CN109266935A - A kind of wrought magnesium alloy and preparation method thereof with nano-structure - Google Patents
A kind of wrought magnesium alloy and preparation method thereof with nano-structure Download PDFInfo
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- CN109266935A CN109266935A CN201811360466.7A CN201811360466A CN109266935A CN 109266935 A CN109266935 A CN 109266935A CN 201811360466 A CN201811360466 A CN 201811360466A CN 109266935 A CN109266935 A CN 109266935A
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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
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
A kind of wrought magnesium alloy and preparation method thereof with nano-structure.The ingredient of the alloy is by mass percentage are as follows: aluminium 0.8~1.5%, zinc 1.5~2.5%, calcium 0.15~0.4%, manganese 0.2~0.4%, gadolinium 0.15~0.3%, magnesium are surplus, and impurity iron content controls below 0.003%.Preparation method: 1, melting raw material Mg ingot, Al ingot, Zn ingot, Mg-Ca and Mg-Gd intermediate alloy；2, MnCl is added in low temperature2Except iron；3, shorten the double refining time added after Mg-Ca, the casting yield of Ca reaches 50~60%；4, electromagnetism semi-continuous casting；5, Homogenization Treatments；6, extrusion process obtains wrought magnesium alloy extruded bars.The present invention prepares wrought magnesium alloy ingot casting base, it can be achieved that low-temp. extrusion, squeeze wood are nanoscale perfect recrystallization tissue using low frequency electromagnetic casting technology, and room-temperature mechanical property is excellent.
Description
Technical field
The invention belongs to metal material and metallurgical technology fields, and in particular to a kind of to have the characteristics that the deformed Mg of nano-structure
Alloy and preparation method thereof.
Background technique
Magnesium alloy is with density is small, specific strength is high and damping, electromagnetic wave shielding, machining property is excellent and is easy to
The advantages that recycling is structure lightened ideal material.In recent years, as aerospace, 3C electronic product and military project are led
Domain is growing to magnesium alloy demand, and the mechanical property of cast magnesium alloy has been unable to satisfy the demand of people, by squeezing, rolling
After the plastic processing methods deformation such as system, forging, the comprehensive mechanical property of magnesium alloy, which is improved, can be better met as knot
The requirement of structure material.But due to the close-packed hexagonal structure of magnesium alloy, magnesium alloy has strong anisotropy and poor
Plastic deformation ability, these two issues all seriously limit the forming property of magnesium alloy.Common AZ series becomes at this stage
Its main component of shape magnesium alloy such as AZ31 is the Al containing 2.5~3.5%, and 0.7~1.3% Zn, 0.2% Mn, remaining is
Mg, the temperature range of deformation is not suitable for deforming under low temperature between 250~450 DEG C, so the crystallite dimension of deformation AZ31 magnesium alloy
Universal bigger than normal, substantially between 5~25 μm, intensity is lower than 280MPa more, and elongation is generally less than 20%.Generally, at present
AZ system magnesium alloy plasticity it is poor, forming difficulty, intensity is not high, using limited.Therefore mining inetesity is higher or plasticity is better
New A Z system alloy is the striving direction of industry research person always.The present invention is on the basis of AZ31, by suitably reducing Al content
Simultaneously properly increase Zn content, in conjunction with the micro combined alloy of Ca and Gd, novel Mg-Zn-Al alloy obtained, it can be achieved that
Low-temp. extrusion shapes and can get the extruding tissue of nanoscale perfect recrystallization, and squeeze wood surface quality is bright and clean, room temperature mechanics
Function admirable.In addition, combining secondary refining process to adjust by the adjustment of alloying order, when significantly improving Ca microalloying
The casting yield and its stability of Mg-Ca intermediate alloy.
Magnesium alloy plastic deformation ability is poor, and other than Mg-Li alloy, most of AZ system industrial magnesium alloys can only at present
Be plastically deformed at 250 DEG C or more, and general deformation temperature is even higher at 300~400 DEG C, but high temperature deformation often because
The mechanical property of deformation material is grown up and significantly reduced to recrystallization for Deformation structure.On the other hand, numerous studies have shown that, magnesium
Alloy plastic deformation has biggish deformation heat, and deformation heat is significantly improved with the reduction of deformation temperature, therefore, if passed through
Alloying component adjusts and combines the optimization of blank preparation process, and casting ingot obtained can be realized cold plasticity deformation
Words control the combination that can pass through deformation temperature and deflection and rate of deformation, effectively to adjust plastic deformation behavior and change
Shape heat, so that the deformed recrystallized structure of Effective Regulation, realizes significantly improving for squeeze wood mechanical property.
