CN103981416B - A kind of Mg-Zn-RE-Zr series magnesium alloy and preparation method thereof - Google Patents

A kind of Mg-Zn-RE-Zr series magnesium alloy and preparation method thereof Download PDF

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CN103981416B
CN103981416B CN201410250496.8A CN201410250496A CN103981416B CN 103981416 B CN103981416 B CN 103981416B CN 201410250496 A CN201410250496 A CN 201410250496A CN 103981416 B CN103981416 B CN 103981416B
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magnesium alloy
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series magnesium
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CN103981416A (en
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孟健
邱鑫
程丽任
牛晓东
杜海
张德平
张洪杰
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps: 1), by Mg source, Zn source, Y source, Gd source, La source and Zr source melt, obtain aluminium alloy;2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C;3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C.The present invention uses Y source, Gd source and La source to prepare Mg-Zn-RE-Zr series magnesium alloy;And the present invention is by preparing technological parameter in Mg-Zn-RE-Zr series magnesium alloy process, enable method provided by the invention to prepare mechanical property is better and also Mg-Zn-RE-Zr series magnesium alloy that diameter dimension is bigger.

Description

A kind of Mg-Zn-RE-Zr series magnesium alloy and preparation method thereof
Technical field
The present invention relates to field of metal alloy technology, particularly relate to a kind of Mg-Zn-RE-Zr series magnesium alloy and preparation method thereof.
Background technology
Magnesium alloy is the structural metallic materials of a kind of lightweight, has density low, and specific strength and specific stiffness are high, damping capacity is good, and effectiveness is good, and casting character is excellent, the advantages such as good processability, magnesium alloy all has wide practical use in Aero-Space, auto industry and 3C industry.
Magnesium alloy can be divided into Mg-Al series alloy, Mg-Mn series alloy and Mg-Zn-Zr series alloy according to the difference of composition, and wherein Mg-Zn-Zr series alloy is a kind of high-strength-toughness magnesium alloy, and its performance is better than other two serial alloys.By adding rare earth element y or rich Y rare earth compound in Mg-Zn-Zr series alloy, the combination property of Mg-Zn-Zr series alloy can be improved further, such as MB25 alloy and MB26 alloy, particularly MB26 alloy, not only there is higher tensile strength (>=360MPa), yield strength (>=310MPa) and elongation percentage (>=13%), and less costly.MB26 alloy is along with the increase of Zn content, tensile strength and yield strength improve therewith, elongation percentage slightly declines, but the increase being as Zn content can reduce the temperature of solidus in the solid process of setting of alloy, especially when Zn content is more than 4.5wt%, the Production Practice of Casting Technologies of MB26 alloy is poor, it is easy to produce loose and hot tearing;And the addition of rare earth element y or rich Y compound, make the amount of contraction of alloy graining body increase, foundryman's fever stress sharply increases, and causes that MB26 alloy easily produces various casting flaws in casting process, particularly easily produces the casting crack of heart portion or edge;The phase transformation that in MB26 alloy graining process, alloy inside occurs simultaneously is while increasing strength of alloy and yield strength, too increasing the formation of grain boundaries micro-crack, above-mentioned reason makes the Mg-Zn-Zr series magnesium alloy mechanical property that prior art provides poor and smaller.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of Mg-Zn-RE-Zr series magnesium alloy and preparation method thereof, better and diameter dimension is bigger for the Mg-Zn-RE-Zr series magnesium alloy mechanical property that preparation method provided by the invention obtains.
The preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps:
1), by the fusing of Mg source, Zn source, Y source, Gd source, La source and Zr source, mixing, aluminium alloy is obtained;
2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;
3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;
Described Mg-Zn-RE-Zr series magnesium alloy includes: the La of Gd, the 0.2wt% of Y, the 0.4wt% of 0.5wt%~1.2wt%~0.7wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.
Preferably, described step 2) in pouring temperature be 700 DEG C~710 DEG C.
Preferably, described step 2) in poring rate be 30mm/min~36mm/min.
Preferably, described step 2) in rate of cooling be 3K/s~10K/s.
Preferably, described step 2) in liquid point depth be 200mm~280mm.
Preferably, described step 3) in annealing temperature be 260 DEG C~300 DEG C.
Preferably, described step 1) particularly as follows:
At the first temperature, being melted in Mg source and Zn source, obtain the first hybrid metal liquid, described first temperature is 670 DEG C~730 DEG C;
At the second temperature, by described first hybrid metal liquid and Y source, Gd source, the mixing of La source, obtaining the second hybrid metal liquid, described second temperature is 740 DEG C~780 DEG C;
At the 3rd temperature, described second hybrid metal liquid and Zr source being mixed, obtain aluminium alloy, described 3rd temperature is 760 DEG C~820 DEG C.
