CN100513606C - Heat conductive magnesium alloy and method for preparing the same - Google Patents
Heat conductive magnesium alloy and method for preparing the same Download PDFInfo
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- CN100513606C CN100513606C CNB2007101214578A CN200710121457A CN100513606C CN 100513606 C CN100513606 C CN 100513606C CN B2007101214578 A CNB2007101214578 A CN B2007101214578A CN 200710121457 A CN200710121457 A CN 200710121457A CN 100513606 C CN100513606 C CN 100513606C
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Abstract
The invention relates to a heat-conductive magnesium alloy and a preparation method thereof. The heat-conductive magnesium alloy comprises the component content of: 2.5-11wt percent of Zn, 0.15-1.5wt percent of Zr, 0.1-2.5wt percent of Ag, 0.3-3.5wt percent of Ce, 0-1.5wt percent of Nd, 0-2.5wt percent of La, 0-0.5wt percent of Pr, wherein each content of Nd, La, Pr can not be zero at the same time or each content of Nd, La, Pr is zero at the same time, the rest component is Mg. Pure Mg ingot, pure Zn ingot, master alloy of Mg-Zr, pure Ag ingot or master alloy of Mg-Ag and pure Ce ingot or rich-cerium mischmetal ingot or Ce or master alloy of rich-cerium mischmetal ingot and magnesium are used as raw materials; pure Mg ingot is smelted and alloyed; after castings are made, solid dissolving treatment and aging treatment are the next steps; or after making billet, homogenization thermal treatment is the next step; sheet metal, tube, profile, rod, wire or other castings are made by adopting the technologies of rolling, extrusion, drawing, forging or distortion process. The magnesium alloy of the invention, under the temperature of 20 DEG C, has thermal conductivity rate of above 120W. (m.K)-1, tensile strength of above 340 Mpa and yielding strength of above 310 Mpa. The invention can be used as structure material for a heat radiation system of a power supply and an electric device in aviation and aerospace.
Description
Technical field
The present invention relates to a kind of heat conductive magnesium alloy and its preparation method, belong to metal material field.
Background technology
The heat-removal system structured material of the power supply in the aerospace, electron device had both required good heat conductivility, must have also simultaneously that density is little, intensity is high.Therefore, high strength, high heat conductive magnesium alloy have important application background.
The thermal conductivity of pure magnesium is 1.55W. (m.K)
-1, intensity is approximately about 10MPa; After the alloying, intensity increases substantially, and thermal conductivity significantly reduces.For example according to U.S.'s magnesium and alloy handbook (ASM SpecialtyHandbook:Magnesium and magnesiumAlloys), contain the magnesium alloy AZ81 of aluminium, zinc, its tensile strength is 275Mpa, the thermal conductivity 20 ℃ the time is 51.1W. (m.K)
-1Magnesium-rare earth WE43, its intensity is 250Mpa, the thermal conductivity 20 ℃ the time is 51.3W. (m.K)
-1The magnesium alloy ZE41 that contains zinc, rare earth, its tensile strength is 205Mpa, the thermal conductivity 20 ℃ the time is 123.1W. (m.K)
-1The magnesium alloy ZC63 that contains zinc, copper, its tensile strength is 210Mpa, the thermal conductivity 20 ℃ the time is 122W. (m.K)
-1The magnesium alloy QE22 of argentiferous, rare earth, its tensile strength is 260Mpa, the thermal conductivity 20 ℃ the time is 113W. (m.K)
-1
Present existing magnesium alloy, thermal conductivity high such as ZE41, QE22, its intensity is all less than 265Mpa; And intensity higher such as AZ81, WE43, its thermal conductivity is all less than 55W. (m.K)
-1
Summary of the invention
The purpose of this invention is to provide a kind of thermal conductivity and intensity all than higher magnesium alloy, this magnesium alloy materials is under 20 ℃ of conditions, and thermal conductivity is greater than 120W. (m.K)
-1, tensile strength greater than 340Mpa, yield strength greater than 310Mpa.Can be as the power supply in the aerospace, the heat-removal system structured material of electron device.
Another object of the present invention provides a kind of thermal conductivity and intensity all than the preparation method of higher magnesium alloy.
For achieving the above object, the present invention takes following technical scheme:
A kind of heat conductive magnesium alloy, the component content of this magnesium alloy is: the content of Zn is 2.5～11wt%, the content of Zr is 0.15～1.5wt%, the content of Ag is 0.1～2.5wt%, the content of Ce is 0.3～3.5wt%, the content of Nd is 0～1.5wt%, the content of La is 0～2.5wt%, the content of Pr is 0～0.5wt%, wherein, Nd, La, Pr are not equal to 0 simultaneously, and perhaps Nd, La, Pr 0 (promptly contain 3 kinds among Nd, La, the Pr simultaneously, perhaps do not contain Nd, La and Pr3 kind), all the other are Mg.
