CN107326237B - A kind of magnesium alloy and preparation method thereof of low temperature resistant environment - Google Patents

A kind of magnesium alloy and preparation method thereof of low temperature resistant environment Download PDF

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CN107326237B
CN107326237B CN201710538439.3A CN201710538439A CN107326237B CN 107326237 B CN107326237 B CN 107326237B CN 201710538439 A CN201710538439 A CN 201710538439A CN 107326237 B CN107326237 B CN 107326237B
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magnesium
alloy
ingot
magnesium alloy
melt
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CN107326237A (en
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仲志国
卢志文
李婧
屈重年
叶铁
马春华
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Nanyang Normal University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/02Alloys based on magnesium with aluminium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention discloses a kind of magnesium alloy of low temperature resistant environment, the mass fraction of each element is in the magnesium alloy:Al:1.2~2%;Nd:1.4%;Y:2.1%;Ag:0.9~3.5%;Zr:0.2~2%;Surplus is Mg.Also disclose a kind of preparation method of the magnesium alloy of low temperature resistant environment, sequentially add magnesium ingot, aluminium ingot, silver ingot, magnesium yttrium intermediate alloy, magnesium neodymium intermediate alloy and zirconium ingot, it stirs evenly, cast and be heat-treated, and ultrasonic activation is applied to mold in casting process, finally obtain low temperature resistant magnesium alloy, so that the low temperature ductility and tensile strength of alloy are greatly improved, greatly reduce the fracture probability of magnesium alloy parts under low temperature environment, the service life that the outer space has used the magnesium alloy equipment is improved, its failure rate is reduced.

Description

A kind of magnesium alloy and preparation method thereof of low temperature resistant environment
Technical field
The present invention is divisional application, and parent application number is 2016101583088, and the applying date is on March 18th, 2016, female case A kind of magnesium alloy and preparation method thereof of low temperature resistant environment of denomination of invention.The present invention relates to magnesium alloy technical fields, and in particular to A kind of magnesium alloy and preparation method thereof of low temperature resistant environment.
Background technology
Magnesium alloy is as most light structural metallic materials, and, specific stiffness height high with specific strength, shock resistance is good, is electromagnetically shielded It has excellent performance, the advantages that recuperability is good, there is wide application in fields such as automobile, portable instrument, electronics industry, aerospaces Foreground.China possesses magnesium resource the abundantest in the world, and development magnesium alloy processing technology of preparing is to realizing from magnesium resource advantage Conversion to economic advantages is of great significance.
With magnesium alloy applied in society it is more and more extensive, for the guarantor of magnesium alloy alloy property under high temperature environment Hold more and more with Study of Lifting, but magnesium alloy can also be in low-temperature vacuum environment in aerospace field.Because magnesium closes The high-performance and low-density of gold so that the various parts made by magnesium alloy use in satellite, spaceship, various detectors It is more and more, which is chronically in the outer space, and the outer space refers to the area of space except earth dense atmosphere, is Vacuum or environment close to vacuum, and 500 DEG C are may be up in the face temperature of shining upon, but in shadow surface temperature and far from permanent Its local surface of star is minimum close to absolute zero;And for finding that the surrender of magnesium alloy is strong during the performance study of magnesium alloy Degree and tensile strength are gradually increasing as temperature reduces, but elongation is gradually reduced.
Ductility and elongation percentage are closely bound up, are the plasticity for reflecting material in fact, and so-called plasticity is anti-in pressure vessel It is material that face, which is said, can bear great plastic deformation without cracked performance under external force.It was verified that relatively low At a temperature of when working, often there is low stress brittle fracture.There are two the reason of causing this result in fact, and one is with temperature The plastic property of the reduction of degree, material is declined, and second, which is material internal, inevitably certain microdefects, for example small is split Line.The reduction of magnesium alloy parts plasticity can then cause its fracture probability under vacuum low-temperature environment to increase, this is used in the outer space When can substantially reduce the service life of equipment, contingency may be caused suddenly, huge loss is caused and endanger astronaut Life.
Invention content
In view of this, in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of magnesium alloys of low temperature resistant environment And preparation method thereof, the ductility of magnesium alloy at low ambient temperatures is improved, it is crisp at low ambient temperatures to reduce magnesium alloy part Property fracture probability.
In order to solve the above technical problems, the technical solution used in the present invention is:
A kind of magnesium alloy of low temperature resistant environment, the mass fraction of each element is in the magnesium alloy:
Al:1.2~2%;
Rare earth element:1~3.5%;
Ag:0.9~3.5%;
Zr:0.2~2%;
Surplus is Mg.
