CN105274412B - Mg-Zn-Y directional solidification alloy and preparing method thereof - Google Patents

Mg-Zn-Y directional solidification alloy and preparing method thereof Download PDF

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CN105274412B
CN105274412B CN201510673757.1A CN201510673757A CN105274412B CN 105274412 B CN105274412 B CN 105274412B CN 201510673757 A CN201510673757 A CN 201510673757A CN 105274412 B CN105274412 B CN 105274412B
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CN105274412A (en
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林小娉
罗晶
吴厚卜
印策
朱壮
徐献义
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Northeastern University China
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Abstract

The invention discloses Mg-Zn-Y directional solidification alloy and a preparing method thereof. The Mg-Zn-Y directional solidification alloy comprises, by mass, 6.00%-9.00% of Zn, 1.00%-2.00% of Y and the balance Mg. The Mg-Zn-Y directional solidification alloy and the preparing method thereof have the beneficial effects that the Mg-Zn-Y directional solidification alloy has columnar crystal tissue, has high strength and certain plasticity under the room temperature, and more importantly has high-temperature mechanical performance; particularly, the Mg-Zn-Y directional solidification alloy obtains a columnar crystal tissue with specific orientation, wherein in the columnar crystal tissue, primary arm growing is parallel, a longitudinal crystal boundary is straight, and a transverse crystal boundary does not exist. Granular phases are dispersed and distributed in crystals, and the crystal boundary phases and the crystal internal granular phases are icosahedron quasi-crystals I-Mg3Zn6Y; and the problems that in the prior art, Mg-Zn-Y alloy solidification tissue is thick, quasi-crystals are connected into a net shape in an eutectic structure form to be distributed among alpha-Mg dendritic crystals, and the quasi-crystal strengthening function cannot be developed fully are solved.

Description

Mg-Zn-Y directional solidificating alloys and preparation method thereof
Technical field
The present invention relates to a kind of Mg-Zn-Y directional solidificating alloys and preparation method thereof, belong to Mg-Zn-Y alloy technologies neck Domain.
Background technology
Used as most light structural metallic materials, it all has excellent performance to magnesium alloy materials at many aspects, is described as " 21st century green engineering material ".But existing Elevated Temperature Mechanical Properties of Mg Alloys is poor, when temperature is more than 120 DEG C, Its intensity and creep-resistant property often significantly decline so as to be difficult to use for a long time at high temperature.Therefore, magnesium conjunction how is improved The mechanical behavior under high temperature of gold is always the important topic of magnesium alloy research field.
Mg-Zn-Y alloys are exactly a kind of new magnesium alloy materials, have special performance due to its unique structure.Root According to information, quasi-crystalline substance I-Mg in Mg-Zn-Y alloys3Zn6Y is that a kind of high-melting-point strengthens phase, its have icosahedral structure of virus and It is paracycle, mutually more more stable than crystal alloy, while it also has stronger interfacing relationship, pinning crystal boundary and dislocation motion with matrix Effect it is also very strong, thus the high-temperature behavior of magnesium alloy can be effectively improved.But existing quasi-crystalline substance strengthens Mg-Zn-Y alloys Solidified structure is thick, and quasi-crystalline substance is linked to be net distribution in α-Mg interdendritics with eutectic structure form more, and the reinforcing for causing quasi-crystalline substance is made With can not give full play to, then also cannot truly improve the mechanical behavior under high temperature of Mg-Zn-Y alloys.Therefore need Inventor is further improved.
The content of the invention
It is an advantage of the invention to provide a kind of Mg-Zn-Y directional solidificating alloys and preparation method thereof, it is optimized The composition proportion and preparation technology of magnesium alloy and condition so that the Mg-Zn-Y alloys of generation have more preferable mechanical behavior under high temperature.
To solve above-mentioned technical problem, the present invention is adopted the following technical scheme that:A kind of Mg-Zn-Y directional solidificating alloys, Including the component of following mass percent:The Mg of Zn 6.00%~9.00%, Y 1.00%~2.00% and remaining percentage ratio.
Preferably, described Mg-Zn-Y directional solidificating alloys, including the component of following mass percent:Zn 9.00%, Y2.00% and Mg 89.00%, so as to the second magnesium alloy for being only mutually Icosahedral phases can be obtained so that the Mg-Zn-Y of generation is closed Gold utensil has more preferable mechanical behavior under high temperature.
