CN108796328A - A kind of high-strength heat-resistant rare earth magnesium alloy and preparation method thereof - Google Patents

A kind of high-strength heat-resistant rare earth magnesium alloy and preparation method thereof Download PDF

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Publication number
CN108796328A
CN108796328A CN201810715392.8A CN201810715392A CN108796328A CN 108796328 A CN108796328 A CN 108796328A CN 201810715392 A CN201810715392 A CN 201810715392A CN 108796328 A CN108796328 A CN 108796328A
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rare earth
magnesium alloy
sources
heat
strength heat
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CN108796328B (en
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张洪杰
程丽任
车朝杰
佟立波
孟健
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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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 alloys
    • C22C1/02Making alloys by melting
    • 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 present invention provides a kind of high-strength heat-resistant rare earth magnesium alloy, ingredient is:The Sm of 2~6wt%;The Nd of 0~3wt%;The heavy rare earth element of 2~5wt%;The Zn of 0.5~4wt%;The Zr of 0.2~3wt%;Surplus is Mg and inevitable impurity.The present invention makes the Zr in rich Zr rings be precipitated during heat treatment in the conical surface of magnesium alloy substrate in the form of Zn-Zr heat resistive compounds using influence of the elements to the electronic migration state of Zr elements such as Sm, heavy rare earth.Under the high temperature conditions, Zn-Zr, which meets, effectively inhibits non-basal slip, forms the precipitation hardened magnesium alloy substrates of Mg-RE by heat treatment on this basis.The presence of two class phases can effectively inhibit high temperature Prismatic slip, conical surface sliding and basal slip in the magnesium alloy of the present invention, improve magnesium alloy elevated temperature strength.The present invention also provides a kind of preparation methods of high-strength heat-resistant rare earth magnesium alloy.

Description

A kind of high-strength heat-resistant rare earth magnesium alloy and preparation method thereof
Technical field
The present invention relates to magnesium alloy technical fields more particularly to a kind of high-strength heat-resistant rare earth magnesium alloy and preparation method thereof.
Background technology
Magnesium alloy is most light structural metallic materials, has specific strength and specific stiffness height, vibration and noise reducing and electromagnetic wave shielding Can it is good, anti-dynamic impact loads ability is strong, the series of advantages such as resourceful, so that it is had in national economy and national defense construction Major application foreground.Mg-Zn and Mg-Al systems tradition magnesium alloy elevated temperature strength is relatively low, and current application is concentrated mainly on non-bearing In structural member.It is higher and higher to lightweight and intensity requirement with the development of weaponry, in big aircraft, manned space flight, lunar exploration Country's Important Project such as engineering, rail traffic and military field propose lightweight and loss of weight very harsh requirement.Therefore, Magnesium alloy with superior heat resistance performance has become space flight and aviation, national defense and military and the developing important materials of modernization industry.
At present in high-strength magnesium alloy, magnesium-rare earth is best one of the heat resistance magnesium alloy of performance.In magnesium-rare earth Rare earth reinforced is mainly realized by ageing strengthening, i.e., after being dissolved rare earth element under specific aging temp, makes (intermetallic compound) is precipitated in the alloying element of high temperature solid solution with some form, the hard particle of Dispersed precipitate is formed, to dislocation It cuts through and causes resistance, intensity is made to increase.The precipitation-hardening being precipitated in ag(e)ing process mutually effectively can hinder basal plane dislocation to move, Significantly improve the intensity of magnesium alloy.The pick-up behavior for how being regulated and controled precipitated phase using means such as alloying, deformation, is had reached good Good performance is numerous scholars problem of concern.The prior art by rare earth precipitated phase effectively pin basal plane although can be slided Move, if but think the non-basal slip of pinning in the case of a high temperature, need to consume more rare earths, form basal plane precipitated phase, make conjunction The cost of gold increases.
Therefore, how to obtain a kind of high temperature resistance and lower-cost magnesium-rare earth becomes those skilled in the art The hot spot of research.
Invention content
In view of this, the purpose of the present invention is to provide a kind of high-strength heat-resistant rare earth magnesium alloy and preparation method thereof, this hair The high-strength heat-resistant rare earth magnesium alloy of bright offer has good high-temperature behavior and cost is relatively low.
The present invention designs the conjunction of high-strength heat-resistant rare earth magnesium in a manner of Zn-Zr precipitated phases, Mg-RE cylinder precipitated phase complex intensifyings Gold.The present invention provides a kind of high-strength heat-resistant rare earth magnesium alloy, ingredient is:
The Sm of 2~6wt%;
The Nd of 0~3wt%;
The heavy rare earth element of 2~5wt%;
The Zn of 0.5~4wt%;
The Zr of 0.2~3wt%;
Surplus is Mg and inevitable impurity.
In the present invention, the mass content of the Sm is preferably 3~5%, and more preferably 3.5~4.5%, most preferably 4%.
In the present invention, the mass content of the Nd is preferably 0.5~2.5%, and more preferably 1~2%, most preferably 1.5%.In the present invention, the Nd is rare earth element costly, it is contemplated that the cost of magnesium alloy does not preferably add Nd members Element.
