CN101392345A - Nickel-containing heat resisting magnesium-rare earth alloy and preparation method thereof - Google Patents
Nickel-containing heat resisting magnesium-rare earth alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a heat resisting rare earth-magnesium alloy containing nickel in the technical field of metallic materials and a preparation method thereof, pertaining to the metallic material category and the metallurgy field. The magnesium alloy comprises Ni, M, Mg and impurities, wherein, M is one or several components of Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er and Tm, the atomic percent of Ni is a percent and the atomic percent of M is b percent, with a more than or equal to 0.1 and less than or equal to 5 and b more than or equal to 0.5 and less than or equal to 5. The preparation of the magnesium alloy comprises the smelting process and subsequent heat treatment process. The magnesium alloy can not only be used as the cast magnesium alloy but also as the wrought magnesium alloy, and has mechanical property of room temperature and high temperature strength superior to that of traditional WE series of commercial magnesium alloys.
Description
Technical field
The present invention relates to magnesium alloy of a kind of metallic substance technical field and preparation method thereof, specifically, what relate to is a kind of nickel-containing heat resisting magnesium-rare earth alloy and preparation method thereof.
Background technology
Magnesium alloy can satisfy the motor vehicle exhaust requirement of increasingly stringent as the lightest structural metallic materials, can produce in light weight, oil consumption is few, the new automobile of environment-friendly type, thereby in automotive industry, be subjected to paying close attention to widely.Yet mechanical properties such as low normal temperature strength, hot strength and plasticity have restricted its application on engine and power system part.Therefore, the heat resistance magnesium alloy of high-intensity high-tenacity high creep resistance energy has been proposed.Rare earth element is considered to be used for improving the important element of magnesium alloy resistance toheat, has for example obtained the Mg-Y-Nd base alloy WE54 and the WE43 of commercial applications.Traditional WE54 alloy is after T6 handles, and room temperature tensile strength is 250MPa, and yield strength is 172MPa, and unit elongation is 2.0% (ASM Specialty Handbook:Magnesium and Magnesium Alloys).
Find through literature search prior art, in patent documentation CN 1804083A, put down in writing a kind of high-strength heat-resistant rare earth magnesium alloy, it consists of: the Gd of 2～10% weight ratios, the Y of 3～12% weight ratios, the weight sum of Gd and Y accounts for 13～14% of this alloy gross weight, and the Zr of 0.4～0.7% weight ratio and the activating element (Zn that is not more than 0.3% weight ratio, Ag, Cu, Sr, Ca, Ti, Bi, choose any one kind of them among the Cd), or the Mn of 0.6～1.5% weight ratio and the activating element (Sn that is not more than 0.3% weight ratio, Si, Sb, Ca, choose any one kind of them among the Sr), all the other are magnesium.The precipitate of this magnesium-rare earth is always separated out along the prismatic plane of matrix, forms a kind of netted phase structure of intersection, has the alligatoring of energy high resistance particle, provides highly enriched and effect creep resistance.They are under 300 ℃ of application conditions, and instantaneous ultimate tensile strength is 180MPa.Yet in this patent documentation, do not add the Ni element.In fact add a certain proportion of Ni element in rare earth element, utilize ageing strengthening by the method for conventional cast, second strengthens and solution strengthening will be prepared the magnesium-rare earth with high-strength and high-ductility mutually.
In the at present more known patent (patent CN1886528A, patent CN 1886529A, patent CN 101027420A) with Mg-Zn-RE class alloy of high-intensity high-tenacity, by different thermal distortion technology, prepared the high-strength and high ductility heat resisting magnesium-rare earth alloy.But, also do not report at present and relevant patent about utilizing the conventional cast technology to prepare high-strength and high ductility Mg-Ni-RE alloy.