Preferably, described step 1) obtain aluminium alloy after also include standing described aluminium alloy, the temperature of described standing is 720 DEG C~780 DEG C.
The invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, Y including 0.5wt%~1.2wt%, the Gd of 0.4wt%~0.7wt%, the La of 0.2wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.
Preferably, including the Gd of Y, the 0.46wt% of 0.54wt%~0.73wt%~0.62wt%, the Zr of Zn, the 0.43wt% of La, the 4.8wt% of 0.23wt%~0.42wt%~5.2wt%~0.54wt%, impurity element total amount < 0.05wt%, surplus is Mg.
The preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps: 1), by Mg source, Zn source, Y source, Gd source, La source and Zr source melt, mixing, obtain aluminium alloy;2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;Described Mg-Zn-RE-Zr series magnesium alloy includes: the La of Gd, the 0.2wt% of Y, the 0.4wt% of 0.5wt%~1.2wt%~0.7wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.The present invention is in the process preparing Mg-Zn-RE-Zr series magnesium alloy, use Y source, Gd source and La source, rare earth element y, Gd and the La coagulation factor in Mg-Zn-RE-Zr series magnesium alloy is different, decreases present invention tearing tendency of ingot casting in preparing Mg-Zn-RE-Zr series magnesium alloy process;And the present invention passes through to control the technological parameter of pouring temperature, poring rate, rate of cooling, liquid point depth and annealing in the process preparing Mg-Zn-RE-Zr series magnesium alloy, avoid prepare in Mg-Zn-RE-Zr series magnesium alloy process crack, shrinkage porosite, cold shut and segregation defect, enable method provided by the invention prepare mechanical property better and also the bigger Mg-Zn-RE-Zr series magnesium alloy of diameter dimension.
Test result indicate that, the extrusion ratio of the Mg-Zn-RE-Zr series magnesium alloy that method provided by the invention prepares is 16, tensile strength is 361MPa~379MPa, yield strength is 315MPa~328MPa, elongation percentage is 13.4%~16.3%, diameter > 400mm, the length > 4000mm of the Mg-Zn-RE-Zr series magnesium alloy that the present invention prepares.
Detailed description of the invention
The preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps:
1), by the fusing of Mg source, Zn source, Y source, Gd source, La source and Zr source, mixing, aluminium alloy is obtained;
2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;
3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;
Described Mg-Zn-RE-Zr series magnesium alloy includes: the La of Gd, the 0.2wt% of Y, the 0.4wt% of 0.5wt%~1.2wt%~0.7wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.
The present invention is in the process preparing Mg-Zn-RE-Zr series magnesium alloy, use Y source, Gd source and La source, rare earth element y, Gd and the La coagulation factor in Mg-Zn-RE-Zr series magnesium alloy is different, decreases present invention tearing tendency of ingot casting in preparing Mg-Zn-RE-Zr series magnesium alloy process;And the present invention passes through to control the technological parameter of pouring temperature, poring rate, rate of cooling, liquid point depth and annealing in the process preparing Mg-Zn-RE-Zr series magnesium alloy, avoid prepare in Mg-Zn-RE-Zr series magnesium alloy process crack, shrinkage porosite, cold shut and segregation defect, enable method provided by the invention prepare mechanical property better and also the bigger Mg-Zn-RE-Zr series magnesium alloy of diameter dimension.
Mg source, Zn source, Y source, Gd source, La source and Zr source are melted by the present invention, mixing, obtain aluminium alloy.The temperature and time of described fusing, mixing is not had a special restriction by the present invention, described fusing, mixing temperature and time can make above-mentioned Mg source, Zn source, Y source, Gd source, La source and the fusing of Zr source mix homogeneously.The equipment of described fusing, mixing is not had special restriction by the present invention, adopts smelting furnace well known to those skilled in the art.The present invention, preferably in carrying out above-mentioned fusing, mixing in the smelting furnace containing RJ-5 flux, carries out above-mentioned fusing, mixing more preferably in the smelting furnace containing the RJ-5 flux melted.
Mg source and Zn source preferably at the first temperature, are melted, are obtained the first hybrid metal liquid by the present invention, and described first temperature is 670 DEG C~730 DEG C;At the second temperature, by described first hybrid metal liquid and Y source, Gd source, the mixing of La source, obtaining the second hybrid metal liquid, described second temperature is 740 DEG C~780 DEG C;At the 3rd temperature, described second hybrid metal liquid and Zr source being mixed, obtain aluminium alloy, described 3rd temperature is 760 DEG C~820 DEG C.
