CN103042199A - Magnesium alloy physical purification method and device - Google Patents

Magnesium alloy physical purification method and device Download PDF

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Publication number
CN103042199A
CN103042199A CN2012105170635A CN201210517063A CN103042199A CN 103042199 A CN103042199 A CN 103042199A CN 2012105170635 A CN2012105170635 A CN 2012105170635A CN 201210517063 A CN201210517063 A CN 201210517063A CN 103042199 A CN103042199 A CN 103042199A
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crucible
tantalum
magnesium alloy
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tantalum crucible
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CN103042199B (en
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彭秋明
房大庆
蔡康乐
刘丽
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Yanshan University
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Yanshan University
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Abstract

Provided are a magnesium alloy physical purification method and device. The magnesium alloy physical purification method includes that evenly mixed magnesium alloy is obtained through fusion under protection of mixed gases (1% SF6 and argon gases), the mixed melt is poured into a preheated tantalum crucible and is subjected to temperature rising and standing, the crucible is directly placed into a flowing water channel, and high-purity magnesium alloy with a refined structure is obtained. The magnesium alloy physical purification device comprises a water channel, a water inlet/outlet, a tantalum baffle, a tantalum crucible, a thermocouple, a protection gas vent pipe and a sealing cover. The magnesium alloy physical purification method and device are simple to operate, high in safety and yield and applicable to mass production.