People such as Itoi adopt the method for rapid solidification to prepare Mg
90.5Ni
3.25Y
6.25(at.%) alloy.(people Scripta Master (2008) such as T.Itoi, doi:10.1016/j.scriptamat.2008.08.001). the preparation method of this alloy is mainly and at first utilizes pure metal Mg, Ni and Y at CO
2Protection is sense melt furnace the inside system Mg down
90.5Ni
3.25Y
6.25(at.%) ternary alloy, this alloy pig is poured in the water cooled copper mould then fast 700 ℃ of remeltings, has obtained the Mg of rapid solidification
90.5Ni
3.25Y
6.25(at.%) alloy pig.The Mg-Ni-Y of this method preparation utilizes the method for rapid solidification to prepare, and the Y content of alloy has surpassed 5at.%.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, propose a kind of high strength, nickel-containing heat resisting magnesium-rare earth alloy of high tenacity and high creep resistance energy and preparation method thereof.By in magnesium, adding one or more of rare earth elements such as Ni and Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, Tm, and obtain high strength by melting and thermal treatment process condition, high tenacity and high creep resistance can magnesium alloy.The purposes that this metal needle enlarges magnesium alloy, its intensity and toughness all are in can be for practical level.
The present invention is achieved by the following technical solutions:
Nickel-containing heat resisting magnesium-rare earth alloy involved in the present invention and preparation method thereof, comprise Ni, M, all the other are Mg and unavoidable impurities, wherein M is one or more among Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, the Tm, the atom percentage content of Ni is a%, the M atom percentage content is b%, and a and b satisfy: 0.1≤a≤5, and 0.5≤b≤5.
The atom percentage content of described impurity component is: Fe＜0.002% and Cu＜0.005%.
The composition design considerations of alloy is: if the atom percentage content of Ni is more than 5%, then particularly toughness (or ductility) has the tendency of reduction; If rare earth element adds up to atom percentage content more than 5%, then toughness (or ductility) also has the tendency of reduction.If the atom percentage content of Ni is lower than 0.1%, perhaps the rare earth atom degree amounts to and is lower than 0.5%, then intensity and toughness at least either side with insufficient.Therefore, the following of the atom percentage content of Ni is limited to 0.1%, and the rare earth element atomic percent adds up to the following of content to be limited to 0.5%.
Intensity and flexible increase are that the Ni atom percentage content is at 0.5～2.5% o'clock and becomes remarkable.If the Ni atom percentage content is 0.1% near and rare earth element content tails off, then intensity has the tendency of reduction, even still be in the situation of this scope, still demonstrates than high in the past high strength and high tenacity.Therefore, the atom percentage content maximum range of Ni is more than 0.1% in the magnesium alloy of the present invention, below 5%.
Intensity and flexible increase are that rare earth element adds up to atom percentage content to be at 1～3% o'clock and becomes remarkable.If rare earth element adds up to atom percentage content 0.5% near and Ni content tails off, then intensity has the tendency of reduction, even still be in the situation of this scope, still demonstrates than high in the past high strength and high tenacity.Therefore, it is more than 0.5% that magnesium alloy middle-weight rare earths dvielement of the present invention adds up to the atom percentage content maximum range, below 5%.
The preparation method of above-mentioned nickel-containing heat resisting magnesium-rare earth alloy provided by the present invention is divided into two stages, i.e. melting and subsequent heat treatment.Wherein:
Described fusion process is at SF
6/ CO
2Carry out under the gas shield condition, comprise the steps:
(1) melting Mg: in smelting furnace, add the pure magnesium of oven dry, the heating melting;
(2) add Ni: after treating that magnesium melts fully, add the Mg-Ni master alloy down at 660～680 ℃;
(3) add in Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, the Tm element one or more: add one or more of Mg-Y, Mg-Gd, Mg-Sm, Mg-Nd, Mg-Tb, Mg-Dy, Mg-Ho, Mg-Er, Mg-Tm, Mg-La and Mg-Ce master alloy in the magnesium liquid at 700～740 ℃;
(4) casting: rising magnesium liquid temp to 780～800 ℃, be cooled to 740～760 ℃ behind insulation 20～30min, energising refining 6～10min, time of repose after the refining is controlled between 25～40min, treat that skimming surface scum after magnesium liquid is cooled to 700～740 ℃ casts, casting is heated to 200～250 ℃ in advance with steel die, can obtain the magnesium-rare earth alloy ingot blank.
Described melting is carried out follow-up thermal treatment after finishing, be specially: the magnesium-rare earth alloy ingot blank that melting is obtained carries out 490～540 ℃, the solution treatment of 6～30h, alloy after the solution treatment after carrying out the preheating of 0.5～2h, 250～450 ℃ temperature is pushed, then the hot extrude pressure bar is carried out 200～300 ℃, the ageing treatment of 12～100h.
