CN105274412A - Mg-Zn-Y directional solidification alloy and preparing method thereof - Google Patents
Mg-Zn-Y directional solidification alloy and preparing method thereof Download PDFInfo
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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
Technical field
The present invention relates to a kind of Mg-Zn-Y directional solidificating alloy and preparation method thereof, belong to Mg-Zn-Y technical field of alloy.
Background technology
Magnesium alloy materials is as the lightest structural metallic materials, and it all has excellent performance in a lot, 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, and make it be difficult at high temperature use for a long time.Therefore, the mechanical behavior under high temperature how improving magnesium alloy is the important topic of magnesium alloy research field always.
Mg-Zn-Y alloy is exactly a kind of novel magnesium alloy materials, has special performance due to its structure uniqueness.According to made, the brilliant I-Mg of the standard in Mg-Zn-Y alloy
3zn
6y is a kind of high-melting-point wild phase, it has icosahedral structure of virus and quasi-periodicity, more stable mutually than crystal alloy, and itself and matrix also have stronger interfacing relationship simultaneously, the effect of pinning crystal boundary and dislocation motion is also very strong, thus effectively can improve the high-temperature behavior of magnesium alloy.But the solidified structure of existing accurate brilliant enhancing Mg-Zn-Y alloy is thick, and accurate crystalline substance is linked to be net distribution in α-Mg interdendritic mainly with eutectic structure form, cause accurate brilliant strengthening effect not give full play to, so also just truly can not improve the mechanical behavior under high temperature of Mg-Zn-Y alloy.Therefore contriver is needed to improve further.
Summary of the invention
One object of the present invention is, provides a kind of Mg-Zn-Y directional solidificating alloy and preparation method thereof, and it optimizes the composition proportion of magnesium alloy and preparation technology and condition, makes the Mg-Zn-Y alloy generated have better mechanical behavior under high temperature.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of Mg-Zn-Y directional solidificating alloy, comprises the component of following mass percent: the Mg of Zn6.00% ~ 9.00%, Y1.00% ~ 2.00% and residue per-cent.
Preferably, described Mg-Zn-Y directional solidificating alloy, comprise the component of following mass percent: Zn9.00%, Y2.00% and Mg89.00%, thus the magnesium alloy that second-phase is only Icosahedral phases can be obtained, make the Mg-Zn-Y alloy generated have better mechanical behavior under high temperature.
Aforesaid Mg-Zn-Y directional solidificating alloy, the starting material adopted are: purity (massfraction) is Mg ingot, the Zn ingot of 99.9%, Mg-30Y (30%, massfraction) master alloy, thus ensureing that the purity of molten alloy is high, impurity is few.
The preparation method of aforesaid Mg-Zn-Y directional solidificating alloy, comprises the following steps:
A. get Zn, Y, Mg starting material, by the mixing of described starting material, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate;
C. lower link is utilized, what water-cooled copper ring and gallium-indium alloy formed chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when being started by muff and pull rate maintenance casting (forms the thermograde needed for experiment by the cold junction of chilling platform and the liquid alloy of higher pouring temperature, temperature when recycling muff ensures that not solidified liquid metal part is in casting, ensure that cold junction is to the Quench ability of the firm liquid alloy pulled out from muff by controlling pull rate, thus maintain the thermograde that casting starts foundation), promote the crystal unidirectional growth of the alloy of casting, obtain Mg-Zn-Y directional solidificating alloy coupon.
Can prepare by above technique the Mg-Zn-Y directional solidificating alloy coupon that height is 80 ~ 100mm, this directional solidificating alloy coupon has good intensity and plasticity simultaneously, also has good mechanical behavior under high temperature.
Preferably, in step b, c, described pouring temperature is 700 ~ 800 DEG C, pull rate is 5 ~ 30mm/min, thus can make that alloy fully melts, uniform composition, and magnesium alloy volatilization is few, also ensure that thermograde needed for directional freeze (relies on the thermograde that pouring temperature and pull rate control in cold junction-both co-controlling directional freeze processes simultaneously, make thermograde control column crystal growth needed for interval), the directional solidificating alloy of acquisition has good mechanical behavior under high temperature.
