that also the accurate crystalline substance that obtains under the high pressure has thermostability preferably.
Description of drawings
It is the solidified structure pattern with ultra-fine dendrite that figure a among Fig. 1 obtains the Mg-6Zn-3Y alloy structure for the present invention shows under the high pressure, and figure b shows being distributed on the magnesium alloy substrate of a large amount of brilliant even dispersion of tiny standard in pelletized form;
Fig. 2 high pressure is with graphite assembling cover schematic cross-section.
Embodiment
Below through embodiment technical scheme of the present invention is done further description.
1, in melt quality percentage ratio Wt%, takes by weighing Mg: 91.0%, Zn:6.0%, Y:3.0%;
2, magnesium ingot, zinc ingot metal, the pure yttrium metal charge of above-mentionedization mass percent are put into the crucible of baking oven under 200 ℃ and carry out the preheating baking;
3, the Heating temperature with crucible electrical resistance furnace is set at 780 ℃, when crucible temperature rises to 380 ℃, in crucible, adds magnesium ingot and zinc ingot metal; And begin to feed the CO2/SF6 mixed gas as protection gas, continue to heat up, treat that magnesium ingot and zinc ingot metal in this crucible melts fully after; Add pure yttrium; Treat that pure yttrium melts the back fully and stirred 2 ~ 5 minutes,, for use after stirring is accomplished 780 ℃ of insulations 10 ~ 15 minutes;
4, Mg-Zn-Y alloy solution temperature is adjusted to 760 ℃; After leaving standstill 3 ~ 5 minutes, remove the solution surface scum silica frost, again the Mg-Zn-Y alloy solution is cast in the metal pattern; Obtain Mg-6Zn-3Y cast alloy material, again the cast alloy material is carried out abundant diffusion annealing;
5, the Mg-6Zn-3Y cast alloy material after the above-mentioned diffusion annealing is carried out the line cutting, the high pressure that is processed into Ф 4 х 5mm is used sample;
6, the Mg-6Zn-3Y sample of the Ф that processes 4 х 5mm is put into graphite assembling cover; The graphite assembling is mounted on the cavity position of CS-1B type high pressure six top surface; The setting freezing pressure is 6GPa, and Heating temperature is 1300 ℃, is heated rapidly to preset Heating temperature; Make the Mg-6Zn-3Y sample of Ф 4 х 5mm melt fully; And under this temperature heat-insulation pressure keeping 15min, to solidify rate of cooling be 300K/S in control, finally makes the Mg-6Zn-3Y alloy that contains the icosahedral quasicrystal phase and have ultra-fine solidified structure.
In the present embodiment; Quasicrystal reinforced magnesium alloy with ultra-fine solidified structure, its Characteristics of As-cast Structure is made up of granular accurate crystalline substance, α-Mg matrix and Mg-Zn-Y ternary phase, in as-cast structure; The secondary dendrite arm spacing of α-Mg dendrite is 7-10 μ m; Granular accurate crystalline phase is the I-Mg3Zn6Y phase with icosahedral structure of virus, and its diameter is 50-100 μ m, and granular accurate brilliant volume accounts for 25 ~ 35% of this alloy TV.
The graphite of indication assembling cover is seen Fig. 2 in above-mentioned.Described graphite assembling cover; Comprise boron nitride crucible 4; With the plumbago crucible 2 that places boron nitride crucible 4 outsides, complete installation is in WC supercharging post 3, and the symmetrical both sides that are positioned at WC supercharging post 3 are provided with agalmatolite 1; Six faces at said graphite assembling cover are provided with pressure hammer 6, and Mg-6Zn-3Y alloy sample 5 is placed in the boron nitride crucible 4 in the graphite assembling cover.
Explain: the measuring method of temperature in the high pressure process of setting: adopt the punching at place, the big agalmatolite piece right angle of cubes of jig drill head, up to touching sample, then thermocouple wire is put into and touched sample, the other end of thermopair is a temperature recording unit.