In the high creep resistance heat resistance magnesium alloy of high-intensity high-tenacity of the present invention manufacture method, the temperature condition when preferably described magnesium alloy being carried out plastic working is more than 250 ℃.This is because if temperature condition is lower than 250 ℃, then plastic working difficulty.
The present invention is by adding one or more of rare earth elements such as alloying element Ni and Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, Tm in magnesium, and by further optimizing heat treatment of alloy technology and heat processing technique, make full use of the effect of second reinforcement mutually, ageing strengthening and the alloying of alloy, can access higher normal temperature and pyritous tensile property, plasticity and creep-resistant property, obtain excellent heat resisting.Give full play to the comprehensive advantage of rare earth alloy and Ni, available instantaneous ultimate tensile strength reaches as high as 489MPa, and unit elongation is the magnesium alloy of 7.7% high-intensity high-tenacity.Its tensile strength and unit elongation all are higher than existing WE54 alloy far away, are a kind of high-strength-toughness magnesium alloys that has prospect therefore.
Purposes as described above, as can to have enlarged at magnesium alloy according to the present invention provides the manufacture method of the high-intensity high-tenacity high creep resistance Dow metal that a kind of intensity and toughness all is in realistic scale.Compared with prior art, the present invention has marked improvement, the heat resistance magnesium alloy that provides is in light weight except that having, technology is simple, cost can accept, also has good plasticity, excellent hot strength and creep-resistant property.
Magnesium alloy of the present invention just can obtain by the method for conventional cast, handles the high creep resisting heat resistance magnesium alloy of the high strength that can obtain excellent properties by follow-up extruding and thermal treatment process.Be fit to large-scale industrial production, can be applied in industrial circles such as space flight and aviation automobile military project.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Alloying constituent (atomic percent): 2%Y and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y: in magnesium liquid, add the Mg-Y master alloy at 700 ℃; (4) casting: rising magnesium liquid temp to 780 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Y-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 2:
Alloying constituent (atomic percent): 2%Y, 0.5%La and 0.5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and La: in magnesium liquid, add Mg-Y and Mg-La master alloy at 720 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled between the 40min, treat that skimming surface scum after magnesium liquid is cooled to 720 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 30h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 200 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Y-0.5La-0.5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 3:
Alloying constituent (atomic percent): 2%Y, 0.5%Ce and 0.1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Ce: in magnesium liquid, add Mg-Y and Mg-Ce master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind insulation 20～30min, energising refining 10min, the time of repose after the refining is controlled between the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 20h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 250 ℃, the ageing treatment of 32h.Can obtain having concurrently the Mg-2Y-0.5Ce-0.1Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 4:
Alloying constituent (atomic percent): 2%Y, 0.5%Tb and 2%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Tb: in magnesium liquid, add Mg-Yhe and Mg-Tb master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 40h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 235 ℃, the ageing treatment of 80h.Can obtain having concurrently the Mg-2Y-0.5Tb-2Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 5:
Alloying constituent (atomic percent): 3%Y, 0.5%Dy and 5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Dy: in magnesium liquid, add Mg-Y and Mg-Dy master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 550 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-3Y-0.5Dy-5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 6:
Alloying constituent (atomic percent): 5%Y, 0.5%Ho and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Ho: in magnesium liquid, add Mg-Y and Mg-Ho master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 780 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 550 ℃, and the solution treatment of 20h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 245 ℃, the ageing treatment of 80h.Can obtain having concurrently the Mg-5Y-0.5Ho-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 7:
Alloying constituent (atomic percent): 0.5%Y, 0.5%Er and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Er: in magnesium liquid, add Mg-Y and Mg-Er master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 490 ℃, and the solution treatment of 6h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 245 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-0.5Y-0.5Er-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 8:
Alloying constituent (atomic percent): 2%Gd and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Gd: in magnesium liquid, add the Mg-Gd master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 740～760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Gd-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 9:
Alloying constituent (atomic percent): 2%Gd, 5%La and 0.1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Gd and La: in magnesium liquid, add Mg-Gd and Mg-La master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 740～760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Gd-5La-0.1Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 10:
Alloying constituent (atomic percent): 5%Gd, 5%Ce and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Gd and Ce: in magnesium liquid, add Mg-Gd and Mg-Ce master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 740～760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 12h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 245 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-5Gd-5Ce-Ni alloy of high strength and good resistance creep property at last,
The mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 11:
Alloying constituent (atomic percent): 2%Sm and 0.5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Sm: in magnesium liquid, add the Mg-Sm master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Sm-0.5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 12:
Alloying constituent (atomic percent): 5%Sm, 5%Dy and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Sm and Dy: in magnesium liquid, add Mg-Sm and Mg-Dy master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-5Sm-5Dy-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 13:
Alloying constituent (atomic percent): 5%Ho, 0.5%Sm and 5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Sm and Ho: in magnesium liquid, add Mg-Sm and Mg-Ho master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 60h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 48h.Can obtain having concurrently the Mg-5Ho-0.5Sm-5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 14:
Alloying constituent (atomic percent): 5%Er, 2%Nd and 0.5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Nd and Er: in magnesium liquid, add Mg-Nd and Mg-Er master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-5Er-2Nd-0.5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 15:
Alloying constituent (atomic percent): 5%Nd and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Nd: in magnesium liquid, add the Mg-Nd master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-5Nd-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 16:
Alloying constituent (atomic percent): 0.5% Nd and 5%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Nd: in magnesium liquid, add the Mg-Nd master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled at 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-0.5Nd-5Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 17:
Alloying constituent (atomic percent): 2%Y, 1%Gd and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Y and Gd: in magnesium liquid, add Mg-Y and Mg-Gd master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 40h.Can obtain having concurrently the Mg-2Y-Gd-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 18:
Alloying constituent (atomic percent): 2%Tb, 2%Dy and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Tb and Dy: in magnesium liquid, add Mg-Tb and Mg-Dy master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled within the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 20h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 245 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Tb-2Dy-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 19:
Alloying constituent (atomic percent): 2%Ho, 2%Er and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Ho and Er: in magnesium liquid, add Mg-Ho and Mg-Er master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled between the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 540 ℃, and the solution treatment of 20h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 245 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-2Ho-2Er-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Embodiment 20:
Alloying constituent (atomic percent): 1%Tm, 1%La, 1%Ce and 1%Ni; All the other are Mg and unavoidable impurities.Wherein, impurity content is: Fe＜0.002% and Cu＜0.005%.
The melting technology concrete steps of this alloy are: (1) adds pure magnesium according to mentioned component configuration alloy in electrical crucible, adopt SF simultaneously
6/ CO
2Mixed gas is protected; (2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy at 680 ℃; (3) add Tm, La and Ce: in magnesium liquid, add Mg-Tm, Mg-La and Mg-Ce master alloy at 740 ℃; (4) casting: rising magnesium liquid temp to 800 ℃, be cooled to 760 ℃ behind the insulation 30min, energising refining 10min, the time of repose after the refining is controlled between the 40min, treat that skimming surface scum after magnesium liquid is cooled to 740 ℃ casts, casting is heated to 250 ℃ in advance with steel die.
The alloy that melting is obtained carries out 530 ℃, and the solution treatment of 10h (being called for short T4) is pushed under 300 ℃, and extrusion ratio is 10.And then carry out 225 ℃, the ageing treatment of 24h.Can obtain having concurrently the Mg-Tm-La-Ce-Ni alloy of high strength and good resistance creep property at last, the mechanical property of normal temperature and 200 ℃ sees Table 1 and table 2.