Aforesaid Mg-Zn-Y directional solidificating alloys, the raw material for being adopted for:Purity (mass fraction) is 99.9% Mg Ingot, Zn ingots, Mg-30Y (30%, mass fraction) intermediate alloy, so as to the purity for ensureing molten alloy is high, impurity is few.
The preparation method of aforesaid Mg-Zn-Y directional solidificating alloys, comprises the following steps:
A. Zn, Y, Mg raw material is taken, by described raw material mixing, adds heat fusing, obtain alloy liquid;
B. continue to heat described alloy liquid, and controlling alloy liquid, that orientation is cast under different cast temperatures is solidifying In fixed standby lower pull system, while the lower pull system of control is lifted with different pull rate;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Temperature forms thermograde with cold end, and maintains casting to be formed in solid liquid interface when starting by muff and pull rate Thermograde (be made up of the cold end of chilling platform and the liquid alloy of higher cast temperature experiment needed for thermograde, The not solidified liquid metal of recycling muff guarantee is partially in temperature during casting, and by controlling pull rate cold end is ensured The Quench ability of the liquid alloy to just having pulled out from muff, the thermograde begun setting up so as to maintain to cast), promote The crystal unidirectional growth of the alloy of casting, obtains Mg-Zn-Y directional solidificating alloy coupons.
The Mg-Zn-Y directional solidificating alloy coupons of a height of 80~100mm can be prepared by process above, while should Directional solidificating alloy coupon has preferable intensity and plasticity, also with preferable mechanical behavior under high temperature.
Preferably, in step b, c, described cast temperature is 700~800 DEG C, and pull rate is 5~30mm/min, from And alloy can be made fully to melt, composition it is uniform, and magnesium alloy volatilization is few, while also ensure that the temperature needed for directional solidification Gradient (controls the thermograde in cold end-both co- controlling directional solidification process by cast temperature and pull rate, makes Thermograde is controlled in the interval needed for column crystals growth), the directional solidificating alloy of acquisition has preferable mechanical behavior under high temperature.
It is furthermore preferred that in step b, c, described cast temperature is 760~780 DEG C, pull rate is 10~15mm/min, Such that it is able to make alloy melt composition evenly, and magnesium alloy volatilization is less, while also ensure that the temperature needed for directional solidification Degree gradient (controls the solid liquid interface temperature in cold end-both co- controlling directional solidification process by cast temperature and pull rate Degree gradient, makes thermograde control in the interval needed for column crystals growth), the directional solidificating alloy of acquisition is (highly reachable 100mm) there is more preferable mechanical behavior under high temperature.
In said method, vacuum is 2.4 × 10-2Pa in the furnace chamber of described apparatus for directional solidification, reduces waving for magnesium alloy Send out, while ensureing that magnesium alloy does not burn.
In order to verify above content, inventor has also carried out following experimental study:
Experimental example 1:Composition proportion screening experiment
Inventor using Factsage software Phase Diagram (phase module) and thermodynamic data storehouse SGTE (solution, Pure material and compound database) and magnesio data base, draw Zn, Y content under equilibrium condition and Mg-Zn-Y alloy quasi-crystalline substances are formed The impact schematic diagram of quantity.As shown in Figure 14, when Zn contents are 9wt.%, and Y contents are 2wt.%, quasi-crystalline substance quantity is most.To the greatest extent Quasi-crystalline substance when pipe Y contents are 3wt.% is more, but it can be seen from solidification theory, the growth pattern of crystal can be subject to solute The impact of concentration, solute redistribution can be caused when solute concentration is too high, and then can increase constitutional supercooling, be not suitable for column crystal life It is long.Therefore, in the present invention, preferred composition proportion is:Zn contents are 9wt.%, and Y contents are 2wt.%, and surpluses are Mg.
Experimental example 2:Investigate impact of the preparation method to Mg-Zn-Y alloys
1st, technic metal is prepared and experimental technique
Method one:Mg-Zn-Y directional solidificating alloy coupons are prepared using the directional solidifying method for preparing of the present invention.
Method two:Melting is carried out to raw material using 2RRL-M8 type vacuum resistance smelting furnaces, cast temperature is 760 DEG C, will The alloy liquid for having melted is cast in preheated metallic type, and Mg-Zn-Y routine casting alloy cast ingots are obtained.