Preferred, in step b, c, described pouring temperature is 760 ~ 780 DEG C, pull rate is 10 ~ 15mm/min, thus alloy melt composition can be made evenly, and magnesium alloy volatilization is less, also ensure that thermograde needed for directional freeze (relies on the temperature gradient of solid-liquid interface that pouring temperature and pull rate control in cold junction-both co-controlling directional freeze processes simultaneously, make the interval that thermograde controls needed for column crystal growth), the directional solidificating alloy of acquisition (height can reach 100mm) has better mechanical behavior under high temperature.
In aforesaid method, in the furnace chamber of described apparatus for directional solidification, vacuum is 2.4 × 10-2Pa, reduces the volatilization of magnesium alloy, ensures that magnesium alloy does not burn simultaneously.
In order to verify above content, contriver has also carried out following experimental study:
Experimental example 1: composition proportion screening experiment
Contriver adopts Factsage software PhaseDiagram (phase module) and thermodynamic data storehouse SGTE (solution, pure substance and compound database) and magnesium base data storehouse, and drawing Zn, Y content under equilibrium conditions affects schematic diagram to the accurate brilliant quantity of formation of Mg-Zn-Y alloy.As shown in Figure 14, when Zn content be 9wt.%, Y content is 2wt.%, accurate brilliant quantity is maximum.Although standard crystalline substance when Y content is 3wt.% is more, but according to solidification theory, the growth pattern of crystal can be subject to the impact of solute concentration, can cause solute redistribution when solute concentration is too high, and then can constitutional supercooling be increased, be not suitable for column crystal growth.Therefore, in the present invention, preferred composition proportion is: Zn content is 9wt.%, Y content is 2wt.%, and residual content is Mg.
Experimental example 2: investigate preparation method to the impact of Mg-Zn-Y alloy
1, technic metal preparation and experimental technique
Method one: adopt directional solidifying method for preparing of the present invention to prepare Mg-Zn-Y directional solidificating alloy coupon.
Method two: adopt 2RRL-M8 type vacuum resistance smelting furnace to carry out melting to starting material, pouring temperature is 760 DEG C, is cast to by the alloy liquid melted in preheated metallic type, obtained Mg-Zn-Y routine casting alloy cast ingot.
The column crystal stable growth district of described Mg-Zn-Y directional solidificating alloy coupon or region and Mg-Zn-Y routine casting alloy cast ingot being cut into diameter is 10m, the high sample for 15mm, adopt WDW3100 microcomputer controlled electronic universal tester to carry out room temperature compression experiment, strain rate ε is 0.001s
-1; In addition, Gleeble-3500D hot modeling test machine carries out mechanical behavior under high temperature experiment, experimental temperature is set as 200 DEG C, 250 DEG C and 300 DEG C respectively, and strain rate is set as 1.0s respectively
-1~ 1 × 10
-3s
-1, sample is heated, is incubated 50s after heating 2min reaches target temperature, and then compresses; Wherein, for preventing sample to be oxidized in compression process, adopt argon shield.Utilize LEOJSM5400 type scanning electron microscopic observation and analysis design mothod alloy microscopic structure, utilize 2500/PC type X-ray diffractometer to carry out material phase analysis, scanning step is 0.3 ° simultaneously, between 20 ° and 90 ° (2 θ), measure XRD diffraction spectra.