In the present invention, the heavy rare earth element is preferably selected from one or more of Gd, Y, Dy, Ho and Er, more preferably For one or both of Gd and Y.Present invention preferably employs above-mentioned specific heavy rare earth elements, in the present invention, Sm with it is specific Heavy rare earth element mating reaction can preferably promote Zn-Zr phases to be precipitated, to make high-strength temperature-resistant magnesium provided by the invention close Gold utensil has better performance.In the present invention, the mass content of the heavy rare earth element is preferably 3~5%, and more preferably 3.5 ~4.5%, most preferably 4%.
In the present invention, the mass content of the Zn is preferably 1~3%, and more preferably 1.5~2.5%, most preferably 2%.
In the present invention, the mass content of the Zr is preferably 0.5~2.5%, and more preferably 1~2%, most preferably 1.5%.
In the present invention, the mass content of Zn and Zr is preferably more, so as to which more Zn-Zr precipitated phases are precipitated, carries The performance of high high-strength heat-resistant magnesium alloy provided by the invention.
In the present invention, the ratio of the mass percentage of the Zn and Zr is preferably (1~3):1, more preferably (1.5 ~2.5):1, most preferably 2:1.The ratio of the mass percentage of Zn and Zr is preferably greater than 1 in the present invention:1 (Zn constituent contents It is on the high side compared with Zr elements), it can be more conducive to the generation of Zn-Zr conical surface precipitated phases, it is high-strength to make the present invention be prepared Heat resisting magnesium-rare earth alloy has better performance.
In the present invention, the ingredient of the high-strength heat-resistant rare earth magnesium alloy is preferably:
The Sm of 3~5wt%;
The heavy rare earth element of 3~5wt%;
The Zn of 1~3wt%;
The Zr of 0.2~2wt%;
Surplus is Mg and inevitable impurity.
In the present invention, the ingredient of the high-strength heat-resistant rare earth magnesium alloy is most preferably:
The Sm of 4.5wt%;
The heavy rare earth element of 3.5wt%, the heavy rare earth element are preferably Gd or Y;
The Zn of 2wt%;
The Zr of 1.5wt%;
Surplus is Mg and inevitable impurity.
The present invention provides a kind of preparation methods of the high-strength heat-resistant rare earth magnesium alloy described in above-mentioned technical proposal, including with Lower step:
(1) sources Mg, the sources Nd, the sources Sm, the sources Zn, the sources Zr and heavy rare earth source are subjected to dispensing;
(2) sources Mg are subjected to melting, obtain Mg aluminium alloys;
(3) the Mg aluminium alloys and the sources Sm, the sources Nd, the sources Zn and heavy rare earth source are subjected to melting, obtain mixed liquor;
(4) mixed liquor and the sources Zr are subjected to melting, obtain aluminium alloy;
(5) aluminium alloy is cast, obtains as-cast magnesium alloy;
(6) as-cast magnesium alloy is heat-treated, obtains high-strength heat-resistant rare earth magnesium alloy.
The present invention does not have special limitation to the sources Mg, and it is conventional use of to prepare magnesium alloy using those skilled in the art High-purity magnesium ingot such as can be used in the sources Mg.
The present invention does not have special limitation to the sources Zn, and preparing magnesium alloy using this law field technology personnel routinely uses The sources Zn, high purity zinc such as can be used.
The present invention does not have special limitation to the sources Sm, and preparing magnesium-rare earth routinely using those skilled in the art makes Mg-Sm intermediate alloys such as can be used in the sources Sm;In the Mg-Sm intermediate alloys mass content of Sm be preferably 20~ 30%, more preferably 22~28%, most preferably 24~26%.
The present invention does not have special limitation to the sources Nd, and preparing magnesium-rare earth routinely using those skilled in the art makes Mg-Nd intermediate alloys such as can be used in the sources Nd;In the Mg-Nd intermediate alloys mass content of Nd be preferably 20~ 30%, more preferably 22~28%, most preferably 24~26%.
The present invention does not have special limitation to the heavy rare earth source, and it is normal to prepare magnesium-rare earth using those skilled in the art The heavy rare earth source used is advised, Mg- heavy rare earth intermediate alloys such as can be used;The heavy rare earth element is among Mg- heavy rare earth Mass content in alloy is preferably 25~35%, more preferably 28~32%, most preferably 30%.
The present invention does not have special limitation to the sources Zr, and preparing magnesium-rare earth routinely using those skilled in the art makes Mg-Zr intermediate alloys such as can be used in the sources Zr;In the Mg-Zr intermediate alloys mass content of Zr be preferably 20~ 30%, more preferably 22~28%, most preferably 24~26%.
In the present invention, the dosage in the sources Mg, the sources Sm, the sources Nd, the sources Zn, the sources Zr and heavy rare earth source makes the height being prepared The ingredient of strong heat resisting magnesium-rare earth alloy meets the component requirements described in above-mentioned technical proposal.
In the present invention, preferably by the sources Mg, the sources Sm, the sources Nd, the sources Zn, the sources Zr and heavy rare earth source in the blending process It removes the oxide skin on its surface and is preheated;The temperature of the preheating is preferably 200~300 DEG C, more preferably 220~280 DEG C, most preferably 240~260 DEG C.