Because in the process of preparation magnesium alloy, the composition Ce in the magnesium alloy adds with pure Ce ingot or cerium-rich mischmetal ingot mode, in the cerium-rich mischmetal that is added, the content of Ce is more than 40 weight %, and all the other are Nd, La and Pr rare earth element.Therefore, the composition Ce of magnesium alloy is adding fashionablely in pure cerium-rich mischmetal ingot mode, all contain Nd, La and Pr3 kind when containing Ce in the composition of magnesium alloy again, and promptly the Nd in the technical scheme, La, Pr are not equal to 0 simultaneously; Composition Ce in the magnesium alloy is adding fashionablely in pure Ce ingot mode, only contain Ce in the composition of magnesium alloy, does not contain Nd, La and Pr3 kind, and promptly the Nd in the technical scheme, La, Pr are 0 simultaneously.
In heat conductive magnesium alloy of the present invention, the content of described Zn is preferably 3.5～6.5wt%.
In heat conductive magnesium alloy of the present invention, the content of described Zr is preferably 0.45～1.0wt%.
In heat conductive magnesium alloy of the present invention, the content of described Ag is preferably 0.5～1.5wt%.
In heat conductive magnesium alloy of the present invention, the content of described Ce is preferably 1.5～3.0wt%.
In heat conductive magnesium alloy of the present invention, the total content of described Nd, La and Pr is preferably 0～3.5wt%.
A kind of method for preparing heat conductive magnesium alloy of the present invention, this method comprises the steps:
(1), be raw material with the master alloy of pure magnesium ingot, pure Zn ingot, Mg-Zr master alloy, pure Ag ingot or Mg-Ag master alloy and pure Ce ingot or cerium-rich mischmetal ingot or Ce or cerium-rich mischmetal and magnesium, get the raw materials ready by the weight percent of the composition of above-mentioned magnesium alloy; Wherein, cerium-rich mischmetal is that the content of Ce is more than 40 weight %, all the other are Nd, La and Pr rare earth element, Nd, La and the Pr content in cerium-rich mischmetal is not fixed, the cerium-rich mischmetal that different manufacturers and same manufacturer different time are produced, and wherein the content of Nd, La and Pr may be also inequality, but basically all within a scope, the content of Nd is 10～20wt%, and the content of La is 20～35wt%, and the content of Pr is 3～10wt%;
(2), with whole pure magnesium ingots with as far as possible closely mode pile up in the fusion crucible in smelting furnace, fusing fully under the protection of shielding gas, the magnesium melt temperature is controlled at 680～800 ℃, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
(3), preheating oven is warmed up to 160～580 ℃, the master alloy of pure Zn ingot, Mg-Zr master alloy, pure Ag ingot or Mg-Ag master alloy and pure Ce ingot or cerium-rich mischmetal ingot or Ce or cerium-rich mischmetal and magnesium put into add charging basket, adding charging basket is that soft steel or high chromium steel are made, be thick with a large amount of apertures on it, above-mentioned raw materials is put into preheating oven together with the charging basket that adds that holds these raw materials, be preheating to 100～580 ℃;
(4), the pure Zn ingot with after the preheating, Mg-Zr master alloy, pure Ag ingot or Mg-Ag master alloy and pure Ce ingot or cerium-rich mischmetal ingot or Ce or cerium-rich mischmetal submerge in the magnesium melt together with the charging basket that adds that holds these raw materials with the master alloy of magnesium, is convenient to the dissolving and the diffusion of the master alloy of pure Zn ingot, Mg-Zr master alloy, pure Ag ingot or Mg-Ag master alloy and pure Ce ingot or cerium-rich mischmetal ingot or Ce or cerium-rich mischmetal and magnesium;
(5), the magnesium melt temperature is controlled at 720～800 ℃, after the master alloy for the treatment of Zn, Mg-Zr master alloy, Ag or Mg-Ag master alloy and Ce or cerium-rich mischmetal or Ce or cerium-rich mischmetal and magnesium dissolves fully, taking-up adds charging basket, 730～800 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, according to the composition of sample and content decision reinforced adjustment the whether, reaches the composition and the content of magnesium alloy of the present invention until the magnesium alloy liquation;
(6), the magnesium alloy liquation is poured in the permanent mold casting mould of abundant preheating or the sand mold casting mould and is frozen into foundry goods; Perhaps the magnesium alloy liquation is poured in extrusion casting machine or the pressure die-casting machine in batches extrusion casting or be cast into foundry goods according to casting weight; Perhaps adopt low-pressure casting process that casting of magnesium alloy is caused foundry goods;
(7), the foundry goods of above-mentioned steps preparation is carried out solution treatment, its solution treatment process is foundry goods to be heated to 350～500 ℃, insulation 3～30 hours, hardening;
(8), the foundry goods after the solution treatment is carried out ageing treatment, its timeliness treating processes is that foundry goods was heated to 155～235 ℃, insulation 2～46 hours.