Description

A kind of magnesium alloy physical purification method and purification devices thereof
Technical field: the invention belongs to metal material field, particularly a kind of preparation method of magnesium alloy.
Background technologyMagnesium alloy has that density is little, specific strength is high, processing welding and damping capacity well reach dimensionally stable, cheap, the advantage such as can recycle, more and more be subject to people's attention, be subject in the world great attention, be regarded as " green engineering material of 21 century ".
But the shortcoming of ordinary magnesium alloy is corrosion-resistant (Qiuming Peng et.al, Biomaterials, 2010), in humidity or salt mist environment, can cause part failure because of the impure point corrosion in a shorter period.If in magnesium alloy, be mingled with impurity, in extruding and rolling process, can obvious affect the mechanical property (Li Hualun of magnesium alloy, Special Processes of Metal Castings and non-ferrous alloy, 2003), this application to magnesium alloy is very disadvantageous, and is opposite, if magnesium alloy flux is mingled with and forms the Impurity Fe of micro cell, Ni, Cu, the strict limited content such as Si, magnesium alloy purity is improved, just can be good at improving corrosion resistance and the morphotropism of magnesium alloy.Therefore, prepare the important directions that high purity magnesium alloy has become the magnesium alloy development.
At present, the main purification process of magnesium alloy has solvent method (Lorentz Petter Lossius et.al, Acta Materials, 1996), the way of distillation (Zofia Kowalewska et.al, Acta Materials, 1999) and semi-continuous process (Zhang Zhiqiang et.al, Trans. Nonferrous Met.Soc.China, 2010).Solvent method normally passes through to add chloride and fluoride salt in the magnesium alloy smelting process, makes it to generate the multicomponent complex precipitation with oxide impurity and removes.Main shortcoming has been introduced the halogen ion exactly, brings secondary impurities into, causes the corrosion resistance of alloy sharply to descend.Compare with solvent method, way of distillation temperature is high, simultaneously because the fusing point of each element is different, therefore is difficult to obtain organizing consistent alloy material.The method of at present general semicontinuous ingot casting, can greatly put forward heavy alloyed purity, but this method normally directly is poured into the ingot casting surface with the water that flows, condition is very harsh, potential safety hazard is large, and solidifies normally lateral solidified inside of field, causes the center to be mingled with, or the bottom solidifies to top and forms a large amount of column crystals, and tissue odds is even.
Summary of the invention
The object of the present invention is to provide a kind of simple to operately, safe, yield rate is high, is fit to magnesium alloy physical purification method and the purification devices thereof of large-scale production.The present invention mainly is by special purification devices, and control setting temperature field discharged to the outside, finally obtains even tissue, the magnesium alloy that melt is clean, fine and close at the lower impurity of the effect of alloy graining auto purification.
Purification process of the present invention is as follows: with raw material magnesium alloy magnesium; aluminium; zinc etc. are at 300-400 ℃ of preheating 30-60 min; at 750 ℃; under mist-1%SF6+ argon shield; adopt the common graphite crucible for smelting; stir 30 min after adding successively fully; with the above-mentioned melt that mixes; be poured in the tantalum crucible of the purification devices of 620-700 ℃ of preheating 60-120 min; build the seal cover of crucible; in tantalum crucible, pass into mist-1%SF6+ argon gas by the protection breather pipe simultaneously; be warming up to 720 ℃ after the cast; left standstill 60-120 minute, and crucible was put into the tank of water filling with the speed of 10-100 mm/s.
Purification devices of the present invention mainly comprises: tank, intake-outlet, tantalum baffle plate, tantalum crucible, thermocouple, protection gas breather pipe and seal cover.Wherein, be provided with water inlet on the top of tank, be provided with delivery port in its underpart, tantalum crucible is located at above the above-mentioned tank, and the bottom of above-mentioned tantalum crucible is taper, and its angle is 120-175 °; Be arranged with inside and outside 2 layers of baffle plate at above-mentioned tantalum crucible bottom outer, angle between this baffle plate and the tantalum crucible is 45-90 °, the aspect ratio of Internal baffle and tantalum crucible is 1:1-2, the aspect ratio of outer baffle and Internal baffle is 1:2-3, distance between internal layer baffle plate and the sidewall of crucible is 400-500 mm, and the distance between the ectonexine baffle plate is 200-300 mm.Be provided with seal cover at above-mentioned tantalum crucible pot mouth, sealing covers and is provided with thermocouple and the protection breather pipe that inserts in the tantalum crucible, and above-mentioned thermocouple lower end can not contact the tantalum crucible limit, in order to observe the temperature of molten state alloy in the tantalum crucible.
The present invention compared with prior art has following advantage:
1, simple to operate, safe, yield rate is high, is fit to large-scale production.
2, can prevent that too much residue is arranged in the crucible, from the inside to the outside, form that inner impurity is few, the alloy of even tissue, stable performance.
3, utilize Temperature Field Control impurity clotting method, avoided secondary impurities.
Description of drawings
Fig. 1 is purification devices simplified schematic diagram of the present invention.
Fig. 2 be the AZ31 that obtains of the embodiment of the invention 1 with without impurity content column comparison diagram among the AZ31 of purification process.
Fig. 3 is the Mg-6Zn that obtains of the embodiment of the invention 2 and the corrosive nature column comparison diagram of Mg-6Zn in 3.5%NaCl solution without purification process.
Specific embodiment
Embodiment 1
In a kind of magnesium alloy physical purification device simplified schematic diagram shown in Figure 1, be provided with water inlet 2 on the top of tank 1, be provided with delivery port 8 in its underpart, tantalum crucible 4 is located at above the above-mentioned tank, the bottom of above-mentioned tantalum crucible is taper, its angle beta is 120 °, the height of tantalum crucible is 800 mm, be arranged with inside and outside 2 layers of baffle plate 3 at above-mentioned tantalum crucible bottom outer, angle [alpha] between this baffle plate and the tantalum crucible is 45 °, and the height of Internal baffle is 400 mm, and the height of outer baffle is 133 mm, distance between the ectonexine baffle plate is 300 mm, and the distance between internal layer baffle plate and the sidewall of crucible is 400 mm.Be provided with seal cover 7 at above-mentioned tantalum crucible pot mouth, sealing covers and is provided with thermocouple 5 and the protection breather pipe 6 that inserts in the tantalum crucible.
Get fine aluminium 0.15kg; zinc 0.05kg; magnesium 4.8kg; at 400 ℃ of preheating 30 min; at 750 ℃; under mist-1%SF6+ argon shield; adopt the common graphite crucible for smelting; stir 30 min after adding successively fully; with the above-mentioned melt that mixes; be poured in the tantalum crucible of the purification devices of 620 ℃ of preheating 60 min; build the seal cover of crucible, in tantalum crucible, pass into mist-1%SF6+ argon gas by the protection breather pipe simultaneously, be warming up to 720 ℃ after the cast; left standstill 60 minutes; crucible is put into the tank of water filling with the speed of 10 mm/s, just obtained even tissue, the AZ31 magnesium alloy that melt is clean.
As shown in Figure 2, compare with the magnesium alloy through purification process not through the magnesium alloy of purification process, obviously reduce through the impurity content of the magnesium alloy of purification process, and and alloy phase ratio on every side, the impurity content of core is on the low side, proves that the setting temperature field becomes all around and disperses distribution.
Embodiment 2
A kind of magnesium alloy physical purification device, top at tank is provided with water inlet, be provided with delivery port in its underpart, tantalum crucible is located at above the above-mentioned tank, the angle of the bottom taper of above-mentioned tantalum crucible is 150 °, the height of tantalum crucible is 600 mm, be arranged with inside and outside 2 layers of baffle plate at above-mentioned tantalum crucible bottom outer, angle between this baffle plate and the tantalum crucible is 90 °, the height of Internal baffle is 600 mm, the height of outer baffle is 300 mm, and the distance between the ectonexine baffle plate is 200 mm, and the distance between internal layer baffle plate and the sidewall of crucible is 500 mm.Be provided with seal cover at above-mentioned tantalum crucible pot mouth, sealing covers and is provided with thermocouple and the protection breather pipe that inserts in the tantalum crucible.
Get pure zinc 0.3kg; magnesium 4.7kg; with raw material magnesium alloy magnesium; zinc etc. are at 300 ℃ of preheating 60 min; at 750 ℃; under mist-1%SF6+ argon shield; adopt the common graphite crucible for smelting; stir 30 min after adding successively fully; with the above-mentioned melt that mixes; be poured in the tantalum crucible of the purification devices of 700 ℃ of preheating 120 min; build the seal cover of crucible; in tantalum crucible, pass into mist-1%SF6+ argon gas by the protection breather pipe simultaneously; be warming up to 720 ℃ after the cast, left standstill 120 minutes, crucible is put into the tank of water filling with the speed of 100 mm/s.
As shown in Figure 3, will put into 3.5%NaCl solution through Mg-6Zn magnesium alloy and the undressed Mg-6Zn magnesium alloy of purification process, and compare, the corrosion resistance of the alloy after the process purification process obviously improves, and proves that the setting temperature field becomes all around and disperses distribution.

