CN105463279B - A kind of nanometer enhances magnesium alloy and preparation method thereof - Google Patents
A kind of nanometer enhances magnesium alloy and preparation method thereof Download PDFInfo
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- CN105463279B CN105463279B CN201610026103.4A CN201610026103A CN105463279B CN 105463279 B CN105463279 B CN 105463279B CN 201610026103 A CN201610026103 A CN 201610026103A CN 105463279 B CN105463279 B CN 105463279B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
A kind of nanometer of enhancing magnesium alloy and preparation method thereof, the present invention have obtained a kind of magnesium alloy of high intensity using nanometer additive is mixed in the magnesium alloy, and the average crystal grain of obtained magnesium alloy is at 100 nanometers hereinafter, the yield strength of alloy is up to more than 450MPa.The magnesium alloy by melting, incorporation nano particle and disperse, cool down, torsional deformation, asymmetrical rolling and etc. be prepared.
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 enhancing magnesium alloy
And preparation method thereof.
Background technology
As aerospace structure material, the intensity on the one hand requiring material is high, and the density on the other hand requiring material is small.
Magnesium alloy is a kind of very small metal material of density, but due to the atomic structure feature of magnesium alloy, plasticity is poor, at present
Manufacturing process cannot obtain the material of high intensity.The intensity of magnesium alloy how is improved, is the focus of current people's research.
103031452 A of Chinese patent CN disclose a kind of SiC particles reinforced magnesium-based composite material and preparation method,
The invention prepares carbonization using pure Mg powder, Al powder and SiC particulate micro mist as raw material, using powder metallurgy and multiway forging method
Silicon particle enhances magnesium-based composite material.By two kinds of forming methods of powder metallurgy and multiway forging, make magnesium alloy substrate and SiC
Between grain there is good wellability and associativity, and eliminate the hole that powder metallurgy forming remains in material internal in the process
Gap is finally obtained SiC particulate and is uniformly distributed, the tiny magnesium-based composite material of magnesium alloy substrate crystal grain, has the composite material
There is better mechanical property.The tensile strength of the magnesium alloy of the invention is less than 200MPa.
Chinese patent 104109790A provides a kind of high-strength magnesium alloy material and preparation method thereof, the magnesium alloy materials group
Aluminium (Al), zinc (Zn), manganese chloride (MnCl are included in point2), silicon carbide (SiC) crystal grain, beryllium (Be), magnesium (Mg), wherein, magnesium alloy
Material each group is grouped as is respectively by weight percentage：Aluminium (Al)：10.5-12%, zinc (Zn)：6-7%, manganese chloride (MnCl2)：
0.6-1.5%, silicon carbide (SiC) crystal grain：2-3.5%, beryllium (Be)：0.01-0.03%, surplus are magnesium (Mg).The alloy passes through
The mode of continuously casting replaces traditional extrusion process, and the production of magnesium alloy is completed in a manner of short route, shortens production stream
Journey, has saved cost, and prepared magnesium alloy materials in tensile strength, yield strength, prolong compared to traditional magnesium alloy materials
Rate, elasticity modulus, hardness etc. is stretched to be significantly improved.
Chinese patent 102766774A provides a kind of Enhancement Method of magnesium alloy doping SiC particulate, for magnesium alloy mould
The situation that low, intensity is low, easy to wear, high temperature resistance is poor, coefficient of thermal expansion is high is measured, is mixed using during Melting Magnesium alloy block
Then miscellaneous thin silicon carbide and thick silicon-carbide particle are cast, are pressurizeed and hot extrusion molding, increase substantially the surrender of magnesium alloy
Intensity, hardness and wear-resisting property, making yield strength, hardness reaches 120HV ± 5HV, and wearability improves up to 328MPa ± 2MPa
80%。
Above invention is devoted to improve the performance particularly strength character of magnesium alloy, by the room-temperature yield strength of magnesium alloy
It has been increased to megapascal more than 300.But, the intensity of the materials such as current steel, titanium alloy, aluminium alloy generally all 400 megapascal with
On, the intensity of magnesium alloy also has a certain distance with these common engineering material.
Invention content：
Goal of the invention：The advantages of in order to expand the application field of magnesium alloy, play its low-density, the present invention provides one kind
High-strength magnesium alloy and preparation method thereof.
