CN105463279A - Nanometer enhanced magnesium alloy and preparation method thereof - Google Patents
Nanometer enhanced magnesium alloy and preparation method thereof Download PDFInfo
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- CN105463279A CN105463279A CN201610026103.4A CN201610026103A CN105463279A CN 105463279 A CN105463279 A CN 105463279A CN 201610026103 A CN201610026103 A CN 201610026103A CN 105463279 A CN105463279 A CN 105463279A
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- C22C23/00—Alloys based on magnesium
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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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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
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Abstract
The invention discloses a nanometer enhanced magnesium alloy and a preparation method thereof. A nanometer additive is added into magnesium alloy, and high-strength magnesium alloy is obtained. The average crystalline grain of the magnesium alloy is 100 nanometers or below, the yield strength of the alloy can reach 450 MPa or above. The preparation method comprises the steps of smelting, adding of nanometer particles, dispersion, cooling, distortion, asymmetrical rolling and the like.
Description
Technical field
The present invention relates to a kind of high-strength magnesium alloy and preparation method thereof, especially a kind of nanometer additive strengthens magnesium alloy and preparation method thereof.
Background technology
As aerospace structure material, require that the intensity of material is high on the one hand, require that the density of material is little on the other hand.Magnesium alloy be a kind of density very little metallic substance, but due to the atomic structure feature of magnesium alloy, its plasticity is poor, and current processing means can not obtain the material of high strength.How improving the intensity of magnesium alloy, is the focus of current people research.
Chinese patent CN103031452A discloses a kind of SiC particles reinforced magnesium base composite material and preparation method, this invention for starting material, adopts powder metallurgy and multiway forging legal system for SiC particles reinforced magnesium base composite material with pure Mg powder, Al powder and SiC particle micro mist.By powder metallurgy and multiway forging two kinds of forming methods, make, between magnesium alloy substrate and SiC particle, there is good wetting property and associativity, and eliminate the hole remaining in material internal in powder metallurgy forming process, finally obtain the distribution of SiC uniform particles, the magnesium base composite material that magnesium alloy substrate crystal grain is tiny, makes this matrix material have better mechanical property.The tensile strength of the magnesium alloy of this invention is lower than 200MPa.
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%.
More than invent the performance particularly strength property being all devoted to improve magnesium alloy, the room-temperature yield strength of magnesium alloy has been brought up to MPa more than 300.But, the intensity of the materials such as current iron and steel, titanium alloy, aluminium alloy is general all more than 400 MPas, and the intensity of magnesium alloy and these conventional engineering materialss also have a certain distance.
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 a kind of high-strength magnesium alloy and preparation method thereof.
Technical scheme of the present invention is as follows:
Adopt the method at nano-particle reinforcement, in the process of melting, in magnesium alloy, mix additive, be uniformly dispersed, Slow cooling also vacuumizes and allows nano particle improve concentration further, then under high pressure adopt the mode of torsional deformation, further crystal grain thinning, put forward heavy alloyed intensity.According to the present invention, a kind of high-strength magnesium alloy of nano-particle reinforcement can be prepared.Average crystal grain diameter in its microstructure is below 60 nanometers, and the diameter of nano particle is below 100 nanometers, and the yield strength of magnesium alloy is at more than 450MPa.
Concrete preparation method comprises the following steps:
(1) raw material is prepared: prepare high purity magnesium and the high purity alloys element of more than 99.9%, and median size is the nanometer additive of below 100 nanometers;
(2) molten alloy: high purity magnesium and alloying element are prepared burden according to certain atomic ratio, melting in protective atmosphere, adds nanometer additive 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; 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.
Nanometer additive of the present invention is including but not limited to silicon carbide, silicon oxide, titanium oxide; Alloying element of the present invention is including but not limited to zinc, aluminium, copper, iron, manganese, molybdenum, titanium.
As preferably, CO
250:1 ~ 100:1 with the scope of the volume ratio of SF6;
As preferably, the massfraction that the additive particles added in step (2) accounts for alloy is 1.5 ~ 5%;
As preferably, the speed of rotation in step (5) is per minute 2 ~ 5 turns, rotates altogether 3-20 circle.
Useful effect:
The present invention adopts the particle of the nanometer additive 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 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; The content of alloying element also can increase simultaneously.
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 60 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 alloy prepared by the present invention, its yield strength up to more than 450MPa, can be applied to the field such as automotive light weight technology engineering, space flight and aviation engineering.
