CN102766791B - 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, specifically a kind of brilliant Mg-6Zn-3Y of enhancing of standard Alloy And Preparation Method with ultra-fine solidified structure.
Background technology
Magnesium alloy has the features such as good electric conductivity, thermal conductivity, capability of electromagnetic shielding and high specific tenacity, specific rigidity, damping property, the lightest structural metallic materials of current practical application, at aerospace, automobile and 3C(computer, communicate by letter and consumption electronic product) etc. industry have broad application prospects.But, magnesium alloy because intensity is lower, the problem such as poor toughness, the good high temperature creep property of plastic working difficulty be poor, limited it in industrial further application.Therefore, by various technologies of preparing, improve magnesium alloy mechanical property, expand the emphasis that magnesium alloy range of application is the research and development of magnesium alloy technical field.
Since people such as the Xie Qieman of National Bureau of Standards (NBS) (D.shechtman) etc. in 1984 finds first accurate crystalline substance in the Al-Mn of chilling alloy, in aluminium base, magnesium base and other alloy, in succession found a variety of accurate brilliant.1993, first the Luo Zhi equality people of China Beijing Inst. of Aeronautical Materials determined that the Mg3Zn6Y ternary phase in Mg-Zn-Y alloy is icosahedral quasicrystal, and was that accurate crystalline substance has carried out a large amount of research work to Mg-Zn-RE.Accurate crystalline phase, because having unique atomic arrangement structure, makes it have excellent mechanical property and physicals, as high strength, low-friction coefficient, lower thermal conductivity, low conductivity, anti-oxidant, corrosion-resistant etc.Research shows, thinning microstructure is one of topmost enhancement method of magnesium alloy, and as accurate crystalline form looks, size, quantity and the distribution of wild phase, the performance of Magnuminium is had to important impact, on magnesium alloy substrate, the granular accurate crystalline phase of disperse distribution, is expected to obtain high-performance quasicrystal particle reinforced magnesium matrix alloy material and matrix material.
Through retrieval, find, in disclosed technology, as CN 101705405 A disclose magnesium base spherical quasi crystal intermediate alloy and preparation method thereof, adopt the method for controlling rate of cooling to prepare five yuan of magnesium base icosahedron spherical quasi crystal master alloys of Mg-Zn-Y-Mn-Cu, its chemical composition is (wt. %): Mg 55.0 ~ 65.0%, Zn 30.0 ~ 40.0%, Y 2.5 ~ 5.5%, Mn 0.10 ~ 1.50%, Cu 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 2 ~ 7, and volume accounts for 35 ~ 45% of cumulative volume.
As, CN 101705406 A disclose magnesium base spherical quasi crystal intermediate alloy and preparation method thereof, adopt the method for controlling rate of cooling to prepare Mg-Zn-Y-C quaternary magnesium base icosahedron spherical quasi crystal master alloy, its chemical composition is (wt. %): Mg 55.0 ~ 65.0%, Zn 30.0 ~ 40.0%, Y 2.5 ~ 5.5%, C 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 2 ~ 7, and volume accounts for 40 ~ 48% of cumulative volume.
As, CN 101705407 A disclose magnesium base spherical quasi crystal intermediate alloy and method for making thereof, adopt the method for controlling rate of cooling to prepare Mg-Zn-Y-Ti quaternary magnesium base icosahedron spherical quasi crystal master alloy, its chemical composition is (wt. %): Mg 55.0 ~ 65.0%, Zn 30.0 ~ 40.0%, Y 2.5 ~ 5.5%, Ti 0.10 ~ 0.50%.The spherical quasi crystal diameter of preparation is 6 ~ 10, and volume accounts for 30 ~ 40% of cumulative volume.
As, CN 102212727 A disclose a kind of Authigenic quasicrystal-reinforced Mg-Zn-Y alloy and melting method, employing adds the method for Al-Ti-C to prepare Authigenic quasicrystal-reinforced Mg-Zn-Y alloy in melt, its chemical composition is (wt. %): Zn 3.0 ~ 10.0%, Y 0.5 ~ 3.0%, Al-Ti-C 0.05 ~ 1.0%.