In the present invention, it is preferably by the method that the sources Mg carry out melting:
Mg source meltings are added after crucible is preheated and are passed through protective gas.
In the present invention, the temperature of the crucible preheating is preferably 500~600 DEG C, more preferably 520~580 DEG C, optimal It is selected as 540~560 DEG C.
In the present invention, the temperature that the sources Mg carry out melting is preferably 720~740 DEG C, more preferably 725~735 DEG C, optimal It is selected as 730 DEG C.
In the present invention, the protective gas is preferably SF6And CO2Gaseous mixture.In the present invention, the protective gas Middle SF6And CO2Volume ratio be preferably 1:(80~120), more preferably 1:(90~110), most preferably 1:100.
In the present invention, the Sm after above-mentioned preheating preferably being added into obtained Mg aluminium alloys after the sources Mg are completely melt Source, the sources Nd, the sources Zn and heavy rare earth source carry out melting.In the present invention, uniform stirring is preferably carried out during the melting.? In the present invention, the time of the stirring is preferably 5~15 minutes, more preferably 8~12 minutes, most preferably 10 minutes.
In the present invention, the sources Zr for obtaining being preferably added to after mixed liquor above-mentioned preheating carry out melting.In the present invention, described Uniform stirring is preferably carried out during melting, the temperature of the melting is preferably 760~800 DEG C, more preferably 770~790 DEG C, most preferably 780 DEG C.In the present invention, the time of the stirring is preferably 5~15 minutes, more preferably 8~12 minutes, Most preferably 10 minutes.
In the present invention, dehydrogenation preferably is carried out to the aluminium alloy after obtaining aluminium alloy.In the present invention, described to remove Hydrogen processing method be preferably:
It is passed through argon gas into the aluminium alloy and carries out dehydrogenation.
In the present invention, the temperature for argon gas being passed through into the aluminium alloy is preferably 740~760 DEG C, more preferably 745~ 755 DEG C, most preferably 750 DEG C.
In the present invention, preferably the aluminium alloy is refined after carrying out dehydrogenation to the aluminium alloy.In this hair In bright, the method for the refining is preferably:
It is stood after flux is added into the aluminium alloy.
The present invention does not have the flux special limitation, and magnesium alloy process is prepared using well known to those skilled in the art In flux.In the present invention, the flux is preferably No. 6 flux, and the flux preferably includes MgCl2、CaCl2、KCl、 BaCl2、CaF2And NaCl.
In the present invention, the time of the standing is preferably 40~60min, more preferably 45~55min, most preferably 50min。
The present invention does not have the method for the casting special limitation, the present invention different casting methods can be used and be prepared into To as-cast magnesium alloy, the method that gravitational casting such as can be used obtains as-cast magnesium alloy, and the mode that counter-pressure casting can also be used obtains As-cast magnesium alloy, the mode that die casting also can be used obtain as-cast magnesium alloy.
In the present invention, the method for the casting is preferably:
It is cast in mold after the aluminium alloy is kept the temperature at 720~740 DEG C.
In the present invention, the holding temperature of the aluminium alloy is preferably 725~735 DEG C, more preferably 730 DEG C;The guarantor The time of temperature is preferably 10~15min, more preferably 11~14min, most preferably 12~13min.
In the present invention, the mold is preferably steel water cooling mold.
In the present invention, the heat-treating methods are preferably:
The as-cast magnesium alloy is first carried out to solution treatment and carries out ageing treatment again, obtains high-strength heat-resistant rare earth magnesium alloy.
In the present invention, the method for the solution treatment is preferably:
Temperature range by the as-cast magnesium alloy at 300~530 DEG C heats up step by step, is analysed step by step while solid solution with realizing Go out Zn-Zr conical surface phases, obtains intermediate product.
In the present invention, the method for the actual effect processing is preferably:
By the intermediate product in 170~230 DEG C of temperature range inside holding, high-strength heat-resistant rare earth magnesium alloy is obtained.
In this present invention, the as-cast magnesium alloy is preferably to heat up step by step in 350~500 DEG C of temperature range, more excellent It is selected as heating up step by step in 400~450 DEG C of temperature range.In the present invention, the heating step by step is to realize that gradient is dissolved. In the present invention, the specific method to heat up step by step is preferably:
The as-cast magnesium alloy is warming up to second temperature after the first temperature first time and kept the temperature for the second time, so It is warming up to the third temperature third time again afterwards, obtains intermediate product.
In the present invention, first temperature is preferably 300~450 DEG C, more preferably 350~400 DEG C, most preferably 360~380 DEG C;The first time is preferably 2~10 hours, more preferably 3~8 hours, most preferably 4~6 hours.At this In invention, the second temperature is preferably 450~500 DEG C, more preferably 460~490 DEG C, most preferably 470~480 DEG C;Institute It is preferably 5~15 hours to state for the second time, more preferably 8~12 hours, most preferably 10 hours.In the present invention, described Three temperature are preferably 500~540 DEG C, more preferably 510~530 DEG C, most preferably 515~525 DEG C;The third time is preferred It is 5~15 hours, more preferably 8~12 hours, most preferably 10 hours.
