CN105177384A - Mg-RE-Zr system multielement magnesium alloy and preparation method thereof - Google Patents
Mg-RE-Zr system multielement magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Mg-RE-Zr system multielement magnesium alloy and a preparation method thereof. The magnesium alloy comprises, by weight, 0.5%-6% of RE, 0.4%-0.8% of Zr, 0.001%-2% of Zn, 0.001%-1% of Ca, and the balance Mg. The magnesium alloy is prepared by taking Mg-RE intermediate alloy, Mg-Zr intermediate alloy and pure Mg ingots as raw materials and adding pure ingots or intermediate alloy containing three elements including Ca and Zn. According to the magnesium alloy, under the condition of 25 DEG C, the thermal conductivity after aging is larger than 100 W/(m*K), the corrosion rate in a 72-hour standard neutral salt spray test is smaller than 1 mg/cm<2>*D, the tensile strength of cast ingots is 140-190 MPa, the yield strength is larger than 100 MPa, and the percentage of elongation is larger than 4%.
Description
Technical field
The present invention relates to a kind of magnesium alloy and manufacture method thereof, be specifically related to a kind of Mg-RE-Zr system complex magnesium alloy and preparation method thereof, belong to metal material field.
Background technology
The heat sink material that aerospace, automobile and 3C Product use not only requires to have good heat conductivility, and requires that density is low, intensity is high.Under room temperature, the thermal conductivity of (20 DEG C) pure magnesium is 156W/ (mK), and after magnesium carries out alloying, its intensity increases substantially, and thermal conductivity is different with the alloying element added, and it is also slightly different, totally on a declining curve that it reduces degree.Commercial magnesium alloy Mg-Al system AZ91, AM60B, AZ80 over-all properties is well found broad application, but its room temperature (20 DEG C) thermal conductivity is less than 61W/ (mK); WE cording has excellent mechanical property, can carry out Die Casting, but its 20 DEG C of room temperature thermal conductivities of WE43, WE91, EW75 are all less than 51W/ (mK); Common Mg-Zn system, room temperature thermal conductivity (20 DEG C) as ZK60, ZE41A, ZC63A is all greater than 100W/ (mK), show that the thermal conductivity impact of the Zn element in Mg-Zn system on pure Mg is more slow, as contained Zn alloy CN101709418A (a kind of heat conductive magnesium alloy and preparation method thereof), thermal conductivity when 20 DEG C is greater than 100W/ (mK); But Mg-Zn system freezing range is large, coarse grains, and easy to crack in the course of processing, the Mg-Zn alloy for die casting does not almost have.And RE alloy melt decontamination effect improving is outstanding, can improve the mobility of magnesium alloy, it declines impact not quite (ZE41, thermal conductivity when 20 DEG C is 123.1W/ (mK)) to room temperature thermal conductivity, therefore, Mg-RE-Zn alloy is the important goal of die casting high thermal conductivity alloy research.
But, Mg-RE diecast magnesium alloy poor corrosion resistance, wherein impurity element Ni Co Fe the galvanic corrosion that causes of Cu be an important factor.Adding appropriate alloying element by the impurity element displacement in melt, is a direction of improving alloy corrosion resistance to improve the purity of melt.Ca element not only can reduce its concentration with impurity element reaction, can also play the effect of grain refining, improve mechanical property, and it is more slow to reduce degree to magnesium alloy thermal conductivity; Zn and Mg has identical hcp structure, has very strong Precipitation effect, and a small amount of Zn obviously can strengthen the tensile strength of Mg-RE; Therefore can to attempt in Mg-RE alloy corrosion-resistantly adding with the requirement of mechanical property Ca one or more in Zn.Zr element is then proved to be can remarkable refinement Mg-RE system alloy, is the excellent alterant of Mg-RE alloy.Therefore the thought of this patent is basis with Mg-RE-Zr, according to different performance requriements choose reasonable Zn one or more in Ca, to prepare the diecast magnesium alloy of high heat-conducting and corrosion-resistant.