By the stable vitellarium of the column crystal of described Mg-Zn-Y directional solidificating alloy coupons or region and Mg-Zn-Y routines Casting alloy ingot casting cuts into a diameter of 10m, the sample of a height of 15mm, using WDW3100 microcomputer controlled electronic universal testers Room temperature compression experiment is carried out, strain rate ε is 0.001s-1;In addition, carrying out on Gleeble-3500D hot modeling test machines Mechanical behavior under high temperature is tested, and experimental temperature is respectively set as 200 DEG C, 250 DEG C and 300 DEG C, and strain rate is respectively set as 1.0s-1 ~1 × 10-3s-1, sample is heated, heating 2min reaches and be incubated after target temperature 50s, is then compressed again;Wherein, To prevent sample from aoxidizing in compression process, protected using argon.Using the type scanning electron microscopic observations of LEO JSM 5400 and analyze reality Alloy microscopic structure is tested, while carrying out material phase analysis using 2500/PC types X-ray diffractometer, scanning step is 0.3 °, at 20 ° XRD diffraction spectra is measured between 90 ° (2 θ).
2nd, experimental result and analysis
2.1 oriented freezing organizations are analyzed
Fig. 1~Fig. 4 is Mg-Zn-Y Solidification Structures.As shown in Figure 1, made using the method (method one) in the present invention The standby Mg-Zn-Y alloys for obtaining, obtain a secondary arm Parallel Growth, and longitudinal crystal boundary is straight, take with specific without transverse grain boundaries To columanar structure, Jing determines, and its column crystal length is about 35~60mm;Fig. 2 is Mg-Zn-Y directional solidificating alloys in Fig. 1 Cross section solidified structure schematic diagram, as shown in Figure 2, the present invention Mg-Zn-Y directional solidificating alloys there is columanar structure, and The cross-sectional grain of the column crystal is born of the same parents' shape, while granular phase in the transgranular Dispersed precipitate of going back of column.Additionally, such as Fig. 3, Fig. 4 institute Show, under the conditions of identical amplification, compared with the solidified structure (as shown in Figure 4) of routine casting alloy, institute in the present invention The average-size of crystal grain is thicker on the cross section (as shown in Figure 3) of the directional solidificating alloy tissue for obtaining, and crystal boundary phase area subtracts It is little, more elongated;Additionally, the intergranular second in routine casting alloy structure is mutually with lamellar eutectic tissue signature (in Fig. 4 Shown in illustration), and the phase of intergranular second in directional solidificating alloy tissue is then more presented divorsed eutectic tissue signature (such as Fig. 3 In illustration shown in).Finally, EDS analyses show (as shown in Figure 5, Figure 6), in the directional solidificating alloy tissue in the present invention The atomic percent of Mg, Zn and Y of Grain-Boundary Phase and transgranular granular phase is respectively 28.25%, 60.70%, 11.05% and 32.55%th, 57.30%, 10.15%, Mg:Zn:Y≈3:6:1 (for the stoichiometric proportion of icosahedral quasicrystal phase), shows that it is brilliant Boundary's phase with it is transgranular it is granular be mutually icosahedral quasicrystal, thus can be very good to play the invigoration effect of quasi-crystalline substance, improve Mg-Zn-Y The mechanical behavior under high temperature of alloy.
Fig. 7 is that routine casting alloy is closed from the solidification that the directional solidificating alloy of the present invention is obtained under different curing conditions The XRD diffraction spectra contrast schematic diagrams of gold, as shown in Figure 7, routine casting alloy and directional solidificating alloy are organized by α-Mg and standard Brilliant I-Mg3Zn6The phase compositions of Y two, but the conical surface compared with the XRD spectral lines of routine casting alloy, in directional solidificating alloy tissue (102) crystal face and cylinder (100) diffraction maximum are more higher, while solid matter face (002) crystallographic plane diffraction peak is weaker.Normal freezing When, atom is grown in the way of solid matter face, surface density highest, during combining in atom, is released in unit area Latent heat be higher than non-solid matter face.And during directional solidification, then (closed with cooling water or gallium indium by controlling certain thermograde Gold forms thermograde as the cold end of chilling platform using alloy liquid temperature and cold end, and by muff and pull rate The thermograde for maintaining casting to be formed in solid liquid interface when starting), so as to ensure that crystal along the elevated direction life of temperature It is long.