The measuring method of pressure: resistance strain gage is bonded on the top press matrix through tackiness agent closely; When the stressed generation strain variation of matrix; Resistance strain gage also produces deformation together, and the resistance of foil gauge is changed, and is added in ohmically voltage and changes thereby make; Again this data variation is passed to treatment circuit, can show the on-load pressure of six-plane piercer.
The measurement of rate of cooling: measure cooling curve with X-Y recorder, calculate rate of cooling according to cooling curve.
For the effect that proves absolutely that the present invention has, referring to accompanying drawing.
Fig. 1 has ultra-fine solidified structure and contains the displaing micro tissue topography (SEM) of the Mg-6Zn-3Y alloy of icosahedral quasicrystal phase for what this enforcement made.
Figure a shows that it is the dendrite pattern with solidified structure of ultra-fine crystalline substance that high pressure obtains the Mg-6Zn-3Y alloy structure down.
Figure b shows being distributed on the magnesium alloy substrate of a large amount of brilliant even dispersion of tiny standard in pelletized form.
Claims (3)
1. the accurate crystalline substance with ultra-fine solidified structure strengthens the Mg-6Zn-3Y alloy, and it is characterized in that: chemical ingredients is counted by mass percent wt%: Mg: 87.0 ~ 93.0%, Zn: 3.0 ~ 10.0%, Y:0.5 ~ 3.0%.
2. be used for the preparation method that claim 1 has the accurate brilliant Mg-6Zn-3Y of the enhancing alloy of ultra-fine solidified structure, comprise the steps:
(1) as cast condition Mg-Zn-Y alloy material under the preparation normal pressure:
Getting and accounting for raw material total amount mass percent is 91.0% magnesium ingot, 6.0% zinc ingot metal, 3.0% pure yttrium, puts into baking oven and under 200 ℃, carries out the preheating baking; It is 760 ~ 780 ℃ that crucible electrical resistance furnace is set at Heating temperature, when crucible temperature rises to 350 ~ 400 ℃, in crucible, adds magnesium ingot and zinc ingot metal; Begin to feed the CO2/SF6 mixed gas as protection gas, continue to heat up, treat that magnesium ingot and zinc ingot metal in the crucible melts fully after; Add pure yttrium, treat that pure yttrium melts the back fully and stirred 2 ~ 5 minutes, 760 ~ 780 ℃ of insulations 10 ~ 15 minutes; Remove the solution surface scum silica frost; The Mg-Zn-Y alloy solution is cast in the metal pattern, obtains Mg-6Zn-3Y cast alloy material, then as cast condition Mg-6Zn-3Y is carried out diffusion annealing;
(2) control freezing pressure, Heating temperature and solidify rate of cooling preparation and contain the granular accurate brilliant Mg-6Zn-3Y alloy of nano level under GPa level ultra-high voltage with ultra-fine solidified structure:
The Mg-6Zn-3Y cast alloy material of step (1) is carried out the line cutting; The high pressure that is processed into Ф 4 х 5mm is used sample, puts into graphite assembling cover, the graphite assembling is mounted on the cavity position of CS-1B type high pressure six top surface; The setting freezing pressure is 6GPa, and Heating temperature is 1300 ℃; Be heated rapidly to preset Heating temperature, make sample melt fully, and under this temperature heat-insulation pressure keeping 15min, to solidify rate of cooling be 300K/S in control, finally makes the Mg-6Zn-3Y alloy that contains the accurate brilliant ultra-fine solidified structure of nano level.
3. the preparation method with the accurate brilliant Mg-6Zn-3Y of enhancing alloy of ultra-fine solidified structure according to claim 2; It is characterized in that: Characteristics of As-cast Structure is made up of granular accurate crystalline substance, α-Mg matrix and Mg-Zn-Y ternary phase; In as-cast structure, the secondary dendrite arm spacing of α-Mg dendrite is 7-10 μ m, and granular accurate crystalline phase is the I-Mg3Zn6Y phase with icosahedral structure of virus; Its diameter is 50-100 μ m, and granular accurate brilliant volume accounts for 25 ~ 35% of this alloy TV.