2, experimental result and analysis
2.1 oriented freezing organization analyses
Fig. 1 ~ Fig. 4 is Mg-Zn-Y Solidification Structure.As shown in Figure 1, the Mg-Zn-Y alloy adopting the method (method one) in the present invention to prepare, obtains a secondary arm Parallel Growth, and longitudinal crystal boundary is straight, without the columanar structure with specific orientation of transverse grain boundaries, after measured, its column crystal length is about 35 ~ 60mm; Fig. 2 is the cross section solidified structure schematic diagram of Mg-Zn-Y directional solidificating alloy in Fig. 1, as shown in Figure 2, Mg-Zn-Y directional solidificating alloy of the present invention has columanar structure, and the cross-sectional grain of this column crystal is born of the same parents' shape, and in column crystal, go back Dispersed precipitate granular phase simultaneously.In addition, as shown in Figure 3, Figure 4, under identical magnification condition, compared with the solidified structure (as shown in Figure 4) of routine casting alloy, the mean sizes of the upper crystal grain of the cross section (as shown in Figure 3) of the directional solidificating alloy tissue obtained in the present invention is thicker, and Grain-Boundary Phase area reduces, more elongated; In addition, intergranular second-phase in routine casting alloy structure has lamellar eutectic tissue signature (as shown in the illustration in Fig. 4), and the intergranular second-phase in directional solidificating alloy tissue then more presents divorced eutectic tissue signature (as shown in inset of fig. 3).Finally, EDS analyzes display (as shown in Figure 5, Figure 6), the atomic percent of Mg, Zn and Y of the Grain-Boundary Phase in the directional solidificating alloy tissue in the present invention and the granular phase of intracrystalline is respectively 28.25%, 60.70%, 11.05% and 32.55%, 57.30%, 10.15%, Mg:Zn:Y ≈ 3:6:1 (stoichiometric ratio for icosahedral quasicrystal phase), show that its Grain-Boundary Phase and intracrystalline are granular and be icosahedral quasicrystal mutually, thus can well play accurate brilliant strengthening effect, improve the mechanical behavior under high temperature of Mg-Zn-Y alloy.
Fig. 7 is that the XRD diffraction spectra of the solidified superalloy that routine casting alloy obtains under different curing conditions from directional solidificating alloy of the present invention contrasts schematic diagram, and as shown in Figure 7, routine casting alloy and directional solidificating alloy tissue are by α-Mg and the brilliant I-Mg of standard
3zn
6y two phase composite, but compared with the XRD spectral line of routine casting alloy, the conical surface (102) crystal face in directional solidificating alloy tissue and cylinder (100) diffraction peak are stronger, and solid matter face (002) crystallographic plane diffraction peak is more weak simultaneously.During normal freezing, atom grows in the mode in solid matter face, and area density is the highest, thus in the process of atom combination, in unit surface, d/d latent heat is higher than non-solid matter face.And during directional freeze, then by controlling certain thermograde (using water coolant or gallium-indium alloy as the cold junction of chilling platform, utilize alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate), thus ensure that crystal is along the direction growth that temperature raises.
The mechanical property of 2.2 directional solidificating alloys
2.21 room-temperature mechanical property
Fig. 8 is normal temperature (20 DEG C) engineering stress-strain curve comparison diagram of employing directional solidification technique of the present invention (method one) alloy sample prepared and the alloy sample adopting routine techniques (method two) to cast, from the curve in Fig. 8, the maximum drag that breaks of the alloy sample adopting directional solidification technique of the present invention to prepare is 357MPa, and the maximum drag that breaks of the alloy sample adopting routine techniques to cast is only 232MPa, the maximum drag that breaks improves about 54%; The section rate of expansion of the alloy sample adopting directional solidification technique of the present invention to prepare is 21%, and compared with the alloy sample (section rate of expansion is 16%) adopting routine techniques to cast, its section rate of expansion improves 31%.