Present invention preferably employs the above-mentioned gradient solid solution treatment methods to heat up step by step to prepare high-strength heat-resistant rare earth magnesium alloy, adopts It can be made that Zn-Zr phases and Mg-RE phases are preferably precipitated in magnesium alloy substrate with this special solid dissolving method, to make this hair The bright high-strength heat-resistant magnesium alloy being prepared is with good performance.
In the present invention, it is ageing treatment the intermediate product to be kept the temperature at 170~230 DEG C.In the present invention, in described Between the holding temperature of product be preferably 180~220 DEG C, more preferably 190~210 DEG C, most preferably 200 DEG C.In the present invention, The soaking time of the intermediate product is preferably 10~40 hours, more preferably 20~30 hours, most preferably 25 hours.
In the present invention, crystalline material is divided into polycrystalline material and monocrystal material.Atom in crystalline material can approximate quilt It is considered as rigid sphere.In crystallographic theory, according to symmetry principle, rigid bead shares 14 kinds of arrangement modes, all lists Crystal structure is included.Metal material belongs to close-packed structure, it can be understood as atomic response rigidity bead is equally close Be arranged together, metal material plastic deformation when these atoms be still closely spaced, so metal material is in any case Deformation, volume is constant.Due to solid matter, the monoclinic crystal structure of usual metal material belongs to 3 kinds in 14 kinds of crystal structures:Face Heart cubic crystal structure, Patterns for Close-Packed Hexagonal Crystal structure, body-centered cubic crystal structure.Alloy is the polycrystalline being made of multiple monocrystal Body.Each monocrystal becomes crystal grain, and the Atomic Arrangement rule in each crystal is consistent.The boundary of monocrystal is known as crystal boundary. For magnesium alloy, the Atomic Arrangement of each crystal grain meets the arrangement rule of Patterns for Close-Packed Hexagonal Crystal structure, as shown in Figure 1, Fig. 1 In a, b, c belong to Patterns for Close-Packed Hexagonal Crystal structure, the hexahedron in figure is the crystal structure model of magnesium alloy, wherein each top Point position all represents an atom, and each edge length of hexagon all represents the sum of two magnesium atom radiuss of sphericity, and each edge length is close Approximately equal to magnesium atom diameter length.The diplopia of a represents the basal plane in crystal structure in figure, and b represents cylinder, and c represents the conical surface, cylinder There are two types of altogether, the common conical surface shares 3 kinds, and b, c are a certain position view, are easy to understand.Crystal face analysis in the present invention Go out the compound being exactly precipitated on these crystal faces mutually referred to.
Magnesium is Patterns for Close-Packed Hexagonal Crystal structure, and traditional heat resisting magnesium-rare earth alloy is relied on along prismatic surface and basal plane in the prior art The rare earth compound of precipitation inhibits high temperature crystal-plane slip to need to consume although magnesium alloy heat resistance can be effectively improved Expensive rare earth element, the costs such as a large amount of Gd, Y, Nd are higher.The present invention is complete using lower-cost rare-earth Sm element It substitutes or major part substitutes Nd, mixed with a small amount of Gd, Y element, change the electronic migration state of Zr elements in the magnesium alloy, The heat-resisting precipitated phases of completely new Zn-Zr have been synthesized at the magnesium alloy crystal grain conical surface, by being heat-treated to as-cast magnesium alloy, are being closed The cylinder precipitated phase of Mg-Gd or Mg-Y is formd in gold.The reinforcing effect of conical surface precipitated phase is far superior to common in magnesium alloy Basal plane precipitated phase.The present invention improves the heat-resisting of magnesium alloy simultaneously using completely new conical surface precipitated phase and traditional cylinder precipitated phase Performance reduces the addition of expensive rare earth, cost is greatly reduced while improving magnesium alloy heat resistance.
The present invention makes the Zr in rich Zr rings in heat using influence of the elements to the electronic migration state of Zr elements such as Sm, Gd It is precipitated in the conical surface of magnesium alloy substrate in the form of Zn-Zr heat resistive compounds in processing procedure.Under the high temperature conditions, Zn-Zr phases Non- basal slip can effectively be inhibited, on this basis by heat treatment formed Mg-RE precipitated phases (most of is β cylinder precipitated phases, It is γ basal planes precipitated phase on a small quantity), while reinforced magnesium alloy matrix.The presence of two class phases can be effective in magnesium alloy in the present invention Inhibit high temperature Prismatic slip, conical surface sliding and basal slip, improves magnesium alloy elevated temperature strength.
Magnesium-rare earth in currently available technology is although can be by rare earth precipitated phase effectively pin basal slip, such as Fruit thinks non-basal slip in the case of a high temperature, then needs to consume more rare earths, form basal plane precipitated phase, the cost of alloy is made to increase Add.The present invention makes the magnesium-rare earth shape being prepared by controlling various composition and component content in magnesium-rare earth At the conical surface precipitated phase of Zn-Zr, heat-resisting conical surface precipitated phase is precipitated in this magnesium-rare earth first during solution treatment, Later in conjunction with the ageing treatment after solution treatment, the cylinder precipitated phase of Mg-RE has been precipitated, has inhibited high temperature basal slip.The present invention This magnesium-rare earth provided can reduce the use of high cost rare earth element, while this magnesium-rare earth is with higher Room temperature and elevated temperature strength.
