CN102251137B - Flux-free smelting method for AZ31 magnesium alloy - Google Patents
Flux-free smelting method for AZ31 magnesium alloy Download PDFInfo
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- CN102251137B CN102251137B CN 201110260451 CN201110260451A CN102251137B CN 102251137 B CN102251137 B CN 102251137B CN 201110260451 CN201110260451 CN 201110260451 CN 201110260451 A CN201110260451 A CN 201110260451A CN 102251137 B CN102251137 B CN 102251137B
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Abstract
The invention discloses a flux-free smelting method for AZ31 magnesium alloy and solves the problems of inclusion, pores and environmental pollution in the conventional AZ31 magnesium alloy smelting method. The flux-free smelting method comprises the following steps of: a, preheating a graphite, loading, and introducing tetrafluoroethane mixed gas for smelting; b, alloying and performing cost analysis; c, rotationally blowing argon for refining an alloy solution; and d, removing impurities, filtering by using a MgO foamed ceramic filter, and pouring for forming. A combined purification process of rotationally blowing the argon and filtering by using MgO ceramics under the protection of the tetrafluoroethane mixed gas is adopted, the ductility and toughness of the magnesium alloy are improved, the magnesium alloy is promoted to expand to the field of deep processing such as press working and the like, and the application range of the magnesium alloy is widened; the purity and mechanical properties of the AZ31 magnesium alloy are greatly improved, the tensile strength and elongation are improved from 152.65MPa and 3.2 percent before refining to 177.45MPa and 8 percent, and are improved by 16 percent and 150 percent; meanwhile, the environmental pollution is reduced.
Description
Technical field
The present invention relates to the AZ31 magnesium alloy smelting method, be specially a kind of AZ31 magnesium alloy without the flux melting method.
Background technology
Protective method for smelting of magnesium alloy and magnesium alloy purifying method are the important component part in the magnesium alloy smelting method.Gas protection method is present most widely used protective method for smelting of magnesium alloy.Gas protection method is at liquid magnesium alloy surface coverage one deck rare gas element or can generates with reactive magnesium the gas of dense oxidation film, thus the contacting of the oxygen in the secluding air and magnesium liquid.Industrial available shielding gas mainly contains CO
2, SO
2, SF
6, CHF-134a, Novec
TM612 etc.
In these shielding gas, when melt temperature is higher than 700 ℃, CO
2And SO
2The surface film thickening, become fragile, cracking loses provide protection gradually easily; And SF
6Higher with the CHF-134a Greenhouse effect; Novec
TM612 operations are more numerous and diverse, and processing unit is more.
The flux refining method is because dust removal rate is high, low, the easy to operate purifying method that generally adopts in the magnesium alloy production that becomes of cost, the deficiencies such as but flux refining exists metal loss to increase, flux is mingled with, can not degass, especially when the melting magnesium-rare earth, strict to flux component.Because non-flux refining technique can remedy the deficiency of flux refining technique, thereby obtain further investigation, developed at present multiple purification style, such as blowing gas purification, filtration, purification, vacuum-treat, ultrasonication, electromagnetic field purification and composite purification etc.
At present, the filtration, purification method because magnesia ceramics strainer fragility is large, production cost is high, is used also fewer now; The vacuum purification method, because the higher alloying elements such as Mg of saturated vapor pressure, vaporization losses very easily during vacuum melting, thus cause the fluctuation of metal loss and alloying constituent; Simultaneously vacuum smelting equipment is complicated, expensive, thereby the vacuum purification of magnesium alloy is processed at present not yet large-scale application in industrial production; The ultrasonic purification method, because the limitation of ultrasonic generator, the method also is difficult to be applied to large batch of magnesium cleaning molten and processes.
For the melting method of AZ31 magnesium alloy, aspect melt protecting, adopt at present traditional flux protection aspect, flux brings is mingled with that to decompose the gas that produces with flux be environment; Aspect cleaning molten, traditional flux-refining, bring simultaneously be mingled with, pore and environmental pollution.