Mg source and Zn source preferably at the first temperature, are melted, are obtained the first hybrid metal liquid by the present invention, and described first temperature is 670 DEG C~730 DEG C;More preferably Mg source is melted, in the Mg liquid obtained, add Zn source, obtain the first hybrid metal liquid.In the present invention, described first temperature is more preferably 680 DEG C~720 DEG C, it is most preferred that be 690 DEG C~700 DEG C.
After obtaining the first hybrid metal liquid, the present invention preferably at the second temperature, by described first hybrid metal liquid and Y source, Gd source, the mixing of La source, obtains the second hybrid metal liquid, and described second temperature is 740 DEG C~780 DEG C;More preferably Y source, Gd source and La source are joined in described first hybrid metal liquid, obtain the second hybrid metal liquid.In the present invention, described second temperature is more preferably 750 DEG C~770 DEG C.
After obtaining the second hybrid metal liquid, the present invention is preferably in, at the 3rd temperature, mixing described second hybrid metal liquid and Zr source, obtain aluminium alloy, and described 3rd temperature is 760 DEG C~820 DEG C;More preferably in, at the 3rd temperature, Zr source being joined in described second hybrid metal liquid, obtain aluminium alloy.In the present invention, described 3rd temperature is more preferably 780 DEG C~810 DEG C, it is most preferred that be 790 DEG C~800 DEG C.
In the present invention, described Mg source is preferably high purity magnesium.In the present invention, described Zn source is preferably high purity zinc.The source in described Mg source and Zn source is not had special restriction by the present invention, can be bought by market and obtain.Kind and the source in described Y source, Gd source, La source and Zr source are not had special restriction by the present invention, adopt Y source well known to those skilled in the art, Gd source, La source and Zr source, can be bought by market and obtain.In the present invention, described Y source is preferably Mg-Y intermediate alloy.In the present invention, in described Mg-Y intermediate alloy, the mass content of Y is preferably 20%~30%, more preferably 24%~28%, it is most preferred that be 25%.
In the present invention, described Gd source is preferably Mg-Gd intermediate alloy.In the present invention, in described Mg-Gd intermediate alloy, the mass content of Gd is preferably 20%~30%, more preferably 24%~28%, it is most preferred that be 25%.In the present invention, described La source is preferably Mg-La intermediate alloy.In the present invention, in described Mg-La intermediate alloy, the mass content of La is preferably 20%~30%, more preferably 24%~28%, it is most preferred that be 25%.In the present invention, described Zr source is preferably Mg-Zr intermediate alloy.In the present invention, in described Mg-Zr intermediate alloy, the mass content of Zr is preferably 20%~30%, more preferably 24%~28%, it is most preferred that be 25%.
Before the fusing of described Mg source, Zn source, Y source, Gd source, La source and Zr source, mixing, described Mg source, Zn source, Y source, Gd source, La source and Zr source are preferably preheated by the present invention.In the present invention, the temperature of described preheating is preferably 150 DEG C~280 DEG C, more preferably 160 DEG C~260 DEG C, it is most preferred that be 170 DEG C~240 DEG C, is the most preferably 170 DEG C~220 DEG C.The time of described preheating is not had special restriction, described preheating time to make above-mentioned Mg source, Zn source, Y source, Gd source, La source and Zr source reach described preheating temperature by the present invention.
After obtaining aluminium alloy, described aluminium alloy is preferably carried out refine, skims by the present invention.Described refine and the method skimmed are not had special restriction by the present invention, adopt the refine used by well known to those skilled in the art preparation in magnesium alloy process and the technical scheme skimmed.Described aluminium alloy is preferably carried out blowing argon gas refine by the present invention, skims after the aluminium alloy after refine is removed argon.
After obtaining aluminium alloy, described aluminium alloy is preferably stood by the present invention, and the temperature of described standing is 720 DEG C~780 DEG C.The present invention by carrying out the bubble that standing can be removed in described aluminium alloy to described aluminium alloy, and makes the impurities sink down in aluminium alloy.The present invention stands after preferably described aluminium alloy being carried out above-mentioned refine, skimmed.In the present invention, the temperature of described standing is more preferably 740 DEG C~770 DEG C, it is most preferred that be 750 DEG C~760 DEG C.In the present invention, the time of described standing is preferably 0.5 hour~2 hours, more preferably 1 hour~1.5 hours.
