CN105568104A - Rare earth strengthened magnesium alloy and preparation method thereof - Google Patents
Rare earth strengthened magnesium alloy and preparation method thereof Download PDFInfo
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- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses rare earth strengthened magnesium alloy and a preparation method thereof. According to the rare earth strengthened magnesium alloy and the preparation method thereof, nanoscale silicon carbide and rare earth element niobium are mixed into magnesium alloy, and high-strength magnesium-zinc alloy is obtained. The magnesium-zinc alloy is composed of the elements of magnesium, zinc and niobium and the nanoscale silicon carbide. The atom ratio of the magnesium to the zinc is between 3:1 and 1.5:1. The mass percentage content of the element niobium is 1%-5%. The average diameter of the silicon carbide is 200 nanometers or less. The average crystal size of the magnesium-zinc alloy is 80 nanometers or less, the yield strength of the magnesium-zinc alloy is 500 MPa or above, and the elongation of the magnesium-zinc alloy is 38% or above. The magnesium-zinc alloy is prepared through the steps of smelting, nano-particle mixing and dispersing, cooling, distorting, asymmetrical rolling and the like.
Description
Technical field
The present invention relates to a kind of high-strength high-ductility magnesium alloy and preparation method thereof, high-performance magnesium-zinc alloy that especially a kind of rare earth strengthens and preparation method thereof.
Background technology
Magnesium alloy is applied at present in the fields such as hand-hold electronic equipments, automobile, aerospace.Magnesium be a kind of density very little metallic substance, as engineering materials, people expect the material of high strength usually, but processing means traditional at present can not obtain the magnesium alloy of high strength.
Chinese patent 104109790A provides a kind of high-strength magnesium alloy material and preparation method thereof, comprises aluminium (Al) in this magnesium alloy materials component, zinc (Zn), Manganous chloride tetrahydrate (MnCl
2), silicon carbide (SiC) crystal grain, beryllium (Be), magnesium (Mg), wherein, each component composition of magnesium alloy materials is respectively by weight percentage: aluminium (Al): 10.5-12%, zinc (Zn): 6-7%, Manganous chloride tetrahydrate (MnCl
2): 0.6-1.5%, silicon carbide (SiC) crystal grain: 2-3.5%, beryllium (Be): 0.01-0.03%, surplus is magnesium (Mg).This alloy replaces traditional extrusion process by the mode of continuous casting, the production of magnesium alloy is completed in the mode of short route, shorten Production Flow Chart, save cost, prepared magnesium alloy materials compared to traditional magnesium alloy materials, in tensile strength, yield strength, unit elongation, Young's modulus, hardness etc. all be improved significantly.
Chinese patent 102766774A provides a kind of Enhancement Method of magnesium alloy doped SIC particle, the situation low for magnesium alloy modulus, intensity is low, easy to wear, resistance to elevated temperatures is poor, thermal expansivity is high, adopt adulterate in Melting Magnesium alloy block process thin silicon carbide and thick silicon-carbide particle, then carry out casting, pressurizeing and hot extrusion molding, increase substantially the yield strength of magnesium alloy, hardness and wear resisting property, yield strength is made to reach 328MPa ± 2MPa, hardness reaches 120HV ± 5HV, and wear resistance improves 80%.
Chinese patent 104213008A discloses a kind of novel high-strength magnesium alloy and preparation method thereof.Its composition weight percent is: tungsten-titanium alloy is 5% ~ 35%, and magnalium is 65% ~ 95%.Adding of tungsten-titanium alloy, improve solid solution and the ag(e)ing behavio(u)r of magnalium, improve its structure and properties.Its tensile strength and yield strength are respectively (486 ~ 378) MPa and (400 ~ 320) MPa, compare 320MPa and 269MPa of magnalium, improve 52% ~ 18% and 48% ~ 18% respectively.
Chinese patent 101177752 proposes a kind of magnesium-zinc-lanthanon alloy containing zinc 4.5% and preparation method thereof, particularly relates in magnesium-zincium-rare earth system to add Magnuminium of heavy rare earth yttrium or gadolinium and light rare earths lanthanum or neodymium and preparation method thereof.The magnesium-zinc-lanthanon alloy of interpolation four kinds of rare earths that this invention provides is respectively MG-4.5WT%ZN-(0.2WT% ~ 2WT%) LA; MG-4.5WT%ZN-(0.2WT% ~ 2WT%) ND; MG-4.5WT%ZN-(0.2WT% ~ 4.8WT%) GD and MG-4.5WT%ZN-(0.2WT% ~ 2.8WT%) Y, can solve the problem of industrial alternative magnesium-zincium-rare earth system alloy kind few and rare earth resources Selection utilization or alternative usability difference.But, its yield strength is at below 200MPa.
