CN101532107B - Heat resisting rare earth magnesium alloy and preparation method thereof - Google Patents

Heat resisting rare earth magnesium alloy and preparation method thereof Download PDF

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Publication number
CN101532107B
CN101532107B CN2009100646268A CN200910064626A CN101532107B CN 101532107 B CN101532107 B CN 101532107B CN 2009100646268 A CN2009100646268 A CN 2009100646268A CN 200910064626 A CN200910064626 A CN 200910064626A CN 101532107 B CN101532107 B CN 101532107B
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alloy
rare earth
magnesium
heat resisting
magnesium alloy
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CN101532107A (en
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李全安
李克杰
陈君
张兴渊
张清
任文亮
李跃华
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Henan University of Science and Technology
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Henan University of Science and Technology
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Abstract

The invention discloses a heat resisting rare earth magnesium alloy, in particular to a magnesium alloy with compositions of Mg, Gd, Y, Sm, Zr and Sb. The alloy consists of the following compositions in percentage by weight: 8 to 15 percent of Gd, 2 to 5 percent of Y, 0.4 to 4.5 percent of Sm, 0.3 to 0.7 percent of Zr, 0.3 to 2 percent of Sb, less than 0.02 percent of gross amount of impurity elements, namely Si, Fe, Cu and Ni, and the balance being Mg. The invention also discloses a method for preparing the heat resisting rare earth magnesium alloy. The heat resisting casting rare earth magnesium alloy has high tensile strength, in a range between room temperature and 250 DEG C, the tensile strength of the alloy has anomalous temperature effect, which means that the tensile strength rises along with rise of tensile temperature. The heat resisting casting rare earth magnesium alloy has the highest tensile strength reaching 346MPa at 250 DEG C, still has 309MPa at 300 DEG C. Compared with commercial heat resisting magnesium alloy WE54, the rare earth magnesium alloy has higher high-temperature-strength, and has good application prospect in aero-space, automobile industry, weaponry and other fields.

Description

A kind of heat resisting magnesium-rare earth alloy
Technical field
The present invention relates to a kind of heat resisting magnesium-rare earth alloy.
Background technology
Magnesium is the lightest structural metallic materials, uses increasing on automobile.The every loss of weight 100Kg of automobile, then 100Km fuel-economizing 0.5L has reduced exhaust emissions simultaneously, and therefore carrying out the Mg Alloy Research exploitation has significance for save energy, inhibition environmental pollution.But, its application in aerospace, military project, automobile and other industry of the not good serious obstruction of the intensity of magnesium alloy and thermotolerance, therefore improve magnesium alloy intensity and heat-resisting be the important topic of development magnesium alloy materials.
Existing heat resistance magnesium alloy is mainly started with from restriction dislocation motion and reinforcement crystal boundary, by suitable alloying, by introduce the second high phase of thermostability, reduce element in magnesium matrix rate of diffusion or improve the purpose that means such as grain boundary structure state and tissue morphology realize improving magnesium alloy heat resistance and high temperature creep drag.At present, in all alloying elements, rare earth (RE) is to improve the most effective alloying element of magnesium alloy resistance toheat, except having degasification, removal of impurities, raising casting fluidity, corrosion resisting property, most of rare earth element has bigger solid solubility limit to rare earth element in magnesium simultaneously in magnesium alloy; And descend with temperature, solid solubility sharply reduces, and can obtain bigger degree of supersaturation, thus in ag(e)ing process subsequently diffusion-precipitation, dystectic rare earth compound phase; The all right crystal grain thinning of rare earth element, raising room temperature strength, and be distributed in intracrystalline and crystal boundary (mainly being crystal boundary) disperse, the high-melting-point rare earth compound, still can pinning intracrystalline dislocation and crystal boundary slippage when high temperature, thereby improved the hot strength of magnesium alloy, the rate of diffusion of RE element in magnesium matrix is slower simultaneously, and this makes the Mg-RE alloy be suitable for long term operation under the comparatively high temps environment.Mg-RE (as Mg-Gd system) alloy is important refractory alloy system, has higher high temperature strength and good creep property.It is alloy that current magnesium alloy component in 200~300 ℃ of following long term operations are Mg-RE, because its special valence electron structure and the significant strengthening effect in magnesium alloy are tied to form to developing an important alloy system of high-strength heat-resisting magnesium alloy Mg-RE.
