CN101693957B - Al-Co grain refiner of Mg-Al-based alloy, preparation method and using method thereof - Google Patents
Al-Co grain refiner of Mg-Al-based alloy, preparation method and using method thereof Download PDFInfo
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- CN101693957B CN101693957B CN2009101878648A CN200910187864A CN101693957B CN 101693957 B CN101693957 B CN 101693957B CN 2009101878648 A CN2009101878648 A CN 2009101878648A CN 200910187864 A CN200910187864 A CN 200910187864A CN 101693957 B CN101693957 B CN 101693957B
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Abstract
The invention relates to an Al-Co grain refiner of Mg-Al-based alloy, a preparation method and a using method thereof. The refiner comprises the components by weight percent: 20-34% of Al and 66-80% of Co which have the grain diameter of 25-35[mu]m. The preparation method comprises the following steps: (1) blending according to the weight percent of the components of the Al-Co grain refiner: 20-34% of Al and 66-80% of Co, and obtaining mixed metal; (2) washing the mixed metal; and (3) putting the washed mixed metal into an electric arc furnace, vacuumizing and filling argon gas into the electric arc furnace for smelting for four times, and finally crushing into grains with the grain diameter of 25-35[mu]m by a physical method. The preparation method and the using method of the Al-Co grain refiner of the Mg-Al-based alloy are simple, and the volume of addition and the refining effect of the Al-Co grain refiner are easily controlled, so that the aim of very good refining can be achieved by adding trace of the Al-Co grain refiner, and the refining effect does not fade within 1h.
Description
Technical field
The present invention relates to a kind of grain-refining agent and preparation method thereof and using method, be specifically related to the aluminium Co grain refiner and preparation method thereof and the using method of a kind of Mg-Al base alloy.
Background technology
Though magnesium alloy has wide application prospect in all fields of traffic, aerospace and communication, enlarge the Application of Magnesium scope, also must solve the problem that magnesium and alloy self thereof exist.Magnesium and alloy substrate thereof are close-packed hexagonal structure, have only a basal slip system under the room temperature, and the deformation at room temperature ability is difficult to shape; The chemical property of magnesium is active, and standard potential is very low, and the natural oxide film of formation is fine and close inadequately, so corrosion stability of magnesium alloy is very poor; The room temperature strength of magnesium alloy is low, the not enough 300MPa of the tensile strength of cast magnesium alloys, and wrought magnesium alloys undercapacity 400MPa can not satisfy the performance requriements of load spare.And grain refining is to address the above problem, and improves the important means of as-cast magnesium alloy and over-all properties thereof.
At present, the method for Mg-Al based alloy grain refinement has a variety of, and as overheated method, carbonaceous breeds method, microalloying etc.Generally to breed method be to add C in magnesium alloy to the carbonaceous of Cai Yonging
2Cl
6Or CCl
4, these alterants produce chlorine after adding, environment and human body are produced serious harm, and (20～30min) its thinning effects are taking off easily just, need carry out secondary metamorphic and handle in very short time.Some investigators also by adding Mg-Al-C, Al-C, Al-Ti-C master alloy, add pure Al
4C
3, mode refining Mg-Al-based alloy such as SiC particle, but these alloys and particle preparation technology are comparatively complicated.
Summary of the invention
At the problem of the grain-refining agent complicated process of preparation of existing Mg-Al base alloy, the invention provides a kind of aluminium Co grain refiner and preparation method thereof and using method of Mg-Al base alloy.
The composition of aluminium Co grain refiner of the present invention is Al 20～34% by weight percentage, and Co 66～80%, and particle diameter is 25～35 μ m.
1, be Al 20～34% by weight percentage with metallic aluminium and cobalt metal, Co 66～80% batchings obtain hybrid metal.
2, hybrid metal is cleaned, purging method is to be under the ultrasonic wave condition of 40～60KHz in frequency with hybrid metal, cleans with organic solvent ethanol or acetone, and scavenging period is 3～5min.
3, the hybrid metal after will cleaning places electric arc furnace, and electric arc furnace is vacuumized, and charging into argon gas to electric arc furnace internal gas pressure again is 0.02～0.04MPa; Wherein to vacuumize and require air pressure be 1 * 10 to electric arc furnace
-3～5 * 10
-3MPa.Hybrid metal is carried out four meltings, and the voltage that applies during melting is 20～45V, and electric current is 200～350A, each melting time spent 2～3min.Alloy physics after the melting is broken into the particle that particle diameter is 25～35 μ m, obtains the aluminium Co grain refiner.
