CN102672146A - Method for compositely refining solidification structure of magnesium alloy by combination of current and Zr - Google Patents
Method for compositely refining solidification structure of magnesium alloy by combination of current and Zr Download PDFInfo
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- CN102672146A CN102672146A CN2012101393668A CN201210139366A CN102672146A CN 102672146 A CN102672146 A CN 102672146A CN 2012101393668 A CN2012101393668 A CN 2012101393668A CN 201210139366 A CN201210139366 A CN 201210139366A CN 102672146 A CN102672146 A CN 102672146A
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Abstract
The invention relates to a method for compositely refining a solidification structure of a magnesium alloy by combination of current and Zr. A Zr refiner is added in a smelting process of the magnesium alloy and current is introduced in a solidification process of the magnesium alloy till the magnesium alloy is solidified completely. The method provided by the invention comprises the specific steps of: (1) placing an electrode in a cast, and connecting the electrode with a power supply and pre-adjusting current parameters; (2) smelting the magnesium alloy by regular smelting, refining, drossing and peeling steps; (3) adding the Zr refiner till temperature of a mother solution of the magnesium alloy is adjusted to a predetermined temperature, and agitating and standing; and (4) pouring the mother solution of the magnesium alloy to the cast and turning on a power supply switch to introduce current from the beginning of pouring to complete solidication of the cast so as to obtain the refined solidification structure of the magnesium alloy. The method provided by the invention adopts a composite method which combines physical refining with chemical refining, is able to obtain the structure of the magnesium alloy with more smaller grains, more uniform structure and remarkably reduced deficiency, improves the mechanical property of the magnesium alloy, and is suitable for solidification and refining of the magnesium alloy.
Description
Technical field
The present invention relates to a kind of thinning process of magnesium alloy solidification tissue, specifically, relate to the method for a kind of electric current and Zr coupling composite refining magnesium alloy solidification tissue, belong to metal material and metallurgical technology field.
Background technology
Remarkable advantage such as magnesium and magnesium alloy have that density is little, specific strength and specific stiffness height and the prices of raw and semifnished materials are lower receives attention more and more widely.Magnesium alloy has broad application prospects in fields such as automobile, Aero-Space, military project, 3C Products.China is magnesium resource and magnesium alloy big producing country, and magnesium and magnesium alloy ingot output account for the over half of Gross World Product, further develops the novel reinforced technology of magnesium alloy and meets magnesium alloy national project research and development strategic demand.
As everyone knows, grain refinement technology is the unique channel that effectively improves material plasticity under the intensity index prerequisite not sacrificing, and no matter is as-cast structure or the heat-treated sturcture after Overheating Treatment.At present, cast magnesium alloy is mainly through adding Zr to realize the refinement of solidified structure.In fusion process, the Zr recovery rate is extremely low, is generally less than 30%, and therefore, Zr is also very limited to the influence of magnesium alloy solidification structure refinement degree.
There are some researches show that electric current is with its distinctive energy way of output refinement alloy graining tissue more effectively, its mechanism of action is: reduce phase driving force, improve nucleation rate; Segregation is grown up, is reduced in the broken dendrite of mangneto blockage effect and shear stress, nodularization crystal grain, inhibition.Electric current itself has environmental friendliness, applies easy, obvious results characteristics, iron and steel, aluminium alloy, existing a small amount of application the in titanium alloy solidified structure refinement field, but still is in the scientific research stage in the magnesium alloy field.
Summary of the invention
The objective of the invention is to be directed against the single use of above-mentioned prior art Zr carries out refinement to the magnesium alloy solidification tissue deficiency; The method of a kind of electric current and Zr coupling composite refining magnesium alloy solidification tissue is provided; Adopt physical thinning and the complex method that chemical refinement combines, reach the effect of outburst forming core, nucleus propagation, further refinement magnesium alloy solidification tissue; Improve magnesium alloy mechanical property, widen the Application of Magnesium scope.
For realizing above purpose, the present invention solves its technical problem through following technical scheme:
The method of a kind of electric current and Zr coupling composite refining magnesium alloy solidification tissue is characterized in that: in the magnesium alloy smelting process, add the Zr fining agent, in magnesium alloy in course of solidification, feed electric current and solidify fully until magnesium alloy.