As rare earth resources first big country, China is that the research of alloy is on the increase in recent years and is goed deep into about Mg-RE, and the successful research and development of magnesium-rare earth alloy will help us to utilize this advantage.Present commercial heat resistance magnesium alloy such as WE54, the main deficiency of its existence is, strength degradation is still more during high temperature, in the time of can't satisfying it fully and in aerospace, military project, automobile and other industry, use under the high temperature to the higher requirement of intensity.
Summary of the invention
The purpose of this invention is to provide a kind of high-strength heat-resistant magnesium-rare earth.
Another object of the present invention provides a kind of preparation method of this heat resisting magnesium-rare earth alloy.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of heat resisting magnesium-rare earth alloy, form by following component by mass percent: 8~15%Gd, 2~5%Y, 0.4~4.5%Sm, 0.3~0.7%Zr, 0.3~2%Sb, impurity element Si, Fe, Cu and Ni total amount are less than 0.02%, and surplus is Mg.
Described Gd, Y, the mass percent sum of Sm is 13~18%.
Described heat resisting magnesium-rare earth alloy is by magnesium, antimony and master alloy Mg-Gd, and Mg-Y, Mg-Sm, Mg-Zr forms for the raw material melting.
The preparation method of heat resisting magnesium-rare earth alloy of the present invention comprises the steps:
1. with magnesium, antimony, master alloy Mg-Gd, Mg-Y, Mg-Sm and Mg-Zr preheating;
2. with magnesium and antimony at CO 2+ SF 6Mixed gas protected fusing down in 720~740 ℃ of adding master alloy Mg-Gd, Mg-Y, Mg-Sm, rises to 740~760 ℃ with temperature and adds the Mg-Zr master alloys;
3. after Mg-Zr fusing, remove surface scum, stop to heat up after temperature is risen to 770~780 ℃;
4. cast after cooling the temperature to 690~730 ℃, obtain cast alloy;
5. obtain heat resisting magnesium-rare earth alloy after cast alloy being heat-treated.
The 1. described preheating temperature of step is 150~220 ℃.
Described thermal treatment is that cast alloy is carried out solution treatment and ageing treatment successively.
The treatment temp of described solution treatment is 500~550 ℃, and the treatment time is 8~20 hours.
The treatment temp of described ageing treatment is 200~250 ℃, and the treatment time is 10~40 hours.
During described casting casting die is preheated to 180~250 ℃.
Alloy compositions of the present invention is Mg-Gd-Y-Sm-Zr-Sb.It is first component that the present invention adopts Gd, the maximum solid solution degree of Gd in Mg sosoloid is 20.3wt%, 200 ℃ of solid solubility in Mg sosoloid are 3.8wt%, for guaranteeing that alloy obtains good timeliness precipitation strength and solid solution strengthening effect, the add-on of Gd is not less than 8wt%, and too many for fear of the alloy density increase, and the undue embrittlement of alloy, therefore Gd add-on of the present invention is not higher than 15wt%; Adopting Y is second component, and adopting Sm is the 3rd component, and Y, Sm can reduce the solid solubility of Gd in Mg, thereby increases the timeliness precipitation strength effect of Gd; The maximum solid solution degree of Sm in Mg is 5.7wt%, and therefore Sm add-on of the present invention is not higher than 4.5wt%; Adopt Zr as grain-refining agent, with toughness that improves alloy and the processing performance of improving alloy; Sb as solution strengthening, dispersion-strengthened and with the constituent element of rare earth cooperative reinforcing magnesium alloy, further improve the hot strength of alloy.