The using method of aluminium Co grain refiner of the present invention is:
During melting Mg-Al base alloy, at Mg-Al base alloy melt temperature is under 700～750 ℃ of conditions, to place Mg-Al base alloy liquation with the aluminium Co grain refiner of aluminium foil parcel, leave standstill 20～60min after stirring then, the add-on of aluminium Co grain refiner is 0.5～2.5% of a Mg-Al base alloy liquation gross weight.
Leave standstill and finish back slagging-off, cast, the average refinement rate of crystal grain of the Mg-Al base alloy of acquisition is about 50%.
The aluminium Co grain refiner that preparation method of the present invention obtains is block aluminium cobalt master alloy product.Product preparation method of the present invention and using method are simple, and the addition of product and thinning effect are easy to control, add the purpose can reach fine refinement with trace, and thinning effect taking off not in 1h.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the aluminium Co grain refiner of preparation in the embodiment of the invention 1, and a is an aluminium cobalt phase among the figure.
Fig. 2 is the metallography microscope photo of the 0#AZ31 magnalium base alloy in the embodiment of the invention 1.
Fig. 3 is the metallography microscope photo of the 1#AZ31 magnalium base alloy in the embodiment of the invention 1.
Fig. 4 is the metallography microscope photo of the 2#AZ31 magnalium base alloy in the embodiment of the invention 1.
Fig. 5 is the metallography microscope photo of the 3#AZ31 magnalium base alloy in the embodiment of the invention 1.
Fig. 6 is the metallography microscope photo of the 4#AZ31 magnalium base alloy in the embodiment of the invention 1.
Fig. 7 is the metallography microscope photo of the 5#AZ31 magnalium base alloy in the embodiment of the invention 1.
Embodiment
Weight purity 〉=99.99% of the metallic aluminium that adopts in the embodiment of the invention, weight purity 〉=99.88% of cobalt metal, weight purity 〉=99.99% of metallic zinc, weight purity 〉=99.95% of MAGNESIUM METAL.
The ethanol that adopts in the embodiment of the invention is industrial spirit, and the acetone of employing is industrial acetone.
The ultrasonic equipment model that adopts in the embodiment of the invention is KUDOS-SK3300LHC.
The encloses container that adopts in the embodiment of the invention is a silica tube.
The resistance furnace that adopts in the embodiment of the invention is a MRL-8 type well formula resistance furnace.
The crucible that adopts in the embodiment of the invention is the high-strength graphite crucible.
The angle grinding machine that adopts in the embodiment of the invention is the solid VG100DE type angle of a German prestige grinding machine, and working conditions is 500r/min.
Embodiment 1
With metallic aluminium and cobalt metal mix, wherein metallic aluminium accounts for 30% of mixture by weight percentage, and cobalt metal accounts for 70% of mixture by weight percentage, obtains hybrid metal.
Be to clean with organic solvent under the ultrasonic wave condition of 40KHz in frequency with hybrid metal, scavenging period is 3min, and organic solvent is an ethanol.
Hybrid metal after cleaning is placed electric arc furnace, electric arc furnace is vacuumized, charging into argon gas to electric arc furnace internal gas pressure again is 0.02MPa; Wherein to be evacuated to air pressure be 1 * 10 to electric arc furnace
-3MPa.
Hybrid metal is carried out melting, and the voltage that applies during melting is 45V, and electric current is 200A, melting time spent 2min, and melt back is four times in a manner described; Physics is broken into the particle that particle diameter is 25～35 μ m then, obtains the aluminium Co grain refiner, and its composition is Al 30% by weight percentage, and Co 70%, and the X-ray diffraction spectrogram as shown in Figure 1.
Adopt metallic aluminium, MAGNESIUM METAL, metallic zinc to prepare AZ31 magnalium base alloy; with metallic aluminium, MAGNESIUM METAL, metallic zinc as requested proportioning get the raw materials ready; then respectively with angle grinding machine polishing light; put into loft drier again, under 200 ℃ of conditions, heat 10min, put into the crucible that cleans up then; crucible is placed resistance furnace; be heated to 400～500 ℃ to resistance furnace, feed shielding gas, shielding gas is N
2+ SF
6Mixed gas, nitrogen and SF in the mixed gas
6The blending ratio of gas is 1000: 2 by volume.