Summary of the invention
For the present invention for AZ system magnesium alloy strength is low and the problem of plasticity difference, providing a kind of has the characteristics that the change of nano-structure
Shape magnesium alloy and preparation method thereof.The alloy is cast using low frequency electromagnetic casting technique, while in smelting operation
The method of smelting of Mg-Ca intermediate alloy casting yield and stability can be improved in Shi Caiyong.
The present invention, which provides, a kind of has the characteristics that the wrought magnesium alloy of nano-structure, the ingredient of the alloy are by mass percentage
Al:0.8~1.5%, Zn:1.5~2.5%, Ca:0.15~0.4%, Mn:0.2~0.4%, Gd:0.15~0.3%, Mg are
Surplus, impurity F e content control below 0.003%.
Described to have the characteristics that the wrought magnesium alloy of nano-structure, average grain size are 300~1250nm, tensile strength is
280~330MPa, yield strength are 260~310MPa, and elongation at break is 16~25%.
The present invention also provides a kind of preparation methods with the wrought magnesium alloy of nano-structure, and steps are as follows:
(1) melting raw material: according to the mass percent of wrought magnesium alloy, Mg ingot being heated to melting, and Al ingot is then added
With Zn ingot, 20min is refined, Mg-Gd intermediate alloy is added when temperature is 720~740 DEG C, stirs evenly, obtains Mg-Al-Zn-Gd
Melt；
(2) cooling is except iron processing: Mg-Al-Zn-Gd melt obtained by step (1) being cooled to 660~670 DEG C, is added
MnCl2It carries out except Fe；
(3) adding raw materials Ca: will be obtained by step (2) except adding Mg-Ca when melt temperature is increased to 700~720 DEG C after iron
Intermediate alloy stirs evenly, and the time≤10min obtains Mg-Al-Zn-Gd-Mn-Ca melt；
(4) electromagnetism semi-continuous casting: Mg-Al-Zn-Gd-Mn-Ca melt is cooled to 680~700 DEG C, in N2+SF6Mixing
Electromagnetism semi-continuous casting is carried out under gas shield, obtains magnesium alloy ingot base；
(5) Homogenization Treatments: carrying out 16~20h of Homogenization Treatments for magnesium alloy ingot base under the conditions of 380~400 DEG C,
Ingot casting after Homogenization Treatments is subjected to turning, obtains the good casting ingot of turning；
(6) extrusion process: the good casting ingot of turning being put into resistance furnace and is heated to 110~250 DEG C, and heat preservation 120~
180min obtains magnesium alloy extrusion blank, squeezes it, and extrusion ratio is 16~25, and extrusion speed is 1.0~2.0m/
Min obtains the extruded bar from magnesium alloy that specification is 20~75mm of Φ.
In the step (3), the casting yield of Ca reaches 50~60%.
In the step (4), electromagnetism semi-continuous casting condition are as follows: magnet exciting coil number of ampere turns is 3000~12000AN, electromagnetism
Frequency is 15~30Hz, and casting speed is 60~150mm/min, and water is 100~450L/min.
In the step (6), pressurizing unit is put into heating furnace before extrusion operation and is preheated, reaches extruding and requires temperature,
Using grease based on molybdenum disulfide lithium as lubricant, it is uniformly applied to extrusion die inner wall, magnesium alloy extrusion blank surface
On extrusion cylinder inner wall.