The mechanical property of 2.2 directional solidificating alloys
2.21 room-temperature mechanical property
Fig. 8 is using the alloy sample of directional solidification technique (method one) preparation of the present invention and using routine techniquess (side Method two) casting alloy sample room temperature (20 DEG C) engineering stress-strain curve comparison diagram, from the curve in Fig. 8, employing It is 357MPa that the maximum of alloy sample prepared by the directional solidification technique of the present invention breaks drag, and adopts what routine techniquess cast It is only 232MPa that the maximum of alloy sample breaks drag, and maximum breaks drag and improves about 54%;Coagulated using the orientation of the present invention Gu the section expansion rate of alloy sample prepared by technology is 21%, (section expands with the alloy sample cast using routine techniquess Rate is 16%) to compare, and its section expansion rate improves 31%.
Organization decided performance, due to being linked to be netted the crystal boundary quasi-crystalline substance in routine casting alloy structure, thus quasi-crystalline substance is acted on more It is difficult to play;And preparation-obtained directional solidificating alloy in the present invention, it is organized as column crystal in the directional solidificating alloy, and The orientation of column crystal is consistent with Impact direction during compression, and most boundary is parallel to Impact direction, thus laterally phase boundary Face is few, is more beneficial for resisting plastic deformation, and making the compressive strength of alloy substantially increases, additionally, the present invention is preparation-obtained fixed To solidified superalloy, the crystal boundary quasi-crystalline substance in the directional solidificating alloy is greatly reduced, and grain particles shape Icosahedral phases increase, thus quasi-crystalline substance Effect is given full play to;In addition, the transverse grain boundaries of the columanar structure of preparation-obtained directional solidificating alloy of the invention are few, Grain boundary area is also less, dislocation motion along parallel columnar crystal direction by crystal boundary resistance it is less so that dislocation mobility is good and be difficult to Pile up, the difficulty that the strain for causing the high stress concentrations region inner product that dislocation pile up is formed tired reaches crack nucleation is bigger, thus Make it be less susceptible to rupture, improve the plasticity of Mg-Zn-Y alloys.Additionally, compared with routine casting alloy, the present invention is made The tissue of the standby directional solidificating alloy for obtaining is finer and close, and microdefect is less, and this also improves to a certain extent the property of alloy Energy.
2.22 thermal compaction energy
Fig. 9~Figure 11 is respectively directional solidificating alloy and routine casting alloy respectively in 200 DEG C, 250 DEG C and 300 DEG C hot pressing Under the conditions of contracting, the curve chart that its peak stress changes with strain rate;Figure 12 is for deformation temperature to technic metal differently strained Peak stress under speed affects schematic diagram.As shown in Figure 9, the conjunction for being prepared using the directional solidification technique (method one) of the present invention Golden sample is in 200 DEG C of -1.0s-1Under, its peak stress is up to 245MPa, relatively using the alloy examination of routine techniquess (method two) casting Sample (its peak stress is 155MPa) improves about 58%;When temperature-resistant, the peak value of alloy is with the reduction of strain rate Reduce, when strain rate is 0.001s-1When, the peak of the alloy sample prepared using the directional solidification technique (method one) of the present invention Value stress is 171MPa, relatively improves about 46% using the alloy sample (117MPa) of routine techniquess (method two) casting.With The rising of experimental temperature, the peak stress of alloy is in be gradually reduced trend, in 250 DEG C of -0.1s-1Under, using the orientation of the present invention The peak stress of alloy sample prepared by solidification technology (method one) is 207MPa, relatively using routine techniquess (method two) casting Alloy sample (129MPa) improves about 60%;Additionally, in 250 DEG C of -0.001s-1Under, using the directional solidification technique of the present invention The peak stress of alloy sample prepared by (method one) is 114MPa, relatively using the alloy sample of routine techniquess (method two) casting (79MPa) improve about 44% (shown in Figure 10).In 300 DEG C of -1.0s-1Under, using the directional solidification technique (method of the present invention One) peak stress of the alloy sample for preparing is 156MPa, and adopts the peak of the alloy sample of routine techniquess (method two) casting Value stress is only 94MPa (shown in Figure 11), and its peak stress improves about 66%.As can be seen here, the directional solidification in the present invention The more conventional casting alloy of alloy has higher elevated temperature strength.