The method of electric current of the present invention and Zr coupling composite refining magnesium alloy solidification tissue, it comprises following concrete steps:
(1) in the casting mold of mould, settles electrode, and electrode and power supply are joined, regulate current parameters in advance;
(2) fusing, the refining through routine successively, skim and peeler's ordered pair magnesium alloy carries out melting;
(3) treat that magnesium alloy mother liquor temperature is adjusted to design temperature, interpolation Zr fining agent also stirs, leaves standstill;
(4) cast magnesium alloy mother liquor in the casting mold of mould turns on the power switch simultaneously, continues to feed electric current until the complete solidificating period of foundry goods from the cast beginning, obtains the magnesium alloy solidification tissue of refinement.
The material of said electrode is magnesium, aluminium, zinc, copper, graphite or steel.
Design temperature in the said step (3) is 780～800 ℃.
Said Zr fining agent is that sponge Zr, compound add Zr, salt-mixture and add Zr and intermediate alloy and add one or more the mixture among the Zr.
Said electric current is DC current, alternating current, pulse current or lightning current.
Described DC current is 60A.
Described pulse current is peak value 100A, and frequency is 200Hz.
Described alternating current is 1000A, 1000Hz.
Thinking of the present invention is novel, integrates chemistry, physical thinning is technological, has the composite refining function, adopts basic casting technique and simple production equipment, realized the refinement of magnesium alloy solidification tissue, thereby the present invention has the following advantages:
1, the present invention is merged Zr thinning method and electric current refinement technology first; The disperse that has realized second phase distributes; Disturbance through electric current has reduced casting inherent shortcomings such as cold shut, shrinkage porosite and segregation better, has significantly improved the quality of magnesium alloy ingot and the strength and toughness of foundry goods.
2, in the galvanization, the diffusion couple magnesium alloy of electrode material has played the effect of a small amount of compensator alloy element.
Description of drawings
Fig. 1 is the current treatment device sketch map.
Fig. 2 is among the embodiment one, the WE43 magnesium alloy solidification tissue that obtains under the identical Zr content different disposal technology, wherein,
The 1# foundry goods that Fig. 2 (a) obtains for the Zr thinning processing, Fig. 2 (b) are that electric current and Zr composite refining are handled the 2# foundry goods that obtains.
The ZM6 magnesium alloy solidification tissue that Fig. 3 obtains for identical Zr content different disposal technology among the embodiment two, wherein,
The 1# ingot casting that Fig. 3 (a) obtains for the Zr thinning processing, Fig. 3 (b) are that electric current and Zr composite refining are handled the 2# ingot casting that obtains.
The ZM2 magnesium alloy solidification tissue that Fig. 4 obtains for identical Zr content different disposal technology among the embodiment three, wherein,
The 1# foundry goods that Fig. 4 (a) obtains for the Zr thinning processing, Fig. 4 (b) are that electric current and Zr composite refining are handled the 2# foundry goods that obtains.
Among the above-mentioned figure, 1-protection gas mixing arrangement, 2-resistance furnace temperature controller, 3-thermocouple, 4-gas blow pipe, 5-melting kettle, 6-electrode holder, 7-electrode, 8-casting mold, 9-power supply.
The specific embodiment
The present invention is merged physical thinning and chemical refinement first, unites through electric current and Zr and uses refinement magnesium alloy solidification tissue, promptly in the magnesium alloy smelting process, adds Zr, in magnesium alloy in course of solidification, feeds electric current and solidifies fully until magnesium alloy.
Below in conjunction with accompanying drawing embodiments of the invention are elaborated, present embodiment is that prerequisite has provided detailed embodiment and concrete operating process with technical scheme of the present invention, but protection scope of the present invention is not limited only to following embodiment.
The method of electric current according to the invention and Zr coupling composite refining magnesium alloy solidification tissue adopts current treatment device as shown in Figure 1 to realize.This current treatment device comprises protection gas mixing arrangement 1, resistance furnace temperature controller 2, thermocouple 3, gas blow pipe 4, melting kettle 5, electrode holder 6, electrode 7, casting mold 8 and power supply 9.Melting kettle 5 is used for the melting magnesium alloy, and it is positioned in the resistance furnace; Resistance furnace temperature controller 2 is in order to the temperature of melt in the control melting kettle 5, and links to each other with thermocouple 3 in being placed in melting kettle 5; Protection gas mixing arrangement 1 is in order to hybrid protection gas, and links to each other with gas blow pipe 4 in feeding melting kettle 5; Casting mold 8 is in order to pouring cast part; Electrode 7 is placed in the casting mold 8, and is connected to feed electric current with power supply 9; Electrode holder 6 is in order to holding electrode 7.