Compared with prior art, beneficial effects of the present invention:
(1) as-cast magnesium alloy of the invention has compared with high plastic deformation's ability, can carry out extrusion molding at a lower temperature,
It is formulated as on the basis of AZ31, the appropriate Al content that reduces properly increases Zn content simultaneously, and combines the micro combination of Ca and Gd
Alloying, wherein rare metal Gd additive amount is no more than 0.3%, and alloy material is low in cost；
(2) present invention uses low frequency electromagnetic casting technology, obtained extruding casting ingot any surface finish, vehicle pin
It measures small；
(3) using cooling and plus MnCl in fusion process of the present invention2Mode except the order for adding Ca after Fe operation, and it is tight
Lattice control adds the double refining time after Ca, and the stability of the casting yield and casting yield that significantly improve Mg-Ca intermediate alloy is (real
Yield spectra is 50~60%)；
(4) magnesium alloy ingot prepared by the present invention can realize that low-temp. extrusion, obtained squeeze wood have nanoscale completely again
Crystalline structure, and surface quality is bright and clean, room-temperature mechanical property is excellent；
(5) magnesium alloy of the present invention can be squeezed in minimum extruding temperature for 110 DEG C, can obtain minimum average B configuration crystal grain ruler
Very little is 300nm, highest tensile strength 330Mpa (for 1.2~1.7 times of AZ31 alloy), highest yield strength 310MPa, is preferably broken
Split the performance indicator that elongation is 25% (for 1.2~1.8 times of AZ31 alloy).
Detailed description of the invention
Fig. 1 is the ingot casting picture of magnesium alloy in embodiment 1；
Fig. 2 is the typical as-cast microstructure picture of magnesium alloy in embodiment 1；
Fig. 3 is the homogenization state microscopic structure picture of magnesium alloy in embodiment 1；
Fig. 4 is extruded bars picture in embodiment 1；
Fig. 5 is extruded bars picture in embodiment 2；
Fig. 6 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 1, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture；
Fig. 7 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 2, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture；
Fig. 8 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 3, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture；
Fig. 9 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 4, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture；
Figure 10 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 5, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture；
Figure 11 is that the microscopic structure of extruded bars and stretching fracture scan pattern picture in embodiment 6, wherein (a) is micro-
Picture is organized, (b) scans pattern picture for stretching fracture.
Specific embodiment
Mg, Al, Zn are added using level-one magnesium ingot, aluminium ingot, zinc ingot metal pure metal in the present embodiment, and Mn uses MnCl2Form adds
Enter, Ca and Gd are added using intermediate alloy form, and flux is market purchase.
Embodiment 1
Wrought magnesium alloy ingredient is Al:0.8%, Zn:2.5%, Ca:0.15%, Mn:0.2%, Gd by mass percentage:
0.3%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Mg ingot is heated to 720 DEG C of fusings, Al ingot, Zn ingot are added in the magnesium liquid melted, with No. five flux-refining 20min, temperature
When degree rises to 730 DEG C, the intermediate alloy of Mg-25%Gd is added, stirs evenly, obtains Mg-Al-Zn-Gd melt；
(2) cooling is except iron processing: Mg-Al-Zn-Gd melt is cooled to 660 DEG C and MnCl is added2It carries out dual except iron, guarantor
It demonstrate,proves Fe content in magnesium alloy and is less than 0.003%；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 705 DEG C after iron, the secondary fine of 10min is carried out
Refining, the casting yield of Ca are 50%；
(4) when being cooled to 700 DEG C, in N2+SF6Mixed gas protected lower progress electromagnetism semi-continuous casting applies electromagnetic conditions
Are as follows: number of ampere turns 3000AN, electromagnetic frequency 30Hz, duty ratio 20%, casting speed 120mm/min, water 140L/
Min, obtaining diameter of section is 110mm, and length is the magnesium alloy ingot base of 6000mm, and chemical analysis group becomes Mg-0.8Al-
2.5Zn-0.2Mn-0.15Ca-0.3Gd；
(5) magnesium alloy ingot photo as shown in Figure 1, by magnesium alloy ingot segmentation be put into heat-treatment furnace carry out 395 ± 5 DEG C ×
The Homogenization Treatments of 16h, typical as cast condition and homogenization state microscopic structure difference are as shown in Figures 2 and 3, and Homogenization Treatments are complete
Ingot casting carry out sawing, according to the sawing of extrusion die size and be turned into Φ 98mm × 600mm cylinder blank in case squeeze
It is used；
(6) the good casting ingot of turning is heated in furnace 110 DEG C and keeps the temperature 120min, obtain magnesium alloy extrusion base
Material, while extrusion cylinder, extrusion die and extruding pad are heated to 110 DEG C, then used in extrusion die inner wall, magnesium alloy extrusion
Blank surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with
The extrusion speed of 1.0m/min squeezes, extrusion ratio 25, squeezes and obtains the magnesium alloy extrusion stick that diameter as shown in Figure 4 is 20mm
Material, microscopic structure and stretching fracture the scanning pattern picture of gained extruded bars are as shown in fig. 6, wherein microscopic structure such as Fig. 6 (a)
Shown, extruded bar from magnesium alloy sampling is processed into tensile sample, carried out on stretching-machine by average grain size 330nm
Room temperature tensile, tensile speed 1.0mm/min, room temperature tensile mechanical property is as shown in table 1, stretching fracture pattern such as Fig. 6 (b)
It is shown.