Knowable to fabric analysiss above, the Mg-Zn- prepared under the conditions of the directional solidification technique of method one (present invention) Y alloy, based on solid solution α-Mg, forms the columanar structure with same direction, and its Grain-Boundary Phase is quasi-crystalline substance I- Mg3Zn6Y, and have granular quasi-crystalline substance I-Mg3Zn6Y Dispersed precipitates are in column crystal intergranular.And obtained using the conventional casting technique of method two The Mg-Zn-Y alloys for arriving, are that polycrystalline alloy is organized, and are linked to be netted its phase of intergranular second more, and the crystal boundary vertical with stress axiss is high The master " source " cracked under warm stress.Additionally, the alloy sample prepared using the directional solidification technique (method one) of the present invention, Its column crystal crystal boundary is aligned and behind parallel principal axis of stress direction, and the stress acted under high temperature on fragile crystal boundary can be minimum, So as to delay crackle to be formed, the elevated temperature strength of alloy is improve.Additionally, the thermal deformation of metal is come real by the motion of dislocation Existing, dislocation after product blocked, forms high density dislocation area in motor process, the dynamic when dislocation density reaches certain marginal value Recrystallization starts forming core, compared with the Mg-Zn-Y alloys under the conditions of routine casting, the Mg-Zn-Y with continuous cylindrical crystalline texture Alloy transverse grain boundaries are few, and grain boundary area is less, and dislocation motion is less by crystal boundary resistance along parallel columnar crystal direction, makes dislocation movable Property it is good and be difficult to pile up, cause dislocation density to be difficult to reach the marginal value needed for occurrence dynamics Recrystallization nucleation;On the other hand, by Misorientation is cut in the Mg-Zn-Y alloy interior tissues with continuous columnar less, during the pressurized compression deformation of sample, its need to be made parallel The misorientation for organizing the formation of deformation band, increasing regional area of arrangement, is beneficial to the formation of high-angle boundary, is its occurrence dynamics Recrystallization provides essential condition;And the grain boundary area of the initial structure of the Mg-Zn-Y alloys under the conditions of routine casting is big and brilliant The misorientation of intergranular is larger, and it is more likely formed substantial amounts of high density dislocation area and high-angle boundary, therefore phase in compression Compared with Mg-Zn-Y alloys under the conditions of routine casting, the recrystallization of the Mg-Zn-Y alloys occurrence dynamics with continuous cylindrical crystalline texture is needed Energy that will be higher, then be more difficult to dynamic recrystallization, and the emollescence for making the dynamic recrystallization that alloy is subject to reduces.Furthermore, it is fixed It is mutually granular icosahedral quasicrystal phase of the Dispersed precipitate on matrix to transgranular second in solidified structure, because quasi-crystalline substance has preferably height Temperature stability, quasi-crystalline substance can still hinder dislocation motion under high temperature, improve alloy strength.
4 conclusions
(1) Mg-Zn-Y alloys obtain a secondary arm Parallel Growth, longitudinal crystal boundary Jing after method of the present invention directional solidification Straight, the columanar structure with specific orientation without transverse grain boundaries, while granular phase, crystal boundary in the transgranular Dispersed precipitate of column Icosahedral quasicrystal I-Mg is with transgranular granular phase3Zn6Y;
(2) under room temperature, adopt the present invention directional solidification technique prepare alloy sample maximum break drag for 357MPa, more conventional casting alloy intensity (232MPa) improves about 54%;Dependent variable is 21% when breaking, and more conventional casting is closed Gold (dependent variable is 16% when breaking) improves about 31%;
(3) under high temperature, using the alloy of directional solidification technique preparation of the invention in 200 DEG C of -1.0s-1Under peak stress Up to 245MPa, more conventional casting alloy (peak stress is 155MPa) improves about 58%;When temperature-resistant, the peak of alloy Value reduces with strain rate and reduces;When strain rate is 0.001s-1When, the conjunction prepared using the directional solidification technique of the present invention The peak stress of gold is 171MPa, and more conventional casting alloy (peak stress is 117MPa) improves about 46%.With experiment temperature The rising of degree, the peak stress of alloy is in be gradually reduced trend;In 250 DEG C of -0.1s-1Under, using the directional solidification skill of the present invention The peak stress of alloy sample prepared by art is 207MPa, is relatively improve using the alloy sample (129MPa) of routine techniquess casting About 60%;Additionally, in 250 DEG C of -0.001s-1Under, the peak value of the alloy sample prepared using the directional solidification technique of the present invention should Power is 114MPa, relatively improves about 44% using the alloy sample (79MPa) of routine techniquess casting.In 300 DEG C of -1.0s-1Under, adopt The peak stress of the alloy prepared with the directional solidification technique of the present invention is 156MPa, and the peak stress of routine casting alloy is only For 94MPa, peak stress improves about 66%.It can thus be appreciated that:Coagulated using the orientation obtained with when preparation technology of the present invention Gu the more conventional casting alloy of alloy has more preferable mechanical behavior under high temperature.