Table 1 shows is mechanical property after the alloy extruding, with extrusion temperature and the extrusion ratio shown in the table, with the 2.5mm/ extrusion speed of second, the casting material of the Ni various Mg-Ni-RE alloys different with the addition of RE carried out extrusion processing after, stretching experiment result at room temperature.As following table 1
| Embodiment | Form (atom %) | Extrusion temperature ℃ | Extrusion ratio | Experimental temperature ℃ | Yield strength MPa | Tensile strength MPa | Unit elongation % |
| Embodiment 1 | Mg-2Y-1Ni | 300 | 10. | Normal temperature | 365 | 413 | 4.4 |
| Embodiment 2 | Mg-2Y-0.5La-0.5Ni | 300 | 10 | Normal temperature | 377 | 421 | 5.6 |
| Embodiment 3 | Mg-2Y-0.5Ce-0.1Ni | 300 | 10 | Normal temperature | 380 | 431 | 7.2 |
| Embodiment 4 | Mg-2Y-0.5Tb-2Ni | 300 | 10 | Normal temperature | 397 | 429 | 4.7 |
| Embodiment 5 | Mg-3Y-0.5Dy-5Ni | 300 | 10 | Normal temperature | 382 | 401 | 4.9 |
| Embodiment 6 | Mg-5Y-0.5Ho-1Ni | 300 | 10 | Normal temperature | 396 | 455 | 7.6 |
| Embodiment 7 | Mg-0.5Y-0.5Er-1Ni | 300 | 10 | Normal temperature | 328 | 399 | 9.3 |
| Embodiment 8 | Mg-2Gd-1Ni | 300 | 10 | Normal temperature | 357 | 402 | 7.1 |
| Embodiment 9 | Mg-2Gd-5La-0.1Ni | 300 | 10 | Normal temperature | 334 | 428 | 11.8 |
| Embodiment 10 | Mg-5Gd-5Ce-1Ni | 300 | 10 | Normal temperature | 405 | 489 | 7.7 |
| Embodiment 11 | Mg-2Sm-0.5Ni | 300 | 10 | Normal temperature | 321 | 376 | 4.8 |
| Embodiment 12 | Mg-5Dy-5Sm-1Ni | 300 | 10 | Normal temperature | 344 | 427 | 6.1 |
| Embodiment 13 | Mg-5Ho-0.5Sm-5Ni | 300 | 10 | Normal temperature | 305 | 399 | 7.9 |
| Embodiment 14 | Mg-5Er-2Nd-0.5Ni | 300 | 10 | Normal temperature | 321 | 376 | 4.8 |
| Embodiment 15 | Mg-5Nd-1Ni | 300 | 10 | Normal temperature | 347 | 419 | 5.1 |
| Embodiment 16 | Mg-0.5Nd-5Ni | 300 | 10 | Normal temperature | 312 | 389 | 8.9 |
| Embodiment 17 | Mg-2Y-1Gd-1Ni | 300 | 10 | Normal temperature | 339 | 401 | 5.7 |
| Embodiment 18 | Mg-2Tb-2Dy-1Ni | 300 | 10 | Normal temperature | 355 | 406 | 6.8 |
| Embodiment 19 | Mg-2Ho-2Er-1Ni | 300 | 10 | Normal temperature | 354 | 417 | 6.0 |
| Embodiment 20 | Mg-1Tm-1La-1Ce-1Ni | 300 | 10 | Normal temperature | 371 | 423 | 5.3 |
Table 2 shows is mechanical property after the alloy extruding, with extrusion temperature and the extrusion ratio shown in the table, with the 2.5mm/ extrusion speed of second, the casting material of the Ni various Mg-Ni-RE alloys different with the addition of RE carried out extrusion processing after, the stretching experiment result under 200 ℃.As following table 2:
| Embodiment | Form (atom %) | Extrusion temperature ℃ | Extrusion ratio | Experimental temperature ℃ | Yield strength MPa | Tensile strength MPa | Unit elongation % |
| Embodiment 1 | Mg-2Y-1Ni | 300 | 10 | 200 | 218 | 290 | 11.6 |
| Embodiment 2 | Mg-2Y-0.5La-0.5Ni | 300 | 10 | 200 | 234 | 302 | 13.1 |
| Embodiment 3 | Mg-2Y-0.5Ce-0.1Ni | 300 | 10 | 200 | 268 | 300 | 15.8 |
| Embodiment 4 | Mg-2Y-0.5Tb-2Ni | 300 | 10 | 200 | 254 | 312 | 20.7 |
| Embodiment 5 | Mg-3Y-0.5Dy-5Ni | 300 | 10 | 200 | 231 | 279 | 15.3 |
| Embodiment 6 | Mg-5Y-0.5Ho-1Ni | 300 | 10 | 200 | 244 | 305 | 14.0 |
| Embodiment 7 | Mg-0.5Y-0.5Er-1Ni | 300 | 10 | 200 | 276 | 299 | 16.9 |
| Embodiment 8 | Mg-2Gd-1Ni | 300 | 10 | 200 | 207 | 278 | 13.2 |
| Embodiment 9 | Mg-2Gd-5La-0.1Ni | 300 | 10 | 200 | 206 | 278 | 11.8 |