The extruded bar from magnesium alloy room temperature tensile mechanical property of 1 embodiment 1 of table
Embodiment 2
Wrought magnesium alloy ingredient is Al:0.9%, Zn:2.2%, Ca:0.2%, Mn:0.2%, Gd by mass percentage:
0.2%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Magnesium ingot is heated to 720 DEG C of fusings, according to the mass percentage composition of wrought magnesium alloy, Al ingot, Zn ingot is added to having melted
Magnesium liquid in, with No. five flux-refining 20min, when temperature rises to 730 DEG C, the intermediate alloy of Mg-25%Gd is added, stirring is equal
It is even, obtain Mg-Al-Zn-Gd melt；
(2) low temperature is except iron processing: Mg-Al-Zn-Gd melt being cooled to 660 DEG C and MnCl is added2Carry out it is dual except iron,
Guarantee that Fe content is less than 0.003% in magnesium alloy；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 705 DEG C after iron, the two of 8min is then carried out
Secondary refining, the casting yield of Ca are 52%；
(4) when being cooled to 700 DEG C, in N2+SF6Mixed gas protected lower beginning electromagnetism semi-continuous casting starts electromagnetism and partly connects
Continuous casting, applies electromagnetic conditions are as follows: number of ampere turns 9000AN, electromagnetic frequency 20Hz, duty ratio 20%, casting speed are
90mm/min, water 200L/min, obtaining diameter of section is 160mm, and length is the magnesium alloy ingot base of 6000mm, chemistry
Analysis group becomes Mg-0.9Al-2.2Zn-0.2Mn-0.2Ca-0.2Gd；
(5) segmentation of magnesium alloy ingot base is put into the Homogenization Treatments that heat-treatment furnace carries out 395 ± 5 DEG C × 16h, it will be uniform
Change ingot casting progress sawing handle, according to the sawing of extrusion die size and is turned into the cylinder blank of Φ 148mm × 600mm
It is used in case squeezing；
(6) cylinder blank is heated to 110 DEG C in furnace and keeps the temperature 120min, obtains magnesium alloy extrusion blank, together
When extrusion cylinder, extrusion die and extruding pad be heated to 110 DEG C, then in extrusion die inner wall, magnesium alloy extrusion blank
Surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with 1.3m/min
Extrusion speed squeeze, extrusion ratio 18.9, squeeze obtain diameter be 35mm extruded bar from magnesium alloy, as shown in figure 5, gained
Microscopic structure and stretching fracture the scanning pattern pictures of extruded bars as shown in fig. 7, wherein shown in microscopic structure such as Fig. 7 (a),
Average grain size is 300nm, and extruding is prepared magnesium alloy rod sampling and is processed into tensile sample, room temperature is carried out on stretching-machine
It stretches, tensile speed 1mm/min, room temperature tensile mechanical property is as shown in table 2, shown in stretching fracture pattern such as Fig. 7 (b).