Compared with prior art, the present invention has advantages below:The Mg-Zn-Y directional solidificating alloys of the present invention have column Crystalline substance tissue, not only has at room temperature higher intensity and certain plasticity, and what is more important has preferable high-temperature mechanics Performance;Specifically:
(1) Mg-Zn-Y alloys obtain a secondary arm Parallel Growth, longitudinal crystal boundary Jing after method of the present invention directional solidification Straight, the columanar structure with specific orientation without transverse grain boundaries;It is accurate icosahedron mostly to be in columanar structure's Grain-Boundary Phase Brilliant I-Mg3Zn6Y phases;Therefore overcome that Mg-Zn-Y Solidification Structures of the prior art are thick and quasi-crystalline substance is more with eutectic structure Form is linked to be net distribution in α-Mg interdendritics, the problem that quasi-crystalline substance invigoration effect can not give full play to;
(2) under room temperature, the maximum of the Mg-Zn-Y directional solidificating alloy samples prepared using the directional solidification technique of the present invention It is 357MPa to break drag, and the intensity (232MPa) of more conventional casting alloy improves about 54%;Dependent variable when breaking is 21%, more conventional casting alloy (16%) improves 31%;
(3) under high temperature, using the present invention directional solidification technique prepare Mg-Zn-Y directional solidificating alloys, 200 DEG C- 1.0s-1Under peak stress be up to 245MPa, more conventional casting alloy (155MPa) improves 58%;When temperature-resistant, this The peak value of the Mg-Zn-Y directional solidificating alloys of invention is reduced with the reduction of strain rate;When strain rate is 0.001s-1When, The peak stress of directional solidificating alloy is 171MPa, and more conventional casting alloy (117MPa) improves about 46%.With experiment temperature The rising of degree, the peak stress of alloy is in be gradually reduced trend;300℃-1.0s-1Under, the peak stress of directional solidificating alloy is 156MPa, and the peak stress of routine casting alloy is only 94MPa, peak stress about improves 66%.It can thus be appreciated that:Using this The more conventional casting alloy of directional solidificating alloy that the proportioning of invention, preparation technology are obtained, not only has at room temperature higher strong Degree and plasticity, while also having preferable mechanical behavior under high temperature.
Inventor has been also carried out substantial amounts of experimental study to cast temperature and pull rate, by setting different casting temperature Spend and pull rate, and the alloy to obtaining carries out being learnt after fabric analysiss:When cast temperature is 700~800 DEG C, pull rate For 5~30mm/min when, columanar structure's effect of acquisition is fine, its at room temperature have higher intensity and plasticity, together When there is preferable mechanical behavior under high temperature;When pull rate is more than 30mm/min, because cold end movement velocity is too fast, column crystal is given birth to Long scope can be suppressed;When pull rate is less than 5mm/min, pull rate is excessively slow, is unfavorable for column crystals growth;Work as casting When temperature is less than 700 DEG C, thermograde slope is little, causes constitutional supercooling to increase, and is unfavorable for column crystals growth;When cast temperature it is big When 800 DEG C, magnesium alloy then volatilizees seriously.
Additionally, cast temperature to be chosen for respectively inventor 700,720,740,760,780,800 DEG C, and pour for each Casting temperature, pull rate is set as into 5,10,15,20,25,30mm/min, carry out being learnt after fabric analysiss:When cast temperature is 760~780 DEG C, when pull rate is 10~15mm/min, columanar structure's effect of the Mg-Zn-Y directional solidificating alloys of acquisition More preferably (highly up to 100mm), it has at room temperature higher intensity and plasticity, while having more preferable high-temperature mechanics Energy.