After obtaining aluminium alloy, described aluminium alloy is cast by the present invention, obtains cast alloy, and pouring temperature during described casting is 690 DEG C~720 DEG C, poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm.Described casting is carried out when the present invention is preferably in protective gas.The kind of described protective gas and source are not had special restriction by the present invention, adopt and well known to those skilled in the art prepare protective gas used during magnesium alloy, can be bought acquisition by market.In the present invention, described protective gas is preferably SF6And CO2.The equipment of described casting is not had special restriction by the present invention, adopts casting equipment well known to those skilled in the art.In an embodiment of the present invention, the equipment of described casting can be crystallizer.In the present invention, the chuck of described crystallizer is preferably copper chuck.The diameter of described crystallizer chuck is not had special restriction by the present invention, and those skilled in the art can according to the crystallizer chuck of the size Selection different-diameter of required Mg-Zn-RE-Zr series magnesium alloy.
In the present invention, pouring temperature during described casting is preferably 700 DEG C~710 DEG C.In the present invention, poring rate during described casting is preferably 30mm/min~36mm/min, more preferably 33mm/min~35mm/min.In the present invention, rate of cooling during described casting is preferably 3K/s~10K/s.Present invention preferably employs cooling water and carry out described cooling.In the present invention, the pressure of described cooling water is preferably 0.02MPa~0.05MPa, more preferably 0.03MPa~0.04MPa, it is most preferred that for 0.035MPa~0.038MPa.In the present invention, the flow velocity of described cooling water is preferably 6.9m3/ h~9.3m3/ h, more preferably 7.2m3/ h~8.4m3/ h, it is most preferred that for 7.5m3/ h~8m3/h.In the present invention, when adopting cooling water to carry out described cooling, the temperature of secondary cooling water is preferably 25 DEG C~48 DEG C, more preferably 28 DEG C~42 DEG C, it is most preferred that be 31 DEG C~38 DEG C.In the present invention, liquid point depth during described casting is preferably 200mm~280mm, more preferably 230mm~260mm, it is most preferred that for 240mm~250mm.
After obtaining cast alloy, described cast alloy is annealed processing by the present invention, obtains Mg-Zn-RE-Zr series magnesium alloy, and the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours.The present invention by being annealed described cast alloy processing thus the internal stress removed in described cast alloy.In the present invention, the temperature of described annealing is preferably 260 DEG C~300 DEG C, more preferably 270 DEG C~280 DEG C.In the present invention, the time of described annealing is preferably 9 hours~11 hours, more preferably 10 hours.
In the present invention, described Mg-Zn-RE-Zr series magnesium alloy includes: the Y of 0.5wt%~1.2wt%, the Gd of 0.4wt%~0.7wt%, the La of 0.2wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.The present invention can control the composition of alloy by the addition in Mg source, Zn source, Y source, Gd source, La source and Zr source described in control technique scheme, prepares the Mg-Zn-RE-Zr series magnesium alloy of described composition.
The invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, including: the Y of 0.5wt%~1.2wt%, the Gd of 0.4wt%~0.7wt%, the La of 0.2wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.In the present invention, described Mg-Zn-RE-Zr series magnesium alloy preferably includes: the Y of 0.54wt%~0.73wt%, the Gd of 0.46wt%~0.62wt%, the La of 0.23wt%~0.42wt%, the Zn of 4.8wt%~5.2wt%, the Zr of 0.43wt%~0.54wt%, impurity element total amount < 0.05wt%, surplus is Mg.In the present invention, the preparation method of described Mg-Zn-RE-Zr series magnesium alloy is consistent with the preparation method of Mg-Zn-RE-Zr series magnesium alloy described in technique scheme, does not repeat them here.
The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the standard testing present invention of present invention GB/T228.1-2010 " metal material stretching test part 1: room temperature test method " prepares, test result is the extrusion ratio of the Mg-Zn-RE-Zr series magnesium alloy that the present invention prepares is 16, tensile strength is 361MPa~379MPa, yield strength is 315MPa~328MPa, elongation percentage is 13.4%~16.3%, and mechanical property is better.The Mg-Zn-RE-Zr series magnesium alloy that the present invention is prepared carries out dimensional measurement, and measurement result is diameter > 400mm, the length > 4000mm of the Mg-Zn-RE-Zr series magnesium alloy that the present invention prepares.The Mg-Zn-RE-Zr series magnesium alloy that the present invention is prepared carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the present invention prepares.
The preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps: 1), by Mg source, Zn source, Y source, Gd source, La source and Zr source melt, mixing, obtain aluminium alloy;2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;Described Mg-Zn-RE-Zr series magnesium alloy includes: the La of Gd, the 0.2wt% of Y, the 0.4wt% of 0.5wt%~1.2wt%~0.7wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.The present invention is in the process preparing Mg-Zn-RE-Zr series magnesium alloy, use Y source, Gd source and La source, rare earth element y, Gd and the La coagulation factor in Mg-Zn-RE-Zr series magnesium alloy is different, decreases present invention tearing tendency of ingot casting in preparing Mg-Zn-RE-Zr series magnesium alloy process;And the present invention passes through to control the technological parameter of pouring temperature, poring rate, rate of cooling, liquid point depth and annealing in the process preparing Mg-Zn-RE-Zr series magnesium alloy, avoid prepare in Mg-Zn-RE-Zr series magnesium alloy process crack, shrinkage porosite, cold shut and segregation defect, enable method provided by the invention prepare mechanical property better and also the bigger Mg-Zn-RE-Zr series magnesium alloy of diameter dimension.