Organization decided performance, because the accurate crystalline substance of the crystal boundary in routine casting alloy structure is linked to be netted more, thus accurate brilliant effect is difficult to play; And preparation-obtained directional solidificating alloy in the present invention, column crystal is organized as in this directional solidificating alloy, and the orientation of column crystal and compression time Impact direction consistent, most phase interface is parallel to Impact direction, thus horizontal phase interface is few, more be conducive to resisting viscous deformation, the compressive strength of alloy is obviously increased, in addition, the preparation-obtained directional solidificating alloy of the present invention, the accurate crystalline substance of crystal boundary in this directional solidificating alloy greatly reduces, and grain particles shape Icosahedral phases increases, and thus accurate brilliant effect is given full play to; In addition, the transverse grain boundaries of the columanar structure of the preparation-obtained directional solidificating alloy of the present invention is few, grain boundary area is also less, dislocation motion is along parallel columnar chip to less by crystal boundary resistance, make dislocation mobility good and be difficult to pile up, the difficulty that the strain that the high stress concentrations region inner product causing piling up of dislocations to be formed is tired out reaches crack nucleation is larger, thus makes it more not easily rupture, improves the plasticity of Mg-Zn-Y alloy.In addition, with routine casting alloy phase ratio, organizing of the preparation-obtained directional solidificating alloy of the present invention is finer and close, and microdefect is less, and this also improves the performance of alloy to a certain extent.
2.22 thermo compression performance
Fig. 9 ~ Figure 11 is respectively directional solidificating alloy and routine casting alloy respectively under 200 DEG C, 250 DEG C and 300 DEG C of thermo compression conditions, the graphic representation that its peak stress changes with strain rate; Figure 12 is that deformation temperature affects schematic diagram to the peak stress of technic metal under differently strained speed.As shown in Figure 9, adopt alloy sample prepared by directional solidification technique of the present invention (method one) at 200 DEG C of-1.0s
-1under, its peak stress is up to 245MPa, and the alloy sample (its peak stress is 155MPa) comparatively adopting routine techniques (method two) to cast improves about 58%; When temperature-resistant, the peak value of alloy reduces with the reduction of strain rate, when strain rate is 0.001s
-1time, the peak stress of the alloy sample adopting directional solidification technique of the present invention (method one) to prepare is 171MPa, and the alloy sample (117MPa) comparatively adopting routine techniques (method two) to cast improves about 46%.Along with the rising of experimental temperature, the peak stress of alloy is downtrending gradually, at 250 DEG C of-0.1s
-1under, the peak stress of the alloy sample adopting directional solidification technique of the present invention (method one) to prepare is 207MPa, and the alloy sample (129MPa) comparatively adopting routine techniques (method two) to cast improves about 60%; In addition, at 250 DEG C of-0.001s
-1under, the peak stress of the alloy sample adopting directional solidification technique of the present invention (method one) to prepare is 114MPa, and the alloy sample (79MPa) comparatively adopting routine techniques (method two) to cast improves about 44% (shown in Figure 10).At 300 DEG C of-1.0s
-1under, the peak stress of the alloy sample adopting directional solidification technique of the present invention (method one) to prepare is 156MPa, and the peak stress of the alloy sample adopting routine techniques (method two) to cast is only 94MPa (shown in Figure 11), its peak stress improves about 66%.As can be seen here, the directional solidificating alloy in the present invention has higher hot strength compared with routine casting alloy.