In sum, above-mentioned disclosed patented technology content be mainly common solidify with rapid solidification condition under the magnesium base spherical quasi crystal intermediate alloy that makes, its prepared icosahedral quasicrystal phase yardstick is level, and little at the report of rank about the brilliant yardstick of standard, especially for preparation under ultra-high voltage, there is the accurate brilliant Mg-6Zn-3Y of the enhancing alloy of ultra-fine solidified structure and have no relevant report.
Summary of the invention
In view of above-mentioned present situation, the object of this invention is to provide a kind of brilliant Mg-6Zn-3Y of enhancing of standard magnesium alloy 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 been to provide 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 by controlling the method preparation of freezing pressure, Heating temperature and rate of cooling.
The technical scheme that technical solution problem of the present invention is taked is:
The brilliant alloy that strengthens of standard with ultra-fine solidified structure, its chemical composition 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 described ultra-fine solidified structure, comprises the steps:
1, prepare As-cast Mg-Zn-Y Alloy material under normal pressure:
Get and account for the magnesium ingot that raw material total amount mass percent is 91.0%, 6.0% zinc ingot metal, 3.0% pure yttrium, put into baking oven and at 200 ℃, carry out prewarming baking, the Heating temperature of crucible electrical resistance furnace is set as to 760 ~ 780 ℃, when crucible temperature rises to 350 ~ 400 ℃, first in crucible, add magnesium ingot and zinc ingot metal, start to pass into CO2/SF6 mixed gas as protection gas, continue to heat up, after the magnesium ingot in crucible and zinc ingot metal melt completely, add again pure yttrium, after melting completely, stirs pure yttrium 2 ~ 5 minutes, 760 ~ 780 ℃ of insulations 10 ~ 15 minutes, remove solution surface scum silica frost, Mg-Zn-Y alloy solution is cast in metal pattern, obtain Mg-6Zn-3Y cast alloy material, cast alloy material is carried out to abundant diffusion annealing,
2, in GPa level superelevation press control freezing pressure, Heating temperature and rate of cooling preparation, there is the brilliant Mg-6Zn-3Y of enhancing of the standard alloy of ultra-fine solidified structure:
The Mg-6Zn-3Y alloy material that step 1 is obtained carries out line cutting, be processed into the high pressure sample of Ф 4 х 5mm, and put into graphite assembling and overlap, graphite assembling cover is put into an actor's rendering of an operatic tune of CS-1B type high pressure six-plane piercer, setting freezing pressure is 6GPa, Heating temperature is 1300 ℃, be heated rapidly to default Heating temperature, sample is melted completely, and at this temperature heat-insulation pressure keeping 15min, control solidification cooling rate is 300K/S, finally makes the brilliant Mg-6Zn-3Y of enhancing of the standard alloy of the ultra-fine solidified structure that contains icosahedral quasicrystal phase.
In the present invention, there is the quasicrystal reinforced magnesium alloy of ultra-fine solidified structure, its Characteristics of As-cast Structure is comprised 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 cumulative volume.
In the present invention, related graphite assembling cover, comprises the boron nitride crucible, plumbago crucible, the WC supercharging post that in agalmatolite, set gradually, and six of described graphite assembling cover is faced should hammer, and Mg-6Zn-3Y alloy sample is placed in boron nitride crucible.
The invention has the beneficial effects as follows:
One, one of innovative point that the present invention has the brilliant Mg-6Zn-3Y of enhancing of the standard alloy preparation method of ultra-fine solidified structure is under GPa level superelevation, by controlling freezing pressure, Heating temperature and solidification cooling rate, obtains required alloy material.
1, freezing pressure has great impact to the acquisition of ultra-fine dendritic structure: while solidifying under GPa level high pressure, solute spread coefficient can be index and doubly reduce, in matrix, easily form solute atoms enrichment region, the existence at crystals with heterogeneous forming core particle has increased crystal nucleation rate greatly, the speed of growth of crystal also can be suppressed simultaneously, so solidify under hyperpressure, 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 a best solidification cooling rate in the formation of accurate crystalline phase, and the too low meeting of rate of cooling causes growing up of accurate crystalline phase, affects the performance of alloy, but too high rate of cooling can suppress again accurate brilliant forming core, even cannot obtain accurate crystalline phase.