Summary of the invention
An object of the present invention is to provide a kind of thermal conductivity and the high and corrosion resistant magnesium alloy of specific tenacity, this magnesium alloy materials is under 25 DEG C of conditions, and thermal conductivity is greater than 100W/ (mK), is less than 1g/cm in the erosion rate of 72 hours standard salt fog test
2, ingot casting tensile strength 140 ~ 190MPa, yield strength is greater than 100MPa, and unit elongation is greater than 4%, can be used as the cooling system structure material of electron device, also can be used for all to corrosive nature and the high occasion of heat conductivility requirement.The technical scheme had is as follows:
A kind of Mg-RE-Zr system complex magnesium alloy, composition is as follows:
The content of RE be 0.5 ~ 6wt.%, RE be selected from La Nd Ce Pr Sm one or more arbitrary combination in Y;
The content of Zr is 0.4 ~ 0.8wt.%;
The content of Zn is 0.001 ~ 2wt.%;
The content of Ca is 0.001 ~ 1wt.%;
All the other are Mg and inevitable impurity element.
Another object of the present invention is to provide a kind of thermal conductivity and all higher and preparation method of corrosion resistant magnesium alloy of intensity.The technical scheme had is as follows:
A preparation method for Mg-RE-Zr system complex magnesium alloy, comprises the steps:
(1) under protective atmosphere, pure magnesium ingot melts obtain magnesium melt completely, and the temperature of magnesium melt controls between 700 ~ 780 DEG C;
(2) magnesium melt temperature remains on more than 700 DEG C, and the raw material of Zr element is added magnesium melt, obtains the second alloy molten solution;
(3) second alloy molten solution temperature remain on more than 710 DEG C, the raw material of the raw material of Zn element, Ca element, the raw material of RE element are added the second alloy molten solution, obtains the 3rd alloy molten solution; RE be selected from La Nd Ce Pr Sm one or more combination in Y;
(4) the 3rd alloy molten solution temperature remain on more than 730 DEG C, refining agent are added the 3rd alloy molten solution, continue to spread refining flux at the liquid level of the 3rd alloy molten solution, until specular gloss appears in liquid level, obtain the 4th alloy molten solution while stirring;
(5) remove the refining solvent on the liquid level of the 4th alloy molten solution and scum silica frost, sprinkle insulating covering agent at liquid level; Leave standstill cooling, treat that impurity fully floats or sinks, removing impurity, obtains the 5th alloy molten solution;
Be poured in fully preheated metal casting mould after (6) the 5th alloy molten solutions are adjusted to suitable temp and be frozen into foundry goods; Or the 5th alloy molten solution is poured in pressure die-casting machine carries out high-pressure casting or low-pressure casting produces die casting; Or extrusion production magnesium alloy member is carried out after the 5th alloy molten solution cooled and solidified; Or be rolled after the 5th alloy molten solution cooled and solidified, forge.
Preferably, pure magnesium ingot melts completely in well formula resistance crucible furnace.
Preferably, shielding gas is SF
6and N
2.
Preferably, in step (2), the raw material of Zr element is Mg-Zr master alloy.
Preferably, the raw material of Zn element is pure Zn ingot in step (3), and the raw material of Ca element is the raw material of Mg-Ca master alloy or pure Ca, RE element is Mg-RE master alloy.
More preferably, pure Zn ingot, Mg-Ca master alloy and Mg-RE master alloy are preheated to suitable temp, then add in the second alloy molten solution, insulation for some time is until pure Zn ingot, Mg-Ca master alloy and Mg-RE master alloy all melt.