The method for preparing heat conductive magnesium alloy of the present invention includes fusion process and last handling process, wherein, last handling process can be divided into two kinds: a kind of is that the foundry goods after the cast is carried out aftertreatment, another kind is that the billet after the cast is carried out aftertreatment, therefore, because of different last handling processes, the method for preparing heat conductive magnesium alloy of the present invention also is divided into two kinds, and the method for aforesaid preparation heat conductive magnesium alloy of the present invention is wherein a kind of, is the method for first kind of heat conductive magnesium alloy of the present invention.Second kind of method for preparing heat conductive magnesium alloy of the present invention is:
A kind of method for preparing heat conductive magnesium alloy of the present invention, wherein, step (1)-(5) of the fusion process and the method for first kind of heat conductive magnesium alloy of the present invention are identical, the Therefore, omited, its step (6)-(8) are:
(6), the magnesium alloy liquation is poured into is frozen into the billet of using for follow-up deformation processing in the permanent mold casting mould of abundant preheating or the sand mold casting mould, perhaps the magnesium alloy liquation is transported in the crystallizer, carry out continuous or semicontinuous casting, be prepared into the billet of using for follow-up deformation processing;
(7), the billet with the above-mentioned steps preparation carries out homogenizing thermal treatment, its homogenizing heat treatment process is that billet is heated to 350～500 ℃, is incubated 3～30 hours, directly adopt rolling, extruding, drawing or forging process deformation processing to become sheet material, tubing, section bar, bar, wire rod or various forging then, promptly adopt extruding or drawing process that the billet deformation processing is become bar or wire rod, or billet is processed into sheet material with rolling deformation, or adopt crimp that billet is processed into tubing or section bar, or adopt forging press that billet is forged into forging;
(8), sheet material, tubing, section bar, bar, wire rod or various forging that deformation processing is become carry out ageing treatment, its timeliness treating processes is that sheet material, tubing, section bar, bar, wire rod or various forging were heated to 155～235 ℃, insulation 2～36 hours.
In the method for preparation heat conductive magnesium alloy of the present invention; in described step (2); during pure magnesium ingot melts under the protection of shielding gas; be evenly to sprinkle SULPHUR POWDER in crucible bottom and pure magnesium ingot surface; the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion, and is with crucible cover that crucible is airtight, heat temperature raising; make the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, open crucible cover again.Wherein the consumption of SULPHUR POWDER can roughly be estimated as follows: the oxidizing fire reaction of sulphur is S+O
2=SO
2, the nucleidic mass of S and O
2Molecular weight all be 32, promptly material equates with the oxygen level in the external space in the consumption of SULPHUR POWDER and the crucible; Oxygen accounts for 1/5 greatly in air, and density of air is approximately 1 grams per liter; For example the space beyond the material is 200 liters in the crucible, and wherein oxygen is 40 liters, i.e. 40 grams, so the consumption of SULPHUR POWDER are 40 grams.In addition, the oxygen of small amount of residual or sulphur can be ignored the influence of magnesium alloy smelting.In actually operating,, calculate the space beyond the material in the crucible, and, calculate oxygen weight and SULPHUR POWDER weight according to the space beyond the material in the crucible according to the volume of crucible and the cumulative volume of pure magnesium ingot.
In the method for preparation heat conductive magnesium alloy of the present invention, in described step (2), the shielding gas that feeds to smelting furnace is preferably and contains 0.2～0.5 volume %SF
6N
2Be designated hereinafter simply as shielding gas (0.2～0.5%SF
6+ N
2).
Advantage of the present invention is: magnesium alloy of the present invention is under 20 ℃ of conditions, and thermal conductivity is greater than 120W. (m.K)
-1, tensile strength greater than 340Mpa, yield strength greater than 310Mpa.Can be as the power supply in the aerospace, the heat-removal system structured material of electron device.
Embodiment
Embodiment 1:1000 kilogram Mg-2.5Zn-1.5Zr-2.5Ag-3.5Ce heat conductive magnesium alloy (promptly the component content of this magnesium alloy is: 2.5wt%Zn, 1.5wt%Zr, 2.5wt%Ag, 3.5wt%Ce, surplus is Mg) and the plate rolling preparation method.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of pure Ce ingot
Adopt preheating oven that 25 kilograms of pure Zn ingots, 50 kilograms of Mg-30Zr master alloys, 25 kilograms of pure Ag ingots, 35 kilograms of pure Ce ingots are preheating to 120～180 ℃, wherein pure Zn ingot, Mg-30Zr master alloy (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), pure Ag ingot, pure Ce ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt the thick Cr13 steel plate of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 865 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight; heat temperature raising; make the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots; the magnesium melt temperature is controlled at 680～800 ℃; open crucible cover; the scum silica frost of molten surface is cleaned out, fed shielding gas (0.2～0.5%SF to smelting furnace
6+ N
2);
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, pure Ce ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that Zn, Mg-Zr master alloy, Ag, Ce dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, billet casting
With the melt transfer pump magnesium alloy liquation is transported in the crystallizer, carries out semicontinuous casting, be prepared into the billet of plate rolling processing usefulness.