The extruded bar from magnesium alloy room temperature tensile mechanical property of 2 embodiment 2 of table
Embodiment 3
Wrought magnesium alloy ingredient is Al:1.2%, Zn:1.9%, Ca:0.3%, Mn:0.3%, Gd by mass percentage:
0.2%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Magnesium ingot is heated to 720 DEG C of fusings, according to the mass percentage composition of wrought magnesium alloy, Al ingot, Zn ingot is added to having melted
Magnesium liquid in, with No. five flux-refining 20min, when temperature rises to 730 DEG C, the intermediate alloy of Mg-25%Gd is added, stirring is equal
It is even, it obtains Mg-Al-Zn-Gd melt；
(2) low temperature is except iron processing: Mg-Al-Zn-Gd melt obtained by step (1) being cooled to 660 DEG C and MnCl is added2Into
Row is dual to remove iron, and Fe content is less than 0.003% in magnesium alloy；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 705 DEG C after iron, the two of 8min is then carried out
Secondary refining, the casting yield of Ca are 52%；
(4) when being cooled to 695 DEG C, in N2+SF6Mixed gas protected lower beginning electromagnetism semi-continuous casting starts electromagnetism and partly connects
Continuous casting, applies electromagnetic conditions are as follows: number of ampere turns 12000AN, electromagnetic frequency 15Hz, duty ratio 20%, casting speed are
60mm/min, water 450L/min, obtaining diameter of section is 312mm, and length is the magnesium alloy ingot base of 6000mm, chemistry
Analysis group becomes Mg-1.2Al-1.9Zn-0.3Mn-0.3Ca-0.2Gd；
(5) segmentation of magnesium alloy ingot base is put into the Homogenization Treatments that heat-treatment furnace carries out 395 ± 5 DEG C × 18h, it will be uniform
Change ingot casting progress sawing handle, according to the sawing of extrusion die size and is turned into the cylinder blank of Φ 295mm × 600mm
It is used in case squeezing；
(6) cylinder blank is heated to 170 DEG C in furnace and keeps the temperature 180min, obtains magnesium alloy extrusion blank, together
When extrusion cylinder, extrusion die and extruding pad be heated to 170 DEG C, then in extrusion die inner wall, magnesium alloy extrusion blank
Surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with 1.6m/min
Extrusion speed extrusion magnesium alloy sample, extrusion ratio 16, squeeze obtain diameter be 75mm extruded bar from magnesium alloy, gained squeeze
Microscopic structure and stretching fracture the scanning pattern picture of pressure bar material are put down as shown in figure 8, wherein shown in microscopic structure such as Fig. 8 (a)
Equal crystallite dimension is 620nm, and extruding is prepared magnesium alloy rod sampling and is processed into tensile sample, room temperature drawing is carried out on stretching-machine
It stretches, tensile speed 1mm/min, room temperature tensile mechanical property is as shown in table 3, shown in stretching fracture pattern such as Fig. 8 (b).
The extruded bar from magnesium alloy room temperature tensile mechanical property of 3 embodiment 3 of table
Embodiment 4
Wrought magnesium alloy ingredient is Al:1.5%, Zn:1.5%, Ca:0.2%, Mn:0.25%, Gd by mass percentage:
0.3%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Magnesium ingot is heated to 720 DEG C of fusings, according to the mass percentage composition of wrought magnesium alloy, Al ingot, Zn ingot is added to having melted
Magnesium liquid in, with No. five flux-refining 20min, when temperature rises to 730 DEG C, the intermediate alloy of Mg-25%Gd is added, stirring is equal
It is even, it obtains Mg-Al-Zn-Gd melt；
(2) low temperature is except iron processing: Mg-Al-Zn-Gd melt obtained by step (1) being cooled to 660 DEG C and MnCl is added2Into
Row is dual to remove iron, and Fe content is less than 0.003% in magnesium alloy；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 705 DEG C after iron, the two of 8min is then carried out
Secondary refining, the casting yield of Ca are 53%；
(4) when being cooled to 700 DEG C, in N2+SF6Mixed gas protected lower beginning electromagnetism semi-continuous casting starts electromagnetism and partly connects
Continuous casting, applies electromagnetic conditions are as follows: number of ampere turns 3000AN, electromagnetic frequency 30Hz, duty ratio 20%, casting speed are
120mm/min, water 140L/min, obtaining diameter of section is 110mm, and length is the magnesium alloy ingot base of 6000mm, is changed
Credit analysis group becomes Mg-1.5Al-1.5Zn-0.25Mn-0.2Ca-0.3Gd；
(5) segmentation of magnesium alloy ingot base is put into the Homogenization Treatments that heat-treatment furnace carries out 390 ± 5 DEG C × 18h, it will be uniform
Change ingot casting progress sawing handle, according to the sawing of extrusion die size and is turned into the cylinder blank of Φ 98mm × 600mm
It is used in case squeezing；
(6) cylinder blank is heated to 170 DEG C in furnace and keeps the temperature 180min, obtains magnesium alloy extrusion blank, together
When extrusion cylinder, extrusion die and extruding pad be heated to 170 DEG C, then in extrusion die inner wall, magnesium alloy extrusion blank
Surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with 1.0m/min
Extrusion speed squeezed, extrusion ratio 25, squeeze obtain diameter be 20mm extruded bar from magnesium alloy, gained extruded bars
Microscopic structure and stretching fracture scanning pattern picture as shown in figure 9, wherein shown in microscopic structure such as Fig. 9 (a), average crystal grain
Having a size of 550nm, extruding is prepared into magnesium alloy rod sampling and is processed into tensile sample, room temperature tensile is carried out on stretching-machine, is drawn
Stretching speed is 1mm/min, and room temperature tensile mechanical property is as shown in table 4, shown in stretching fracture pattern such as Fig. 9 (b).