Preferably, in step (6), the 5th alloy molten solution is poured in pressure die-casting machine and carries out high-pressure casting or low-pressure casting production die casting, concrete steps are: by die heater, the temperature of die-cast metal mould is adjusted to more than 160 DEG C, adjustment low speed speed is to suitable, and high speed speed is 2 ~ 10m/s, and joint face casting pressure is 60 ~ 100Mpa, 5th alloy molten solution is poured into injection mouth, determine each to water fluence according to the volume size of mould product, then carry out injection, obtain die casting.
Advantage of the present invention is: this high heat conduction die casting Corrosion resistant magnesium alloy material is under 25 DEG C of conditions, and thermal conductivity is greater than 100W/ (mK), is less than 1g/cm in the erosion rate of 72 hours standard salt fog test
2, tensile strength 140MP ~ 190MPa, yield strength is greater than 100MPa, and unit elongation is greater than 4%, can be used as the cooling system structure material of electron device and require high occasion for corroding.This high heat conduction die casting corrosion-resistant magnesium alloy is simply shaping, can Die Casting thin-wall part.
Be described further below with reference to the technique effect of accompanying drawing to design of the present invention, concrete structure and generation, to understand object of the present invention, characteristic sum effect fully.
Accompanying drawing explanation
Fig. 1 is the stress strain curve of complex magnesium alloy prepared by a preferred embodiment of the present invention;
Fig. 2 is the metallograph of complex magnesium alloy prepared by a preferred embodiment of the present invention;
Fig. 3 is the thermal capacitance curve of complex magnesium alloy prepared by a preferred embodiment of the present invention.
Embodiment
It is below the embodiment of invention.The example done in embodiment, only as example, object of protection involved in the present invention, is not limited to example, comprises all by the alloying constituent configured in claims and illustrated working method.
Embodiment 1:25 kilogram of Mg-1Nd-1Y-0.5Zr height heat conduction die casting corrosion-resistant magnesium alloy (namely the component content of this magnesium alloy is: 2wt.%RE, 0.5wt.%Zr, and surplus is Mg and other inevitable impurity elements) and diecast parts preparation method thereof.
1, get the raw materials ready:
Consider that suitable burn out rate is got the raw materials ready according to weight percent, preheating is carried out to Mg-30wt.%Zr master alloy, Mg-wt.90%Nd master alloy and Mg-25wt.%Y master alloy.The purity of master alloy is 99.9wt.%, and except RE element and inevitable impurity, other element is pure Mg.
2, pure magnesium ingot fusing
Put whole pure magnesium ingot into well formula electrical crucible in mode closely of trying one's best, sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface uniform.With crucible cover by crucible, pass into by SF
6and N
2the shielding gas of composition, heat temperature raising, makes whole pure magnesium ingot melt completely under sulfurous gas and shielding gas, magnesium melt temperature is controlled at 700 ~ 780 DEG C;
3, alloying element Nd, Y is added
Alloying element Nd Y by adding Mg-25wt.%Y and Mg-90wt.%Nd master alloy to realize.Magnesium liquid temp rises to more than 700 DEG C, is joined in magnesium melt by preheated Mg-RE master alloy in batches, and insulation is until master alloy all melts;
4, alloy element Zr is added
Magnesium liquid temp rises to more than 710 DEG C, adds in above-mentioned magnesium melt respectively by the Mg-30%Zr master alloy after preheating, and insulation is until an alloy all melts;
5, magnesium alloy refining
Magnesium liquid temp rises to more than 730 DEG C, starts to add the special refining agent of magnesium alloy and carries out refining.In refining process, refining spoon immerses 2/3 place of liquid magnesium alloy, and the fierce aluminium alloy of stirring is from top to bottom till specular gloss appears in liquid level.In stirring, constantly on alloy liquid level, spread refining flux.Refining is complete, removes the solvent on liquid level and scum silica frost, then sprinkles one deck insulating covering agent gently.Cooling to optimal temperature leaves standstill until be mingled with and fully float or sink, after skim;
6, magnesium alloy high-pressure casting
High heat conduction die casting corrosion-resistant magnesium alloy temperature good for refining is adjusted to suitable teeming temperature; Abundant preheating die-cast metal mould; Adjustment pressure die-casting machine parameter is to optimum: if setting low speed speed is 0.1 ~ 0.6m/s, high speed speed is 1 ~ 8m/s, and casting pressure is 60 ~ 110MPa.Die-casting technological parameter should according to the practical situation of pressure die-casting machine, to advance adjustment, until obtain qualified die casting within the scope of above-mentioned die-casting technological parameter to die-casting technological parameter.