5, homogenizing thermal treatment, plate rolling deformation processing and ageing treatment
The billet of above-mentioned steps preparation is carried out homogenizing thermal treatment, exactly billet is heated to 450～500 ℃, is incubated 26～30 hours, billet rolling deformation after directly adopting plate mill with homogenizing thermal treatment after coming out of the stove is processed into sheet material, then this sheet material is carried out ageing treatment, ageing treatment is heated to this sheet material 215～235 ℃ exactly, is incubated 2～5 hours hours.
Have following performance after Mg-2.5Zn-1.5Zr-2.5Ag-3.5Ce magnesium alloy process homogenizing of the present invention thermal treatment, plate rolling distortion and the ageing treatment: under 20 ℃ of conditions, thermal conductivity is approximately 125W. (m.K)
-1, tensile strength is that 360～370Mpa, yield strength are greater than 325～335Mpa.
Embodiment 2:1000 kilogram Mg-11Zn-0.15Zr-0.1Ag-0.3Ce heat conductive magnesium alloy (promptly the component content of this magnesium alloy is: 11wt%Zn, 0.15wt%Zr, 0.1wt%Ag, 0.3wt%Ce, surplus is Mg) and the diecast parts preparation method.
1, pure Zn ingot, Mg-30Zr master alloy, Mg-25Ag master alloy, the preheating of Mg-30Ce master alloy
Adopt preheating oven with 110 kilograms of pure Zn ingots, (promptly the component content of this master alloy is 5 kilograms of Mg-30Zr: 30wt%Zr, surplus is Mg) master alloy, (promptly the component content of this master alloy is 4 kilograms of Mg-25Ag: 25wt%Ag, surplus is Mg) master alloy, (promptly the component content of this master alloy is 10 kilograms of Mg-30Ce master alloys: 30wt%Ce, surplus is Mg) be preheating to 530～570 ℃, wherein pure Zn ingot, the Mg-30Zr master alloy, the Mg-25Ag master alloy, the Mg-30Ce master alloy all is contained in and adds in the charging basket, puts into the preheating oven preheating together with adding charging basket.Add charging basket and adopt No. 20 thick boiler sheets of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 871 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight; heat temperature raising; make the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots; the magnesium melt temperature is controlled at 680～800 ℃; open crucible cover; the scum silica frost of molten surface is cleaned out, fed shielding gas (0.2～0.5%SF to smelting furnace
6+ N
2);
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, Mg-25Ag master alloy, Mg-30Ce master alloy are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, Mg-25Ag master alloy, Mg-30Ce master alloy dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, casting forming
According to casting weight, with the melt quantitative shifting pump magnesium alloy liquation is poured in the pressure chamber of cold-chamber die casting machine in batches, be cast into foundry goods.
5, thermal treatment
Thermal treatment comprises solution treatment and ageing treatment; Solution treatment is exactly that foundry goods with above-mentioned steps die casting was heated to 350～380 ℃, insulation 25～28 hours, hardening; Then the foundry goods after the solution treatment is carried out ageing treatment, ageing treatment is heated to foundry goods 155～175 ℃ exactly, is incubated 32～36 hours.
Have following performance after Mg-11Zn-0.15Zr-0.1Ag-0.3Ce magnesium alloy process die cast of the present invention and the thermal treatment: under 20 ℃ of conditions, thermal conductivity is approximately 120W. (m.K)
-1, tensile strength is that 340～350Mpa, yield strength are greater than 320～325Mpa.
Embodiment 3:1000 kilogram Mg-3.5Zn-0.45Zr-1.5Ag-3Ce-1.5Nd-2.5La-0.5Pr (promptly the component content of this magnesium alloy is: 3.5wt%Zn, 0.45wt%Zr, 1.5wt%Ag, 3wt%Ce, 1.5wt%Nd, 2.5wt%La, 0.5wt%Pr, surplus is Mg) heat conductive magnesium alloy and bar, tubing, section bar or wire rod extruding production.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of cerium-rich mischmetal ingot
Adopt preheating oven that 35 kilograms of pure Zn ingots, 15 kilograms of Mg-30Zr master alloys (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), 15 kilograms of pure Ag ingots, 75 kilograms of cerium-rich mischmetal ingots are preheating to 260～360 ℃, wherein the content of Ce is that the content of 40wt%, Nd is that the content of 20wt%, La is that the content of 33.4wt%, Pr is 6.6wt% in the cerium-rich mischmetal; Pure Ag ingot, Mg-Zr master alloy, cerium-rich mischmetal ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt the thick Cr13 steel plate of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 860 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight, heat temperature raising makes the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, the magnesium melt temperature is controlled at 680～800 ℃, open crucible cover, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, billet casting
The magnesium alloy liquation is poured into the billet that is frozen in the permanent mold casting mould of abundant preheating for follow-up crimp processing usefulness with the melt transfer pump.