More than invent the performance particularly strength property being all devoted to improve magnesium alloy, but the yield strength of magnesium alloy prepared by current techniques is all at below 400MPa, and its intensity and current long engineering materials also have larger gap.
Summary of the invention:
Goal of the invention: in order to expand the Application Areas of magnesium alloy, plays its low-density advantage, the invention provides high-strength magnesium alloy of a kind of rare earth enhancing and preparation method thereof.
Technical scheme of the present invention is as follows:
By the melting in a vacuum of magnesium, zinc, niobium, SiC nano particle is mixed in the process of melting, be uniformly dispersed, Slow cooling also vacuumizes and allows nano particle improve concentration further, then the mode of torsional deformation is under high pressure adopted, adopt asymmetrical rolling again, further crystal grain thinning, put forward heavy alloyed intensity.According to the present invention, a kind of high-strength magnesium-zinc alloy can be prepared.Average crystal grain diameter in its microstructure below 80 nanometers, the diameter of nano particle below 200 nanometers, the yield strength of magnesium-zinc alloy at more than 500MPa, unit elongation more than 38%.
Concrete preparation method comprises the following steps:
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the nano SiC of below 200 nanometers;
(2) molten alloy: by magnesium, zinc, niobium according to certain atomic ratio batching, melting in protective atmosphere, adds nano SiC in fusion process, maintains the temperature at 700 ° of C, adopts ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, and keep vacuumizing state in the process of cooling, low vacuum is in 5torr;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies high pressure, and rotates pressure anvil to reverse alloy disks, makes it the deformation that is distorted;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.1-1.5; Setting each rolling deformation amount is 1-8%; The speed of setting low speed roller is 0.5-2 meter per second;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (2) (3) process more than 15 times is repeated;
(9) full annealed thermal treatment is carried out.
Wherein, the shielding gas in step (1) is CO
2with the mixed gas of SF6, in step (3), speed of cooling is less than 0.5k per second; The pressure that step (5) interalloy bears is 1.5-5GPa; Speed of rotation per minute 2 ~ 5 turns, rotates altogether 3-20 circle; Rolling temperature in step (8) is room temperature: the recrystallization temperature in step (9) is 1/3 ~ 1/4 of the fusing point of magnesium, time 3-20 minute.
As preferably, CO
250:1 ~ 100:1 with the scope of the volume ratio of SF6.
As preferably, the atomic ratio of high purity magnesium and zinc is 3 ~ 6:1.
As preferably, the mass percentage of the niobium added is 1 ~ 5%.
As preferably, the massfraction of the SiC particle added in step (2) is 1.5 ~ 5%.
As preferably, the granularity average out to 60-120 nanometer of the silicon carbide adopted.
Useful effect:
The present invention adopts the particle of the nanometer silicon carbide of high strength as enhanced granule, not only can play the effect of crystal grain thinning, and as the obstacle of dislocation motion, can stop the dislocation moving of metal, thus reinforced metal; Meanwhile, crystal grain thinning can play the effect improving alloy plasticity.
The present invention additionally uses rare earth element niobium as enhancing element.Niobium defines rare earth precipitated phase in the magnesium alloy, can play the effect of pinning dislocation, crystal grain thinning further, thus strengthens the intensity of alloy.
The present invention carries out ultrasonic disperse under adopting high temperature metal liquid state, efficiently solves nano particle and is difficult to finely dispersed problem in a metal.Ultrasonic disperse is used under liquid metal state, can be even by nanoparticulate dispersed, to solve the defect that in the technology such as conventional hybrid, stirring, nanoparticulate dispersed is bad.Adopt Slow cooling after melting, keep vacuum tightness simultaneously, the metallic vapor of magnesium can be made constantly to be drawn out of, reduce the content of magnesium in alloy, thus improve the volume fraction of nano particle in alloy, strengthen the effect of reinforced by nanoparticles further.In the present invention, although the magnesium zinc ratio added is 3 ~ 6:1, in the alloy finally obtained, the atomic ratio of magnesium zinc is between 3:1 to 1.5:1.