Two, the brilliant Mg-6Zn-3Y of enhancing of the standard alloy that the present invention has a 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 normal pressure on the one hand, and dendritic structure obtains significant refinement; On the other hand, being distributed on α-Mg matrix of a large amount of, tiny brilliant even dispersion of granular standard, causing the microhardness of this alloy can reach under HV89(normal pressure is HV68), than having improved 31% under normal pressure; Young's modulus is reduced to 62GPa by the 68GPa under normal pressure, shows that this what gold utensil has good intensity and good plasticity.
2, the brilliant enhancing of the standard with the ultra-fine solidified structure alloy obtaining under high pressure is carried out to long-time ageing treatment at 200 ℃, experimental result demonstration, this alloy structure has good thermostability.DSC detection is analyzed also and is shown, the brilliant solvent temperature that starts of standard obtaining under high pressure is compared with high 5 ℃ of left and right under normal pressure, and heat enthalpy value increase, and this also shows that the standard crystalline substance obtaining under high pressure has good thermostability.
Accompanying drawing explanation
Figure a in Fig. 1 is that the present invention shows that under high pressure, obtaining Mg-6Zn-3Y alloy structure is the Solidification Microstructure Morphology with ultra-fine dendrite, and figure b shows being distributed on magnesium alloy substrate of a large amount of brilliant even dispersion of tiny standard in pelletized form;
Graphite assembling cover schematic cross-section for Fig. 2 high pressure.
Embodiment
By the following examples technical scheme of the present invention is further described.
1, in melt quality percentage ratio Wt%, take Mg: 91.0%, Zn:6.0%, Y:3.0%;
2, the magnesium ingot of above-mentionedization mass percent, zinc ingot metal, pure yttrium metal charge are put into the crucible of baking oven at 200 ℃ and carry out prewarming baking;
3, the Heating temperature of crucible electrical resistance furnace is set as to 780 ℃, when crucible temperature rises to 380 ℃, in crucible, add magnesium ingot and zinc ingot metal, and start to pass into CO2/SF6 mixed gas as protection gas, continue to heat up, after the magnesium ingot in this crucible and zinc ingot metal melt completely, add pure yttrium, after melting completely, stirs pure yttrium 2 ~ 5 minutes, and 780 ℃ of insulations 10 ~ 15 minutes, stand-by after having stirred;
4, Mg-Zn-Y alloy solution temperature is adjusted to 760 ℃, after standing 3 ~ 5 minutes, remove solution surface scum silica frost, then Mg-Zn-Y alloy solution is cast in metal pattern, obtain Mg-6Zn-3Y cast alloy material, then cast alloy material is carried out to abundant diffusion annealing;
5, the Mg-6Zn-3Y cast alloy material after above-mentioned diffusion annealing is carried out to line cutting, be processed into the high pressure sample of Ф 4 х 5mm;
6, the Mg-6Zn-3Y sample of the Ф processing 4 х 5mm is put into graphite assembling cover, graphite assembling is mounted on to the cavity position of CS-1B type high pressure cubic apparatus, setting freezing pressure is 6GPa, Heating temperature is 1300 ℃, be heated rapidly to default Heating temperature, the Mg-6Zn-3Y sample of Ф 4 х 5mm is melted completely, and at this temperature heat-insulation pressure keeping 15min, control solidification cooling rate is 300K/S, finally makes the Mg-6Zn-3Y alloy that contains icosahedral quasicrystal phase and have ultra-fine solidified structure.
In the present embodiment, there is the quasicrystal reinforced magnesium alloy of ultra-fine solidified structure, its Characteristics of As-cast Structure is comprised 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 cumulative volume.