Technical scheme is as follows:
Using the method in nano-particle reinforcement, additive is mixed into magnesium alloy during melting, is uniformly dispersed,
Slow cooling simultaneously vacuumizes nano particle is allowed to further improve concentration, then under high pressure by the way of torsional deformation, into one
Crystal grain thinning is walked, improves the intensity of alloy.According to the present invention it is possible to prepare a kind of high-strength magnesium alloy of nano-particle reinforcement.Its
Average crystal grain diameter in microscopic structure at 60 nanometers hereinafter, the diameter of nano particle at 100 nanometers hereinafter, the surrender of magnesium alloy
Intensity is in more than 450MPa.
Specific preparation method includes the following steps：
（1）Prepare raw material：The high purity magnesium and high purity alloys element and average grain diameter for preparing more than 99.9% are 100 nanometers
Following nanometer additive；
（2）Molten alloy：By high purity magnesium and alloying element according to certain atomic ratio dispensing, melted in protective atmosphere
It refines, adds in nanometer additive in fusion process, maintain the temperature at 700 °C, the method using ultrasound is disperseed；
（3）Slow cooling is carried out to alloy pig, keeps vacuumizing state during cooling, vacuum degree is less than 5torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, high pressure is applied, and rotate anvil to reverse alloy disks to alloy, is allowed to the deformation that is distorted；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.1-1.5;Setting is rolled every time
Deformation quantity processed is 1-8%；The speed of low speed roller is set as 0.5-2 meter per seconds；
（7）Start main driving motor, start the operation of rolling;
（8）It treats after once rolling, repeats（6）（7）Process 15 times or more；
（9）Carry out full annealed heat treatment.
Wherein, step（1）In protective gas be CO2With SF6Mixed gas, step（3）In, cooling velocity is less than every
Second 0.5K；Step（5）The pressure that middle alloy is born is 1.5-5GPa；Step（8）In rolling temperature be room temperature：Step（9）In
Recrystallization temperature for magnesium fusing point 1/3 ~ 1/4, time 3-20 minute.
Nanometer additive of the present invention is including but not limited to silicon carbide, silica, titanium oxide；The present invention is used
Alloying element including but not limited to zinc, aluminium, copper, iron, manganese, molybdenum, titanium.
Preferably, CO2With SF6The range of volume ratio be 50:1~100:1；
Preferably, step（2）The mass fraction that middle added in additive particles account for alloy is 1.5 ~ 5%；
Preferably, step（5）In rotary speed for 2 ~ 5 turns per minute, corotating 3-20 circles.
Beneficial effect：
The present invention, as enhancing particle, can not only play crystal grain thinning using the particle of the nanometer additive of high intensity
Effect, and the dislocation of metal as the obstacle of dislocation motion, can be prevented to move, so as to reinforced metal；Meanwhile crystal grain thinning
It can play the role of improving alloy plasticity.
The present invention efficiently solves nano particle in a metal very using ultrasonic disperse is carried out under high temperature metal liquid state
The problem of difficulty is uniformly dispersed.Using ultrasonic disperse under liquid metal state, nano particle can be uniformly dispersed, to solve to pass
The defects of nano particle dispersion is bad in the technologies such as system mixing, stirring.Using Slow cooling after melting, while vacuum degree is kept,
The metallic vapour of magnesium can be made constantly to be extracted, the content of magnesium in alloy is reduced, so as to improve the body of nano particle in alloy
Fraction further enhances the effect of reinforced by nanoparticles；The content of alloying element can also increase simultaneously.
During high pressure twist distortion is applied, larger crystal grain is broken down into more tiny nanocrystalline in alloy substrate
Grain.In addition, the present invention is processed further material using asymmetrical rolling, this milling method can further refine crystalline substance
Grain, and thickness crystal grain distribution can be formed in portion within the organization, this material structure can reach greatly back of the body processing hardening, this
It is to be not present in the material of even grained or the material of conventional machining.The present invention is using micro Process, multi-pass, suitable for obtaining
Destination organization.For the average crystal grain diameter of final alloy generally at 60 nanometers hereinafter, according to Hall-with strange relationship, crystal grain becomes thin
It is small, it can cause the intensity higher of alloy, it is also possible to improve the plasticity of alloy.The magnesium alloy prepared by the present invention,
Yield strength can be up to more than 450MPa, can be applied to the fields such as automotive light weight technology engineering, space flight and aviation engineering.
Specific embodiment
Below by embodiment detailed description of the present invention preparation method, but it is not construed as limiting the invention.