Sm, heavy rare earth element, Zn and Zr in high-strength heat-resistant rare earth magnesium alloy provided by the invention and the use between them Amount ratio have synergistic effect, the present invention under the action of element consumption proportion of specific Sm, heavy rare earth element, Zn and Zr, Enable the magnesium alloy being prepared that the strip compound of Zn-Zr is precipitated in the conical surface and combines the Mg-RE of cylinder precipitation (heavy dilute Earth elements) compound simultaneously reinforced rare earth magnesium alloy.
The present invention provides a kind of heat resisting magnesium-rare earth alloys of medium content of rare earth, with commercial WE43 magnesium-rare earths phase Than the present invention abandons the use of expensive light rare earth neodymium, (is aoxidized in the market using cheap samarium element substitution neodymium element The price of samarium is about at 1.5 ten thousand yuan/ton, and the price of neodymia is at 40~500,000 yuan/ton).The high temperature of traditional commercial WE43 is strong Change phase based on cylinder precipitated phase, is aided with a small amount of basal plane precipitated phase.The present invention is used cooperatively by introducing Zn, Zr element Sm and heavy rare earth element form the heat-resisting hardening constituent of the Zn-Zr conical surfaces by heat treatment, while light dilute using heavy rare earth element combination Earth elements Sm promotes to form cylinder precipitated phase.The common work that the present invention passes through basal plane precipitated phase and cylinder precipitated phase in magnesium alloy With effective pinning high temperature crystal-plane slip, magnesium-rare earth ratio WE43 magnesium alloys provided by the invention have more outstanding resistance to Hot property, and considerably reduce cost.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis The attached drawing of offer obtains other attached drawings.
Fig. 1 is magnesium alloy crystal face schematic diagram in the present invention;
Fig. 2 is the transmission electron micrograph for the high-strength heat-resistant rare earth magnesium alloy that the embodiment of the present invention 3 is prepared.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
The sources Mg used in following embodiment of the present invention are pure Mg ingots, and the high-purity Zn in the sources Zn, the sources Sm are that Sm mass contents are 25% Mg-Sm intermediate alloys, the sources Gd are the Mg-Gd intermediate alloys that Gd mass contents are 30%, and the sources Zr are that Zr mass contents are 25% Mg-Zr intermediate alloys, the sources Y are the Mg-Y intermediate alloys that Y mass contents are 30%.No. 6 solvents used are that Liaoning is new The RJ-6 flux that roc high-tech metal Co., Ltd provides.
Embodiment 1
It is divided into according to being preset to:Sm2wt%, Gd2wt%, Zn 0.5wt%, Zr 0.5wt%, surplus are Mg and can not keep away The impurity exempted from, synthesis point, the sources Mg, the sources Zn, the sources Sm, the sources Gd and the sources Zr are subjected to dispensing, each stock chart is removed in blending process The oxide skin in face, and they are preheated to 200 DEG C;
Crucible is preheated to 500 DEG C, the sources Mg of above-mentioned preheating are added, furnace temperature rises to 720 DEG C, and it is 1 to be passed through volume ratio: 100 SF6And CO6Gaseous mixture carry out magnesium melting;
After the sources Mg are completely melt, Mg aluminium alloys are obtained;The sources Sm, the sources Zn of above-mentioned preheating are added into the Mg aluminium alloys Uniform stirring is carried out with the sources Gd and carries out melting within 10 minutes, obtains mixed liquor;
Furnace temperature is risen to 760 DEG C, the sources Zr of above-mentioned preheating are added into the mixed liquor, uniform stirring is melted for 10 minutes Refining, obtains aluminium alloy;
Furnace temperature is down to 750 DEG C, argon gas dehydrogenation is passed through into the aluminium alloy;
No. 6 flux standings are added into the aluminium alloy after the dehydrogenation to be refined within 40 minutes;
Furnace temperature is set as 720 DEG C the aluminium alloy heat preservation after refining is cast for 10 minutes, aluminium alloy is cast to steel In water cooling mold processed, as-cast magnesium alloy is obtained;
It the as-cast magnesium alloy at 400 DEG C is kept the temperature 5 hours then heats to 470 DEG C and keep the temperature 10 hours, finally heat up again 10 hours are kept the temperature to 520 DEG C, obtains intermediate product;
The intermediate product is kept the temperature 30 hours at 180 DEG C, obtains high-strength heat-resistant rare earth magnesium alloy.
Using domestic DDL-100 electronic universal testers, the high-strength heat-resistant rare earth that the embodiment of the present invention 1 is prepared is tested Mechanical property of the magnesium alloy at room temperature and 300 DEG C, testing result is as shown in table 1, and table 1 is the embodiment of the present invention and comparative example system The mechanics properties testing result of standby obtained high-strength heat-resistant rare earth magnesium alloy.