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 and the high purity zinc of more than 99.9%, and median size is the nano SiC of 90 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden, at CO according to the atomic ratio of 6:1
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 1.5; 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 2
(1) raw material is prepared: prepare high purity magnesium and the high purity zinc of more than 99.9%, and median size is the nano SiC of 80 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden, at CO according to the atomic ratio of 4:1
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 1.4; 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 3
(1) raw material is prepared: prepare high purity magnesium and the rafifinal of more than 99.9%, and median size is the Nano-meter SiO_2 of 80 nanometers
2;
(2) molten alloy: high purity magnesium and zinc are prepared burden, at CO according to the atomic ratio of 3:1
2with melting in the mixed gas of SF6, wherein CO
2100:1 with SF6 volume ratio; The Nano-meter SiO_2 accounting for alloy mass mark 4.2% is added in fusion process
2, 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 4.5GPa 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 3 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 4
(1) raw material is prepared: prepare high purity magnesium and the high purity zinc of more than 99.9%, and median size is the nano-TiO of 80 nanometers
2;
(2) molten alloy: high purity magnesium and copper are prepared burden, at CO according to the atomic ratio of 5:1
2with melting in the mixed gas of SF6, wherein CO
260:1 with SF6 volume ratio; The nano-TiO accounting for alloy mass mark 2.5% is added in fusion process
2, 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 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 3GPa high pressure, and rotate pressure anvil to reverse alloy disks with the speed of per minute 2.5 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 5
(1) raw material is prepared: prepare high purity magnesium and the high purity zinc of more than 99.9%, and median size is the nano SiC of 60 nanometers;
(2) molten alloy: high purity magnesium and zinc are prepared burden, at CO according to the atomic ratio of 3.5:1
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 1.3; 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; Adopt TEM (transmission electron microscope) analysis, obtain the crystal grain diameter of alloy; Result is as following table:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Yield strength (MPa) | 510 | 492 | 492 | 515 | 494 |
| Average crystal grain diameter (micron) | 53 | 52 | 47 | 56 | 46 |
Can see from upper table, adopt the present invention, the yield strength doing the magnesium alloy prepared, at more than 450MPa, 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 (9)
1. nanometer strengthens a magnesium alloy, it is characterized in that: this magnesium alloy is made up of magnesium and alloying element thereof and nanometer additive; The mean diameter of nanometer additive is below 100 nanometers, and the average crystal grain of magnesium alloy is below 60 nanometers.
2. magnesium alloy as claimed in claim 1, its manufacture method comprises following steps:
(1) prepare raw material: the high purity magnesium and the high purity alloys element that prepare purity more than 99.9%, and median size is the nanometer additive of below 200 nanometers;
(2) molten alloy: high purity magnesium and alloying element are prepared burden according to certain atomic ratio, melting in protective atmosphere, adds nanometer additive 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.
3.(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;
Start main driving motor, start the operation of rolling;
After treating a rolling, repeat (2) (3) process more than 15 times;
(9) full annealed thermal treatment is carried out.
4. magnesium alloy as claimed in claim 1, is characterized in that: described nanometer additive is including but not limited to silicon carbide, silicon oxide, titanium oxide.
5. magnesium alloy as claimed in claim 1, is characterized in that: described alloying element is including but not limited to zinc, aluminium, copper, iron, manganese, molybdenum, titanium.
6. 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.
7. 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.
8. 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.
9. 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521222A (en) * | 2016-10-28 | 2017-03-22 | 北京新能源汽车股份有限公司 | Magnesium alloy plate machining method and magnesium alloy plate |
| CN115852181A (en) * | 2022-11-28 | 2023-03-28 | 重庆大学 | Preparation method of micron-sized titanium particle reinforced magnesium-based composite material |
-
2016
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521222A (en) * | 2016-10-28 | 2017-03-22 | 北京新能源汽车股份有限公司 | Magnesium alloy plate machining method and magnesium alloy plate |
| CN106521222B (en) * | 2016-10-28 | 2018-01-19 | 北京新能源汽车股份有限公司 | The processing method and magnesium alloy plate of a kind of magnesium alloy plate |
| CN115852181A (en) * | 2022-11-28 | 2023-03-28 | 重庆大学 | Preparation method of micron-sized titanium particle reinforced magnesium-based composite material |
| CN115852181B (en) * | 2022-11-28 | 2023-09-01 | 重庆大学 | Preparation method of micron-sized titanium particle reinforced magnesium-based composite material |
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