Volume size according to mould product determines each liquid inlet volume, high heat conduction die casting corrosion-resistant magnesium alloy liquid is poured into injection mouth and carries out injection, namely obtains high heat conduction die casting corrosion-resistant magnesium alloy die casting.
Mg-1Nd-1Y-0.5Zr height heat conduction die casting Corrosion resistant magnesium alloy material tensile strength of the present invention is 164.6MPa, yield strength is greater than 100MPa, unit elongation is 9.7%, its die casting appearance component and stress strain curve and metallographic are shown in Fig. 1, die casting complete appearance, without cracking, average grain size is 15-20um.
Fig. 1 is the stress strain curve of Mg-1Nd-1Y-0.5Zr prepared by the present embodiment, and Fig. 2 is the metallograph of Mg-1Nd-1Y-0.5Zr prepared by the present embodiment.
Fig. 3 is room temperature (25 DEG C) the thermal capacitance curve of Mg-1Nd-1Y-0.5Zr prepared by the present embodiment, surveys its density be about 1.83g/cm with Archimedes method
3, can use as dissipation from electronic devices structural part completely.
Embodiment 2-3:
25 kilograms of Mg-2Nd-1Y-0.5Zr and Mg-3Y-1Nd-0.5Zr are respectively prepared in an identical manner.Record both yield strengths and be all greater than 120Mpa, tensile strength is all greater than 170Mpa, and unit elongation is all greater than 6%, and 25 DEG C of thermal conductivities are all greater than 100W/ (mK).72h standard Neutral salt-fog test records erosion rate and is less than 1mg/cm
2.D, wherein, Mg-2Nd-1Y-0.5Zr erosion rate, close to commercial AZ91, has excellent over-all properties.
Embodiment 4:
(namely the component content of this magnesium alloy is 25 kilograms of Mg-2Nd-1Y-0.1Ca-0.5Zr height heat conduction die casting corrosion-resistant magnesium alloys: 2wt.%Nd, 1wt.%Y, 0.1wt.%Ca and 0.5wt.%Zr, surplus is inevitable impurity and Mg element) and diecast parts preparation method.
1, consider that suitable burn out rate is got the raw materials ready according to weight percent, preheating is carried out to Mg-30wt.%Zr master alloy, Mg-wt.90%Nd master alloy and Mg-25wt.%Y master alloy and Mg-30wt.% master alloy.The purity of master alloy is 99.9wt.%, and except RE element and inevitable impurity, other element is pure Mg.