Sb is a kind of magnesium alloy strengthening element and surface active element, energy refinement magnesium alloy crystal grain, and also dystectic Sb-RE compound of disperse has the intensive strengthening effect to matrix and crystal boundary.Sb and Mg form the hexagonal structure Mg of good stability 3Sb 2Compound, Mg 3Sb 2Less with the face mismatch of Mg, part Mg 3Sb 2Can become the forming core substrate of α-Mg, make alloy nucleation under less condensate depression, crystal grain thinning, the intensity of raising magnesium alloy; The Mg of disperse 3Sb 2Not only can strengthen the Mg matrix, also be distributed in crystal boundary and make its reinforcement, also make the upper semi-continuous netted compound of crystal boundary be transformed into particulate state simultaneously, further improve the hot strength of alloy.
The assistant alloy element sb that the present invention adds in containing magnesium alloy can form with RE with rare earth (RE) 2Sb is main high-melting-point diffusing particle particle, is distributed in the Mg matrix, and this particle particle is mainly RE mutually 2The Sb phase, but measure when higher when containing Sb, this particle matter is mainly RE 2Sb phase and RESb mixture mutually, disperse RE 2Sb particle particle quantity and size increase, and the quantity that the crystal boundary place sporadicly scatters divorced eutectic β phase also improves.An amount of Sb has also improved the flowability of alloy liquid.Because the solution strengthening effect of dispersion-strengthened action, Sb and the RE of RE-Sb particle improves the normal temperature of alloy and mechanical behavior under high temperature, and effectively improves the alloy high-temp creep resisting ability.
Heat resisting magnesium-rare earth alloy of the present invention has an outstanding feature on mechanical property, in room temperature to 250 ℃ scope, tensile strength of alloys has the abnormal temperature effect, promptly along with the raising of draft temperature, tensile strength also improves thereupon, and in the time of 250 ℃, tensile strength can reach 346MPa.Heat resisting magnesium-rare earth alloy of the present invention is example with Mg-10Gd-3.5Y-2.5Sm-0.3Zr-1Sb, its room temperature tensile strength is 270MPa after solution treatment and ageing treatment, unit elongation is 3.4%, 200 ℃ of tensile strength are 300MPa, 250 ℃ of tensile strength are 346Mpa, and tensile strength is still up to arriving 309MPa in the time of 300 ℃.And under the same conditions, the room temperature tensile strength of WE54 magnesium alloy is 280MPa, and unit elongation is that 4.0%, 200 ℃ of tensile strength is 241MPa, and 250 ℃ of tensile strength are 230MPa.Heat resisting magnesium-rare earth alloy of the present invention and commercial heat resistance magnesium alloy WE54 alloy phase ratio have higher hot strength, at aspects such as aerospace, automotive industry, weaponrys wide application prospect will be arranged.
Embodiment
The raw material magnesium (Mg) that relates in the embodiment of the invention, antimony (Sb), Mg-Gd, Mg-Y, Mg-Sm, Mg-Zr is the commercially available prod.The purity of described raw material is 99.9% Mg, 99.9% Sb, 99.5% Mg-25.26%Gd, 99.5% Mg-24.54%Y, 99.5% Mg-25.11%Sm, 99.5% Mg-30.00%Zr.
Embodiment 1
The heat resisting magnesium-rare earth alloy of present embodiment is made up of following component by mass percent: 8%Gd, and 2%Y, 4%Sm, 0.5%Zr, 0.5%Sb, impurity element Si, Fe, Cu and Ni total amount are less than 0.02%, and surplus is Mg.Its middle-weight rare earths total content is 14%.
Press the mentioned component alloyage, its founding is: adopt corundum crucible, medium-frequency induction furnace melting.Earlier magnesium, antimony, master alloy Mg-Gd, Mg-Y, Mg-Sm and Mg-Zr are preheating to 190 ℃, magnesium, antimony are put into be preheating to 500 ℃ crucible then, at CO 2+ SF 6Mixed gas protected down, high-power rapid heating fusing, treat the fusing of magnesium and antimony after, add Mg-Gd, Mg-Y master alloy at 730 ℃, small power slowly heats, and treats that its fusing back and magnesium liquid temp add the Mg-Sm master alloy again when ging up to 730 ℃; Be warmed up to 760 ℃ and add the Mg-Zr master alloy, treat its fusing back removal surface scum, temperature is risen to 780 ℃ again, close governor circuit, leave standstill; Treat that magnesium liquid is cooled to 710 ℃ and casts, casting is heated to 180 ℃ in advance with steel die.Obtain the Mg-8Gd-2Y-4Sm-0.5Zr-0.5Sb as-cast magnesium alloy at last.The thermal treatment of as-cast magnesium alloy: 500 ℃ of solution treatment 20 hours, 225 ℃ of isothermal agings were handled 25 hours.