5, the homogenizing thermal treatment of billet; The crimp processing of bar, tubing, section bar or wire rod and timeliness are handled
The billet of above-mentioned steps preparation is carried out homogenizing thermal treatment, exactly billet is heated to 410～430 ℃, is incubated 10～15 hours, bar, tubing, section bar or wire rod are processed in billet crimp after directly adopting extrusion machine with homogenizing thermal treatment after coming out of the stove, then this bar, tubing, section bar or wire rod are carried out ageing treatment, ageing treatment is heated to this bar, tubing, section bar or wire rod 180～200 ℃ exactly, is incubated 5～6 hours.
Mg-3.5Zn-0.45Zr-1.5Ag-3Ce-1.5Nd-2.5La-0.5Pr magnesium alloy of the present invention is through homogenizing thermal treatment, have following performance after bar, tubing, section bar or wire rod crimp processing and the ageing treatment: under 20 ℃ of conditions, thermal conductivity is approximately 127W. (m.K)
-1, tensile strength is that 350～355Mpa, yield strength are 320～325Mpa.
Embodiment 4:1000 kilogram Mg-4Zn-0.6Zr-1Ag-1.1Ce-0.3Nd-0.5La-0.1Pr (promptly the component content of this magnesium alloy is: 4wt%Zn, 0.6wt%Zr, 1wt%Ag, 1.1wt%Ce, 0.3wt%Nd, 0.5wt%La, 0.1wt%Pr, surplus is Mg) heat conductive magnesium alloy and part forging preparation method thereof.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of cerium-rich mischmetal ingot
Adopt preheating oven that 40 kilograms of pure Zn ingots, 20 kilograms of Mg-30Zr master alloys (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), 10 kilograms of pure Ag ingots, 20 kilograms of cerium-rich mischmetal ingots are preheating to 260～360 ℃, wherein the content of Ce is that the content of 55wt%, Nd is that the content of 15wt%, La is that the content of 25wt%, Pr is 5wt% in the cerium-rich mischmetal; Pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt the thick Cr13 steel plate of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 910 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight, heat temperature raising makes the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, the magnesium melt temperature is controlled at 680～800 ℃, open crucible cover, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, billet casting
The magnesium alloy liquation is poured into the billet that is frozen in the sand mold casting mould for follow-up forging deformation processing usefulness with the melt transfer pump.
5, homogenizing thermal treatment, the processing of part forging deformation and ageing treatment
The billet of above-mentioned steps preparation is carried out homogenizing thermal treatment, exactly billet is heated to 435～460 ℃, is incubated 15～17 hours, billet forging deformation after directly adopting forging press with homogenizing thermal treatment after coming out of the stove is processed into part, then this part is carried out ageing treatment, ageing treatment is heated to this part 190～210 ℃ exactly, is incubated 7～9 hours.
Have following performance after Mg-4Zn-0.6Zr-1Ag-1.1Ce-0.3Nd-0.5La-0.1Pr magnesium alloy process homogenizing of the present invention thermal treatment, the processing of part forging deformation and the ageing treatment: under 20 ℃ of conditions, thermal conductivity is approximately 125W. (m.K)
-1, tensile strength is that 355～365Mpa, yield strength are 325～335Mpa.
Embodiment 5:1000 kilogram Mg-4.5Zn-0.9Zr-0.5Ag-0.9Ce-0.3Nd-0.6La-0.2Pr (promptly the component content of this magnesium alloy is: 4.5wt%Zn, 0.9wt%Zr, 0.5wt%Ag, 0.9wt%Ce, 0.3wt%Nd, 0.6wt%La, 0.2wt%Pr, surplus is Mg) heat conductive magnesium alloy and bar or wire rod extruding and drawing preparation method.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of cerium-rich mischmetal ingot
Adopt preheating oven that 45 kilograms of pure Zn ingots, 30 kilograms of Mg-30Zr master alloys (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), 5 kilograms of pure Ag ingots, 20 kilograms of cerium-rich mischmetal ingots are preheating to 260～360 ℃, wherein the content of Ce is that the content of 45wt%, Nd is that the content of 15wt%, La is that the content of 30wt%, Pr is 10wt% in the cerium-rich mischmetal; Pure Ag ingot, Mg-Zr master alloy, cerium-rich mischmetal ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt No. 20 thick boiler sheets of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 900 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight, heat temperature raising makes the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, the magnesium melt temperature is controlled at 680～800 ℃, open crucible cover, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, billet casting
The magnesium alloy liquation is poured into the billet that is frozen in the permanent mold casting mould of abundant preheating for follow-up crimp processing usefulness with the melt transfer pump.