In order to further appreciate that the present invention, below in conjunction with embodiment, Mg-Zn-RE-Zr series magnesium alloy provided by the invention and preparation method thereof is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Raw material used in following example of the present invention is commercial goods, Mg used is high purity magnesium, Zn is high purity zinc, in Mg-Zr intermediate alloy, the mass content of Zr is 25%, in Mg-Y intermediate alloy, the mass content of Y is 20%, in Mg-Gd intermediate alloy, the mass content of Gd is 25%, and in Mg-La intermediate alloy, the mass content of La is 20%.
Embodiment 1
The Mg-Zr intermediate alloy of Zn, 160kg of Mg, 105kg of 1565kg, the Mg-Y intermediate alloy of 100kg, the Mg-Gd intermediate alloy of 45kg and the Mg-La intermediate alloy of 25kg are preheating to 200 DEG C;
At 680 DEG C, the Mg after above-mentioned preheating is put into and melts containing in the smelting furnace of the RJ-5 flux melted, after described Mg is completely melt, in the Mg liquid obtained, adds the Zn of above-mentioned preheating, obtain the first hybrid metal liquid;
At 760 DEG C, in above-mentioned first hybrid metal liquid, add the Mg-Y intermediate alloy of above-mentioned preheating, Mg-Gd intermediate alloy and Mg-La intermediate alloy, obtain the second hybrid metal liquid;
At 780 DEG C, in above-mentioned second hybrid metal liquid, add the Mg-Zr intermediate alloy of above-mentioned preheating, obtain aluminium alloy;
Skim after described aluminium alloy blowing argon gas refine, removing argon, the aluminium alloy after skimming is stood 1h in the standing furnace of 760 DEG C;
At SF6Gas and CO2Under the protection of gas; aluminium alloy after above-mentioned standing is imported in the diverter at crystallizer center; enter after making the shunting of described aluminium alloy in the copper chuck of crystallizer that diameter is 480mm, pouring temperature be 700 DEG C, the dummy ingot decrease speed of crystallizer is 36mm/min, water pressure of cooling water be 0.03MPa, cooling water flow velocity is 7.2m3/ h, secondary cooling water water temperature be 38 DEG C, liquid point depth when being 250mm, described aluminium alloy is cast, obtain cast alloy;
Described cast alloy is carried out at 232 DEG C the annealing of 12h, obtains Mg-Zn-RE-Zr series magnesium alloy.
The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 is obtained by spectroanalysis instrument is adopted to carry out composition detection, testing result is that the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 obtains includes: the Y of 0.73wt%, the Gd of 0.56wt%, the La of 0.23wt%, the Zn of 5.2wt%, the Zr of 0.54wt%, surplus is Mg.The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the method test embodiment of the present invention 1 described in technique scheme obtains, test result is as shown in table 1, the mechanical experimental results of the Mg-Zn-RE-Zr series magnesium alloy that table 1 obtains for the embodiment of the present invention.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 is obtained carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 obtains.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 is obtained carries out dimensional measurement, and measurement result is the diameter of the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 1 obtains is 465mm, and length is 4175mm, larger in size.
Embodiment 2
The Mg-Zr intermediate alloy of Zn, 150kg of Mg, 100kg of 1585kg, the Mg-Y intermediate alloy of 90kg, the Mg-Gd intermediate alloy of 40kg and the Mg-La intermediate alloy of 35kg are preheating to 180 DEG C;
At 700 DEG C, the Mg after above-mentioned preheating is put into and melts containing in the smelting furnace of the RJ-5 flux melted, after described Mg is completely melt, in the Mg liquid obtained, adds the Zn of above-mentioned preheating, obtain the first hybrid metal liquid;
At 750 DEG C, in above-mentioned first hybrid metal liquid, add the Mg-Y intermediate alloy of above-mentioned preheating, Mg-Gd intermediate alloy and Mg-La intermediate alloy, obtain the second hybrid metal liquid;
At 800 DEG C, in above-mentioned second hybrid metal liquid, add the Mg-Zr intermediate alloy of above-mentioned preheating, obtain aluminium alloy;
Skim after described aluminium alloy blowing argon gas refine, removing argon, the aluminium alloy after skimming is stood 1.5h in the standing furnace of 770 DEG C;
At SF6Gas and CO2Under the protection of gas; aluminium alloy after above-mentioned standing is imported in the diverter at crystallizer center; enter after making the shunting of described aluminium alloy in the copper chuck of crystallizer that diameter is 480mm, pouring temperature be 705 DEG C, the dummy ingot decrease speed of crystallizer is 33mm/min, water pressure of cooling water be 0.035MPa, cooling water flow velocity is 7.8m3/ h, secondary cooling water water temperature be 36 DEG C, liquid point depth when being 280mm, described aluminium alloy is cast, obtain cast alloy;
Described cast alloy is carried out at 260 DEG C the annealing of 11h, obtains Mg-Zn-RE-Zr series magnesium alloy.