The extruded bar from magnesium alloy room temperature tensile mechanical property of 4 embodiment 4 of table
Embodiment 5
Wrought magnesium alloy ingredient is Al:1.0%, Zn:2.2%, Ca:0.4%, Mn:0.4%, Gd by mass percentage:
0.15%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Magnesium ingot is heated to 730 DEG C of fusings, according to the mass percentage composition of wrought magnesium alloy, Al ingot, Zn ingot is added to having melted
Magnesium liquid in, with No. five flux-refining 30min, when temperature rises to 730 DEG C, Mg-25% is added according to 0.4%Gd mass percent
The intermediate alloy of Gd, stirs evenly, and obtains Mg-Al-Zn-Gd melt；
(2) low temperature is except iron processing: Mg-Al-Zn-Gd melt being cooled to 670 DEG C, and MnCl is added2Carry out it is dual except iron,
Guarantee that Fe content is less than 0.003% in magnesium alloy；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 700 DEG C after iron, the two of 8min is then carried out
Secondary refining, the casting yield of Ca are 57%；
(4) when melt temperature is 700 DEG C, in N2+SF6Mixed gas protected lower beginning electromagnetism semi-continuous casting starts electricity
Magnetic semi-continuous casting applies electromagnetic conditions are as follows: number of ampere turns 9000AN, electromagnetic frequency 20Hz, duty ratio 20%, casting speed
Degree is 90mm/min, water 200L/min, and obtaining diameter of section is 160mm, and length is the magnesium alloy ingot base of 6000mm,
Chemical analysis group becomes Mg-1.0Al-2.0Zn-0.4Mn-0.4Ca-0.15Gd；
(5) segmentation of magnesium alloy ingot base is put into the Homogenization Treatments that heat-treatment furnace carries out 395 ± 5 DEG C × 20h, it will be uniform
Change ingot casting progress sawing handle, according to the sawing of extrusion die size and is turned into the cylinder blank of Φ 148mm × 600mm
It is used in case squeezing；
(6) cylinder blank is heated to 210 DEG C in furnace and keeps the temperature 180min, obtains magnesium alloy extrusion blank, together
When extrusion cylinder, extrusion die and extruding pad be heated to 210 DEG C, then in extrusion die inner wall, magnesium alloy extrusion blank
Surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with 2.0m/min
Extrusion speed extrusion magnesium alloy sample, extrusion ratio 18.9, squeeze obtain diameter be 35mm extruded bar from magnesium alloy, gained
Microscopic structure and stretching fracture the scanning pattern picture of extruded bars are as shown in Figure 10, wherein shown in microscopic structure such as Figure 10 (a),
Its average grain size is 880nm, and extruding is prepared magnesium alloy rod sampling and is processed into tensile sample, room is carried out on stretching-machine
Temperature stretches, and tensile speed 1mm/min, room temperature tensile mechanical property is as shown in table 5, stretching fracture pattern such as Figure 10 (b) institute
Show.
The magnesium alloy of 5 embodiment 5 of table squeezes bar room temperature tensile mechanical property
Embodiment 6
Wrought magnesium alloy ingredient is Al:1.3%, Zn:1.8%, Ca:0.25%, Mn:0.25%, Gd by mass percentage:
0.3%, Mg are surplus, and impurity F e content controls below 0.003%.