Further, the rare earth element includes Nd and Y.
Further, the mass fraction of Nd is 0.1~3.4% in the magnesium alloy, the mass fraction of Y in the magnesium alloy It is 0.1~3.4%.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 745 DEG C~755 DEG C, be again stirring for uniformly, most Melt is carried out afterwards zirconium ingot is added after being warming up to 760 DEG C~775 DEG C, 5~10min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, in the step 2) protective gas be purity 99.9% argon gas.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.1mm~1mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process.
Further, the casting temperature in casting process is monitored, ultrasonic transducer is contacted with mold, works as casting When part temperature is cooled to 650 DEG C~740 DEG C, it is 40KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to At 550 DEG C~650 DEG C, it is 80KHz that ultrasonic transducer, which applies ultrasonic frequency,.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 330 DEG C~360 DEG C to keep temperature, and the time is 1~3h, then be warming up to 530 DEG C~ 560 DEG C, 8~9h is kept, then be cooled to 170 DEG C~180 DEG C, keep 30~40h, finally taken out and carry out room temperature water cooling.
Further, the room temperature ensures temperature at 18 DEG C~24 DEG C.
The main problem that the present invention is directed to is the ductility of magnesium alloy under vacuum low-temperature environment, and the slip system of magnesium causes less Its plastic deformation ability force difference obtains reason, can generate additional sliding in crystal under higher temperature so that magnesium is when the temperature rises Plasticity enhances, and ductility is poor under low temperature, although yield strength and tensile strength all get a promotion, but this kind of magnesium alloy The outer space using when be susceptible to brittle fracture.Silver ingot is added after magnesium ingot fusing, can make magnesium alloy crystal axis Than reducing, to activate prism slip system, ensure that magnesium alloy still has preferable ductility at low ambient temperatures.
Rare earth neodymium forms new compound Al with aluminium in the magnesium alloy11Nd3, reduce Mg17Al12The quantity and size of phase, make It becomes Dispersed precipitate from discontinuous net distribution, can effectively hinder grain-boundary sliding and crack propagation, to refining alloy group It knits, the mechanical property of magnesium alloy is made to get a promotion.Rare-earth yttrium has the function of crystal grain thinning, enhances tensile strength and improves compacted Become performance, additionally it is possible to improve corrosion, make up the defect of silver in the magnesium alloy.In melting, rare-earth yttrium is subcooled by crystallization front The increase of degree has refined casting grain structure, and hinders recrystallization and crystal grain long in hot procedure and in annealing process Greatly, to realize the purpose of refinement magnesium and magnesium alloy crystal grain, increase the alloy property of magnesium alloy.
Zirconium is most effective grain refiner in the magnesium alloy, moreover it is possible to is purged to the impurity in melt, enhancing magnesium closes The tensile strength of gold, improves its corrosion resistance.Therefore zirconium powder is finally added in the present invention, and the addition of zirconium is by powdered Zirconium powder is uniformly sprinkling upon bath surface by addition, and stirring can allow zirconium uniformly dispersing in melt in two minutes, to gas and Fe etc. Impurity is purged, and can accelerate the speed of final step, and magnesium alloy burning is avoided so that oxidation is serious.
Infrared temperature sensor can be used for the casting temperature monitoring in casting process to realize that non-contact temperature is adopted Collection, ultrasonic transducer are controlled by supersonic generator, are changed to the frequency of ultrasonic wave.Casting process applies super Sound wave, which improves the performance of magnesium alloy, has prodigious facilitation, when magnesium alloy temperature is very high and also in molten condition when to it The ultrasonic frequency of application is larger, and the acoustic pressure that ultrasonic wave will produce positive and negative alternation when propagating reaches to generate cavitation effect Tissue, crystal grain thinning are purified, stirring melt makes the effect of microstructure homogenization;Start to solidify when Mg alloy castings temperature is reduced to When, the frequency of ultrasonic wave suitably increases amplitude and suitably reduces, and on the one hand ensures the smoothness of cast(ing) surface, on the other hand improves magnesium Effective degree of supercooling of alloy molten solution, reduces critical nucleus radius, and to increase nucleation rate, crystal grain thinning enhances the power of alloy Learn performance.