According to GB/T 2039-2012《Metal material simple tension creep test method》Standard, test the present invention implement Croop property of the high-strength heat-resistant rare earth magnesium alloy that example 1 is prepared under the conditions of 200 DEG C, 100MPa, testing result such as 2 institute of table Show, table 2 is the croop property testing result for the high-strength heat-resistant rare earth magnesium alloy that the embodiment of the present invention and comparative example are prepared.
Embodiment 2
It is divided into according to being preset to:Sm3wt%, Gd3wt%, Zn 1.5wt%, Zr 1.5wt%, surplus are Mg and can not keep away The impurity exempted from, synthesis point, the sources Mg, the sources Zn, the sources Sm, the sources Gd and the sources Zr are subjected to dispensing, each stock chart is removed in blending process The oxide skin in face, and they are preheated to 300 DEG C;
Crucible is preheated to 500 DEG C, the sources Mg of above-mentioned preheating are added, furnace temperature rises to 730 DEG C, and it is 1 to be passed through volume ratio: 100 SF6And CO6Gaseous mixture carry out magnesium melting;
After the sources Mg are completely melt, Mg aluminium alloys are obtained;The sources Sm, the sources Zn of above-mentioned preheating are added into the Mg aluminium alloys Uniform stirring is carried out with the sources Gd and carries out melting within 5 minutes, obtains mixed liquor;
Furnace temperature is risen to 770 DEG C, the sources Zr of above-mentioned preheating are added into the mixed liquor, uniform stirring is melted for 5 minutes Refining, obtains aluminium alloy;
Furnace temperature is down to 750 DEG C, argon gas dehydrogenation is passed through into the aluminium alloy;
No. 6 flux standings are added into the aluminium alloy after the dehydrogenation to be refined within 45 minutes;
Furnace temperature is set as 740 DEG C the aluminium alloy heat preservation after refining is cast for 10 minutes, aluminium alloy is cast to steel In water cooling mold processed, as-cast magnesium alloy is obtained;
It the as-cast magnesium alloy at 300 DEG C is kept the temperature 2 hours is warming up to 450 DEG C and keep the temperature 5 hours, then heat to 500 DEG C Heat preservation 5 hours, obtains intermediate product;
The intermediate product is kept the temperature 20 hours at 200 DEG C, obtains high-strength heat-resistant rare earth magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 2 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 2 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 3
It is divided into according to being preset to:Sm 5wt%, Y 3wt%, Zn 2wt%, Zr 1.5wt%, surplus are Mg and can not keep away The impurity exempted from, synthesis point, the sources Mg, the sources Zn, the sources Sm, the sources Y and the sources Zr are subjected to dispensing, each raw material surface is removed in blending process Oxide skin, and they are preheated to 300 DEG C;
Crucible is preheated to 500 DEG C, the sources Mg of above-mentioned preheating are added, furnace temperature rises to 760 DEG C, and it is 1 to be passed through volume ratio: 100 SF6And CO6Gaseous mixture carry out magnesium melting;
After the sources Mg are completely melt, Mg aluminium alloys are obtained;The sources Sm, the sources Zn of above-mentioned preheating are added into the Mg aluminium alloys Uniform stirring is carried out with the sources Y and carries out melting within 15 minutes, obtains mixed liquor;
Furnace temperature is risen to 770 DEG C, the sources Zr of above-mentioned preheating are added into the mixed liquor, uniform stirring is melted for 15 minutes Refining, obtains aluminium alloy;
Furnace temperature is down to 750 DEG C, argon gas dehydrogenation is passed through into the aluminium alloy;
No. 6 flux standings are added into the aluminium alloy after the dehydrogenation to be refined within 45 minutes;
Furnace temperature is set as 740 DEG C the aluminium alloy heat preservation after refining is cast for 10 minutes, aluminium alloy is cast to steel In water cooling mold processed, as-cast magnesium alloy is obtained;
It the as-cast magnesium alloy at 400 DEG C is kept the temperature 10 hours is warming up to 500 DEG C and keep the temperature 15 hours, be then warming up to again 540 DEG C keep the temperature 15 hours, obtain intermediate product;
The intermediate product is kept the temperature 25 hours at 215 DEG C, obtains high-strength heat-resistant rare earth magnesium alloy.
According to GB/T 13298-2015《The metal microstructure method of inspection》Standard, the embodiment of the present invention 3 is prepared into The high-strength heat-resistant rare earth magnesium alloy arrived carries out tissue detection, and testing result is as shown in Fig. 2, Fig. 2 is prepared into for the embodiment of the present invention 3 The transmission electron micrograph of the high-strength heat-resistant rare earth magnesium alloy arrived, figure it is seen that the present invention be prepared it is high-strength resistance to Contain Zn-Zr conical surfaces precipitated phase (i in figure), Mg-Y-Sm cylinders precipitated phase (ii in figure) and a small amount of Mg- in hot magnesium-rare earth Y basal planes precipitated phase (iii in figure).
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 3 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 3 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 4
High-strength heat-resistant rare earth magnesium alloy is prepared according to method described in embodiment 3, with embodiment 3 difference lies in, Dispensing is carried out according to following target components:
Sm:4wt%;Y:4wt%;Zn:0.5wt%, Zr:0.5wt%, surplus are Mg and inevitable impurity.