The method of the tensile strength test of present embodiment heat resisting magnesium-rare earth alloy: the sample after solid solution aging is handled, be processed into 5 times of standard tensile samples according to standard GB 6397-86 " metal stretching experimental sample ".Tension specimen at high temperature need be in the requirement of sample two ends machining screw with the clamping device that satisfies the drawing by high temperature sample.Electronics is stretching on the accurate universal testing machine of day island proper Tianjin AG-I 250kN and carries out, and draw speed is 1mm/min.During drawing by high temperature, to tension specimen insulation 15 minutes, temperature fluctuation ± 1 ℃ stretched then under relevant temperature.
The heat resisting magnesium-rare earth alloy of present embodiment gained, its room temperature tensile strength is 264MPa, and unit elongation is that 3.2%, 200 ℃ tensile strength is 300MPa, and 250 ℃ tensile strength is 338Mpa, and tensile strength is still up to arriving 293MPa in the time of 300 ℃.The tensile strength of this example heat resisting magnesium-rare earth alloy improves along with the rising of draft temperature in room temperature to 250 ℃, still has very high tensile strength under 300 ℃ high temperature, has satisfied its requirement in aerospace, military project, automobile and other industry.
Embodiment 2
The composition of heat resisting magnesium-rare earth alloy of the present invention (weight percent) is: 10%Gd, and 3.5%Y, 2.5%Sm, 0.3%Zr, 1%Sb, impurity element Si, Fe, Cu and Ni total amount are less than 0.02%, and surplus is Mg.Its middle-weight rare earths total content is 16%.
Press the mentioned component alloyage, its founding is: adopt corundum crucible, medium-frequency induction furnace melting.Earlier magnesium, antimony, master alloy Mg-Gd, Mg-Y, Mg-Sm and Mg-Zr are preheating to 220 ℃, magnesium, antimony are put into be preheating to 500 ℃ of left and right sides crucibles then, at CO 2+ SF 6Under mixed gas protected; high-power rapid heating fusing; after treating the fusing of magnesium ingot and antimony; add Mg-Gd, Mg-Y master alloy at 740 ℃, small power slowly heats, and treats that its fusing back and magnesium liquid temp add the Mg-Sm master alloy again when ging up to 740 ℃; be warmed up to 750 ℃ and add the Mg-Zr master alloy; treat its fusing back removal surface scum, again the magnesium liquid temp is risen to 775 ℃, close governor circuit, leave standstill.Treat that magnesium liquid is cooled to 730 ℃ and casts.Casting is heated to 210 ℃ in advance with steel die.Obtain the Mg-10Gd-3.5Y-2.5Sm-0.3Zr-1Sb cast alloy at last.Cast alloy is heat-treated: 530 ℃ of solution treatment 12 hours, 200 ℃ of isothermal agings were handled 40 hours.
The method of the tensile strength test of present embodiment heat resisting magnesium-rare earth alloy is with embodiment 1.
The alloy of present embodiment gained, its room temperature tensile strength is 270MPa, and unit elongation is that 3.4%, 200 ℃ of tensile strength is 300MPa, and 250 ℃ of tensile strength are 346MPa, tensile strength 309MPa in the time of 300 ℃.The tensile strength of this example heat resisting magnesium-rare earth alloy improves along with the rising of draft temperature in room temperature to 250 ℃, still has very high tensile strength under 300 ℃ high temperature, has satisfied its requirement in aerospace, military project, automobile and other industry.