The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 is obtained by method described in embodiment 1 carries out composition detection, testing result is that the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 obtains includes: the Y of 0.67wt%, the Gd of 0.46wt%, the La of 0.34wt%, the Zn of 4.8wt%, the Zr of 0.43wt%, surplus is Mg.The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the method test embodiment of the present invention 2 described in technique scheme obtains, test result is as shown in table 2.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 is obtained carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 obtains.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 is obtained carries out dimensional measurement, and measurement result is the diameter of the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 2 obtains is 465mm, and length is 4780mm, larger in size.
Embodiment 3
The Mg-Zr intermediate alloy of Zn, 160kg of Mg, 90kg of 1570kg, the Mg-Y intermediate alloy of 80kg, the Mg-Gd intermediate alloy of 55kg and the Mg-La intermediate alloy of 45kg are preheating to 220 DEG C;
At 690 DEG C, the Mg after above-mentioned preheating is put into and melts containing in the smelting furnace of the RJ-5 flux melted, after described Mg is completely melt, in the Mg liquid obtained, adds the Zn of above-mentioned preheating, obtain the first hybrid metal liquid;
At 780 DEG C, in above-mentioned first hybrid metal liquid, add the Mg-Y intermediate alloy of above-mentioned preheating, Mg-Gd intermediate alloy and Mg-La intermediate alloy, obtain the second hybrid metal liquid;
At 810 DEG C, in above-mentioned second hybrid metal liquid, add the Mg-Zr intermediate alloy of above-mentioned preheating, obtain aluminium alloy;
Skim after described aluminium alloy blowing argon gas refine, removing argon, the aluminium alloy after skimming is stood 2h in the standing furnace of 740 DEG C;
At SF6Gas and CO2Under the protection of gas; aluminium alloy after above-mentioned standing is imported in the diverter at crystallizer center; enter after making the shunting of described aluminium alloy in the copper chuck of crystallizer that diameter is 480mm, pouring temperature be 710 DEG C, the dummy ingot decrease speed of crystallizer is 30mm/min, water pressure of cooling water be 0.038MPa, cooling water flow velocity is 8.4m3/ h, secondary cooling water water temperature be 31 DEG C, liquid point depth when being 240mm, described aluminium alloy is cast, obtain cast alloy;
Described cast alloy is carried out at 280 DEG C the annealing of 8h, obtains Mg-Zn-RE-Zr series magnesium alloy.
The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 is obtained by method described in embodiment 1 carries out composition detection, testing result is that the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 obtains includes: the Y of 0.54wt%, the Gd of 0.62wt%, the La of 0.42wt%, the Zn of 4.5wt%, the Zr of 0.63wt%, surplus is Mg.The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the method test embodiment of the present invention 3 described in technique scheme obtains, test result is as shown in table 1.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 is obtained carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 obtains.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 is obtained carries out dimensional measurement, and measurement result is the diameter of the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 3 obtains is 466mm, and length is 4990mm, larger in size.
Embodiment 4
The Mg-Zr intermediate alloy of Zn, 120kg of Mg, 100kg of 1660kg, the Mg-Y intermediate alloy of 65kg, the Mg-Gd intermediate alloy of 35kg and the Mg-La intermediate alloy of 20kg are preheating to 220 DEG C;
At 670 DEG C, the Mg after above-mentioned preheating is put into and melts containing in the smelting furnace of the RJ-5 flux melted, after described Mg is completely melt, in the Mg liquid obtained, adds the Zn of above-mentioned preheating, obtain the first hybrid metal liquid;
At 740 DEG C, in above-mentioned first hybrid metal liquid, add the Mg-Y intermediate alloy of above-mentioned preheating, Mg-Gd intermediate alloy and Mg-La intermediate alloy, obtain the second hybrid metal liquid;
At 760 DEG C, in above-mentioned second hybrid metal liquid, add the Mg-Zr intermediate alloy of above-mentioned preheating, obtain aluminium alloy;
Skim after described aluminium alloy blowing argon gas refine, removing argon, the aluminium alloy after skimming is stood 2h in the standing furnace of 720 DEG C;
At SF6Gas and CO2Under the protection of gas; aluminium alloy after above-mentioned standing is imported in the diverter at crystallizer center; enter after making the shunting of described aluminium alloy in the copper chuck of crystallizer that diameter is 480mm, pouring temperature be 690 DEG C, the dummy ingot decrease speed of crystallizer is 27mm/min, water pressure of cooling water be 0.02MPa, cooling water flow velocity is 6.9m3/ h, secondary cooling water water temperature be 25 DEG C, liquid point depth when being 160mm, described aluminium alloy is cast, obtain cast alloy;
Described cast alloy is carried out at 300 DEG C the annealing of 10h, obtains Mg-Zn-RE-Zr series magnesium alloy.
