CN105695829B - A kind of magnesium alloy of low temperature resistant environment and preparation method thereof - Google Patents

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

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Publication number
CN105695829B
CN105695829B CN201610158308.8A CN201610158308A CN105695829B CN 105695829 B CN105695829 B CN 105695829B CN 201610158308 A CN201610158308 A CN 201610158308A CN 105695829 B CN105695829 B CN 105695829B
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magnesium
alloy
ingot
magnesium alloy
melt
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CN105695829A (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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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%;Rare earth element:1~3.5%;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, stir, cast and be heat-treated, obtain low temperature resistant magnesium alloy, so that the low temperature ductility and tensile strength of alloy are greatly improved, the fracture probability of magnesium alloy parts under low temperature environment is greatly reduced, the life-span that the outer space has used the magnesium alloy equipment is improved, reduces its fault rate.

Description

A kind of magnesium alloy of low temperature resistant environment and preparation method thereof
Technical field
The present invention relates to magnesium alloy technical field, and in particular to a kind of magnesium alloy of low temperature resistant environment and preparation method thereof.
Background technology
Magnesium alloy is as most light structural metallic materials, with specific strength is high, specific stiffness is high, shock resistance is good, electromagnetic shielding The advantages of excellent performance, recuperability are good, there is wide application in fields such as automobile, portable instrument, electronics industry, Aero-Space Prospect.China possesses the magnesium resource enriched the most in the world, and development magnesium alloy processing technology of preparing is to realizing from magnesium resource advantage It is significant to the conversion of economic advantages.
With magnesium alloy applied in society more and more extensively, for the guarantor of magnesium alloy alloy property in high temperature environments Hold more and more with Study of Lifting, but magnesium alloy can also be in low-temperature vacuum environment in aerospace field.Because magnesium is closed The high-performance and low-density of gold so that the various parts made by magnesium alloy are used in satellite, spaceship, various detectors It is more and more, the part is chronically in the outer space, and the outer space refers to the area of space outside earth dense atmosphere, is Vacuum or the 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 away 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 is reduced, 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 that material can bear great plastic deformation and occur without the performance of crackle under external force that face, which is said,.It was verified that relatively low At a temperature of when working, often there is low stress brittle fracture.The reason for causing this result in fact has two, and one is with temperature The reduction of degree, the plastic property of material has declined, and second is that material internal has some microdefects unavoidably, such as small to split Line.The reduction of magnesium alloy parts plasticity, then can 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, cause it is huge loss and harm astronaut Life.
The content of the invention
In view of this, the purpose of the present invention is that there is provided a kind of magnesium alloy of low temperature resistant environment in view of the shortcomings of the prior art And preparation method thereof, the ductility of magnesium alloy at low ambient temperatures is improved, magnesium alloy part is reduced crisp at low ambient temperatures Property fracture probability.
In order to solve the above technical problems, the technical solution used in the present invention is:
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment, 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 that Nd mass fraction is Y in 0.1~3.4%, the magnesium alloy in the magnesium alloy For 0.1~3.4%.
A kind of preparation method of the magnesium alloy of low temperature resistant environment, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 745 DEG C~755 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, most Melt is carried out afterwards to add zirconium ingot after being warming up to 760 DEG C~775 DEG C, 5~10min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 2) in protective gas be purity 99.9% argon gas.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.1mm~1mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle.
Further, the casting temperature in casting cycle is monitored, by ultrasonic transducer and contacting dies, 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 step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 330 DEG C~360 DEG C, 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, 30~40h of holding, finally taking-up progress room temperature water cooling.
Further, the room temperature ensures temperature at 18 DEG C~24 DEG C.