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| CN105256262A (en) * | 2015-10-29 | 2016-01-20 | 东北大学 | Method for improving aging hardening effect of Mg-Zn-Y alloy through presetting of twin crystals |
| CN105603249A (en) * | 2016-01-07 | 2016-05-25 | 燕山大学 | Preparation method of terrace-shaped appearance Al-Cu-Fe quasi crystal block material |
| CN106925955A (en) * | 2017-02-22 | 2017-07-07 | 成都青石激光科技有限公司 | Sphere material quasi-crystalline lattice is distributed in the processing method in matrix material |
| CN108467962A (en) * | 2018-04-13 | 2018-08-31 | 中北大学 | A kind of preparation method of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites |
| CN109280829A (en) * | 2018-12-14 | 2019-01-29 | 东北大学秦皇岛分校 | A kind of high-strength casting Mg-Zn-Cu-Zr alloy and preparation method thereof |
| CN109355540A (en) * | 2018-12-14 | 2019-02-19 | 东北大学 | A kind of high intensity Mg-Zn-Cu-Zr-Cr-Ca alloy and preparation method thereof |
| CN110079751A (en) * | 2019-04-22 | 2019-08-02 | 上海工程技术大学 | A kind of preparation method of made of Al-Cu alloy supersaturated solid solution |
| US10799947B2 (en) * | 2018-12-28 | 2020-10-13 | North University Of China | Method of semi-solid indirect squeeze casting for magnesium-based composite material |
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| CN105274412B (en) * | 2015-10-16 | 2017-05-17 | 东北大学 | Mg-Zn-Y directional solidification alloy and preparing method thereof |
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| CN1789458A (en) * | 2005-12-12 | 2006-06-21 | 西安理工大学 | In-situ synthesizing quasi-crystal and approximate phase reinforced high-strength ultra-tough magnesium alloy and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1789458A (en) * | 2005-12-12 | 2006-06-21 | 西安理工大学 | In-situ synthesizing quasi-crystal and approximate phase reinforced high-strength ultra-tough magnesium alloy and preparation method thereof |
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| CN105256262A (en) * | 2015-10-29 | 2016-01-20 | 东北大学 | Method for improving aging hardening effect of Mg-Zn-Y alloy through presetting of twin crystals |
| CN105603249A (en) * | 2016-01-07 | 2016-05-25 | 燕山大学 | Preparation method of terrace-shaped appearance Al-Cu-Fe quasi crystal block material |
| CN106925955A (en) * | 2017-02-22 | 2017-07-07 | 成都青石激光科技有限公司 | Sphere material quasi-crystalline lattice is distributed in the processing method in matrix material |
| CN108467962A (en) * | 2018-04-13 | 2018-08-31 | 中北大学 | A kind of preparation method of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites |
| CN108467962B (en) * | 2018-04-13 | 2019-12-17 | 中北大学 | Preparation method of magnesium-zinc-yttrium quasicrystal and boron carbide mixed enhanced magnesium-based composite material |
| CN109280829A (en) * | 2018-12-14 | 2019-01-29 | 东北大学秦皇岛分校 | A kind of high-strength casting Mg-Zn-Cu-Zr alloy and preparation method thereof |
| CN109355540A (en) * | 2018-12-14 | 2019-02-19 | 东北大学 | A kind of high intensity Mg-Zn-Cu-Zr-Cr-Ca alloy and preparation method thereof |
| CN109355540B (en) * | 2018-12-14 | 2020-10-16 | 东北大学 | High-strength Mg-Zn-Cu-Zr-Cr-Ca alloy and preparation method thereof |
| US10799947B2 (en) * | 2018-12-28 | 2020-10-13 | North University Of China | Method of semi-solid indirect squeeze casting for magnesium-based composite material |
| CN110079751A (en) * | 2019-04-22 | 2019-08-02 | 上海工程技术大学 | A kind of preparation method of made of Al-Cu alloy supersaturated solid solution |
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