5, homogenizing thermal treatment, bar or wire rod extruding are handled with drawing deformation processing and timeliness
The billet of above-mentioned steps preparation is carried out homogenizing thermal treatment, exactly billet is heated to 425～450 ℃, is incubated 10～15 hours, bar or wire rod are processed in billet crimp after directly adopting extrusion machine with homogenizing thermal treatment after coming out of the stove, and then adopt cold drawing bench that this bar or wire rod are carried out drawing deformation to be processed into littler bar of diameter or wire rod, at last this bar or wire rod are carried out ageing treatment, ageing treatment is heated to this bar or wire rod 180～200 ℃, is incubated 5～6 hours exactly.
Have following performance after Mg-4.5Zn-0.9Zr-0.5Ag-0.9Ce-0.3Nd-0.6La-0.2Pr heat conductive magnesium alloy process homogenizing of the present invention thermal treatment, bar or wire rod extruding and drawing deformation processing and the ageing treatment: under 20 ℃ of conditions, thermal conductivity is approximately 123W. (m.K)
-1, tensile strength is that 380～400Mpa, yield strength are 370～390Mpa.
Embodiment 6:1000 kilogram Mg-5.5Zn-0.9Zr-0.5Ag-0.9Ce-0.3Nd-0.6La-0.2Pr (promptly the component content of this magnesium alloy is: 5.5wt%Zn, 0.9wt%Zr, 0.5wt%Ag, 0.9wt%Ce, 0.3wt%Nd, 0.6wt%La, 0.2wt%Pr, surplus is Mg) heat conductive magnesium alloy and and extrusion casting part preparation method thereof.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of cerium-rich mischmetal ingot
Adopt preheating oven that 55 kilograms of pure Zn ingots, 30 kilograms of Mg-30Zr master alloys (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), 5 kilograms of pure Ag ingots, 20 kilograms of cerium-rich mischmetal ingots are preheating to 260～360 ℃, wherein the content of Ce is that the content of 45wt%, Nd is that the content of 15wt%, La is that the content of 30wt%, Pr is 10wt% in the cerium-rich mischmetal; Pure Ag ingot, Mg-Zr master alloy, cerium-rich mischmetal ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt the thick Cr13 steel plate of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 890 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight, heat temperature raising makes the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, the magnesium melt temperature is controlled at 680～800 ℃, open crucible cover, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, extrusion casting is shaped
According to casting weight, with the melt quantitative shifting pump magnesium alloy liquation is poured in the pressure chamber of extrusion casting machine in batches, extrusion casting becomes foundry goods.
5, thermal treatment
Thermal treatment comprises solution treatment and ageing treatment; Solution treatment is exactly that foundry goods with above-mentioned steps extrusion casting was heated to 435～460 ℃, insulation 28～30 hours, hardening; Then the foundry goods after the solution treatment is carried out ageing treatment, ageing treatment is heated to foundry goods 165～180 ℃ exactly, is incubated 42～46 hours.
Have following performance after Mg-5.5Zn-0.9Zr-0.5Ag-0.9Ce-0.3Nd-0.6La-0.2Pr magnesium alloy process extrusion casting moulding of the present invention and the thermal treatment: under 20 ℃ of conditions, thermal conductivity is approximately 121W. (m.K)
-1, tensile strength is that 340～350Mpa, yield strength are 315～325Mpa.
Embodiment 7:1000 kilogram Mg-6.5Zn-0.9Zr-0.5Ag-1Ce-0.2Nd-0.6La-0.2Pr (promptly the component content of this magnesium alloy is: 6.5wt%Zn, 0.9wt%Zr, 0.5wt%Ag, 1wt%Ce, 0.2wt%Nd, 0.6wt%La, 0.2wt%Pr, surplus is Mg) heat conductive magnesium alloy and and low-pressure casting part preparation method thereof.
1, pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, the preheating of cerium-rich mischmetal ingot
Adopt preheating oven that 65 kilograms of pure Zn ingots, 30 kilograms of Mg-30Zr master alloys (promptly the component content of this master alloy is: 30wt%Zr, surplus are Mg), 5 kilograms of pure Ag ingots, 20 kilograms of cerium-rich mischmetal ingots are preheating to 260～360 ℃, wherein the content of Ce is that the content of 50wt%, Nd is that the content of 10wt%, La is that the content of 30wt%, Pr is 10wt% in the cerium-rich mischmetal; Pure Ag ingot, Mg-Zr master alloy, cerium-rich mischmetal ingot all are contained in and add in the charging basket, put into the preheating oven preheating together with adding charging basket.Add charging basket and adopt the thick Cr13 steel plate of 3mm to be processed into, on steel plate, get out the aperture of a large amount of Φ 5mm, make it into sieve-like.