The subject matter that the present invention is directed to is the ductility of magnesium alloy under vacuum low-temperature environment, and the slip system of magnesium is caused less Its plastic deformation ability poor obtain can produce extra sliding under reason, higher temperature in crystal so that magnesium is when temperature is raised Plasticity strengthens, but ductility is poor under low temperature, although yield strength and tensile strength all get a promotion, but this kind of magnesium alloy Easily there is brittle fracture when the outer space is used.Silver ingot is added after magnesium ingot fusing, magnesium alloy crystal axis can be caused Than reduction, so as to activate prism slip system, it is ensured 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 is changed into Dispersed precipitate from discontinuous net distribution, can effectively hinder grain-boundary sliding and Crack Extension, so that refining alloy group Knit, the mechanical property of magnesium alloy is got a promotion.Rare-earth yttrium has the effect of crystal grain thinning, and enhancing tensile strength and improvement are 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, so as to realize the purpose of refinement magnesium and magnesium alloy crystal grain, the alloy property of magnesium alloy is increased.
Zirconium is maximally effective grain refiner in the magnesium alloy, moreover it is possible to which the impurity in melt is purged, and enhancing magnesium is closed The tensile strength of gold, improves its corrosion resistance.Therefore it is last in the present invention to add zirconium powder, and the addition of zirconium is by powdered Addition, is uniformly sprinkling upon bath surface, stirring just can allow zirconium uniformly dispersing for two minutes in melt, to gas and Fe etc. by zirconium powder Impurity is purged, and can accelerate the speed of final step, it is to avoid magnesium alloy burning causes oxidation serious.
It can realize that non-contact temperature is adopted using infrared temperature sensor for the casting temperature monitoring in casting cycle Collection, ultrasonic transducer is controlled by supersonic generator, and the frequency to ultrasonic wave is changed.Casting cycle applies super Sound wave is improved with very big facilitation, when magnesium alloy temperature is very high and also in molten condition to it to the performance of magnesium alloy The ultrasonic frequency of application is larger, and ultrasonic wave can produce the acoustic pressure of positive and negative alternation when propagating, so as to produce cavitation effect, reach Tissue, crystal grain thinning are purified, stirring liquation makes the effect of microstructure homogenization;Start solidification when Mg alloy castings temperature is reduced to When, the frequency of ultrasonic wave suitably increases amplitude and suitably reduced, 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, so as to increase nucleation rate, crystal grain thinning strengthens the power of alloy Learn performance.
Beneficial effects of the present invention:
1st, 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 alloys elongation percentage circulated on the market is 17.4%, and tensile strength is 265MPa, is -196 DEG C in temperature When, magnesium alloy elongation percentage 10.6% of the present invention, tensile strength is 486MPa, and the AZ31B magnesium alloy elongation percentage circulated on the market is 3.8%, tensile strength is 301MPa, greatly reduces the fracture probability of magnesium alloy parts under low temperature environment, and improving the outer space makes With the life-span of the magnesium alloy equipment, its fault rate is reduced;
2nd, add rare earth element in magnesium alloy fused mass have dehydrogenation, deoxygenation, sulphur removal, except iron, except the effect of field trash, Reach refinery by de-gassing, purify the effect of melt;Rare earth element can be put forward the mechanical property of magnesium alloy with refining alloy tissue Rise;And rare earth element has higher solid solubility in the magnesium alloy, rare earth atom is dissolved in magnesium matrix, strengthens interatomic combination Power, makes matrix produce distortion of lattice, slows down atoms permeating speed, hinders dislocation motion, so as to strengthen matrix, improves the strong of alloy Degree and high temperature creep property;
3rd, add zirconium powder to be easy and fast to fuse into magnesium alloy fused mass, last eliminating impurities effect, and energy are played to melt Significantly improve the alloy property and corrosion resistance of magnesium alloy, it is to avoid cause magnesium alloy corrosion resistance poor after addition silver, then Because the corrosion resistance of alloy under vacuum environment can be improved, magnesium alloy of the present invention can be caused to be asked without corrosion of worrying again Topic, beneficial to the permanent work of safety of magnesium alloy part.
4th, by applying ultrasonic activation to mould in casting cycle, and ultrasonic wave is reached inside magnesium alloy, refined The crystal grain of strand, and then improve the plasticity and ductility of alloy so that magnesium alloy possesses higher ductility to adapt to low temperature ring Border.