From fabric analysis above, the Mg-Zn-Y alloy prepared under the directional solidification technique condition of method one (the present invention), with sosoloid α-Mg for matrix, is formed and has the columanar structure of same direction, and its Grain-Boundary Phase is as the criterion brilliant I-Mg
3zn
6y, and have the brilliant I-Mg of granular standard
3zn
6y Dispersed precipitate is in column crystal intergranular.And the Mg-Zn-Y alloy adopting the conventional casting technique of method two to obtain, be polycrystalline alloy tissue, its intergranular second-phase is linked to be netted more, the crystal boundary vertical with stress axis, is the master " source " cracked under high temperature stress.In addition, adopt alloy sample prepared by directional solidification technique of the present invention (method one), its column crystal crystal boundary aligns and behind parallel principal axis of stress direction, the stress acted under high temperature on fragile crystal boundary can be minimum, thus delay crackle and formed, improve the hot strength of alloy.In addition, the thermal distortion of metal is realized by the motion of dislocation, after dislocation is long-pending by obstruction in moving process, form high density dislocation district, when dislocation desity reaches certain threshold value, dynamic recrystallization starts forming core, with the Mg-Zn-Y alloy phase ratio under routine casting condition, the Mg-Zn-Y alloy transverse grain boundaries with continuous cylindrical crystalline texture is few, grain boundary area is less, dislocation motion is along parallel columnar chip to less by crystal boundary resistance, make dislocation mobility good and be difficult to pile up, causing dislocation desity to be difficult to reach the threshold value needed for occurrence dynamics Recrystallization nucleation; On the other hand, due to the Mg-Zn-Y alloy interior tissue with continuous columnar, to cut misorientation less, when sample is out of shape by compression, the organization formation deformed belt that it is arranged in parallel need be made, increase the misorientation of regional area, be beneficial to the formation of high-angle boundary, for its occurrence dynamics recrystallize provides prerequisite; And the grain boundary area of the initial structure of Mg-Zn-Y alloy under routine casting condition is large and intercrystalline misorientation is larger, it more easily forms a large amount of high density dislocation districts and high-angle boundary when compression set, therefore compared to Mg-Zn-Y alloy under routine casting condition, the Mg-Zn-Y alloy occurrence dynamics recrystallize with continuous cylindrical crystalline texture needs higher energy, then more be difficult to dynamic recrystallization, the ramollescence of the dynamic recrystallization that alloy is subject to reduces.Moreover the intracrystalline second-phase in oriented freezing organization is the granular icosahedral quasicrystal phase of Dispersed precipitate on matrix, and because accurate crystalline substance has good high-temperature stability, under high temperature, accurate crystalline substance still can hinder dislocation motion, improves alloy strength.
4 conclusions
(1) Mg-Zn-Y alloy is after method directional freeze of the present invention, obtain a secondary arm Parallel Growth, longitudinal crystal boundary is straight, without the columanar structure with specific orientation of transverse grain boundaries, in column crystal, Dispersed precipitate granular phase simultaneously, and Grain-Boundary Phase is icosahedral quasicrystal I-Mg mutually with intracrystalline is granular
3zn
6y;
(2), under room temperature, the maximum drag that breaks of the alloy sample adopting directional solidification technique of the present invention to prepare is 357MPa, and comparatively routine casting alloy strength (232MPa) improves about 54%; When breaking, dependent variable is 21%, and comparatively routine casting alloy (when breaking, dependent variable is 16%) improves about 31%;
(3), under high temperature, the alloy adopting directional solidification technique of the present invention to prepare is at 200 DEG C of-1.0s
-1under peak stress up to 245MPa, comparatively routine casting alloy (peak stress is 155MPa) improves about 58%; When temperature-resistant, the peak value of alloy reduces with strain rate and reduces; When strain rate is 0.001s
-1time, the peak stress of the alloy adopting directional solidification technique of the present invention to prepare is 171MPa, and comparatively routine casting alloy (peak stress is 117MPa) improves about 46%.Along with the rising of experimental temperature, the peak stress of alloy is in downtrending gradually; At 250 DEG C of-0.1s
-1under, the peak stress of the alloy sample adopting directional solidification technique of the present invention to prepare is 207MPa, comparatively adopts the alloy sample (129MPa) of routine techniques casting to improve about 60%; In addition, at 250 DEG C of-0.001s
-1under, the peak stress of the alloy sample adopting directional solidification technique of the present invention to prepare is 114MPa, comparatively adopts the alloy sample (79MPa) of routine techniques casting to improve about 44%.At 300 DEG C of-1.0s
-1under, the peak stress of the alloy adopting directional solidification technique of the present invention to prepare is 156MPa, and the peak stress of routine casting alloy is only 94MPa, and peak stress improves about 66%.It can thus be appreciated that: the directional solidificating alloy adopting proportioning of the present invention and preparation technology to obtain comparatively routine casting alloy has better mechanical behavior under high temperature.