2, pure magnesium ingot fusing
With whole 880 kilograms of pure magnesium ingots with as far as possible closely mode pile up in fusion crucible, evenly sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface, the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion.With crucible cover that crucible is airtight, heat temperature raising makes the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, the magnesium melt temperature is controlled at 680～800 ℃, open crucible cover, the scum silica frost of molten surface is cleaned out, feed shielding gas to smelting furnace;
3, alloying
Pure Zn ingot after the preheating, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot are submerged in the magnesium melt together with the charging basket that adds that holds them, the magnesium melt temperature is controlled at 780～790 ℃, after treating that pure Zn ingot, Mg-30Zr master alloy, pure Ag ingot, cerium-rich mischmetal ingot dissolve fully, taking-up adds charging basket, 750～780 ℃ of insulations 10～60 minutes, all alloying elements are evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, if composition and content are defective, the adjustment of can feeding in raw material is until qualified;
4, low-pressure casting is shaped
With the melt transfer pump magnesium alloy liquation of above-mentioned steps melting is transferred in the crucible of air injection machine holding furnace, low-pressure casting becomes foundry goods.
5, thermal treatment
Thermal treatment comprises solution treatment and ageing treatment; Solution treatment is exactly that foundry goods with the above-mentioned steps low-pressure casting was heated to 395～420 ℃, insulation 27～29 hours, hardening; Then the foundry goods after the solution treatment is carried out ageing treatment, ageing treatment is heated to foundry goods 165～180 ℃ exactly, is incubated 42～46 hours.
Have following performance after Mg-6.5Zn-0.9Zr-0.5Ag-1Ce-0.2Nd-0.6La-0.2Pr magnesium alloy process low-pressure casting moulding of the present invention and the thermal treatment: under 20 ℃ of conditions, thermal conductivity is approximately 121W. (m.K)
-1, tensile strength is that 340～350Mpa, yield strength are 310～315Mpa.
Claims (10)
1, a kind of heat conductive magnesium alloy, it is characterized in that: the component content of this magnesium alloy is: the content of Zn is 2.5～11wt%, and the content of Zr is 0.15～1.5wt%, and the content of Ag is 0.1～2.5wt%, the content of Ce is 0.3～3.5wt%, the content of Nd is 0～1.5wt%, and the content of La is 0～2.5wt%, and the content of Pr is 0～0.5wt%, wherein, Nd, La, Pr are not equal to 0 simultaneously, and perhaps Nd, La, Pr are 0 simultaneously, and all the other are Mg.
2, heat conductive magnesium alloy according to claim 1 is characterized in that: the content of described Zn is 3.5～6.5wt%.
3, heat conductive magnesium alloy according to claim 1 and 2 is characterized in that: the content of described Zr is 0.45～1.0wt%.
4, heat conductive magnesium alloy according to claim 3 is characterized in that: the content of described Ag is 0.5～1.5wt%.
5, heat conductive magnesium alloy according to claim 4 is characterized in that: the content of described Ce is 1.5～3.0wt%.
6, heat conductive magnesium alloy according to claim 5 is characterized in that: the total content of described Nd, La, Pr is 0～3.5wt%.
7, a kind of method for preparing heat conductive magnesium alloy, this method comprises the steps:
(1), with pure magnesium ingot, pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium be raw material, gets the raw materials ready by the weight percent of the composition of the described magnesium alloy of claim 1; Wherein, cerium-rich mischmetal be the content of Ce more than 40 weight %, all the other are Nd, La and Pr rare earth element;
(2), pure magnesium ingot is piled up in the fusion crucible in smelting furnace, fusing fully is controlled at 680～800 ℃ with the magnesium melt temperature under the protection of shielding gas, the scum silica frost of molten surface is cleaned out, and fed shielding gas to smelting furnace;
(3), preheating oven is warmed up to 160～580 ℃, with pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of the putting in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium add charging basket, and adding charging basket is that soft steel or high chromium steel are made, and is thick with a large amount of apertures on it, above-mentioned raw materials is put into preheating oven together with the charging basket that adds that holds these raw materials, be preheating to 100～580 ℃;
(4), with the pure Zn ingot after the preheating, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of in the master alloy of the master alloy of magnesium and rich cerium mixture rare earth and magnesium of pure Ce ingot, cerium-rich mischmetal ingot, Ce submerged in the magnesium melt together with the charging basket that adds that holds these raw materials, be convenient to pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of dissolving and diffusion in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium;
(5), the magnesium melt temperature is controlled at 720～800 ℃, treat Zn, the Mg-Zr master alloy, a kind of in Ag and the Mg-Ag master alloy, and after a kind of dissolving fully in the master alloy of the master alloy of Ce, cerium-rich mischmetal, Ce and magnesium and rich cerium mixture rare earth and magnesium, taking-up adds charging basket, 730～800 ℃ of insulations 10～60 minutes, all alloying elements is evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, according to the composition of sample and content decision reinforced adjustment the whether, reaches the composition and the content of the described magnesium alloy of claim 1 until the magnesium alloy liquation;
(6), the magnesium alloy liquation is poured in the permanent mold casting mould of preheating or the sand mold casting mould and is frozen into foundry goods; Perhaps the magnesium alloy liquation is poured in extrusion casting machine or the pressure die-casting machine in batches extrusion casting or be cast into foundry goods according to casting weight; Perhaps adopt low-pressure casting process that the magnesium alloy liquation is cast as foundry goods;
(7), the foundry goods of above-mentioned steps preparation is carried out solution treatment, its solution treatment process is foundry goods to be heated to 470～540 ℃, insulation 3～30 hours, hardening;
(8), the foundry goods after the solution treatment is carried out ageing treatment, its timeliness treating processes is that foundry goods was heated to 170～250 ℃, insulation 2～46 hours.