The concrete steps of the method for the invention are summarized as follows:
(1) in the casting mold 8 of mould, settles electrode 7, and electrode 7 and power supply 9 are joined, regulate the electric current technological parameter in advance;
(2) fusing, the refining through routine successively, skim and remove the peel operation, carrying out melting in the magnesium alloy in the melting kettle 5;
(3) treat magnesium alloy mother liquor temperature stabilization to design temperature, add a certain amount of Zr and stir, leave standstill;
When (4) treating that the mother liquor temperature is reduced to 740～760 ℃; Cast magnesium alloy mother liquor in the casting mold 8 of mould; Turn on the power switch simultaneously; Continue to feed electric current until the complete solidificating period of foundry goods from cast beginning, can obtain that crystal grain is tiny, the magnesium alloy solidification tissue of the refinement of second disperse, even tissue.
Through the embodiment of some common cast magnesium alloys, the present invention is further described below.In order the result to be compared analysis, the foundry goods of the also useful conventional Zr process for refining cast of implementing simultaneously with the method for the invention among the embodiment.
Embodiment one
WE43 magnesium alloy (Mg-4wt.%Y-2wt.%Nd-1wt.%Gd-0.5wt.%Zr; Wherein, Wt.% is meant the percentage of the magnesium alloy gross mass that ingredients constitute is prepared) batching fusing refining process is following: all instruments shift to an earlier date swabbing, and instrument, furnace charge, refining agent are all 180 ℃ of oven dry more than 4 hours; Opening resistor stove, preheating stainless steel melting kettle 5 add magnesium ingot to kermesinus, beginning in the time of 500 ℃ to feed volume ratios through protection gas mixing arrangement 1 and gas blow pipe 4 is 100: 1 CO
2+ 5F
6Protective gas is all accomplished until founding work; Melting kettle 5 is warming up to 690 ℃ all melts, temperature is adjusted to 720～740 ℃, add the Mg-25wt.%Y intermediate alloy behind the temperature stabilization until pure magnesium; Treat that it melts fully, when melt temperature is stabilized in 720～740 ℃, add mishmetal intermediate alloy (Mg-25wt.%Nd and Mg-25wt.%Gd), melt the back fully and stirred 2 minutes through the refining spoon; Temperature is adjusted to 800 ℃, and to add quality be that (mass ratio is K for the mixing Zr salt of alloy total amount 1.5%
2ZrF
6: ZrCl
4: KCl=2: 2: 1), drag for the end until completely melted and stirred 7～10 minutes, leave standstill 5～10min then, treating that temperature is reduced in 750～760 ℃ of scopes carries out refining, sinks to refining stirring 8～10min apart from alloy liquid level 2/3rds places with the refining spoon, drags for end scarfing cinder; Temperature is adjusted to 795 ℃ leaves standstill 10～15min, be cooled to 760 ℃ and pour into a mould after removing the liquid level slags.
The conventional method casting obtains foundry goods 1#.In casting mold 8, settle graphite electrode 7 in addition, opening power 9 adopts DC current, and the adjusting electric current is 60A, and mother liquor is poured in the casting mold 8, begins to keep the continuous firing of electric current to finish until whole process of setting from cast, and the powered-down switch obtains foundry goods 2#.Choose two foundry goods same area and carry out fabric analysis, as shown in Figure 2, Fig. 2 (a) is for adopting the WE43 magnesium alloy solidification tissue of Zr refinement, and Fig. 2 (b) is the WE43 magnesium alloy solidification tissue of electric current and Zr composite refining.The ICP-MS composition detection is the result show, the mass percentage content of Zr: 1# is 0.48wt.%, and 2# is 0.49wt.%.
The result shows; Compare with the WE43 magnesium alloy solidification tissue that single use Zr refinement obtains; Primary-Mg all obtains obvious refinement with eutectic structure in the WE43 magnesium alloy tissue that employing the inventive method obtains; Wherein primary-Mg phase crystal grain more rounding, size be reduced to the former 2/3, eutectic structure is disperse and distributes.