Compared with prior art, the present invention has the following advantages: Mg-Zn-Y directional solidificating alloy of the present invention has columanar structure, and not only at room temperature have higher intensity and certain plasticity, what is more important has good mechanical behavior under high temperature; Specifically:
(1) Mg-Zn-Y alloy is after method directional freeze of the present invention, obtain a secondary arm Parallel Growth, longitudinal crystal boundary straight, without the columanar structure with specific orientation of transverse grain boundaries; Icosahedral quasicrystal I-Mg mostly is at this columanar structure's Grain-Boundary Phase
3zn
6y phase; Therefore overcome that Mg-Zn-Y Solidification Structure of the prior art is thick and accurate crystalline substance is linked to be net distribution in α-Mg interdendritic mainly with eutectic structure form, the problem that accurate brilliant strengthening effect can not give full play to;
(2), under room temperature, the maximum drag that breaks of the Mg-Zn-Y directional solidificating alloy sample adopting directional solidification technique of the present invention to prepare is 357MPa, improves about 54% compared with the intensity (232MPa) of routine casting alloy; Dependent variable when breaking is 21%, and comparatively routine casting alloy (16%) improves 31%;
(3) under high temperature, Mg-Zn-Y directional solidificating alloy prepared by directional solidification technique of the present invention is adopted, at 200 DEG C of-1.0s
-1under peak stress up to 245MPa, comparatively routine casting alloy (155MPa) improves 58%; When temperature-resistant, the peak value of Mg-Zn-Y directional solidificating alloy of the present invention reduces with the reduction of strain rate; When strain rate is 0.001s
-1time, the peak stress of directional solidificating alloy is 171MPa, and comparatively routine casting alloy (117MPa) improves about 46%.Along with the rising of experimental temperature, the peak stress of alloy is in downtrending gradually; 300 DEG C of-1.0s
-1under, the peak stress of directional solidificating alloy is 156MPa, and the peak stress of routine casting alloy is only 94MPa, and peak stress about improves 66%.It can thus be appreciated that: adopt proportioning of the present invention, directional solidificating alloy comparatively routine casting alloy that preparation technology obtains, not only at room temperature there is higher intensity and plasticity, also there is good mechanical behavior under high temperature simultaneously.
Contriver has also carried out a large amount of experimental studies to pouring temperature and pull rate, by setting different pouring temperatures and pull rate, and learn after fabric analysis is carried out to the alloy obtained: when pouring temperature is 700 ~ 800 DEG C, when pull rate is 5 ~ 30mm/min, the columanar structure's effect obtained is all fine, it at room temperature has higher intensity and plasticity, has good mechanical behavior under high temperature simultaneously; When pull rate is greater than 30mm/min, because cold junction movement velocity is too fast, column crystal growth scope can be suppressed; When pull rate is less than 5mm/min, pull rate is excessively slow, is unfavorable for that column crystal grows; When pouring temperature is lower than 700 DEG C, thermograde slope is little, causes constitutional supercooling to increase, and is unfavorable for that column crystal grows; When pouring temperature is greater than 800 DEG C, magnesium alloy then volatilizees seriously.
In addition, pouring temperature is chosen for 700,720,740,760,780,800 DEG C by contriver respectively, and for each pouring temperature, pull rate is set as 5,10,15,20,25,30mm/min, learn after carrying out fabric analysis: when pouring temperature is 760 ~ 780 DEG C, when pull rate is 10 ~ 15mm/min, columanar structure's better effects if (height can reach 100mm) of the Mg-Zn-Y directional solidificating alloy obtained, it at room temperature has higher intensity and plasticity, has better mechanical behavior under high temperature simultaneously.