Description of the drawings
Fig. 1 is the longitudinal section solidified structure schematic diagram of directional solidificating alloy;
Fig. 2 is the cross section solidified structure schematic diagram of directional solidificating alloy;
Fig. 3 is the cross section solidified structure schematic diagram of directional solidificating alloy;
Fig. 4 is the solidified structure schematic diagram of routine casting alloy;
Fig. 5 is the power spectrum schematic diagram of Grain-Boundary Phase in oriented freezing organization;
Fig. 6 is the power spectrum schematic diagram of granular phase in oriented freezing organization;
Fig. 7 is the XRD of the solidified superalloy that routine casting alloy is obtained from directional solidificating alloy under different curing conditions Diffraction spectra contrast schematic diagram;
Fig. 8 is the room temperature engineering stress-strain curve of alloy sample prepared by directional solidification and routine casting alloy sample Comparison diagram;
Fig. 9~Figure 11 is respectively directional solidificating alloy and routine casting alloy respectively in 200 DEG C, 250 DEG C and 300 DEG C hot pressing Under the conditions of contracting, the curve chart that its peak stress changes with strain rate;
Figure 12 is that peak stress of the deformation temperature on technic metal under differently strained speed affects schematic diagram;
Figure 13 is method of the present invention flow chart;
Figure 14 is impact schematic diagram of Zn, Y content to Mg-Zn-Y alloy quasi-crystalline substance quantity of formation under equilibrium condition.
With reference to the accompanying drawings and detailed description the present invention is further illustrated.
Specific embodiment
Embodiments of the invention 1:A kind of Mg-Zn-Y directional solidificating alloys, are prepared by the following method and form (such as Figure 13 institutes Show):
A. take in the middle of Mg ingot 88g, Zn ingot 12g that purity (mass fraction) is 99.9%, Mg-30Y (30%, mass fraction) Alloy 2.5g, by the mixing of above-mentioned raw material, adds heat fusing, obtains alloy liquid;
B. continue to heat described alloy liquid, and controlling alloy liquid, that orientation is cast under different cast temperatures is solidifying In fixed standby lower pull system, while the lower pull system of control is lifted with different pull rate;Wherein, described orientation is coagulated Vacuum is 2.4 × 10 in fixed standby furnace chamber-2Pa;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Temperature forms thermograde with cold end, and maintains casting to be formed in solid liquid interface when starting by muff and pull rate Thermograde, promote casting alloy crystal unidirectional growth, obtain the Mg-Zn-Y directional solidificating alloy coupons of a height of 100mm;
In step b, c, described cast temperature is 760~780 DEG C, and pull rate is 10~15mm/min.
The final chemistry of the directional solidificating alloy prepared using ICAP6300 plasma spectroscopy the present embodiment The mass percent of composition is:Zn 9.00%, Y 2.00%, Mg 89.00%.
Involved apparatus for directional solidification can adopt existing equipment in said method.
Embodiment 2:A kind of Mg-Zn-Y directional solidificating alloys, are prepared by the following method and form (as shown in figure 13):
A. take in the middle of Mg ingot 92g, Zn ingot 8g that purity (mass fraction) is 99.9%, Mg-30Y (30%, mass fraction) Alloy 1.2g, by the mixing of above-mentioned raw material, adds heat fusing, obtains alloy liquid;
B. continue to heat described alloy liquid, and controlling alloy liquid, that orientation is cast under different cast temperatures is solidifying In fixed standby lower pull system, while the lower pull system of control is lifted with different pull rate;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Temperature forms thermograde with cold end, and maintains casting to be formed in solid liquid interface when starting by muff and pull rate Thermograde, promote casting alloy crystal unidirectional growth, obtain the Mg-Zn-Y directional solidificating alloys of a height of 80~100mm Coupon;
In step b, c, described cast temperature is 700~760 DEG C, and pull rate is 5~10mm/min.
The final chemistry of the directional solidificating alloy prepared using ICAP6300 plasma spectroscopy the present embodiment The mass percent of composition is:Zn 6.00%, Y 1.00%, Mg 93.00%.
Involved apparatus for directional solidification can adopt existing equipment in said method.
Embodiment 3:A kind of Mg-Zn-Y directional solidificating alloys, are prepared by the following method and form:
A. Mg ingot 89.2g, Zn ingot 9g that purity (mass fraction) is 99.9% are taken, in Mg-30Y (30%, mass fraction) Between alloy 1.8g, by the mixing of above-mentioned raw material, plus heat fusing, obtain alloy liquid;
B. continue to heat described alloy liquid, and controlling alloy liquid, that orientation is cast under different cast temperatures is solidifying In fixed standby lower pull system, while the lower pull system of control is lifted with different pull rate;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Temperature forms thermograde with cold end, and maintains casting to be formed in solid liquid interface when starting by muff and pull rate Thermograde, promote casting alloy crystal unidirectional growth, obtain the Mg-Zn-Y directional solidificating alloys of a height of 80~100mm Coupon;
In step b, c, described cast temperature is 760 DEG C, and pull rate is 10~15mm/min.