Beneficial effects of the present invention:
1, by adding human lymph node its room-temperature ductility and low temperature ductility in magnesium alloy, with existing magnesium alloy phase Than in the tension test for carrying out 1mm/min, when temperature is 0 DEG C, magnesium alloy elongation percentage 29.8% of the present invention, tensile strength is 362MPa, the AZ31B magnesium alloy elongation percentage to circulate on the market are 17.4%, tensile strength 265MPa, are -196 DEG C in temperature When, magnesium alloy elongation percentage 10.6% of the present invention, tensile strength 486MPa, the AZ31B magnesium alloy elongation percentage to circulate on the market is 3.8%, tensile strength 301MPa greatly reduce the fracture probability of magnesium alloy parts under low temperature environment, and improving the outer space makes With the service life of the magnesium alloy equipment, its failure rate is reduced;
2, the rare earth element being added have the function of in magnesium alloy fused mass dehydrogenation, deoxygenation, sulphur removal, except iron, except field trash, Achieve the effect that refinery by de-gassing, purification melt;Rare earth element can be such that the mechanical property of magnesium alloy is carried with refining alloy tissue It rises;And there is rare earth element higher solid solubility, rare earth atom are dissolved in the magnesium alloy in magnesium matrix, enhance interatomic combination Power makes matrix generate distortion of lattice, slows down atoms permeating rate, and dislocation motion is hindered to improve the strong of alloy to strengthen matrix Degree and high temperature creep property;
3, zirconium powder is added to be easy and fast to fuse into magnesium alloy fused mass, eliminating impurities to the end, and energy is served to melt The alloy property and corrosion resistance for significantly improving magnesium alloy avoid causing magnesium alloy corrosion resistance poor after addition silver, then Since the corrosion resistance of alloy under vacuum environment can be improved, magnesium alloy of the present invention can be made to no longer need to misgivings corrosion and ask Topic is conducive to the permanent work of safety of magnesium alloy part.
4, by applying ultrasonic activation to mold in casting process, and ultrasonic wave is reached inside magnesium alloy, is refined The crystal grain of strand, and then improve the plasticity and ductility of alloy so that magnesium alloy has higher ductility to adapt to low temperature ring Border.
Specific implementation mode
For a better understanding of the present invention, present disclosure, but this hair are further fairly set out with reference to embodiment Bright protection content is not limited solely to the following examples, and specific implementation mode is as follows:
Embodiment one
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.3%;Nd:0.5%;Y:0.5%;Ag:1%;Zr:0.3%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment two
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.4%;Nd:1.5%;Y:1.5%;Ag:1.5%;Zr:0.6%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment three
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.5%;Nd:2.1%;Y:1.4%;Ag:2.0%;Zr:0.9%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Example IV
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.6%;Nd:1.4%;Y:2.1%;Ag:3.1%;Zr:1.2%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment five
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.7%;Nd:1.3%;Y:2.2%;Ag:3.3%;Zr:1.6%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment six
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.9%;Nd:3.3%;Y:0.2%;Ag:3.4%;Zr:1.9%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C
Embodiment one to embodiment six is constant to experimental condition progress, is adjusted, does to each component mass percent The experiment obtained.Performance detection is carried out to magnesium alloy made of six embodiments, is machined by numerically controlled lathe, making drawing is National standard tensile sample, long 63mm, stretch section diameter 8mm, fixing end diameter 10mm, by electronic tensile test machine in 1mm/ Mechanical property is tested under the tensile speed of min, emphasis of the present invention is in order to improve the elongation percentage of magnesium alloy under low temperature environment, so dividing It is not tested under 0 DEG C and -196 DEG C of environment, specific data are shown in following table:
The performance most preferably example IV it can be seen from upper figure, tensile strength at 0 DEG C can reach 362MPa, prolong It is 29.8% to stretch rate, and tensile strength can reach 486MPa in the environment of -196 DEG C, although elongation percentage is declined, 10% or more is remained at, this makes the magnesium alloy workpiece under low temperature not have larger probability and brittle fracture occur.
Next using each component mass percent in example IV, change working condition, Properties of Magnesium Alloy is carried out Testing inspection.
Embodiment seven
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.6%;Nd:1.4%;Y:2.1%;Ag:3.1%;Zr:1.2%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment eight
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.6%;Nd:1.4%;Y:2.1%;Ag:3.1%;Zr:1.2%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment nine
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.6%;Nd:1.4%;Y:2.1%;Ag:3.1%;Zr:1.2%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, by ultrasonic transducer and mould Tool contact, it is 40KHz that ultrasonic transducer, which applies ultrasonic frequency,.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then drop Temperature keeps 35h to 175 DEG C, finally takes out and carries out room temperature water cooling, and the room temperature ensures temperature at 21 DEG C.