It is by obtained as-cast magnesium alloy progress heat-treating methods:
In 200 DEG C of timeliness 18 hours after the as-cast magnesium alloy is dissolved 12 hours at 525 DEG C, high-strength heat-resistant rare earth is obtained Magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 4 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 4 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 5
High-strength heat-resistant rare earth magnesium alloy is prepared according to method described in embodiment 3, with embodiment 3 difference lies in, Dispensing is carried out according to following target components:
Sm:2wt%;Nd:2wt%;Gd:3.5wt%;Zn:0.5wt%;Zr:0.5wt%, surplus is for Mg and unavoidably Impurity.
It is by obtained as-cast magnesium alloy progress heat-treating methods:
In 200 DEG C of timeliness 18 hours after the as-cast magnesium alloy is dissolved 14 hours at 525 DEG C, high-strength heat-resistant rare earth is obtained Magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 5 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 5 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 6
High-strength heat-resistant rare earth magnesium alloy is prepared according to method described in embodiment 3, with embodiment 3 difference lies in, Dispensing is carried out according to following target components:
Sm:1wt%;Nd:1wt%;Y:2wt%;Yb:2wt%;Ho:1.5wt%;Zn:0.3wt%;Zr:0.3wt%; Surplus is Mg and inevitable impurity.
It is by obtained as-cast magnesium alloy progress heat-treating methods:
In 200 DEG C of timeliness 18 hours after the as-cast magnesium alloy is dissolved 14 hours at 525 DEG C, high-strength heat-resistant rare earth is obtained Magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 6 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 6 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 7
It is divided into according to being preset to:Sm 6wt%, Gd 3wt%, Zn 3wt%, Zr 3wt%, surplus are for Mg and unavoidably Impurity, alloying component, the sources Mg, the sources Zn, the sources Sm, the sources Gd and the sources Zr are subjected to dispensing, remove each stock chart in blending process The oxide skin in face, and they are preheated to 300 DEG C;
Crucible is preheated to 500 DEG C, the sources Mg of above-mentioned preheating are added, furnace temperature rises to 760 DEG C, and it is 1 to be passed through volume ratio: 100 SF6And CO6Gaseous mixture carry out magnesium melting;
After the sources Mg are completely melt, Mg aluminium alloys are obtained;The sources Sm, the sources Zn of above-mentioned preheating are added into the Mg aluminium alloys Uniform stirring is carried out with the sources Gd and carries out melting within 10 minutes, obtains mixed liquor;
Furnace temperature is risen to 770 DEG C, the sources Zr of above-mentioned preheating are added into the mixed liquor, uniform stirring is melted for 10 minutes Refining, obtains aluminium alloy;
Furnace temperature is down to 750 DEG C, argon gas dehydrogenation is passed through into the aluminium alloy;
No. 6 flux standings are added into the aluminium alloy after the dehydrogenation to be refined within 45 minutes;
Furnace temperature is set as 750 DEG C the aluminium alloy heat preservation after refining is cast for 10 minutes, aluminium alloy is cast to steel In water cooling mold processed, as-cast magnesium alloy is obtained;
It the as-cast magnesium alloy at 380 DEG C is kept the temperature 6 hours is warming up to 470 DEG C and keep the temperature 8 hours, then heat to 515 DEG C Heat preservation 12 hours, obtains intermediate product;
The intermediate product is kept the temperature 35 hours at 200 DEG C, obtains high-strength heat-resistant rare earth magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 7 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 7 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 8
High-strength heat-resistant rare earth magnesium alloy is prepared according to the method for embodiment 7, with embodiment 7 difference lies in, according to Following target components carry out dispensing:
The Zr of Zn, 3wt% of Gd, 0.8wt% of Sm, 3wt% of 6wt%, surplus are Mg and inevitable impurity.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 8 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 8 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Embodiment 9
High-strength heat-resistant rare earth magnesium alloy is prepared according to the method for embodiment 7, with embodiment 7 difference lies in, according to Following target components carry out dispensing:
The Zr of Zn, 3wt% of Yb, 3wt% of Sm, 3wt% of 6wt%, surplus are Mg and inevitable impurity.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 9 is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that the test embodiment of the present invention 9 is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Comparative example 1
High-strength heat-resistant rare earth magnesium alloy is prepared according to the method for embodiment 7, with embodiment 7 difference lies in, according to Following target components carry out dispensing:
The Zr of Zn, 3wt% of Gd, 3wt% of Sm, 0.2wt% of 6wt%, surplus are Mg and inevitable impurity.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that test comparative example 1 of the present invention is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that test comparative example 1 of the present invention is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
Comparative example 2
High-strength heat-resistant rare earth magnesium alloy is prepared according to method described in embodiment 3, with embodiment 3 difference lies in, Dispensing is carried out according to following target components:
Y:4.0wt%;Nd:4.5wt%;Zn:0.5wt%, Zr:0.5wt.%, surplus are Mg and inevitable impurity.
It is by obtained as-cast magnesium alloy progress heat-treating methods:
In 200 DEG C of timeliness 20 hours after the as-cast magnesium alloy is dissolved 12 hours at 520 DEG C, high-strength heat-resistant rare earth is obtained Magnesium alloy.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that test comparative example 2 of the present invention is prepared is in room temperature With the mechanical property at 300 DEG C, testing result is as shown in table 1.