Embodiment
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 embodiment is as follows:
Embodiment one
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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, and each component mass percent is adjusted, done The experiment obtained.The magnesium alloy that six embodiments are made carries out performance detection, is machined by numerically controlled lathe, makes drawing and 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 min draw speed, emphasis of the present invention is in order to improve the elongation percentage of magnesium alloy under low temperature environment, so dividing Do not tested under 0 DEG C and -196 DEG C of environment, specific data are shown in following form:
As can be seen from the above table, performance most preferably example IV, 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 has declined, More than 10% is remained at, this causes 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic waves It is 40KHz that energy device, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies ultrasound Wave frequency rate is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, by ultrasonic transducer and mould Tool contact, it is 40KHz that ultrasonic transducer, which applies ultrasonic frequency,.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 345 DEG C, and the time is 2h, 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
The mass fraction of each element is in a kind of magnesium alloy of low temperature resistant environment of the present embodiment, 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, comprises 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, in the middle of magnesium neodymium Alloy, zirconium ingot and silver ingot, are cleaned to 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 after magnesium ingot fusing, it is 740 DEG C to keep melt temperature, silver ingot and aluminium ingot is added into melt, after stirring Melt be warming up to after 750 DEG C and adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally to melt Progress adds zirconium ingot after being warming up to 770 DEG C, and 8min is stood after stirring.
4) bath surface is skimmed, and melt is cooled, poured into after melt temperature is down to 740 DEG C in mould Carry out casting and Mg alloy castings are made;
5) Mg alloy castings are carried out being thermally treated resulting in final magnesium alloy.
Further, the step 3) in add zirconium ingot before to zirconium ingot carry out powdered processing so that zirconium ingot turn into Granular zirconium powder, and its granularity is 0.2mm.
Further, the zirconium powder adds the method for melt to be uniformly sprinkling upon bath surface, then passes through mixing plant pair Melt Stirring 2min.
Further, the step 4) ultrasonic activation is applied to mould in casting cycle, to the casting in casting cycle Temperature is monitored, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic wave It is 40KHz that transducer, which applies ultrasonic frequency, when casting temperature is cooled to 550 DEG C~650 DEG C, and ultrasonic transducer applies super Frequency of sound wave is 80KHz.
Further, the step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then by magnesium Alloy-steel casting is put into low temperature chamber type electric resistance furnace, and keeping temperature is 545 DEG C, keeps 12h, finally takes out and carries out room temperature water cooling, described Room temperature ensures temperature at 21 DEG C.
Embodiment 11
The difference of itself and example IV is:The step 4) ultrasonic activation is applied to mould in casting cycle, to pouring Casting temperature during casting is monitored, by ultrasonic transducer and contacting dies, 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
The difference of itself and example IV is:The step 4) ultrasonic activation is applied to mould in casting cycle, to pouring Casting temperature during casting is monitored, by ultrasonic transducer and contacting dies, 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
The difference of itself and example IV is:The step 4) ultrasonic activation is applied to mould in casting cycle, to pouring Casting temperature during casting is monitored, by ultrasonic transducer and contacting dies, 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
The difference of itself and example IV is:The step 4) ultrasonic activation is applied to mould in casting cycle, to pouring Casting temperature during casting is monitored, by ultrasonic transducer and contacting dies, 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