(1) using melting resistance furnace under No. five flux protections, according to the mass percent melting raw material of wrought magnesium alloy,
Magnesium ingot is heated to 720 DEG C of fusings, according to the mass percentage composition of wrought magnesium alloy, Al ingot, Zn ingot is added to having melted
Magnesium liquid in, with No. five flux-refining 20min, when temperature rises to 730 DEG C, the intermediate alloy of Mg-25%Gd is added, stirring is equal
It is even, obtain Mg-Al-Zn-Gd melt；
(2) low temperature is except iron processing: Mg-Al-Zn-Gd melt being cooled to 660 DEG C, and MnCl is added2Carry out it is dual except iron,
Guarantee that Fe content is less than 0.003% in magnesium alloy；
(3) except Mg-30%Ca intermediate alloy is added when melt temperature is increased to 705 DEG C after iron, the two of 8min is then carried out
Secondary refining, the casting yield of Ca are 60%；
(4) when melt temperature is 695 DEG C, in N2+SF6Mixed gas protected lower beginning electromagnetism semi-continuous casting starts electricity
Magnetic semi-continuous casting applies electromagnetic conditions are as follows: number of ampere turns 12000AN, electromagnetic frequency 15Hz, duty ratio 20%, casting
Speed is 60mm/min, water 450L/min, and obtaining diameter of section is 312mm, and length is the magnesium alloy ingot base of 6000mm,
Its chemical analysis group becomes Mg-1.3Al-1.8Zn-0.25Mn-0.25Ca-0.3Gd；
(5) segmentation of magnesium alloy ingot base is put into the Homogenization Treatments that heat-treatment furnace carries out 390 ± 5 DEG C × 16h, it will be uniform
Change ingot casting progress sawing handle, according to the sawing of extrusion die size and is turned into the cylinder blank of Φ 295mm × 600mm
It is used in case squeezing；
(6) cylinder blank is heated to 250 DEG C in furnace and keeps the temperature 180min, obtains magnesium alloy extrusion blank, together
When extrusion cylinder, extrusion die and extruding pad be heated to 250 DEG C, then in extrusion die inner wall, magnesium alloy extrusion blank
Surface and extrusion cylinder inner wall are smeared grease based on molybdenum disulfide lithium and are lubricated, then on 500 tons of hydraulic presses, with 1.7m/min
Extrusion speed squeezed, extrusion ratio 16, squeeze obtain diameter be 75mm extruded bar from magnesium alloy, gained extruded bars
Microscopic structure and stretching fracture scanning pattern picture it is as shown in figure 11, wherein shown in microscopic structure such as Figure 11 (a), average crystalline substance
Particle size is 1250nm, and tensile sample is processed into the magnesium alloy rod sampling for squeezing preparation, room temperature drawing is carried out on stretching-machine
It stretches, tensile speed 1mm/min, room temperature tensile mechanical property is as shown in table 6, shown in stretching fracture pattern such as Figure 11 (b).
The extruded bar from magnesium alloy room temperature tensile mechanical property of 6 embodiment 6 of table
Claims (6)
1. a kind of have the characteristics that the wrought magnesium alloy of nano-structure, which is characterized in that the ingredient of the alloy is by mass percentage
Al:0.8~1.5%, Zn:1.5~2.5%, Ca:0.15~0.4%, Mn:0.2~0.4%, Gd:0.15~0.3%, Mg are
Surplus, impurity F e content control below 0.003%.
2. according to claim 1 have the characteristics that the wrought magnesium alloy of nano-structure, which is characterized in that average grain size
For 300~1250nm, tensile strength is 280~330MPa, and yield strength is 260~310MPa, elongation at break is 16~
25%.