Continuing heating resistor stove to temperature is 750 ℃, metal all melts in the crucible, to join in the molten metal with the aluminium Co grain refiner of aluminium foil parcel, it all is 0.5% of Mg-Al base alloy liquation gross weight that add-on is respectively, 1%, 1.5%, 2%, 2.5%, leave standstill 60min after stirring then.
Leaving standstill the oxide slag body of taking the alloy molten surface after the end off, being poured into preheating temperature is in 250 ℃ the irony mold, add-on by the aluminium Co grain refiner is 0.5% of a Mg-Al base alloy liquation gross weight, 1%, 1.5%, 2%, 2.5%, obtain 1#, 2#, 3#, 4#, 5#AZ31 magnalium base alloy respectively, the metallography microscope photo behind 400 ℃ of isothermal processes 4h is respectively shown in Fig. 3,4,5,6,7 then.
Preparation AZ31 magnalium base alloy under the situation that does not add the aluminium Co grain refiner obtains 0#AZ31 magnalium base alloy as stated above, and the metallography microscope photo behind 400 ℃ of isothermal processes 4h as shown in Figure 2 then.
By Fig. 2,3,4,5,6,7 as seen, behind the use aluminium Co grain refiner, compare with not using grain-refining agent, the average grain size of AZ31 magnalium base alloy is reduced to 43～46 μ m by 92 μ m, and refinement efficient reaches 50～53%.
Embodiment 2
With metallic aluminium and cobalt metal mix, wherein metallic aluminium accounts for 20% of mixture by weight percentage, and cobalt metal accounts for 80% of mixture by weight percentage, obtains hybrid metal.
Be to clean with organic solvent under the ultrasonic wave condition of 60KHz in frequency with hybrid metal, scavenging period is 5min, and organic solvent is an ethanol.
Hybrid metal after cleaning is placed electric arc furnace, electric arc furnace is vacuumized, charging into argon gas to electric arc furnace internal gas pressure again is 0.04MPa; Wherein to be evacuated to air pressure be 5 * 10 to electric arc furnace
-3MPa.
Hybrid metal is carried out melting, and the voltage that applies during melting is 30V, and electric current is 270A, melting time spent 3min, and melt back is four times in a manner described; Physics is broken into the particle that particle diameter is 25～35 μ m then, obtains the aluminium Co grain refiner, and its composition is Al 20% by weight percentage, and Co 80%.
Adopt metallic aluminium, MAGNESIUM METAL, metallic zinc to prepare AZ31 magnalium base alloy; with metallic aluminium, MAGNESIUM METAL, metallic zinc as requested proportioning get the raw materials ready; then respectively with angle grinding machine polishing light; put into loft drier again, under 200 ℃ of conditions, heat 10min, put into the crucible that cleans up then; crucible is placed resistance furnace; be heated to 400～500 ℃ to resistance furnace, feed shielding gas, shielding gas is N
2+ SF
6Mixed gas, the blending ratio of nitrogen and SF6 gas is 1000: 2 by volume in the mixed gas.
Continuing heating resistor stove to temperature is 700 ℃, metal all melts in the crucible, to join in the molten metal with the aluminium Co grain refiner of aluminium foil parcel, it all is 0.5% of Mg-Al base alloy liquation gross weight that add-on is respectively, 1%, 1.5%, 2%, 2.5%, leave standstill 40min after stirring then.
After using the aluminium Co grain refiner, compare with not using grain-refining agent, the average crystal grain refinement efficient of AZ31 magnalium base alloy reaches 50～53%.
Embodiment 3
With metallic aluminium and cobalt metal mix, wherein metallic aluminium accounts for 34% of mixture by weight percentage, and cobalt metal accounts for 66% of mixture by weight percentage, obtains hybrid metal.
Be to clean with organic solvent under the ultrasonic wave condition of 50KHz in frequency with hybrid metal, scavenging period is 4min, and organic solvent is an acetone.
Hybrid metal after cleaning is placed electric arc furnace, electric arc furnace is vacuumized, charging into argon gas to electric arc furnace internal gas pressure again is 0.03MPa; Wherein to be evacuated to air pressure be 3 * 10 to electric arc furnace
-3MPa.