In the process applying high pressure twist distortion, crystal grain larger in alloy substrate is broken down into more tiny nanocrystal.In addition, the present invention adopts asymmetrical rolling to process further material, this rolling method can crystal grain thinning further, and the distribution of thickness crystal grain can be formed at organization internal, this material structure can reach carries on the back work hardening greatly, and this is non-existent in the material of even grained or the material of conventional machining.The present invention adopts micro Process, multi-pass, is suitable for obtaining destination organization.The average crystal grain diameter of final alloy is generally below 80 nanometers, and according to Hall-join strange relation, crystal grain becomes tiny, and the intensity of alloy can be made higher, meanwhile, also can improve the plasticity of alloy.By magnesium-zinc alloy prepared by the present invention, its yield strength up to more than 500MPa, can possess excellent plasticity simultaneously, and unit elongation, up to more than 38%, can be applied to the field such as automobile, space flight and aviation.
Embodiment
Describe preparation method of the present invention in detail below by embodiment, but be not construed as limiting the invention.
Embodiment 1
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the SiC of 150 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden according to the atomic ratio of 3:1, then adds the niobium accounting for alloy mass mark 3%, at CO
2with melting in the mixed gas of SF6, wherein CO
250:1 with SF6 volume ratio; Add the nano SiC accounting for alloy mass mark 3% in fusion process, maintain the temperature at 700 ° of C, adopt ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, speed of cooling 0.2k per second; Keep vacuumizing state in the process of cooling, low vacuum is in 4torr;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies 2GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 2 turns, make it the deformation that is distorted, rotation 20 is enclosed altogether;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.1; Setting each rolling deformation amount is 8%; The speed of setting low speed roller is 0.5 meter per second;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (6) (7) process 23 times are repeated;
(9) full annealed thermal treatment is carried out at 180 degrees Celsius, 8 minutes time.
Embodiment 2
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the SiC of 90 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden according to the atomic ratio of 6:1, then adds the niobium accounting for alloy mass mark 2%, at CO
2with melting in the mixed gas of SF6, wherein CO
280:1 with SF6 volume ratio; Add the nano SiC accounting for alloy mass mark 1.5% in fusion process, maintain the temperature at 700 ° of C, adopt ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, speed of cooling 0.3k per second; Keep vacuumizing state, vacuum tightness 3torr in the process of cooling;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies 5GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 5 turns, make it the deformation that is distorted, rotation 8 is enclosed altogether;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.1; Setting each rolling deformation amount is 1%; The speed of setting low speed roller is 0.5 meter per second;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (6) (7) process 25 times are repeated;
(9) full annealed thermal treatment is carried out at 200 degrees Celsius, 8 minutes time.
Embodiment 3
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the SiC of 60 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden according to the atomic ratio of 3.5:1, then adds the niobium accounting for alloy mass mark 5%, at CO
2with melting in the mixed gas of SF6, wherein CO
250:1 with SF6 volume ratio; Add the nano SiC accounting for alloy mass mark 1.8% in fusion process, maintain the temperature at 700 ° of C, adopt ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, speed of cooling 0.5k per second; Keep vacuumizing state, vacuum tightness 3torr in the process of cooling;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies 1.5GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 2 turns, make it the deformation that is distorted, rotation 20 is enclosed altogether;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.4; Setting each rolling deformation amount is 3%; The speed of setting low speed roller is 2 meter per seconds;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (6) (7) process 25 times are repeated;
(9) full annealed thermal treatment is carried out at 190 degrees Celsius, 10 minutes time.
Embodiment 4
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the nano SiC of 110;
(2) molten alloy: high purity magnesium and zinc are prepared burden according to the atomic ratio of 5:1, then adds the niobium accounting for alloy mass mark 2%, at CO
2with melting in the mixed gas of SF6, wherein CO
2100:1 with SF6 volume ratio; Add the nano SiC accounting for alloy mass mark 3.2% in fusion process, maintain the temperature at 700 ° of C, adopt ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, speed of cooling 0.2k per second; Keep vacuumizing state, vacuum tightness 4torr in the process of cooling;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies 5GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 2 turns, make it the deformation that is distorted, rotation 3 is enclosed altogether;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.5; Setting each rolling deformation amount is 3%; The speed of setting low speed roller is 2 meter per seconds;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (6) (7) process 20 times are repeated;
(9) full annealed thermal treatment is carried out at 170 degrees Celsius, 20 minutes time.