The difference of itself and example IV is:The step 4) ultrasonic activation is applied to mould in casting cycle, to pouring Casting temperature during casting is monitored, by ultrasonic transducer and contacting dies, 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 that production technology is changed, and embodiment seven is not carried out at powdered to zirconium ingot Zirconium ingot, is directly put into melt by reason;Embodiment eight does not use ultrasonic activation to handle in casting cycle;Embodiment nine exists Handled in casting cycle using ultrasonic activation, but the frequency of ultrasonic transducer, which is maintained at 40KHz, not to be changed;Embodiment ten Change last heat treatment process, only with conventional heat treatment method, rather than the multi-temperature segmentation heat treatment in the present invention, Embodiment 11 to 15 changes ultrasonic frequency, and 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 difficult to be quickly dispersed in melt, reduces to alloy melt Clean-up effect, cause alloy property to decline.Ultrasonic activation is not added in casting cycle in embodiment eight, causes alloy Hydraulic performance decline is more, although and embodiment nine adds ultrasonic activation, not as temperature change is to ultrasonic frequency It is adjusted, solidification of the ultrasonic wave of lower frequency to magnesium alloy does not have more preferable facilitation in alloy graining process, It is also easy to so that slab oscillation mark depth increased, play magnesium alloy adverse effect;Heat treatment is conventional skill in embodiment ten Art, and example IV is placed by multi-temperature rapid lapse of time and is heat-treated, and reduces alloy internal stress and fragility, increase alloy Toughness and ductility, have very big 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 cause what the present invention obtained end properties to produce very big change, only exist It could obtain optimal 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 raising effect, and the effect mutually cooperateed with advanced preparation technology, 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, the especially ultralow temperature in Aero-Space Environment.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, this area is common Other modifications or equivalent substitution that technical staff is made to technical scheme, without departing from technical solution of the present invention Spirit and scope, all should cover among scope of the presently claimed invention.

Claims (7)

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 that Nd mass fraction is Y in 0.1~3.4%, the magnesium alloy in the magnesium alloy is 0.1~3.4%;
The preparation method of the magnesium alloy of the low temperature resistant environment, comprises the following steps:
1) magnesium ingot, aluminium ingot, magnesium yttrium intermediate alloy, the conjunction of magnesium neodymium centre are weighed according to the mass fraction of each element in above-mentioned magnesium alloy Gold, zirconium ingot and silver ingot, are cleaned to equipment and keep 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 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 Body, which be warming up to after 745 DEG C~755 DEG C, adds magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy, is again stirring for uniformly, finally right Melt is carried out adding zirconium ingot after being warming up to 760 DEG C~775 DEG C, and 5~10min is stood after stirring;
4) bath surface is skimmed, and melt is cooled, poured into mould 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 step 5) heat treatment process covered by graphite powder for Mg alloy castings first, then Mg alloy castings are put into low Temperature type resistance furnace, keeping temperature is 330 DEG C~360 DEG C, and the time is 1~3h, then is warming up to 530 DEG C~560 DEG C, keep 8~ 9h, then it is cooled to 170 DEG C~180 DEG C, 30~40h of holding, finally taking-up progress room temperature water cooling.
2. the magnesium alloy of low temperature resistant environment as claimed in claim 1, it is characterised in that:The step 2) in protective gas to be pure The argon gas of degree 99.9%.
3. the magnesium alloy of low temperature resistant environment as claimed in claim 1, it is characterised in that:The step 3) in add zirconium ingot before Powdered processing is carried out to zirconium ingot so that zirconium ingot turns into graininess zirconium powder, and its granularity is 0.1mm~1mm.
4. the magnesium alloy of low temperature resistant environment as claimed in claim 3, it is characterised in that:The method that the zirconium powder adds melt is Bath surface uniformly is sprinkling upon, then by mixing plant to Melt Stirring 2min.
5. the magnesium alloy of low temperature resistant environment as claimed in claim 1, it is characterised in that:The step 4) in casting cycle to mould Tool applies ultrasonic activation.
6. the magnesium alloy of low temperature resistant environment as claimed in claim 5, it is characterised in that:Casting temperature in casting cycle is entered Row monitoring, by ultrasonic transducer and contacting dies, when casting temperature is cooled to 650 DEG C~740 DEG C, ultrasonic transducer is applied Plus ultrasonic frequency is 40KHz, when casting temperature is cooled to 550 DEG C~650 DEG C, ultrasonic transducer applies ultrasonic frequency For 80KHz.
7. the magnesium alloy of low temperature resistant environment as claimed in claim 1, it is characterised in that:The room temperature ensure temperature 18 DEG C~ 24℃。
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