According to the method for embodiment 1, the high-strength heat-resistant rare earth magnesium alloy that test comparative example 2 of the present invention is prepared is 200 DEG C, the croop property under the conditions of 100MPa, testing result is as shown in table 2.
The mechanical property for the high-strength heat-resistant magnesium alloy that 1 embodiment of the present invention of table and comparative example are prepared
The croop property for the high-strength heat-resistant magnesium alloy that 2 embodiment of the present invention of table and comparative example are prepared
As seen from the above embodiment, the present invention provides a kind of high-strength heat-resistant rare earth magnesium alloy, ingredient is:2~6wt%'s Sm;The Nd of 0~3wt%;The heavy rare earth element of 2~5wt%;The Zn of 0.5~4wt%;The Zr of 0.2~3wt%;Surplus be Mg and Inevitable impurity.The present invention makes rich Zr rings using influence of the elements to the electronic migration state of Zr elements such as Sm, heavy rare earth In Zr during heat treatment in the form of Zn-Zr heat resistive compounds the conical surface of magnesium alloy substrate be precipitated.In hot conditions Under, Zn-Zr, which meets, effectively inhibits non-basal slip, forms the precipitation hardened magnesium alloys of Mg-RE by heat treatment on this basis Matrix.The presence of two class phases can effectively inhibit high temperature Prismatic slip, conical surface sliding and basal slip in the magnesium alloy of the present invention, Improve magnesium alloy elevated temperature strength.
The above is the preferred embodiments of the invention, it is noted that for the general technical staff of the art For, under the premise of not departing from the principle and core concept of patent of the present invention, several modification and improvement can also be made, this A little modifications and improvement are also considered as within the protection domain of patent of the present invention.

Claims (10)

1. a kind of high-strength heat-resistant rare earth magnesium alloy, ingredient are:
The Sm of 2~6wt%;
The Nd of 0~3wt%;
The heavy rare earth element of 2~5wt%;
The Zn of 0.5~4wt%;
The Zr of 0.2~3wt%;
Surplus is Mg and inevitable impurity.
2. high-strength heat-resistant rare earth magnesium alloy according to claim 1, which is characterized in that the heavy rare earth element be selected from Gd, Y, one or more of Dy, Ho and Er.
3. high-strength heat-resistant rare earth magnesium alloy according to claim 1, which is characterized in that the quality percentage of the Zn and Zr contains The ratio of amount is (1~3):1.
4. high-strength heat-resistant rare earth magnesium alloy according to claim 1, which is characterized in that the high-strength heat-resistant rare earth magnesium alloy Ingredient be:
The Sm of 3~5wt%;
The heavy rare earth element of 3~5wt%;
The Zn of 1~3wt%;
The Zr of 0.2~2wt%;
Surplus is Mg and inevitable impurity.
5. a kind of preparation method of high-strength heat-resistant rare earth magnesium alloy described in claim 1, includes the following steps:
(1) sources Mg, the sources Nd, the sources Sm, the sources Zn, the sources Zr and heavy rare earth source are subjected to dispensing;
(2) sources Mg are subjected to melting, obtain Mg aluminium alloys;
(3) the Mg aluminium alloys and the sources Sm, the sources Nd, the sources Zn and heavy rare earth source are subjected to melting, obtain mixed liquor;
(4) mixed liquor and the sources Zr are subjected to melting, obtain aluminium alloy;
(5) aluminium alloy is cast, obtains as-cast magnesium alloy;
(6) as-cast magnesium alloy is heat-treated, obtains high-strength heat-resistant rare earth magnesium alloy.
6. according to the method described in claim 5, it is characterized in that, the temperature of melting is 720~740 DEG C in the step (2).
7. according to the method described in claim 5, it is characterized in that, the temperature of melting is 760~800 DEG C in the step (4).
8. according to the method described in claim 5, it is characterized in that, the heat treatment in the step (6) is:
The as-cast magnesium alloy is first carried out to solution treatment and carries out ageing treatment again, obtains high-strength heat-resistant rare earth magnesium alloy.
9. according to the method described in claim 8, it is characterized in that, the solution treatment is:
The as-cast magnesium alloy is heated up step by step in 300~530 DEG C of temperature range.
10. according to the method described in claim 8, it is characterized in that, the temperature of the ageing treatment is 170~230 DEG C;
The time of the ageing treatment is 10~40 hours.
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CN109666832A (en) * 2019-02-22 2019-04-23 中国科学院长春应用化学研究所 High-intensity thermal deformation resistant magnesium alloy and preparation method thereof
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CN110284035A (en) * 2019-08-07 2019-09-27 中国科学院长春应用化学研究所 A kind of heat resistance magnesium alloy and preparation method thereof
CN111172442A (en) * 2020-01-09 2020-05-19 西安建筑科技大学 Rare earth magnesium alloy powder for 3D printing and preparation method thereof
CN111172442B (en) * 2020-01-09 2021-05-25 西安建筑科技大学 Rare earth magnesium alloy powder for 3D printing and preparation method thereof

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