2, pure magnesium ingot fusing
Put whole pure magnesium ingot into well formula electrical crucible in mode closely of trying one's best, sprinkle some SULPHUR POWDER in crucible bottom and pure magnesium ingot surface uniform.With crucible cover by crucible, pass into by body SF
6and N
2the shielding gas of composition, heat temperature raising, makes whole pure magnesium ingot melt completely under sulfurous gas and shielding gas, magnesium melt temperature is controlled at 700 ~ 780 DEG C;
3, alloying element Nd, Y is added
Alloying element Nd Y Ca by adding Mg-25wt.%Y, Mg-90wt.%Nd and Mg-30wt.%Ca master alloy to realize.Magnesium liquid temp rises to more than 700 DEG C, joins in magnesium melt by preheated Mg-RE master alloy and Mg-Ca master alloy, and insulation is until master alloy all melts;
4, alloy element Zr is added
Magnesium liquid temp rises to more than 710 DEG C, adds in above-mentioned magnesium melt respectively by the Mg-30%Zr master alloy after preheating, and insulation is until an alloy all melts;
5, magnesium alloy refining
Magnesium liquid temp rises to more than 730 DEG C, starts to add the special refining agent of magnesium alloy and carries out refining, and in refining process, refining spoon immerses 2/3 place of liquid magnesium alloy, and the fierce aluminium alloy of stirring is from top to bottom till specular gloss appears in liquid level.In stirring, constantly on alloy liquid level, spread refining flux.Refining is complete, removes the solvent on liquid level and scum silica frost, then sprinkles one deck insulating covering agent gently.Temperature is down to and is mingled with abundant floating or sinking standing the making of optimal temperature, skims;
6, magnesium alloy high-pressure casting
High heat conduction die casting corrosion-resistant magnesium alloy temperature good for refining is adjusted to suitable teeming temperature; Abundant preheating die-cast metal mould; Adjustment pressure die-casting machine parameter is to optimum: if setting low speed speed is 0.1 ~ 0.6m/s, high speed speed is 1 ~ 8m/s, and casting pressure is 60 ~ 110MPa.Die-casting technological parameter should according to the practical situation of pressure die-casting machine, to advance adjustment, until obtain qualified die casting within the scope of above-mentioned die-casting technological parameter to die-casting technological parameter.
Volume size according to mould product determines each liquid inlet volume, high heat conduction die casting corrosion-resistant magnesium alloy liquid is poured into injection mouth and carries out injection, namely obtains high heat conduction die casting corrosion-resistant magnesium alloy die casting.
Mg-2Nd-1Y-0.1Ca-0.5Zr height heat conduction die casting Corrosion resistant magnesium alloy material die cast of the present invention is good, and accessory appearance is complete without cracking.Under 25 DEG C of conditions, thermal conductivity is 104.3W/ (mK), is less than 1g/cm in the erosion rate of 72 hours standard salt fog test
2, tensile strength is greater than 150MPa, and yield strength is greater than 130MPa, and unit elongation is greater than 4%, can be used as the cooling system structure material of electron device.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (8)
1. a Mg-RE-Zr system complex magnesium alloy, is characterized in that, the composition of described magnesium alloy is as follows:
The content of RE be 0.5 ~ 6wt.%, RE be selected from La Nd Ce Pr Sm one or more combination in Y;
The content of Zr is 0.4 ~ 0.8wt.%;
The content of Zn is 0.001 ~ 2wt.%;
The content of Ca is 0.001 ~ 1wt.%;
All the other are Mg and inevitable impurity element.
2. the preparation method of a kind of Mg-RE-Zr system according to claim 1 complex magnesium alloy, is characterized in that, comprise the steps:
(1) under protective atmosphere, pure magnesium ingot melts obtain magnesium melt completely, and the temperature of described magnesium melt controls between 700 ~ 780 DEG C;
(2) described magnesium melt temperature remains on more than 700 DEG C, and the raw material of Zr element is added described magnesium melt, obtains the second alloy molten solution;
(3) described second alloy molten solution temperature remains on more than 710 DEG C, and one or more in the raw material of the raw material of the raw material of Zn element, Ca element, RE element are added described second alloy molten solution, obtains the 3rd alloy molten solution; Wherein said RE element be selected from La Nd Ce Pr Sm one or more arbitrary combination in Y;
(4) described 3rd alloy molten solution temperature remains on more than 730 DEG C, refining agent is added described 3rd alloy molten solution, continue while stirring to spread refining flux at the liquid level of described 3rd alloy molten solution, until specular gloss appears in liquid level, obtain the 4th alloy molten solution;
(5) remove the refining solvent on the liquid level of described 4th alloy molten solution and scum silica frost, sprinkle insulating covering agent at described liquid level; Leave standstill cooling, treat that impurity fully floats or sinks, remove described impurity, obtain the 5th alloy molten solution;
(6) be poured in fully preheated metal casting mould after described 5th alloy molten solution is adjusted to suitable temp and be frozen into foundry goods; Or described 5th alloy molten solution is poured in pressure die-casting machine carries out high-pressure casting or low-pressure casting produces die casting; Or extrusion production magnesium alloy member is carried out after described 5th alloy molten solution cooled and solidified; Or be rolled after described 5th alloy molten solution cooled and solidified, forge.