Embodiment 1
（1）Prepare raw material：The high purity magnesium and high purity zinc and average grain diameter of more than 99.9% preparation are 90 nanometers of nanometer
SiC；
（2）Molten alloy：By high purity magnesium and zinc according to 6:1 atomic ratio dispensing, in CO2With SF6Mixed gas in
Melting, wherein CO2With SF6Volume ratio is 80:1；The nano SiC for accounting for alloy mass score 1.5% is added in fusion process, keeps temperature
Degree at 700 °C, disperseed by the method using ultrasound；
（3）Slow cooling, cooling velocity 0.3K per second are carried out to alloy pig；It keeps vacuumizing shape during cooling
State, vacuum degree 3torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, apply 5GPa high pressures to alloy, and anvil is rotated to reverse alloy disks with 5 turns per minute of speed, be allowed to be distorted
Deformation, a corotating 8 are enclosed；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.5;Set each rolling deformation
Measure is 3%；The speed of low speed roller is set as 2 meter per seconds；
（7）Start main driving motor, start the operation of rolling；
（8）It treats after once rolling, repeats（6）（7）Process 20 times；
（9）Full annealed heat treatment, 20 minutes time are carried out at 170 degrees Celsius.
Embodiment 2
（1）Prepare raw material：The high purity magnesium and high purity zinc and average grain diameter of more than 99.9% preparation are 80 nanometers of nanometer
SiC；
（2）Molten alloy：By high purity magnesium and zinc according to 4:1 atomic ratio dispensing, in CO2With SF6Mixed gas in
Melting, wherein CO2With SF6Volume ratio is 80:1；The nano SiC for accounting for alloy mass score 5% is added in fusion process, keeps temperature
At 700 °C, the method using ultrasound is disperseed；
（3）Slow cooling, cooling velocity 0.4K per second are carried out to alloy pig；It keeps vacuumizing shape during cooling
State, vacuum degree 5torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, apply 1.5GPa high pressures to alloy, and anvil is rotated to reverse alloy disks with 3 turns per minute of speed, be allowed to turn round
Curved change, a corotating 10 are enclosed；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.4;Set each rolling deformation
Measure is 3%；The speed of low speed roller is set as 2 meter per seconds；
（7）Start main driving motor, start the operation of rolling;
（8）It treats after once rolling, repeats（6）（7）Process 25 times；
（9）Full annealed heat treatment, 10 minutes time are carried out at 190 degrees Celsius.
Embodiment 3
（1）Prepare raw material：The high purity magnesium and rafifinal and average grain diameter of more than 99.9% preparation are 80 nanometers of nanometer
SiO2；
（2）Molten alloy：By high purity magnesium and zinc according to 3:1 atomic ratio dispensing, in CO2With SF6Mixed gas in
Melting, wherein CO2With SF6Volume ratio is 100:1；The Nano-meter SiO_2 for accounting for alloy mass score 4.2% is added in fusion process2, keep
Temperature at 700 °C, disperseed by the method using ultrasound；
（3）Slow cooling, cooling velocity 0.2K per second are carried out to alloy pig；It keeps vacuumizing shape during cooling
State, vacuum degree 4torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, apply 4.5GPa high pressures to alloy, and anvil is rotated to reverse alloy disks with 3 turns per minute of speed, be allowed to turn round
Curved change, a corotating 3 are enclosed；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.1;Set each rolling deformation
Measure is 1%；The speed of low speed roller is set as 0.5 meter per second；
（7）Start main driving motor, start the operation of rolling;
（8）It treats after once rolling, repeats（6）（7）Process 25 times；
（9）Full annealed heat treatment, 8 minutes time are carried out at 200 degrees Celsius.
Embodiment 4
（1）Prepare raw material：The high purity magnesium and high purity zinc and average grain diameter of more than 99.9% preparation are 80 nanometers of nanometer
TiO2；
（2）Molten alloy：By high purity magnesium and copper according to 5:1 atomic ratio dispensing, in CO2With SF6Mixed gas in
Melting, wherein CO2With SF6Volume ratio is 60:1；The nano-TiO for accounting for alloy mass score 2.5% is added in fusion process2, keep
Temperature at 700 °C, disperseed by the method using ultrasound；
（3）Slow cooling, cooling velocity 0.3K per second are carried out to alloy pig；It keeps vacuumizing shape during cooling
State, vacuum degree are less than 4torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, apply 3GPa high pressures to alloy, and anvil is rotated to reverse alloy disks with 2.5 turns per minute of speed, be allowed to turn round
Curved change, a corotating 20 are enclosed；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.1;Set each rolling deformation
Measure is 8%；The speed of low speed roller is set as 0.5 meter per second；
（7）Start main driving motor, start the operation of rolling;
（8）It treats after once rolling, repeats（6）（7）Process 23 times；
（9）Full annealed heat treatment, 8 minutes time are carried out at 180 degrees Celsius.