Embodiment ten
A kind of magnesium alloy of low temperature resistant environment of the present embodiment, the mass fraction of each element is in the magnesium alloy:
Al:1.6%;Nd:1.4%;Y:2.1%;Ag:3.1%;Zr:1.2%;Surplus is Mg.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, includes the following steps:
1) according to the mass fraction of each element in above-mentioned magnesium alloy weigh magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, among magnesium neodymium Alloy, zirconium ingot and silver ingot, clean equipment and keep drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to injection protection gas in graphite crucible Body simultaneously starts melting, and protective gas is the argon gas of purity 99.9%;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring evenly Melt is carried out magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, be again stirring for uniformly, finally to melt It carries out that zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly.
4) it skims to bath surface, and cools down to melt, poured into mold after melt temperature is down to 740 DEG C Carry out obtained Mg alloy castings of casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, powdered processing is carried out to zirconium ingot before zirconium ingot is added in the step 3) so that zirconium ingot becomes Granular zirconium powder, and its granularity is 0.2mm.
Further, the method that melt is added in the zirconium powder is uniformly to be sprinkling upon bath surface, then passes through mixing plant pair Melt stirs 2min.
Further, ultrasonic activation is applied to mold in the step 4) casting process, to the casting in casting process Temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and it is 545 DEG C to keep temperature, keeps 12h, finally takes out and carries out room temperature water cooling, described Room temperature ensures temperature at 21 DEG C.
Embodiment 11
Its with example IV difference lies in:Ultrasonic activation is applied to mold in the step 4) casting process, to pouring Casting temperature during casting is monitored, and ultrasonic transducer is contacted with mold, when casting temperature be cooled to 650 DEG C~ At 740 DEG C, it is 80KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasound It is 80KHz that wave transducer, which applies ultrasonic frequency,.
Embodiment 12
Its with example IV difference lies in:Ultrasonic activation is applied to mold in the step 4) casting process, to pouring Casting temperature during casting is monitored, and ultrasonic transducer is contacted with mold, when casting temperature be cooled to 650 DEG C~ At 740 DEG C, it is 40KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasound It is 90KHz that wave transducer, which applies ultrasonic frequency,.
Embodiment 13
Its with example IV difference lies in:Ultrasonic activation is applied to mold in the step 4) casting process, to pouring Casting temperature during casting is monitored, and ultrasonic transducer is contacted with mold, when casting temperature be cooled to 650 DEG C~ At 740 DEG C, it is 40KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasound It is 70KHz that wave transducer, which applies ultrasonic frequency,.
Embodiment 14
Its with example IV difference lies in:Ultrasonic activation is applied to mold in the step 4) casting process, to pouring Casting temperature during casting is monitored, and ultrasonic transducer is contacted with mold, when casting temperature be cooled to 650 DEG C~ At 740 DEG C, it is 30KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasound It is 80KHz that wave transducer, which applies ultrasonic frequency,.
Embodiment 15
Its with example IV difference lies in:Ultrasonic activation is applied to mold in the step 4) casting process, to pouring Casting temperature during casting is monitored, and ultrasonic transducer is contacted with mold, when casting temperature be cooled to 650 DEG C~ At 740 DEG C, it is 50KHz that ultrasonic transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasound It is 80KHz that wave transducer, which applies ultrasonic frequency,.
Embodiment seven to embodiment 15 is changed to production technology, and embodiment seven does not carry out at powdered zirconium ingot Zirconium ingot, is directly put into melt by reason;Embodiment eight does not use ultrasonic activation to handle in casting process;Embodiment nine is being poured It is handled using ultrasonic activation during casting, but the frequency of ultrasonic transducer, which is maintained at 40KHz, not to be changed;Embodiment ten changes Become last heat treatment process, the multi-temperature segmentation heat treatment only with conventional heat treatment method, rather than in the present invention is real It applies example 11 to 15 and changes ultrasonic frequency, the experimental data of nine groups of experiments and example IV is as follows:
As seen from the above table, zirconium ingot does not do powdered processing, is not easy to be quickly dispersed in melt, reduces to alloy melt Clean-up effect, cause alloy property to be declined.Ultrasonic activation is not added in casting process in embodiment eight, leads to alloy Performance decline it is more, although and embodiment nine adds ultrasonic activation, not as temperature change is to ultrasonic frequency It being adjusted, the ultrasonic wave of lower frequency does not have better facilitation to the solidification of magnesium alloy in alloy graining process, It is also easy to that so that slab oscillation mark depth increased, adverse effect is played to magnesium alloy;Heat treatment is conventional skill in embodiment ten Art, and example IV is heat-treated by the placement of multi-temperature rapid lapse of time, is reduced alloy internal stress and brittleness, is increased alloy Toughness and ductility have prodigious facilitation to the raising of alloy property;It can be seen that from embodiment 11 to 15 The change of frequency and other combined transformations can all lead to the prodigious variation of generation of the obtained end properties of the present invention, only exist It could obtain best effect under the frequency that the present invention is set;The present invention is by each component in magnesium alloy to Properties of Magnesium Alloy Play the role of raising, and mutually cooperateed with advanced preparation process, so that the low temperature ductility of magnesium alloy and anti- Tensile strength is greatly improved, the perfect utilization of magnesium alloy at low ambient temperatures, especially in the ultralow temperature of aerospace Environment.