3. the preparation method of a kind of Mg-RE-Zr system according to claim 2 complex magnesium alloy, is characterized in that, described pure magnesium ingot melts completely in well formula resistance crucible furnace.
4. the preparation method of a kind of Mg-RE-Zr system according to claim 2 complex magnesium alloy, it is characterized in that, described shielding gas is SF
6and N
2.
5. the preparation method of a kind of Mg-RE-Zr system according to claim 2 complex magnesium alloy, it is characterized in that, described in step (2), the raw material of Zr element is Mg-Zr master alloy, add in described magnesium melt after described Mg-Zr master alloy is preheated to suitable temp, insulation for some time is until described Mg-Zr master alloy all melts.
6. the preparation method of a kind of Mg-RE-Zr system according to claim 2 complex magnesium alloy, it is characterized in that, the raw material of Zn element described in step (3) is pure Zn ingot, the raw material of described Ca element is Mg-Ca master alloy or pure Ca, and the raw material of described RE element is Mg-RE master alloy.
7. the preparation method of a kind of Mg-RE-Zr system according to claim 6 complex magnesium alloy, it is characterized in that, the raw material of described Ca element is Mg-Ca master alloy, described pure Zn ingot, described Mg-Ca master alloy and described Mg-RE master alloy are preheated to suitable temp, then add in described second alloy molten solution, insulation for some time is until described pure Zn ingot, described Mg-Ca master alloy and described Mg-RE master alloy all melt.
8. the preparation method of a kind of Mg-RE-Zr system according to claim 2 complex magnesium alloy, it is characterized in that, in step (6), described 5th alloy molten solution is poured in pressure die-casting machine and carries out high-pressure casting or low-pressure casting production die casting, concrete steps are: by die heater, the temperature of die-cast metal mould is adjusted to more than 160 DEG C, adjustment low speed speed is to suitable, high speed speed is 2 ~ 10m/s, joint face casting pressure is 60 ~ 100Mpa, described 5th alloy molten solution is poured into injection mouth, determine each to water fluence according to the volume size of mould product, then injection is carried out, obtain described die casting.
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| CN107475589A (en) * | 2017-08-08 | 2017-12-15 | 上海大学 | Rare earth and magnesium-based alloys of Mg La Zr and preparation method thereof |
| CN107541631A (en) * | 2016-06-29 | 2018-01-05 | 北京美中双和医疗器械股份有限公司 | A kind of biological medical degradable corrosion-proof and high-strength tough magnesium alloy and preparation method thereof |
| CN110284035A (en) * | 2019-08-07 | 2019-09-27 | 中国科学院长春应用化学研究所 | A kind of heat resistance magnesium alloy and preparation method thereof |
| CN110468319A (en) * | 2019-08-13 | 2019-11-19 | 中国兵器科学研究院宁波分院 | A kind of novel Mg-Y-Nd- (La+Ce)-Zr biodegradable magnesium alloy and preparation method thereof |
| CN111364066A (en) * | 2018-12-25 | 2020-07-03 | 有研工程技术研究院有限公司 | Short-process preparation method of rare earth magnesium alloy |
| CN114635068A (en) * | 2022-03-11 | 2022-06-17 | 上海交通大学 | High-strength and high-toughness cast magnesium rare earth alloy and preparation method thereof |
| CN115961196A (en) * | 2022-10-19 | 2023-04-14 | 厦门大学 | System for improving corrosion resistance of AZ magnesium alloy and preparation method thereof |
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Application publication date: 20151223 |