Summary of the invention
The present invention is mingled with for the melting that solves existing AZ31 magnesium alloy exists, the problem of pore and environmental pollution, provides a kind of AZ31 magnesium alloy without the flux melting method.
The present invention adopts following technical scheme to realize: the AZ31 magnesium alloy is feeded and is passed into the Tetrafluoroethane mixed gas after employing following steps: a, the crucible preheating and dissolve without the flux melting method; Carry out cost analysis after b, the alloying; C, rotary blowing argon gas refined magnesium alloy solution; Filter casting by the MgO floamed ceramics filtrating piece after d, the removal of impurities.Adopt advanced in the world Tetrafluoroethane mixed gas protected, the rotary blowing argon gas carries out the refining degassing processing in conjunction with the composite purifying process of ceramic filter to magnesium alloy fused mass, reduces the pollution to environment when improving magnesium alloy quality and purity.
Charging and pass into the concrete steps that the Tetrafluoroethane mixed gas dissolves and be after the crucible preheating: after crucible is preheated to garnet, the MAG block, the aluminium block that add preheating, temperature setting is set to 650 ℃ and dissolves, described Tetrafluoroethane mixed gas is comprised of pressurized air, carbonic acid gas and Tetrafluoroethane, and temperature passes into pressurized air and carbonic acid gas in time more than 400 ℃; Temperature reaches more than 500 ℃; then pass into Tetrafluoroethane; the crucible preheating is in order to remove the steam of surface attachment; temperature is more than 400 ℃ the time; the magnesium alloy oxidation rate increases obviously; pass into pressurized air and carbon dioxide gas mixture and just can well protect the melting of magnesium alloy; simultaneously can save the more expensive Tetrafluoroethane of price; more than 500 ℃ the time; need to continue to pass into the Tetrafluoroethane of protection better effects if for fear of the oxidization burning loss of fusion process, the mixed gas total flux that passes in the furnace chamber is decided to be: the mixed gas volume that per minute passes into is in the burner hearth in the crucible on the liquid level; 5% of the following enclosed cavity volume of seal closure.Temperature setting is set to 650 ℃, is conducive to accurately control the temperature of smelting furnace.
During the refining of rotary blowing argon gas, jet amount is 1.7-2.3L/min, and speed of rotation is 120 r/min-140r/min, and refining temperature is 710 ℃-730 ℃.Jet amount too hour, and is faint to the decontamination effect improving of liquation, and the destruction that can cause the molten surface protective membrane when excessive is caused oxidation and the air-breathing decontamination effect improving that affects of liquation; Speed of rotation hour can not be broken into bubble very much the micro-bubble that disperse distributes, and decontamination effect improving is bad, and along with the increase of rotating speed, the slosh degree strengthens, and the air-breathing of melt also increases; Do not causing that liquid level acutely rocks in the situation of protective membrane destruction, both larger decontamination effect improvings might as well.When temperature was 710 ℃-730 ℃, molten metal not only can not burn under the gas shield condition, and under this temperature condition, the flowability of molten metal is also fine, was conducive to the bubble in the molten metal and is mingled with float to liquid level.
Being cooled to 715 ℃-725 ℃ pours into a mould, the hole density of MgO floamed ceramics filtrating piece is 10PPi during cast, and the preheating temperature to 140 of MgO floamed ceramics filtrating piece ℃-160 ℃, MgO floamed ceramics filtrating piece hole density too hour, easy passage when molten metal passes through causes and can not pour into a mould or misrun; When hole density was too large, filter effect was bad.The control of the preheating temperature of teeming temperature and MgO floamed ceramics filtrating piece records through test of many times, and words molten metal and filter Quench that teeming temperature is crossed low or not preheating of filter are solidified, and block the filter hole, the situation that will generation can not pour into a mould or misrun.