Embodiment two
ZM6 magnesium alloy (Mg-2.6wt.%Nd-0.6wt.%Zn-0.8wt.%Zr) batching fusing refining process is following: all instruments shift to an earlier date swabbing, and instrument, furnace charge, refining agent are all dried more than 4 hours at 180 ℃; Opening resistor stove, preheating stainless steel melting kettle 5 add magnesium ingot to kermesinus, begin to feed volume ratio in the time of 500 ℃ and be 100: 1 CO
2+ SF
6Protective gas is all accomplished until founding work; Melting kettle 5 is warming up to 690 ℃ all melts, temperature is adjusted to 720～740 ℃, add Zn behind the temperature stabilization until pure magnesium; Treat that Zn melts fully, when melt temperature is stabilized in 720～740 ℃, add the Mg-30wt.%Nd intermediate alloy, melt the back fully and stirred 2 minutes through the refining spoon; With temperature be adjusted to 790 ℃ add quality be alloy total amount 3.5% contain Zr compound (mass ratio is K2ZrF6: NaCl: KCl=2: 1: 1), drag for the end until completely melted and stirred 7～10 minutes; Leave standstill 5～10min, treating that temperature is reduced in 750～760 ℃ of scopes carries out refining, sinks to apart from alloy liquid level 2/3rds places refining with the refining spoon and stirs 8～10min, drags for end scarfing cinder; Temperature is adjusted to 790 ℃ leaves standstill 10～15min, be cooled to 750 ℃ and pour into a mould after removing the liquid level slags.
Conventional casting obtains ingot casting 1#.In casting mold 8, settle steel electrode 7 in addition, opening power 9 adopts alternating current; The adjusting electric current is 100A, and frequency is 200Hz, and mother liquor is poured in the casting mold 8; Begin to keep the continuous firing of electric current to finish until whole process of setting from cast, the powered-down switch obtains ingot casting 2#.Choose two ingot casting same area and carry out fabric analysis, as shown in Figure 3, Fig. 3 (a) is for adopting the ZM6 magnesium alloy solidification tissue of Zr refinement, and Fig. 3 (b) is the ZM6 magnesium alloy solidification tissue of electric current and Zr composite refining.The ICP-MS composition detection is the result show, the mass percentage content of Zr: 1# is 0.41wt.%, and 2# is 0.43wt.%.
Compare with the ZM6 magnesium alloy solidification tissue that single use Zr refinement obtains; Primary-Mg all obtains tangible refinement with eutectic structure in the ZM6 magnesium alloy tissue that employing the inventive method obtains; Wherein primary-Mg phase crystal grain more rounding, size be reduced to the former 1/2, eutectic structure is disperse and distributes, is mostly that corynebacterium and content decrease.
Embodiment three
ZM2 magnesium alloy (Mg-4.2wt.%Zn-Nd1.5wt.%-0.6wt.%Zr) batching fusing refining process is following: all instruments shift to an earlier date swabbing, and instrument, furnace charge, refining agent are all dried more than 4 hours at 180 ℃; Opening resistor stove, preheating stainless steel melting kettle 5 add magnesium ingot to kermesinus, begin to feed volume ratio in the time of 500 ℃ and be 100: 1 CO
2+ SF
6Protective gas is all accomplished until founding work; Melting kettle 5 is warming up to 690 ℃ all melts, temperature is adjusted to 720～740 ℃, add Zn behind the temperature stabilization until pure magnesium; Treat that Zn melts fully, when melt temperature is stabilized in 720～740 ℃, add cerium-rich mischmetal, melt the back fully and stirred 2 minutes through the refining spoon; It is the Mg-30wt.%Zr intermediate alloy of alloy total amount 0.8% that temperature is adjusted to 780 ℃ of adding quality, drags for the end until completely melted and stirs 7～10 minutes; Leave standstill 5～10min, treating that temperature is reduced in 750～760 ℃ of scopes carries out refining, sinks to apart from alloy liquid level 2/3rds places refining with the refining spoon and stirs 8～10min, drags for end scarfing cinder; Temperature is adjusted to 780 ℃ leaves standstill 10～15min, be cooled to 740 ℃ and pour into a mould after removing the liquid level slags.
Conventional casting obtains foundry goods 1#.In casting mold 8, settle zinc electrode 7 in addition, opening power 9 adopts pulse current; Electric current is 1000A, and frequency is 1000Hz, and mother liquor is poured in the casting mold 8; Begin to keep the continuous firing of electric current to finish until whole Hirschfeld-Klinger reaction process from cast, the powered-down switch obtains foundry goods 2#.Choose two foundry goods same area and carry out fabric analysis, as shown in Figure 4, Fig. 4 (a) is for adopting the ZM2 magnesium alloy solidification tissue of Zr refinement, and Fig. 4 (b) is the ZM2 magnesium alloy solidification tissue of electric current and Zr composite refining.The ICP-MS composition detection is the result show, the mass percentage content of Zr: 1# is 0.65wt.%, and 2# is 0.66wt.%.