Embodiment 3
The composition of heat resisting magnesium-rare earth alloy of the present invention (weight percent) is: 13%Gd, and 3%Y, 1.5%Sm, 0.5%Zr, 2%Sb, impurity element Si, Fe, Cu and Ni total amount are less than 0.02%, and surplus is Mg.Its middle-weight rare earths total content is 17.5%.
Press the mentioned component alloyage, its founding is: adopt corundum crucible, medium-frequency induction furnace melting.Earlier magnesium, antimony, master alloy Mg-Gd, Mg-Y, Mg-Sm and Mg-Zr are preheating to 150 ℃, magnesium, antimony are put into be preheating to 500 ℃ of left and right sides crucibles then, at CO 2+ SF 6Under mixed gas protected; high-power rapid heating fusing; after treating the fusing of magnesium ingot and antimony; add Mg-Gd, Mg-Y master alloy at 720 ℃, small power slowly heats, and treats that its fusing back and magnesium liquid temp add the Mg-Sm master alloy again when ging up to 720 ℃; be warmed up to 740 ℃ and add the Mg-Zr master alloy; treat its fusing back removal surface scum, again the magnesium liquid temp is risen to 770 ℃, close governor circuit, leave standstill.Treat that magnesium liquid is cooled to 690 ℃ and casts.Casting is heated to 250 ℃ in advance with steel die.Obtain the Mg-13Gd-3Y-1.5Sm-0.5Zr-2Sb cast alloy at last.Cast alloy is heat-treated: 550 ℃ of solution treatment 8 hours, 250 ℃ of isothermal agings were handled 10 hours.
The method of the tensile strength test of present embodiment heat resisting magnesium-rare earth alloy is with embodiment 1.
The alloy of present embodiment gained, its room temperature tensile strength is 281MPa, and unit elongation is that 3.3%, 200 ℃ of tensile strength is 312MPa, and 250 ℃ of tensile strength are 343MPa, tensile strength 304MPa in the time of 300 ℃.The tensile strength of this example heat resisting magnesium-rare earth alloy improves along with the rising of draft temperature in room temperature to 250 ℃, still has very high tensile strength under 300 ℃ high temperature, has satisfied its requirement in aerospace, military project, automobile and other industry.
It should be noted last that, above example only is illustrative rather than definitive thereof technical scheme of the present invention, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.

Claims (2)

1. a heat resisting magnesium-rare earth alloy is characterized in that: be made up of following component by mass percent: 8~15%Gd, 2~5%Y, 0.4~4.5%Sm, 0.3~0.7%Zr, 0.3~2%Sb, impurity element Si, Fe, Cu and Ni total amount are less than 0.02%, and surplus is Mg; Described Gd, Y, the mass percent sum of Sm is 13~18%.
2. heat resisting magnesium-rare earth alloy according to claim 1 is characterized in that: this heat resisting magnesium-rare earth alloy is by magnesium, antimony and master alloy Mg-Gd, and Mg-Y, Mg-Sm, Mg-Zr forms for the raw material melting.
CN2009100646268A 2009-04-13 2009-04-13 Heat resisting rare earth magnesium alloy and preparation method thereof Expired - Fee Related CN101532107B (en)

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CN103146972B (en) * 2013-03-14 2015-12-23 河南科技大学 A kind of Multielement rare-earth magnesium alloy and preparation method thereof
CN103146973B (en) * 2013-03-14 2015-04-29 河南科技大学 High-temperature-resistant rare earth magnesium alloy
CN103757510B (en) * 2014-01-02 2016-08-17 河南科技大学 A kind of multicomponent heat-resistant magnesium alloy
CN104233027B (en) * 2014-06-06 2017-03-22 河南科技大学 Flame-retardant high-strength magnesium alloy and preparation method thereof
CN104060140B (en) * 2014-07-10 2016-08-24 重庆大学 A kind of resistance to high temperature oxidation magnesium alloy
CN104651691B (en) * 2015-02-06 2016-08-24 宁波高新区融创新材料科技有限公司 Fast degradation magnesium alloy materials and manufacture method thereof and application
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