Hybrid metal is carried out melting, and the voltage that applies during melting is 20V, and electric current is 350A, melting time spent 2.5min, and melt back is four times in a manner described; Physics is broken into the particle that particle diameter is 25～35 μ m then, obtains the aluminium Co grain refiner, and its composition is Al 34% by weight percentage, and Co 66%.
Adopt metallic aluminium, MAGNESIUM METAL, metallic zinc to prepare AZ31 magnalium base alloy; with metallic aluminium, MAGNESIUM METAL, metallic zinc as requested proportioning get the raw materials ready; then respectively with angle grinding machine polishing light; put into loft drier again, under 200 ℃ of conditions, heat 10min, put into the crucible that cleans up then; crucible is placed resistance furnace; be heated to 400～500 ℃ to resistance furnace, feed shielding gas, shielding gas is N
2+ SF
6Mixed gas, nitrogen and SF in the mixed gas
6The blending ratio of gas is 1000: 2 by volume.
Continuing heating resistor stove to temperature is 720 ℃, metal all melts in the crucible, to join in the molten metal with the aluminium Co grain refiner of aluminium foil parcel, it all is 0.5% of Mg-Al base alloy liquation gross weight that add-on is respectively, 1%, 1.5%, 2%, 2.5%, leave standstill 20min after stirring then.
After using the aluminium Co grain refiner, compare with not using grain-refining agent, the average crystal grain refinement efficient of AZ31 magnalium base alloy reaches 50～53%.
Claims (3)
1. the preparation method of the aluminium Co grain refiner of Mg-Al base alloy, it is characterized in that carrying out according to the following steps: (1) is Al 20～34% by the moiety weight percent of aluminium Co grain refiner, Co 66～80% batchings obtain hybrid metal; (2) hybrid metal is cleaned; (3) hybrid metal after will cleaning places electric arc furnace, then electric arc furnace is vacuumized, and charging into argon gas to electric arc furnace internal gas pressure again is 0.02～0.04MPa; Hybrid metal is carried out four meltings, and the voltage that applies during melting is 20～45V, and electric current is 200～350A, each melting time spent 2～3min; Alloy physics after the melting is broken into the particle that particle diameter is 25～35 μ m, obtains the aluminium Co grain refiner.
2. the preparation method of the aluminium Co grain refiner of Mg-Al base alloy according to claim 1 is characterized in that electric arc furnace is vacuumized in the described step (3): require air pressure 1 * 10
-3～5 * 10
-3MPa.
3. the preparation method of the aluminium Co grain refiner of Mg-Al base alloy according to claim 1, it is characterized in that described hybrid metal is cleaned is to be under the ultrasonic wave condition of 40～60KHz in frequency with hybrid metal, clean with organic solvent ethanol or acetone, scavenging period is 3～5min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101878648A CN101693957B (en) | 2009-10-14 | 2009-10-14 | Al-Co grain refiner of Mg-Al-based alloy, preparation method and using method thereof |
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|---|---|---|---|
| CN2009101878648A CN101693957B (en) | 2009-10-14 | 2009-10-14 | Al-Co grain refiner of Mg-Al-based alloy, preparation method and using method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102251129A (en) * | 2011-07-15 | 2011-11-23 | 燕山大学 | Refiner for magnesium-aluminum-based alloy and preparation method thereof |
| CN103805795B (en) * | 2014-01-21 | 2015-09-02 | 苏州优诺电子材料科技有限公司 | A kind of alterant for tin-silver-copper solder or Sn-Cu solder melting and using method |
| CN106636701A (en) * | 2016-11-18 | 2017-05-10 | 扶绥县科学技术情报研究所 | Rare earth magnesium alloy fabrication method |
| CN106498250A (en) * | 2016-11-18 | 2017-03-15 | 扶绥县科学技术情报研究所 | The processing method of magnesium alloy |
| CN106756145A (en) * | 2016-11-18 | 2017-05-31 | 扶绥县科学技术情报研究所 | The preparation method of magnesium-rare earth |
| CN106480346A (en) * | 2016-11-18 | 2017-03-08 | 扶绥县科学技术情报研究所 | The preparation method of magnesium alloy |
| CN108754203A (en) * | 2018-07-10 | 2018-11-06 | 上海大学 | A kind of Alar fining agent of degeneration and its preparation method and application |
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