CN101597701B - Grain refiner containing aluminum magnesium alloy and preparation method thereof - Google Patents

Grain refiner containing aluminum magnesium alloy and preparation method thereof Download PDF

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Publication number
CN101597701B
CN101597701B CN 200910115577 CN200910115577A CN101597701B CN 101597701 B CN101597701 B CN 101597701B CN 200910115577 CN200910115577 CN 200910115577 CN 200910115577 A CN200910115577 A CN 200910115577A CN 101597701 B CN101597701 B CN 101597701B
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magnesium alloy
melt
preparation
temperature
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CN101597701A (en
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杨湘杰
郭洪民
罗学泉
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Nanchang University
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Nanchang University
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Abstract

The invention provides a grain refiner containing an aluminum magnesium alloy and a preparation method thereof, and belongs to the field of metal alloy preparation. The grain refiner comprises the following chemical compositions in percentage by weight: 5 to 10 percent of Mg, 5 to 25 percent of SiC, and the balance of Al; and the preparation method comprises the following steps: performing surface cleaning treatment, grinding and screening on SiC particles, heating, melting and superheating the Al to between 720 and 750 DEG C, and then adding Mg into Al melt; after reducing the temperature of the melt to between 650 and 680 DEG C, stirring, simultaneously adding the SiC particles gradually before the temperature of the melt is reduced to between 610 and 590 DEG C, and then continuously stirring for 30 to 45min; and raising the temperature to between 850 and 950 DEG C, and preserving heat for 30 to 90min. The grain refiner has low cost and simple process, is more suitable for industrial mass production, can refine the magnesium alloy, and simultaneously can improve the hardness, strength, abrasion resistance and the like of the alloy; less Al4C3 is obtained on the surfaces of the SiC particles and has small influence on the abrasion resistance of the magnesium alloy; and the SiC has function of strengthening the magnesium alloy.