Embodiment 5
（1）Prepare raw material：The high purity magnesium and high purity zinc and average grain diameter of more than 99.9% preparation are 60 nanometers of nanometer
SiC；
（2）Molten alloy：By high purity magnesium and zinc according to 3.5:1 atomic ratio dispensing, in CO2With SF6Mixed gas
Middle melting, wherein CO2With SF6Volume ratio is 50:1；The nano SiC for accounting for alloy mass score 1.8% is added in fusion process, is kept
Temperature at 700 °C, disperseed by the method using ultrasound；
（3）Slow cooling, cooling velocity 0.5K per second are carried out to alloy pig；It keeps vacuumizing shape during cooling
State, vacuum degree 3torr；
（4）After cooling, alloy pig is processed into discoid；
（5）The space that the groove coarse-grain alloy disks of step (4) processing being put into upper and lower two anvils is formed
It is interior, apply 1.5GPa high pressures to alloy, and anvil is rotated to reverse alloy disks with 2 turns per minute of speed, be allowed to turn round
Curved change, a corotating 20 are enclosed；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.3;Set each rolling deformation
Measure is 2%；The speed of low speed roller is set as 2 meter per seconds；
（7）Start main driving motor, start the operation of rolling;
（8）It treats after once rolling, repeats（6）（7）Process 20 times；
（9）Full annealed heat treatment, 3 minutes time are carried out at 180 degrees Celsius.
Performance detection：Tensile test at room temperature is carried out, obtains the yield strength of alloy prepared by each embodiment；Using transmission electricity
Mirror is analyzed, and obtains the crystal grain diameter of alloy；As a result such 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（Nanometer） | 53 | 52 | 47 | 56 | 46 |
From upper table it can be seen that, using the present invention, the yield strength of the magnesium alloy prepared is done in more than 450MPa, it is significantly high
In state of the art.
The above is only some examples of embodiment of the present invention, it should be pointed out that：For the technology people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of nanometer of enhancing magnesium alloy, it is characterised in that：The magnesium alloy is by magnesium and its alloying element and nanometer additive structure
Into；The average diameter of nanometer additive at 100 nanometers hereinafter, the average crystal grain of magnesium alloy at 60 nanometers hereinafter, its manufacturing method
It comprises the steps of：
（1）Prepare raw material：The high purity magnesium and high purity alloys element and average grain diameter for preparing more than 99.9% purity are 200 nanometers
Following nanometer additive；
（2）Molten alloy：By high purity magnesium and alloying element according to certain atomic ratio dispensing, the melting in protective atmosphere is melted
Nanometer additive is added in during refining, maintains the temperature at 700 °C, the method using ultrasound is disperseed；
（3）Slow cooling is carried out to alloy pig, keeps vacuumizing state during cooling, vacuum degree is less than 5torr；
（4）After cooling, alloy pig is processed into discoid；
（5）It is right in the space that the groove that the coarse-grain alloy disks of step (4) processing are put into upper and lower two anvils is formed
Alloy applies high pressure, and rotates anvil to reverse alloy disks, is allowed to the deformation that is distorted；
（6）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.1-1.5;Setting rolls shape every time
Variable is 1-8%；The speed of low speed roller is set as 0.5-2 meter per seconds；
（7）Start main driving motor, start the operation of rolling；
（8）It treats after once rolling, repeats（6）（7）Process 15 times or more；
（9）Carry out full annealed heat treatment.
2. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：The nanometer additive including but not limited to
Silicon carbide, silica, titanium oxide.
3. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：The alloying element including but not limited to
Zinc, aluminium, copper, iron, manganese, molybdenum, titanium.
4. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：Protective gas is CO2With SF6Mixed gas.
5. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：Cooling velocity is less than 0.5K per second.
6. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：The pressure that alloy is born is 1.5-5GPa, is revolved
2 ~ 5 turns per minute of rotary speed.
7. nanometer as described in claim 1 enhances magnesium alloy, it is characterised in that：The rolling temperature is room temperature.
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