The present invention adopts Tetrafluoroethane mixed gas protected lower, the composite purifying process of rotary blowing argon gas and MgO ceramic filter, and the plasticity and toughness of raising magnesium alloy promote magnesium alloy to the development infiltration in the deep processing fields such as press working, enlarge the range of application of magnesium alloy; Greatly improved purity and the mechanical property of AZ31 magnesium alloy, tensile strength and the elongation respectively front 152.65Mpa and 3.2% of never refining are brought up to 177.45Mpa and 8%, and amplification is respectively 16% and 150%, has reduced simultaneously the pollution to environment.
Embodiment
The AZ31 magnesium alloy is feeded and is passed into the Tetrafluoroethane mixed gas after employing following steps: a, the crucible preheating and dissolve without the flux melting method; Carry out cost analysis after b, the alloying; C, rotary blowing argon gas refined magnesium alloy solution; Filter casting by the MgO floamed ceramics filtrating piece after d, the removal of impurities.
During implementation, the step that alloying adopts is: be warming up to 700 ℃-710 ℃ Al-Mn master alloys that add preheating, be warmed up to 720 ℃ of spelters that add preheating, stir after the fusing, Mn adds with the form of Al-Mn alloy, and temperature of fusion is low, homogeneous chemical composition; Temperature too low fusing and homogenizing not only bad for Al-Mn master alloy, spelter, and the increase of fusing time can aggravate the scaling loss of micro-Mn; Temperature is too high, and the molten metal scaling loss is serious.Pour into a mould 3 samples, through composition analysis, detect the composition requirement that whether reaches AZ31.
During refining; the mixed gas total flux that passes in the furnace chamber is increased to: the mixed gas volume that per minute passes into is in the burner hearth in the crucible on the liquid level, the 10-15% of the following enclosed cavity volume of seal closure; because the slosh oxide film destroys easily, need to increase the shielding gas consumption and make the destruction place in time again form film when preventing refining.It is best that refining purifies 25-30 minute magnesium alloy liquation decontamination effect improving, the time too weak point can not fully purify, the time increases not only not contribution of decontamination effect improving again, and can increase the scaling loss of aluminium alloy and air-breathing.
During removal of impurities, with strainer the impurity of Mg alloy surface is removed after the refining, then be warmed up to 740 ℃-760 ℃ and leave standstill 20-25min, carried out a removal of impurities every 5 minutes, dwell temperature is too low to be unfavorable for entrap bubble in the melt and the abundant come-up that is mingled with, and temperature too Gao Zehui causes the oxidization burning loss of melt, simultaneously too short entrap bubble in the melt and the abundant come-up that is mingled with of being unfavorable for of time of repose, time of repose is oversize no longer to work to gas and the come-up that is mingled with, also may cause the air-breathing of melt on the contrary; With the timely removing that is mingled with that rises to the surface, avoid it to be fused in the liquation again.
Charging and pass into the concrete steps that the Tetrafluoroethane mixed gas dissolves and be after the crucible preheating: after crucible is preheated to garnet, the MAG block, the aluminium block that add preheating, temperature setting is set to 650 ℃ and dissolves, described Tetrafluoroethane mixed gas is comprised of pressurized air, carbonic acid gas and Tetrafluoroethane, and temperature passes into pressurized air and carbonic acid gas in time more than 400 ℃; Temperature reaches more than 500 ℃, then passes into Tetrafluoroethane.
During the refining of rotary blowing argon gas, jet amount is (1.7,1.8,2.1,2.3) L/min, and speed of rotation is (120,123,134,140) r/min, and refining temperature is (710,721,727,730) ℃.
Be cooled to (715,721,724,725) and ℃ pour into a mould, the hole density of MgO floamed ceramics filtrating piece is 10PPi during cast, and the preheating temperature of MgO floamed ceramics filtrating piece is to (140,143,151,160) ℃.
In the specific implementation process, batching is once joined 4 ㎏ raw materials, wherein pure magnesium 3.820 ㎏, pure zinc 44g, alumal 120g, fine aluminium 16g, the volumn concentration of Tetrafluoroethane mixed gas is: Tetrafluoroethane 0.1% ~ 0.2%, carbonic acid gas 20%-25%, surplus is pressurized air.