Finally illustrate, the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, this field is common Other modifications or equivalent replacement that technical staff makes technical scheme of the present invention, without departing from technical solution of the present invention Spirit and scope, be intended to be within the scope of the claims of the invention.

Claims (6)

1. a kind of magnesium alloy of low temperature resistant environment, it is characterised in that:The mass fraction of each element is in the magnesium alloy:
Al:1.2~2%;
Rare earth element:1~3.5%;
Ag:0.9~3.5%;
Zr:0.2~2%;
Surplus is Mg;
The rare earth element includes Nd and Y;
The mass fraction of Nd is 1.4% in the magnesium alloy, and the mass fraction of Y is 2.1% in the magnesium alloy;
The preparation method of the magnesium alloy of the low temperature resistant environment, includes the following steps:
1) magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, the centre conjunction of magnesium neodymium are weighed according to the mass fraction of each element in above-mentioned magnesium alloy The mass fraction of gold, zirconium ingot and silver ingot, each element weighed is Al:1.2~2%;Nd:1.4%;Y:2.1%;Ag:0.9~ 3.5%;Zr:0.2~2%;Surplus is Mg, is cleaned to equipment and keeps drying;
2) magnesium ingot is put into graphite crucible, graphite crucible is put into well formula resistance furnace, to being blown protective gas simultaneously in graphite crucible Start melting;
3) after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, and silver ingot and aluminium ingot are added into melt, to molten after stirring evenly Body carries out that magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy are added after being warming up to 750 DEG C, is again stirring for uniformly, finally carrying out melt Zirconium ingot is added after being warming up to 770 DEG C, 8min is stood after stirring evenly;
4) it skims to bath surface, and cools down to melt, pour into mold and carry out after melt temperature is down to 740 DEG C Mg alloy castings are made in casting;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy;
The heat treatment process of the step 5) is that Mg alloy castings first are covered by graphite powder, then Mg alloy castings are put into low Temperature type resistance furnace, it is 345 DEG C, time 2h to keep temperature, then is warming up to 545 DEG C, keeps 9h, then be cooled to 175 DEG C, is kept 35h finally takes out and carries out water cooling under room temperature environment;
Ultrasonic activation is applied to mold in the step 4) casting process.
2. the preparation method of the magnesium alloy of low temperature resistant environment as described in claim 1, it is characterised in that:In the step 2) Protective gas is the argon gas of purity 99.9%.
3. the preparation method of the magnesium alloy of low temperature resistant environment as described in claim 1, it is characterised in that:Add in the step 3) Powdered processing is carried out to zirconium ingot before entering zirconium ingot so that zirconium ingot becomes graininess zirconium powder, and its granularity is 0.1mm~1mm.
4. the preparation method of the magnesium alloy of low temperature resistant environment as claimed in claim 3, it is characterised in that:The zirconium powder is added molten The method of body is uniformly to be sprinkling upon bath surface, then stirs 2min to melt by mixing plant.
5. the preparation method of the magnesium alloy of low temperature resistant environment as described in claim 1, it is characterised in that:To in casting process Casting temperature is monitored, and ultrasonic transducer is contacted with mold, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasound It is 40kHz that wave transducer, which applies ultrasonic frequency, and when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer is applied It is 80kHz to add ultrasonic frequency.
6. the preparation method of the magnesium alloy of low temperature resistant environment as described in claim 1, it is characterised in that:The room temperature ensures temperature Degree is at 18 DEG C~24 DEG C.
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