The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 is obtained by method described in embodiment 1 carries out composition detection, testing result is that the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 obtains includes: the Y of 0.5wt%, the Gd of 0.4wt%, the La of 0.2wt%, the Zn of 5wt%, the Zr of 0.4wt%, surplus is Mg.The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the method test embodiment of the present invention 4 described in technique scheme obtains, test result is as shown in table 1.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 is obtained carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 obtains.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 is obtained carries out dimensional measurement, and measurement result is the diameter of the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 4 obtains is 464mm, and length is 4250mm, larger in size.
Embodiment 5
The Mg-Zr intermediate alloy of Zn, 180kg of Mg, 130kg of 1424kg, the Mg-Y intermediate alloy of 150kg, the Mg-Gd intermediate alloy of 56kg and the Mg-La intermediate alloy of 60kg are preheating to 220 DEG C;
At 730 DEG C, the Mg after above-mentioned preheating is put into and melts containing in the smelting furnace of the RJ-5 flux melted, after described Mg is completely melt, in the Mg liquid obtained, adds the Zn of above-mentioned preheating, obtain the first hybrid metal liquid;
At 760 DEG C, in above-mentioned first hybrid metal liquid, add the Mg-Y intermediate alloy of above-mentioned preheating, Mg-Gd intermediate alloy and Mg-La intermediate alloy, obtain the second hybrid metal liquid;
At 820 DEG C, in above-mentioned second hybrid metal liquid, add the Mg-Zr intermediate alloy of above-mentioned preheating, obtain aluminium alloy;
Skim after described aluminium alloy blowing argon gas refine, removing argon, the aluminium alloy after skimming is stood 2h in the standing furnace of 780 DEG C;
At SF6Gas and CO2Under the protection of gas; aluminium alloy after above-mentioned standing is imported in the diverter at crystallizer center; enter after making the shunting of described aluminium alloy in the copper chuck of crystallizer that diameter is 480mm, pouring temperature be 720 DEG C, the dummy ingot decrease speed of crystallizer is 40mm/min, water pressure of cooling water be 0.05MPa, cooling water flow velocity is 9.3m3/ h, secondary cooling water water temperature be 48 DEG C, liquid point depth when being 320mm, described aluminium alloy is cast, obtain cast alloy;
Described cast alloy is carried out at 320 DEG C the annealing of 9h, obtains Mg-Zn-RE-Zr series magnesium alloy.
The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 is obtained by method described in above-mentioned skill embodiment 1 carries out composition detection, testing result is that the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 obtains includes: the Y of 1.2wt%, the Gd of 0.7wt%, the La of 0.6wt%, the Zn of 6.4wt%, the Zr of 0.7wt%, surplus is Mg.The mechanical property of the Mg-Zn-RE-Zr series magnesium alloy that the method test embodiment of the present invention 5 described in technique scheme obtains, test result is as shown in table 1.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 is obtained carries out ultrasonic inspection, and result of detection is the internal casting flaw that can not survey of Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 obtains.The Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 is obtained carries out dimensional measurement, and measurement result is the diameter of the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention 5 obtains is 465mm, and length is 4588mm, larger in size.
The mechanical experimental results of the Mg-Zn-RE-Zr series magnesium alloy that table 1 embodiment of the present invention obtains
Extrusion ratio Tensile strength (MPa) Yield strength (MPa) Elongation percentage (%)
Embodiment 1 16 379 328 13.4
Embodiment 2 16 372 317 14.6
Embodiment 3 16 368 318 16.3
Embodiment 4 16 361 315 13.5
Embodiment 5 16 371 317 15.8
As shown in Table 1, the Mg-Zn-RE-Zr series magnesium alloy that the embodiment of the present invention prepares has good mechanical property.