Accompanying drawing explanation
Fig. 1 is the vertical 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 that the XRD diffraction spectra of the solidified superalloy that routine casting alloy obtains under different curing conditions from directional solidificating alloy contrasts schematic diagram;
Fig. 8 is the normal temperature engineering stress-strain curve comparison diagram of the alloy sample prepared of directional freeze and routine casting alloy sample;
Fig. 9 ~ Figure 11 is respectively directional solidificating alloy and routine casting alloy respectively under 200 DEG C, 250 DEG C and 300 DEG C of thermo compression conditions, the graphic representation that its peak stress changes with strain rate;
Figure 12 is that deformation temperature affects schematic diagram to the peak stress of technic metal under differently strained speed;
Figure 13 is method flow diagram of the present invention;
Figure 14 is that under equilibrium conditions, Zn, Y content affects schematic diagram to the accurate brilliant quantity of formation of Mg-Zn-Y alloy.
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
Embodiment
Embodiments of the invention 1: a kind of Mg-Zn-Y directional solidificating alloy, is prepared from (as shown in figure 13) by the following method:
A. get Mg ingot 88g, Zn ingot 12g that purity (massfraction) is 99.9%, Mg-30Y (30%, massfraction) master alloy 2.5g, by above-mentioned starting material mixing, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate; Wherein, in the furnace chamber of described apparatus for directional solidification, vacuum is 2.4 × 10
-2pa;
What c. utilize lower link, water-cooled copper ring and gallium-indium alloy to form chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate, promote the crystal unidirectional growth of the alloy of casting, obtain the high Mg-Zn-Y directional solidificating alloy coupon for 100mm;
In step b, c, described pouring temperature is 760 ~ 780 DEG C, and pull rate is 10 ~ 15mm/min.
The mass percent of the final chemical composition of the directional solidificating alloy utilizing ICAP6300 plasma spectroscopy the present embodiment to prepare is: Zn9.00%, Y2.00%, Mg89.00%.
Apparatus for directional solidification involved in aforesaid method can adopt existing installation.
Embodiment 2: a kind of Mg-Zn-Y directional solidificating alloy, is prepared from (as shown in figure 13) by the following method:
A. get Mg ingot 92g, Zn ingot 8g that purity (massfraction) is 99.9%, Mg-30Y (30%, massfraction) master alloy 1.2g, by above-mentioned starting material mixing, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate;
What c. utilize lower link, water-cooled copper ring and gallium-indium alloy to form chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate, promote the crystal unidirectional growth of alloy of casting, obtaining high is the Mg-Zn-Y directional solidificating alloy coupon of 80 ~ 100mm;
In step b, c, described pouring temperature is 700 ~ 760 DEG C, and pull rate is 5 ~ 10mm/min.
The mass percent of the final chemical composition of the directional solidificating alloy utilizing ICAP6300 plasma spectroscopy the present embodiment to prepare is: Zn6.00%, Y1.00%, Mg93.00%.
Apparatus for directional solidification involved in aforesaid method can adopt existing installation.
Embodiment 3: a kind of Mg-Zn-Y directional solidificating alloy, is prepared from by the following method:
A. get Mg ingot 89.2g, Zn ingot 9g that purity (massfraction) is 99.9%, Mg-30Y (30%, massfraction) master alloy 1.8g, by above-mentioned starting material mixing, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate;
What c. utilize lower link, water-cooled copper ring and gallium-indium alloy to form chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate, promote the crystal unidirectional growth of alloy of casting, obtaining high is the Mg-Zn-Y directional solidificating alloy coupon of 80 ~ 100mm;
In step b, c, described pouring temperature is 760 DEG C, and pull rate is 10 ~ 15mm/min.
The mass percent of the final chemical composition of the directional solidificating alloy utilizing ICAP6300 plasma spectroscopy the present embodiment to prepare is: Zn7.00%, Y1.50% and Mg92.00%.
Apparatus for directional solidification involved in aforesaid method can adopt existing installation.