Compare with the ZM2 magnesium alloy solidification tissue that single use Zr refinement obtains; Primary-Mg all obtains obvious refinement with eutectic structure in the ZM2 magnesium alloy tissue that employing the inventive method obtains; Primary-Mg phase crystal grain rounding, size more is reduced to the former 1/3, and eutectic structure is disperse and distributes, is mostly that intensive corynebacterium and content decrease.
Comprehensive three above-mentioned embodiment; Experimental result proves: compare the magnesium alloy solidification tissue that uses the independent thinning processing of Zr to obtain; The solidified structure that obtains through the method for the invention is more tiny; The nodularization degree is higher, and second has realized the distribution of disperse mutually, and casting inherent shortcomings such as cold shut, shrinkage porosite and segregation all have improvement in various degree.
Claims (9)
1. the method for electric current and Zr coupling composite refining magnesium alloy solidification tissue is characterized in that: in the magnesium alloy smelting process, add the Zr fining agent, in magnesium alloy in course of solidification, feed electric current and solidify fully until magnesium alloy.
2. the method for electric current according to claim 1 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: said method comprises following concrete steps:
(1) in the casting mold of mould, settles electrode, and electrode and power supply are joined, regulate current parameters in advance;
(2) fusing, the refining through routine successively, skim and peeler's ordered pair magnesium alloy carries out melting;
(3) treat that magnesium alloy mother liquor temperature is adjusted to design temperature, interpolation Zr fining agent also stirs, leaves standstill;
(4) cast magnesium alloy mother liquor in the casting mold of mould turns on the power switch simultaneously, continues to feed electric current until the complete solidificating period of foundry goods from the cast beginning, obtains the magnesium alloy solidification tissue of refinement.
3. the method for electric current according to claim 2 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: the material of said electrode is magnesium, aluminium, zinc, copper, graphite or steel.
4. the method for electric current according to claim 2 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: the design temperature in the said step (3) is 780～800 ℃.
5. the method for electric current according to claim 1 and 2 and Zr coupling composite refining magnesium alloy solidification tissue is characterized in that: said Zr fining agent is that sponge Zr, compound add Zr, salt-mixture and add Zr and intermediate alloy and add one or more the mixture among the Zr.
6. according to the method for claim 1 with 2 described electric currents and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: said electric current is DC current, alternating current, pulse current or lightning current.
7. the method for electric current according to claim 6 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: described DC current is 60A.
8. the method for electric current according to claim 6 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: described pulse current is peak value 100A, frequency is 200Hz.
9. the method for electric current according to claim 6 and Zr coupling composite refining magnesium alloy solidification tissue, it is characterized in that: described alternating current is 1000A, 1000Hz.
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| CN103773987A (en) * | 2014-01-20 | 2014-05-07 | 上海交通大学 | Magnesium alloy solidification structure zirconium refining method |
| CN104128592A (en) * | 2014-08-14 | 2014-11-05 | 昆明理工大学 | Device for refining metal solidification structure with electric current pulses |
| CN109266889A (en) * | 2018-12-05 | 2019-01-25 | 四川大学 | A kind of composite refining method of the magnesium alloy containing zirconium |
| CN113774242A (en) * | 2021-08-18 | 2021-12-10 | 北京科技大学 | Method for rapidly eliminating element segregation in rare earth magnesium alloy by using pulse current |
| CN114182130A (en) * | 2021-12-02 | 2022-03-15 | 上海航天精密机械研究所 | Refining agent for magnesium alloy with high rare earth content, preparation method and application method |
| CN115815570A (en) * | 2023-02-15 | 2023-03-21 | 中北大学 | Vacuum electromagnetic low-pressure mold filling device and process for preparing heterogeneous composite structure by adopting same |
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| CN113774242A (en) * | 2021-08-18 | 2021-12-10 | 北京科技大学 | Method for rapidly eliminating element segregation in rare earth magnesium alloy by using pulse current |
| CN114182130A (en) * | 2021-12-02 | 2022-03-15 | 上海航天精密机械研究所 | Refining agent for magnesium alloy with high rare earth content, preparation method and application method |
| CN115815570A (en) * | 2023-02-15 | 2023-03-21 | 中北大学 | Vacuum electromagnetic low-pressure mold filling device and process for preparing heterogeneous composite structure by adopting same |
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Application publication date: 20120919 |