Claims (2)
1. an AZ31 magnesium alloy is without the flux melting method, it is characterized in that: feed after employing following steps: a, the crucible preheating and pass into the Tetrafluoroethane mixed gas and melt, after being specially crucible and being preheated to garnet, the MAG block, the aluminium block that add preheating, temperature setting is set to 650 ℃ and melts, described Tetrafluoroethane mixed gas is comprised of pressurized air, carbonic acid gas and Tetrafluoroethane, and temperature passes into pressurized air and carbonic acid gas in time more than 400 ℃; Temperature reaches more than 500 ℃, then passes into Tetrafluoroethane; Carry out composition analysis after b, the alloying; C, rotary blowing argon gas refined magnesium alloy molten solution, during the refining of rotary blowing argon gas, jet amount is 1.7-2.3L/min, and speed of rotation is 120 r/min-140r/min, and refining temperature is 710 ℃-730 ℃; Filter casting by the MgO floamed ceramics filtrating piece after d, the removal of impurities.
2. AZ31 magnesium alloy according to claim 1 is without the flux melting method, it is characterized in that: be cooled to 715 ℃-725 ℃ and pour into a mould, the hole density of MgO floamed ceramics filtrating piece is 10PPi during cast, and the preheating temperature to 140 of MgO floamed ceramics filtrating piece ℃-160 ℃.
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CN103820657B (en) * | 2014-02-19 | 2016-08-17 | 上海交通大学 | Magnesium alloy fused mass combined method for purifying |
CN103820648B (en) * | 2014-02-19 | 2016-08-17 | 上海交通大学 | Magnesium alloy fused mass purification method |
CN103820665B (en) * | 2014-02-19 | 2016-08-17 | 上海交通大学 | Magnesium alloy fused mass multistage composite purification method |
CN104762495B (en) * | 2015-03-18 | 2017-03-22 | 山东省科学院新材料研究所 | Magnesium and magnesium alloy smelting protective method |
CN105648252B (en) * | 2016-02-03 | 2018-06-08 | 重庆大学 | A kind of gas Modification Manners of Magnesium-aluminum alloys |
CN106222420A (en) * | 2016-08-14 | 2016-12-14 | 河北工业大学 | A kind of recycle and reuse method of waste foam magnesium |
CN106566938A (en) * | 2016-10-30 | 2017-04-19 | 山西汾西重工有限责任公司 | Aluminum-based composite material melt purification method |
CN111041151A (en) * | 2019-12-25 | 2020-04-21 | 安徽应流铸业有限公司 | Metal smelting method for eliminating double-layer oxide film |
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CN1587424A (en) * | 2004-07-08 | 2005-03-02 | 上海交通大学 | Magnesium alloy smelting method using 1,1-difluoroethane as protective atmosphere |
CN1962905A (en) * | 2006-11-29 | 2007-05-16 | 青岛地恩地投资集团有限公司 | Method for protecting tetrafluoroethane gas in magnesium or magnesium alloy smelting furnace |
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CN1587424A (en) * | 2004-07-08 | 2005-03-02 | 上海交通大学 | Magnesium alloy smelting method using 1,1-difluoroethane as protective atmosphere |
CN1962905A (en) * | 2006-11-29 | 2007-05-16 | 青岛地恩地投资集团有限公司 | Method for protecting tetrafluoroethane gas in magnesium or magnesium alloy smelting furnace |
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Effective date of registration: 20190529 Address after: 030003 Room 409, Fourth Floor, New Material Incubator C Block, Area A, Taiyuan Stainless Steel Economic Park, Shanxi Province Patentee after: Shanxi Demagnesene Technology Development Co., Ltd. Address before: 030051 Xueyuan Road 3, pointed lawn area, Taiyuan, Shanxi Patentee before: Zhongbei Univ |
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