Embodiment 4: a kind of Mg-Zn-Y directional solidificating alloy, is prepared from by the following method:
A. get Mg ingot 87g, Zn ingot 12g that purity (massfraction) is 99.9%, Mg-30Y (30%, massfraction) master alloy 1.2g, by above-mentioned starting material mixing, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate;
What c. utilize lower link, water-cooled copper ring and gallium-indium alloy to form chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate, promote the crystal unidirectional growth of alloy of casting, obtaining high is the Mg-Zn-Y directional solidificating alloy coupon of 80 ~ 100mm;
In step b, c, described pouring temperature is 780 DEG C, and pull rate is 15 ~ 30mm/min.
The mass percent of the final chemical composition of the directional solidificating alloy utilizing ICAP6300 plasma spectroscopy the present embodiment to prepare is: Zn9.00%, Y1.00% and Mg85.00%.
Apparatus for directional solidification involved in aforesaid method can adopt existing installation.
Adopt the condition described in embodiment 1 ~ 4 to prepare Mg-Zn-Y directional solidificating alloy coupon, after measured, result is as shown in table 1.Second-phase in the Mg-Zn-Y alloy structure that embodiment 1 obtains is only icosahedral quasicrystal phase; Second-phase in the Mg-Zn-Y alloy structure obtained in embodiment 2,3 mostly is icosahedral quasicrystal phase, a small amount of w phase; Second-phase in the Mg-Zn-Y alloy structure obtained in embodiment 4 only deposits a small amount of icosahedral quasicrystal phase.Although the column crystal in the alloy structure obtained in embodiment 3 is more straight, because volume fraction, especially Icosahedral phases shared by its second-phase are less than embodiment 1, therefore intensity is low compared with the alloy structure in embodiment 1.And only have a small amount of Icosahedral phases in the alloy structure that embodiment 4 obtains, be therefore that room-temperature property or high-temperature behavior are all not as good as embodiment 1.
Table 1
Claims (6)
1. a Mg-Zn-Y directional solidificating alloy, is characterized in that, comprises the component of following mass percent: the Mg of Zn6.00% ~ 9.00%, Y1.00% ~ 2.00% and residue per-cent.
2. Mg-Zn-Y directional solidificating alloy according to claim 1, is characterized in that, comprises the component of following mass percent: Zn9.00%, Y2.00% and Mg89.00%.
3. a preparation method for the Mg-Zn-Y directional solidificating alloy described in claim 1 or 2, is characterized in that, comprise the following steps:
A. get Zn, Y, Mg starting material, by the mixing of described starting material, heat fused, obtain alloy liquid;
B. continue the alloy liquid described in heating, and control alloy liquid and be cast under different pouring temperatures in the lower pull system of apparatus for directional solidification, control lower pull system simultaneously and lift with different pull rate;
What c. utilize lower link, water-cooled copper ring and gallium-indium alloy to form chilling platform can the cold junction of orientation movement, alloy liquid temperature and cold junction formation temperature gradient, and the thermograde formed in solid-liquid interface when casting starts is maintained by muff and pull rate, promote the crystal unidirectional growth of the alloy of casting, obtain Mg-Zn-Y directional solidificating alloy coupon.
4. the preparation method of Mg-Zn-Y directional solidificating alloy according to claim 3, is characterized in that, in step b, c, described pouring temperature is 700 ~ 800 DEG C, and pull rate is 5 ~ 30mm/min.
5. the preparation method of Mg-Zn-Y directional solidificating alloy according to claim 4, is characterized in that, in step b, c, described pouring temperature is 760 ~ 780 DEG C, and pull rate is 10 ~ 15mm/min.
6. the preparation method of Mg-Zn-Y directional solidificating alloy according to claim 3, is characterized in that, in the furnace chamber of described apparatus for directional solidification, vacuum is 2.4 × 10
-2pa.
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| CN109930046A (en) * | 2019-04-22 | 2019-06-25 | 东北大学秦皇岛分校 | A kind of magnesium-rare earth alloy and preparation method thereof with room temperature high-ductility directional solidification |
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