8, a kind of method for preparing heat conductive magnesium alloy, this method comprises the steps:
(1), with pure magnesium ingot, pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium be raw material, gets the raw materials ready by the weight percent of the composition of the described magnesium alloy of claim 1; Wherein, cerium-rich mischmetal be the content of Ce more than 40 weight %, all the other are Nd, La and Pr rare earth element;
(2), pure magnesium ingot is piled up in the fusion crucible in smelting furnace, fusing fully is controlled at 680～800 ℃ with the magnesium melt temperature under the protection of shielding gas, the scum silica frost of molten surface is cleaned out, and fed shielding gas to smelting furnace;
(3), preheating oven is warmed up to 160～580 ℃, with pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of the putting in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium add charging basket, and adding charging basket is that soft steel or high chromium steel are made, and is thick with a large amount of apertures on it, above-mentioned raw materials is put into preheating oven together with the charging basket that adds that holds these raw materials, be preheating to 100～580 ℃;
(4), with the pure Zn ingot after the preheating, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of in the master alloy of the master alloy of magnesium and rich cerium mixture rare earth and magnesium of pure Ce ingot, cerium-rich mischmetal ingot, Ce submerged in the magnesium melt together with the charging basket that adds that holds these raw materials, be convenient to pure Zn ingot, the Mg-Zr master alloy, a kind of in pure Ag ingot and the Mg-Ag master alloy, and a kind of dissolving and diffusion in the master alloy of the master alloy of pure Ce ingot, cerium-rich mischmetal ingot, Ce and magnesium and rich cerium mixture rare earth and magnesium;
(5), the magnesium melt temperature is controlled at 720～800 ℃, treat Zn, the Mg-Zr master alloy, a kind of in Ag and the Mg-Ag master alloy, and after a kind of dissolving fully in the master alloy of the master alloy of Ce, cerium-rich mischmetal, Ce and magnesium and rich cerium mixture rare earth and magnesium, taking-up adds charging basket, 730～800 ℃ of insulations 10～60 minutes, all alloying elements is evenly distributed in the magnesium melt again; Afterwards, cast spectrum sample carries out on-the-spot sample analysis, according to the composition of sample and content decision reinforced adjustment the whether, reaches the composition and the content of the described magnesium alloy of claim 1 until the magnesium alloy liquation;
(6), the magnesium alloy liquation is poured into is frozen into the billet of using for follow-up deformation processing in the permanent mold casting mould of preheating or the sand mold casting mould, perhaps the magnesium alloy liquation is transported in the crystallizer, carry out continuous or semicontinuous casting, be prepared into the billet of using for follow-up deformation processing;
(7), the billet with the above-mentioned steps preparation carries out homogenizing thermal treatment, its homogenizing heat treatment process is that billet is heated to 350～500 ℃, is incubated 3～30 hours, directly adopt rolling, extruding, drawing or forging process deformation processing to become sheet material, tubing, section bar, bar, wire rod or various forging then, promptly adopt extruding or drawing process that the billet deformation processing is become bar or wire rod, or billet is processed into sheet material with rolling deformation, or adopt crimp that billet is processed into tubing or section bar, or adopt forging press that billet is forged into forging;
(8), sheet material, tubing, section bar, bar, wire rod or various forging that deformation processing is become carry out ageing treatment, its timeliness treating processes is that sheet material, tubing, section bar, bar, wire rod or various forging were heated to 155～235 ℃, insulation 2～36 hours.
9, according to claim 7 or the 8 described methods that prepare heat conductive magnesium alloy; it is characterized in that: in described step (2); pure magnesium ingot melts under the protection of shielding gas; be evenly to sprinkle SULPHUR POWDER in crucible bottom and pure magnesium ingot surface; the amount of SULPHUR POWDER can all change into sulfurous gas with the oxygen in the crucible after with oxidizing fire and be as the criterion; with crucible cover that crucible is airtight; heat temperature raising; make the fusing fully under the remaining protection of nitrogen gas of sulfurous gas and burning back of whole pure magnesium ingots, open crucible cover again.
10, the method for preparing heat conductive magnesium alloy according to claim 9 is characterized in that: in described step (2), the shielding gas that feeds to smelting furnace is for containing 0.2～0.5 volume %SF
6N
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