Embodiment 5
(1) raw material is prepared: prepare high purity magnesium, zinc, the niobium of more than 99.9%, and median size is the SiC of 80 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden according to the atomic ratio of 4:1, then adds the niobium accounting for alloy mass mark 1%, at CO
2with melting in the mixed gas of SF6, wherein CO
280:1 with SF6 volume ratio; Add the nano SiC accounting for alloy mass mark 5% in fusion process, maintain the temperature at 700 ° of C, adopt ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, speed of cooling 0.4k per second; Keep vacuumizing state, vacuum tightness 5torr in the process of cooling;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies 1.5GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 3 turns, make it the deformation that is distorted, rotation 10 is enclosed altogether;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.3; Setting each rolling deformation amount is 2%; The speed of setting low speed roller is 2 meter per seconds;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (6) (7) process 20 times are repeated;
(9) full annealed thermal treatment is carried out at 180 degrees Celsius, 3 minutes time.
Performance Detection: carry out tensile test at room temperature, obtains the yield strength of alloy prepared by each embodiment, unit elongation; Adopt TEM (transmission electron microscope) analysis, obtain the crystal grain diameter of alloy; Atomic absorption spectrochemical analysis is adopted to obtain the atomic ratio of magnesium zinc; Result is as following table:
Can see from upper table, adopt the present invention, the yield strength of prepared magnesium-zinc alloy is at more than 500MPa, and unit elongation, more than 38%, is much higher than prior art level.
The above is only some examples of embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. rare earth strengthens a magnesium alloy, it is characterized in that: this magnesium alloy is made up of magnesium, zinc, niobium element and nanometer silicon carbide; The atomic ratio of magnesium zinc is between 3:1 to 1.5:1; The mass percentage of niobium element is between 1 ~ 5%; The mean diameter of silicon carbide below 200 nanometers, the average crystal grain of magnesium-zinc alloy below 80 nanometers, the yield strength of alloy at more than 500MPa, unit elongation more than 38%.
2. magnesium alloy as claimed in claim 1, its manufacture method comprises following steps:
(1) prepare raw material: the high purity magnesium, high purity zinc, the High-purity Niobium that prepare purity more than 99.9%, and median size is the nano SiC of below 200 nanometers;
(2) molten alloy: by high purity magnesium, zinc, niobium according to certain atomic ratio batching, melting in protective atmosphere, adds nano SiC in fusion process, maintains the temperature at 700 ° of C, adopts ultrasonic method to disperse;
(3) involutory ingot carries out Slow cooling, and keep vacuumizing state in the process of cooling, low vacuum is in 5torr;
(4), after cooling, alloy pig is processed into discoid;
(5) space that the groove coarse-grain alloy disks that step (4) processes being put into upper and lower two pressure anvils is formed, alloy applies high pressure, and rotates pressure anvil to reverse alloy disks, makes it the deformation that is distorted;
(6) start Multi-functional rolling system, the speed ratio of setting top and bottom rolls, speed ratio is 1.1-1.5; Setting each rolling deformation amount is 1-8%; The speed of setting low speed roller is 0.5-2 meter per second;
(7) start main driving motor, start the operation of rolling;
(8), after treating a rolling, (2) (3) process more than 15 times is repeated;
(9) full annealed thermal treatment is carried out.
3. the preparation method of magnesium alloy as claimed in claim 2, is characterized in that: shielding gas is CO
2with the mixed gas of SF6.
4. the preparation method of magnesium alloy as claimed in claim 2, is characterized in that: speed of cooling is less than 0.5k per second.
5. the preparation method of magnesium alloy as claimed in claim 2, is characterized in that: the pressure that alloy bears is 1.5-5GPa, speed of rotation per minute 2 ~ 5 turns.
6. the preparation method of magnesium alloy as claimed in claim 2, is characterized in that: in step (2), the atomic ratio of magnesium and zinc is 3 ~ 6:1.
7. magnesium alloy preparation method as claimed in claim 2, is characterized in that: described rolling temperature is room temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110512129A (en) * | 2019-08-30 | 2019-11-29 | 中南大学 | A kind of forging torsion integrated technique preparing superelevation severe deformation magnesium alloy rod |
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| WO2003046239A1 (en) * | 2001-11-27 | 2003-06-05 | Noranda Inc. | Magnesium-based casting alloys having improved elevated temperature performance, oxydation-resistant magnesium alloy melts, magnesium-based alloy castings prepared therefrom and methods for preparing same |
| CN101569892A (en) * | 2009-05-21 | 2009-11-04 | 上海交通大学 | Method for rolling AZ31 magnesium alloy through asynchronous longitudinal and transverse crossing |
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| CN110512129A (en) * | 2019-08-30 | 2019-11-29 | 中南大学 | A kind of forging torsion integrated technique preparing superelevation severe deformation magnesium alloy rod |
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