| Embodiment 10 | Mg-5Gd-5Ce-1Ni | 300 | 10 | 200 | 255 | 339 | 12.7 |
| Embodiment 11 | Mg-2Sm-0.5Ni | 300 | 10 | 200 | 201 | 265 | 13.5 |
| Embodiment 12 | Mg-5Dy-5Sm-1Ni | 300 | 10 | 200 | 239 | 320 | 15.7 |
| Embodiment 13 | Mg-5Ho-0.5Sm-5Ni | 300 | 10 | 200 | 211 | 311 | 17.1 |
| Embodiment 14 | Mg-5Er-2Nd-0.5Ni | 300 | 10 | 200 | 221 | 236 | 12.7 |
| Embodiment 15 | Mg-5Nd-1Ni | 300 | 10 | 200 | 217 | 334 | 14.9 |
| Embodiment 16 | Mg-0.5Nd-5Ni | 300 | 10 | 200 | 201 | 321 | 15.9 |
| Embodiment 17 | Mg-2Y-1Gd-1Ni | 300 | 10 | 200 | 218 | 269 | 13.5 |
| Embodiment 18 | Mg-2Tb-2Dy-1Ni | 300 | 10 | 200 | 200 | 255 | 14.1 |
| Embodiment 19 | Mg-2Ho-2Er-1Ni | 300 | 10 | 200 | 206 | 267 | 15.3 |
| Embodiment 20 | Mg-1Tm-1La-1Ce-1Ni | 300 | 10 | 200 | 221 | 278 | 17.9 |
Claims (5)
1. nickel-containing heat resisting magnesium-rare earth alloy, it is characterized in that, comprise Ni, M, all the other are Mg and impurity, wherein M is one or more among Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, the Tm, and the atom percentage content of Ni is a%, and the M atom percentage content is b%, a and b satisfy: 0.1≤a≤5, and 0.5≤b≤5.
2. nickel-containing heat resisting magnesium-rare earth alloy according to claim 1 is characterized in that, the atom percentage content of described impurity component is: Fe＜0.002% and Cu＜0.005%.
3. the preparation method of a nickel-containing heat resisting magnesium-rare earth alloy as claimed in claim 1 is characterized in that, comprising: two stages of melting and subsequent heat treatment, wherein:
Described fusion process is at SF
6/ CO
2Carry out under the gas shield condition, comprise the steps:
(1) melting Mg: in smelting furnace, add the pure magnesium of oven dry, the heating melting;
(2) add Ni: after treating that magnesium ingot melts fully, add the Mg-Ni master alloy down at 660～680 ℃;
(3) add in Y, Gd, Sm, Nd, La, Ce, Tb, Dy, Ho, Er, the Tm element one or more: add one or more of Mg-Y, Mg-Gd, Mg-Sm, Mg-Nd, Mg-Tb, Mg-Dy, Mg-Ho, Mg-Er, Mg-Tm, Mg-La and Mg-Ce master alloy in the magnesium liquid at 700～740 ℃;
(4) casting: rising magnesium liquid temp to 780～800 ℃, be cooled to 740～760 ℃ after insulation for some time, the energising refining, leave standstill after the refining, treat that skimming surface scum after magnesium liquid is cooled to 700～740 ℃ casts, casting is heated to 200～250 ℃ in advance with steel die, obtains the magnesium-rare earth alloy ingot blank;
Described melting is carried out follow-up thermal treatment after finishing, be specially: the magnesium-rare earth alloy ingot blank that melting is obtained carries out 490～540 ℃, the solution treatment of 6～30h, alloy after the solution treatment is pushed after 250～450 ℃ temperature is carried out the preheating of 0.5～2h, then the hot extrude pressure bar is carried out 200～300 ℃, the ageing treatment of 12～100h.
4. the preparation method of nickel-containing heat resisting magnesium-rare earth alloy according to claim 3 is characterized in that, in the casting step of described melting, is 20～30min 780～800 ℃ of soaking times.
5. the preparation method of nickel-containing heat resisting magnesium-rare earth alloy according to claim 3 is characterized in that, in the casting step of described melting, the energising purified time is 6～10min, and the time of repose after the refining is controlled between 25～40min.
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