As seen from the above embodiment, the preparation method that the invention provides a kind of Mg-Zn-RE-Zr series magnesium alloy, comprise the following steps: 1), Mg source, Zn source, Y source, Gd source, La source and Zr source are melted, mixing, obtain aluminium alloy;2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;Described Mg-Zn-RE-Zr series magnesium alloy includes: the La of Gd, the 0.2wt% of Y, the 0.4wt% of 0.5wt%~1.2wt%~0.7wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.The present invention is in the process preparing Mg-Zn-RE-Zr series magnesium alloy, use Y source, Gd source and La source, rare earth element y, Gd and the La coagulation factor in Mg-Zn-RE-Zr series magnesium alloy is different, decreases present invention tearing tendency of ingot casting in preparing Mg-Zn-RE-Zr series magnesium alloy process;And the present invention passes through to control the technological parameter of pouring temperature, poring rate, rate of cooling, liquid point depth and annealing in the process preparing Mg-Zn-RE-Zr series magnesium alloy, avoid prepare in Mg-Zn-RE-Zr series magnesium alloy process crack, shrinkage porosite, cold shut and segregation defect, enable method provided by the invention prepare mechanical property better and also the bigger Mg-Zn-RE-Zr series magnesium alloy of diameter dimension.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It should be pointed out that, for the person of ordinary skill of the art, under the premise without departing from the principles of the invention, it is also possible to the present invention carries out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.Described above to the disclosed embodiments, makes the special technical staff in this area be capable of or use the present invention, professional and technical personnel in the field be will be apparent from by the multiple amendment of these embodiments.Generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and novel features.

Claims (10)

1. a preparation method for Mg-Zn-RE-Zr series magnesium alloy, comprises the following steps:
1), by the fusing of Mg source, Zn source, Y source, Gd source, La source and Zr source, mixing, aluminium alloy is obtained;
2), being cast by described aluminium alloy, obtain cast alloy, pouring temperature during described casting is 690 DEG C~720 DEG C, and poring rate during described casting is 27mm/min~40mm/min, and rate of cooling during described casting is 1.8K/s~15K/s;Liquid point depth during described casting is 160mm~320mm;
3), by described cast alloy being annealed processing, obtain Mg-Zn-RE-Zr series magnesium alloy, the temperature of described annealing is 230 DEG C~320 DEG C, and the time of described annealing is 8 hours~12 hours;
The composition of described Mg-Zn-RE-Zr series magnesium alloy is: the Y of 0.5wt%~1.2wt%, the Gd of 0.4wt%~0.7wt%, the La of 0.2wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.
2. method according to claim 1, it is characterised in that described step 2) in pouring temperature be 700 DEG C~710 DEG C.
3. method according to claim 1, it is characterised in that described step 2) in poring rate be 30mm/min~36mm/min.
4. method according to claim 1, it is characterised in that described step 2) in rate of cooling be 3K/s~10K/s.
5. method according to claim 1, it is characterised in that described step 2) in liquid point depth be 200mm~280mm.
6. method according to claim 1, it is characterised in that described step 3) in annealing temperature be 260 DEG C~300 DEG C.
7. method according to claim 1, it is characterised in that described step 1) particularly as follows:
At the first temperature, being melted in Mg source and Zn source, obtain the first hybrid metal liquid, described first temperature is 670 DEG C~730 DEG C;
At the second temperature, by described first hybrid metal liquid and Y source, Gd source, the mixing of La source, obtaining the second hybrid metal liquid, described second temperature is 740 DEG C~780 DEG C;
At the 3rd temperature, described second hybrid metal liquid and Zr source being mixed, obtain aluminium alloy, described 3rd temperature is 760 DEG C~820 DEG C.
8. method according to claim 1, it is characterised in that described step 1) obtain aluminium alloy after also include standing described aluminium alloy, the temperature of described standing is 720 DEG C~780 DEG C.
9. a Mg-Zn-RE-Zr series magnesium alloy, composition is: the Y of 0.5wt%~1.2wt%, the Gd of 0.4wt%~0.7wt%, the La of 0.2wt%~0.6wt%, the Zn of 4.5wt%~6.4wt%, the Zr of 0.4wt%~0.7wt%, impurity element total amount < 0.05wt%, surplus is Mg.
10. Mg-Zn-RE-Zr series magnesium alloy according to claim 9, it is characterized in that, the composition of described Mg-Zn-RE-Zr series magnesium alloy is: the Y of 0.54wt%~0.73wt%, the Gd of 0.46wt%~0.62wt%, the Zr of Zn, the 0.43wt% of La, the 4.8wt% of 0.23wt%~0.42wt%~5.2wt%~0.54wt%, impurity element total amount < 0.05wt%, surplus is Mg.
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