Claims (3)

1. the purification process of a magnesium alloy physics; it is characterized in that: with raw material magnesium alloy magnesium; aluminium; zinc etc. are at 300-400 ℃ of preheating 30-60 min; at 750 ℃; under mist-1%SF6+ argon shield; adopt the common graphite crucible for smelting; stir 30 min after adding successively fully; with the above-mentioned melt that mixes; be poured in the tantalum crucible of the purification devices of 620-700 ℃ of preheating 60-120 min; build the seal cover of crucible; in tantalum crucible, pass into mist-1%SF6+ argon gas by the protection breather pipe simultaneously; be warming up to 720 ℃ after the cast, left standstill 60-120 minute, crucible is put into the tank of water filling with the speed of 10-100 mm/s.
2. the used purification devices of the claims 1, it mainly comprises: tank, intake-outlet, tantalum baffle plate, tantalum crucible, thermocouple, protection gas breather pipe and seal cover, it is characterized in that: the top at tank is provided with water inlet, be provided with delivery port in its underpart, tantalum crucible is located at above the above-mentioned tank, the bottom of above-mentioned tantalum crucible is taper, and its angle is 120-175 °; Be arranged with inside and outside 2 layers of baffle plate at above-mentioned tantalum crucible bottom outer, be provided with seal cover at above-mentioned tantalum crucible pot mouth, sealing covers and is provided with thermocouple and the protection breather pipe that inserts in the tantalum crucible, and above-mentioned thermocouple lower end can not contact the tantalum crucible limit.
3. a kind of purification devices according to claim 2, it is characterized in that: the angle between above-mentioned Internal baffle and the tantalum crucible is 45-90 °, the aspect ratio of Internal baffle and tantalum crucible is 1:1-2, the aspect ratio of above-mentioned outer baffle and Internal baffle is 1:2-3, distance between internal layer baffle plate and the sidewall of crucible is 400-500 mm, and the distance between the ectonexine baffle plate is 200-300 mm.
CN201210517063.5A 2012-12-06 2012-12-06 A kind of magnesium alloy physical purification method and purification devices thereof Expired - Fee Related CN103042199B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024866A (en) * 2007-02-14 2007-08-29 西北工业大学 Magnesium alloy smelting and quantitative pouring apparatus
CN102626779A (en) * 2012-04-25 2012-08-08 辽宁工业大学 Method for preparing magnesium alloy ingot and solidification system
CN102672148A (en) * 2012-05-28 2012-09-19 重庆大学 New process for purifying magnesium alloy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024866A (en) * 2007-02-14 2007-08-29 西北工业大学 Magnesium alloy smelting and quantitative pouring apparatus
CN102626779A (en) * 2012-04-25 2012-08-08 辽宁工业大学 Method for preparing magnesium alloy ingot and solidification system
CN102672148A (en) * 2012-05-28 2012-09-19 重庆大学 New process for purifying magnesium alloy

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