The graphite assembling cover of above-mentioned middle indication, is shown in Fig. 2.Described graphite assembling cover, comprise boron nitride crucible 4, with the plumbago crucible 2 that is placed in boron nitride crucible 4 outsides, complete installation is in WC supercharging post 3, the symmetrical both sides that are positioned at WC supercharging post 3 are provided with agalmatolite 1, six faces at described graphite assembling cover are provided with hammer 6, and Mg-6Zn-3Y alloy sample 5 is placed in the boron nitride crucible 4 in graphite assembling cover.
Illustrate: the measuring method of temperature in High Pressure Solidification process: adopt jig drill head in the punching of place, cubes large pyrophyllite block right angle, until touch sample, then thermocouple wire is put into and touched sample, the other end of thermopair is temperature recording unit.
The measuring method of pressure: resistance strain gage is bonded on top press matrix closely by tackiness agent, when the stressed generation strain variation of matrix, resistance strain gage also produces deformation together, the resistance of foil gauge is changed, thereby making to be added in ohmically voltage changes, 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 absolutely proves that the present invention has, referring to accompanying drawing.
Fig. 1 is the displaing micro tissue topography (SEM) of the Mg-6Zn-3Y alloy that has ultra-fine solidified structure and contain icosahedral quasicrystal phase that makes of this enforcement.
Figure a shows that under high pressure, obtaining Mg-6Zn-3Y alloy structure is the dendrite morphology with the solidified structure of Ultra-fine Grained.
Figure b shows being distributed on magnesium alloy substrate of a large amount of brilliant even dispersion of tiny standard in pelletized form.
Claims (1)
1. the brilliant Mg-6Zn-3Y of enhancing of a standard alloy with ultra-fine solidified structure, is characterized in that: its chemical composition is counted by mass percent wt%: Mg: 87.0 ~ 93.0%, Zn: 3.0 ~ 10.0%, Y: 1.0 ~ 3.0%;
The brilliant preparation method who strengthens Mg-6Zn-3Y alloy of the described standard with ultra-fine solidified structure:
(1) prepare As-cast Mg-Zn-Y Alloy material under normal pressure:
Get and account for the magnesium ingot that raw material total amount mass percent is 91.0%, 6.0% zinc ingot metal, 3.0% pure yttrium, put into baking oven and at 200 ℃, carry out prewarming baking; It is 760 ~ 780 ℃ that crucible electrical resistance furnace is set as to Heating temperature, when crucible temperature rises to 350 ~ 400 ℃, in crucible, add magnesium ingot and zinc ingot metal, start to pass into CO2/SF6 mixed gas as protection gas, continue to heat up, after the magnesium ingot in crucible and zinc ingot metal melt completely, add pure yttrium, after melting completely, stirs pure yttrium 2 ~ 5 minutes, 760 ~ 780 ℃ of insulations 10 ~ 15 minutes, remove solution surface scum silica frost, Mg-Zn-Y alloy solution is cast in metal pattern, obtain Mg-6Zn-3Y cast alloy material, then as cast condition Mg-6Zn-3Y is carried out to diffusion annealing;
(2) in GPa level superelevation press control freezing pressure, Heating temperature and solidification cooling rate preparation, contain the granular accurate brilliant Mg-6Zn-3Y alloy with ultra-fine solidified structure of nano level:
The Mg-6Zn-3Y cast alloy material of step (1) is carried out to line cutting, be processed into the high pressure sample of Ф 4 х 5mm, put into graphite assembling cover, graphite assembling is mounted on to the cavity position of CS-1B type high pressure cubic apparatus, setting freezing pressure is 6GPa, and Heating temperature is 1300 ℃; Be heated rapidly to default Heating temperature, sample melted completely, and at this temperature heat-insulation pressure keeping 15min, control solidification cooling rate is 300K/S, finally makes the Mg-6Zn-3Y alloy that contains the accurate brilliant ultra-fine solidified structure of nano level;
(3) the brilliant Mg-6Zn-3Y alloy that strengthens of the standard of prepared ultra-fine solidified structure:
Its Characteristics of As-cast Structure is comprised 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, its diameter is 50-100 μ m, and granular accurate brilliant volume accounts for 25 ~ 35% of this alloy cumulative volume.
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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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