The final chemistry of the directional solidificating alloy prepared using ICAP6300 plasma spectroscopy the present embodiment The mass percent of composition is:Zn 7.00%, Y 1.50% and Mg 92.00%.
Involved apparatus for directional solidification can adopt existing equipment in said method.
Embodiment 4:A kind of Mg-Zn-Y directional solidificating alloys, are prepared by the following method and form:
A. take in the middle of Mg ingot 87g, Zn ingot 12g that purity (mass fraction) is 99.9%, Mg-30Y (30%, mass fraction) Alloy 1.2g, by the mixing of above-mentioned raw material, adds heat fusing, obtains alloy liquid;
B. continue to heat described alloy liquid, and controlling alloy liquid, that orientation is cast under different cast temperatures is solidifying In fixed standby lower pull system, while the lower pull system of control is lifted with different pull rate;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Temperature forms thermograde with cold end, and maintains casting to be formed in solid liquid interface when starting by muff and pull rate Thermograde, promote casting alloy crystal unidirectional growth, obtain the Mg-Zn-Y directional solidificating alloys of a height of 80~100mm Coupon;
In step b, c, described cast temperature is 780 DEG C, and pull rate is 15~30mm/min.
The final chemistry of the directional solidificating alloy prepared using ICAP6300 plasma spectroscopy the present embodiment The mass percent of composition is:Zn 9.00%, Y 1.00% and Mg 85.00%.
Involved apparatus for directional solidification can adopt existing equipment in said method.
Mg-Zn-Y directional solidificating alloy coupons are prepared using the condition described in embodiment 1~4, Jing is determined, as a result such as table 1 It is shown.In the Mg-Zn-Y alloy structures that embodiment 1 is obtained second is only mutually icosahedral quasicrystal phase;Obtained in embodiment 2,3 In Mg-Zn-Y alloy structures second mostly mutually is icosahedral quasicrystal phase, a small amount of w phases;Mg-Zn-Y alloy structures obtained in embodiment 4 In second mutually only deposit a small amount of icosahedral quasicrystal phase.Although the column crystal in alloy structure obtained in embodiment 3 is more straight, Because its volume fraction, especially Icosahedral phases shared by the second phase are less than embodiment 1, therefore intensity is compared with the alloy structure in embodiment 1 It is low.And only have a small amount of Icosahedral phases in the alloy structure that embodiment 4 is obtained, therefore either room-temperature property or high-temperature behavior All not as good as embodiment 1.
Table 1

Claims (4)

1. a kind of preparation method of Mg-Zn-Y directional solidificating alloys, it is characterised in that the Mg-Zn-Y directional solidificating alloys, bag Include the component of following mass percent:The Mg of Zn 6.00%~9.00%, Y 1.00%~2.00% and remaining percentage ratio;Bag Include following steps:
A. Zn, Y, Mg raw material is taken, by described raw material mixing, adds heat fusing, obtain alloy liquid;
B. continue to heat described alloy liquid, and control alloy liquid and be cast to directional solidification under different cast temperatures to set In standby lower pull system, while the lower pull system of control is lifted with different pull rate;
C. the cold end for being capable of directed movement of chilling platform, aluminium alloy body temperature are formed using lower pull bar, water-cooled copper ring and gallium-indium alloy Degree forms thermograde, and the temperature formed in solid liquid interface when maintaining and casting and start by muff and pull rate with cold end Degree gradient, promotes the crystal unidirectional growth of the alloy of casting, obtains Mg-Zn-Y directional solidificating alloy coupons;Wherein, in step b, c, Described cast temperature is 700~800 DEG C, and pull rate is 5~30mm/min.
2. the preparation method of Mg-Zn-Y directional solidificating alloys according to claim 1, it is characterised in that the Mg-Zn-Y Directional solidificating alloy, including the component of following mass percent:Zn 9.00%, Y 2.00% and Mg 89.00%.
3. the preparation method of Mg-Zn-Y directional solidificating alloys according to claim 1, it is characterised in that in step b, c, Described cast temperature is 760~780 DEG C, and pull rate is 10~15mm/min.
4. the preparation method of Mg-Zn-Y directional solidificating alloys according to claim 1, it is characterised in that described orientation Vacuum is 2.4 × 10 in the furnace chamber of solidification equipment-2Pa。
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