3. a kind of preparation method with the wrought magnesium alloy of nano-structure described in claim 1, which is characterized in that step
It is rapid as follows:
(1) melting raw material: according to the mass percent of wrought magnesium alloy, Mg ingot being heated to melting, and Al ingot and Zn is then added
Ingot refines 20min, Mg-Gd intermediate alloy is added when temperature is 720~740 DEG C, is stirred evenly, it is molten to obtain Mg-Al-Zn-Gd
Body；
(2) cooling is except iron processing: Mg-Al-Zn-Gd melt obtained by step (1) being cooled to 660~670 DEG C, and MnCl is added2Into
Row is dual to remove Fe；
(3) adding raw materials Ca: melt temperature is increased at 700~720 DEG C among addition Mg-Ca after removing iron obtained by step (2)
Alloy stirs evenly, and the time≤10min obtains Mg-Al-Zn-Gd-Mn-Ca melt；
(4) electromagnetism semi-continuous casting: Mg-Al-Zn-Gd-Mn-Ca melt is cooled to 680~700 DEG C, in N2+SF6Mixed gas
Protection is lower to carry out electromagnetism semi-continuous casting, obtains magnesium alloy ingot base；
(5) Homogenization Treatments: carrying out 16~20h of Homogenization Treatments for magnesium alloy ingot base under the conditions of 380~400 DEG C, will be equal
Homogenizing treated, ingot casting carries out turning, obtains the good casting ingot of turning；
(6) extrusion process: the good casting ingot of turning being put into resistance furnace and is heated to 110~250 DEG C, and heat preservation 120~
180min obtains magnesium alloy extrusion blank, squeezes it, and extrusion ratio is 16~25, and extrusion speed is 1.0~2.0m/
Min obtains the extruded bar from magnesium alloy that specification is 20~75mm of Φ.
4. preparation method according to claim 3, which is characterized in that in the step (3), the casting yield of Ca reaches 50~
60%.
5. preparation method according to claim 3, which is characterized in that in the step (4), electromagnetism semi-continuous casting condition
Are as follows: magnet exciting coil number of ampere turns is 3000~12000AN, and electromagnetic frequency is 15~30Hz, and casting speed is 60~150mm/min,
Water is 100~450L/min.
6. preparation method according to claim 3, which is characterized in that in the step (6), will squeeze and fill before extrusion operation
It puts into preheating in heating furnace, reaches extruding and require temperature, using grease based on molybdenum disulfide lithium as lubricant, uniformly smear
On extrusion die inner wall, magnesium alloy extrusion blank surface and extrusion cylinder inner wall.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111455245A (en) * | 2020-05-21 | 2020-07-28 | 东北大学 | High-strength Mg-Ca-Mn-Al-Zn series wrought magnesium alloy containing gadolinium-yttrium rare earth elements and preparation method thereof |
| CN111996427A (en) * | 2020-09-03 | 2020-11-27 | 兰州理工大学 | High-strength and high-toughness magnesium alloy capable of being extruded at low temperature and preparation method thereof |
| CN113083930A (en) * | 2021-04-12 | 2021-07-09 | 兰州理工大学 | Differential thermal forming method for preparing high-strength and high-toughness magnesium alloy |
| CN115074563A (en) * | 2022-06-29 | 2022-09-20 | 华南理工大学 | High-strength-toughness low-alloy-content Mg-Zn-Ca alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300918A (en) * | 2017-01-11 | 2018-07-20 | 北京科技大学 | One kind having high room temperature forming property calcic rare earth-magnesium alloy board and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108300918A (en) * | 2017-01-11 | 2018-07-20 | 北京科技大学 | One kind having high room temperature forming property calcic rare earth-magnesium alloy board and preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111455245A (en) * | 2020-05-21 | 2020-07-28 | 东北大学 | High-strength Mg-Ca-Mn-Al-Zn series wrought magnesium alloy containing gadolinium-yttrium rare earth elements and preparation method thereof |
| CN111996427A (en) * | 2020-09-03 | 2020-11-27 | 兰州理工大学 | High-strength and high-toughness magnesium alloy capable of being extruded at low temperature and preparation method thereof |
| CN111996427B (en) * | 2020-09-03 | 2021-11-02 | 兰州理工大学 | High-strength and high-toughness magnesium alloy capable of being extruded at low temperature and preparation method thereof |
| CN113083930A (en) * | 2021-04-12 | 2021-07-09 | 兰州理工大学 | Differential thermal forming method for preparing high-strength and high-toughness magnesium alloy |
| CN115074563A (en) * | 2022-06-29 | 2022-09-20 | 华南理工大学 | High-strength-toughness low-alloy-content Mg-Zn-Ca alloy and preparation method thereof |
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