Description

A kind of grain refiner containing aluminum magnesium alloy and preparation method
Technical field
The invention belongs to the metal alloy preparation field, particularly alloy grain fining agent and preparation method.
Background technology
Unique excellent properties such as the low density of magnesium and alloy thereof, specific tenacity height, good processability, anti-electromagnetic interference is strong, returnability is good determine it in the utilization of fields such as aerospace, automobile, electronic industry more and more widely.But some shortcomings of magnesium and alloy thereof have caused its extensive utilization in actual production, as the magnesium alloy slip system is less at normal temperatures, cause plastic deformation ability very poor, defectives such as the easy alligatoring of crystal grain in castingprocesses, pore are more, macrosegregation, tissue odds are even, surface irregularity.The grain-size size is the key factor of decision magnesium alloy mechanical property, tiny equiax crystal has increased crystal boundary, these crystal boundaries are effective obstacles that slippage is transmitted, the stress concentration of crystal boundary the place ahead generation under external force activates more slip system, improved the plasticity of material, crystal grain thinning helps homogeneous microstructure again simultaneously, reduces the segregation tendency, thereby has more performances and technologic advantage.
The grain refining of magnesia mixture magnesium alloy at present mainly contains: 1) Overheating Treatment, and be heated to magnesium alloy above liquidus temperature 150-160 ℃ and keep for some time, be quickly cooled to teeming temperature then and pour into a mould.2) reach the crystal grain thinning effect by external force field, as mechanical stirring, induction stirring, ultrasonic wave effect etc.3) directly add some solutes in magnesium alloy, this is to play heterogeneous forming core effect in the material magnesium alloy solidification.Studies show that Al in a large number 4C 3Primary-Mg to magnesium and magnesium alloy has fine forming core effect, but directly adds Al in magnesium alloy 4C 3Can not play the effect of refinement, how realize Al 4C 3Thinning effect becomes the focus of present research.The contain Al substance reaction external with containing Al element in the aluminum magnesium alloy or magnesium alloy by carbonaceous materials such as graphite, SiC, TiC obtains Al 4C 3Thereby, can play good forming core effect.These technologies have: powder sintered, mechanical alloying, melt contact reacts etc.
Have some drawbacks in the aforesaid method, Overheating Treatment needs higher temperature and needs cooling fast, and this causes the magnesium alloy degree of oxidation big, and production unit is had relatively high expectations; Because magnesium alloy has good screening of nucleus effect and makes that the induction stirring effect is not fine; Mechanical stirring can cause magnesium alloy oxidation and air-breathing serious, and ultrasonic wave field seriously is not suitable for industrial production because of the extraneous factor decay; Obtain having the Al of forming core effect by powder sintered, mechanical alloying 4C 3, it is to equipment requirements height, cost costliness, inapplicable industrial mass production.
Summary of the invention
The purpose of this invention is to provide a kind of grain refiner containing aluminum magnesium alloy and preparation method.
Grain refiner containing aluminum magnesium alloy of the present invention, its chemical ingredients and weight percent are: Mg is 5-10%, and SiC is 5-25%, and surplus is Al.
The grain-size of SiC of the present invention is best<10 μ m.
The preparation method of magnesium alloy grains agent of the present invention is:
1, carries out the clean processing of SiC particle surface, grinds, screens with ordinary method.
Can use 40% hydrofluoric acid dips SiC, soak time is 6-12h, uses distilled water flushing then, air-dry, grind, the surperficial purified SiC particle of screening;
2, with the Al heat fused and be superheated to 720-750 ℃, the Mg that will account for total mass again and be 5-10wt% joins in the Al melt, makes Al-(5-10wt%) Mg melt;
When 3, treating that Al-(5-10wt%) Mg melt temperature drops to 650-680 ℃, stir, add gradually simultaneously that to account for total mass be the good SiC particle of 5-25% pre-treatment, before the temperature of melt is reduced to 610-590 ℃, add, continue to stir 30-45min again.
4, then, temperature is elevated to 850-950 ℃ and be incubated 30-90min, Al and SiC carry out reaction in (Al+SiC-Al 4C 3+ Si), on the SiC particle surface, form Al with heterogeneous forming core effect 4C 3Finally obtain the Al-Mg-SiC grain-refining agent.
To contain Al 4C 3The Al-Mg-SiC grain-refining agent add in the magnesium alloy fused mass, promptly play the crystal grain refining effect.
The present invention compared with prior art has following advantage:
1, cost is low, and raw material is pure Al, pure Mg, SiC particle, and wherein the rare earth element of SiC and other process for refining employing is cheap, adopts the heating installation of common extensive utilization, does not need the higher sophisticated equipment of composition.
What 2, adopt in preparation process is the stirring casting mode, and comparing powder sintered, pressure permeation, the SiC particle to be added other technologies such as Al melt simple, more suitable industrial mass production.
3, in the Al-Mg melt, in the non-magnesium alloy fused mass, synthesize Al by Al and SiC original position under the high-temperature condition with thinning effect 4C 3, can avoid directly in magnesium alloy fused mass reaction in to cause the drawback of burning oxidation.
4, stir under the semi-solid temperature interval, nascent Al collides mutually to eliminate with SiC and is wrapped in the gas on SiC surface, thereby has improved the wettability between Al-(5-10wt%) Mg and the SiC.
5, the Al that obtains at the SiC particle surface 4C 3Measure less, less to the influence of the corrosion resistance nature of magnesium alloy, and SiC can improve the performance of magnesium alloy, as improving intensity, increase hardness, improving wear resistance etc.
Embodiment
The present invention will be further described by following examples.
Embodiment 1.
Al-Mg-SiC-Al 4C 3Grain-refining agent refinement AZ91 alloy.
1, use 40% hydrofluoric acid dips SiC, soak time is 12h, uses distilled water flushing then 3 times, air-dry, grind, the surperficial purified SiC particle of screening.
2, the 980gAl ingot is placed in the resistance furnace, heat fused also is superheated to 750 ℃, 97gMg is preheating to 250 ℃ and join in the Al melt fusing and insulation 5min, the Al-9wt%Mg melt of system again.
When 3, treating that the Al-9wt%Mg melt temperature drops to 660 ℃, use the twi-tier blade agitator that this melt is stirred, speed with 15g/min adds the good SiC particle of 121.8g pre-treatment gradually, adds before the temperature of melt drops to 605 ℃, continues to stir 45min again.
4, stop to stir, temperature is elevated to 850 ℃ and be incubated 90min, carries out the Al that reaction in has heterogeneous forming core effect 4C 3, finally obtain the Al-Mg-SiC grain-refining agent.
5,690g magnesium heat fused is superheated to 750 ℃, in melt, adds 15.5gAl-10%Mn master alloy, 6.29gZn, 70g Al-Mg-SiC-Al successively 4C 3Grain-refining agent makes and contains the 0.9%SiC magnesium alloy.Insulation 15min is poured in the cavity swage of external diameter 10cm, internal diameter 4cm, high 10cm and obtains magnesium alloy ingot.
6, utilization Image-Pro Plus software measurement grain-size is from the 120 μ m that refine to of original 230 μ m.
Embodiment 2.
Al-Mg-SiC-Al 4C 3Grain-refining agent refinement AZ61 alloy.
1, use 40% hydrofluoric acid dips SiC, soak time is 9h, uses distilled water flushing then 3 times, air-dry, grind, the surperficial purified SiC particle of screening.
2, the 980gAl ingot is placed in the resistance furnace, heat fused also is superheated to 750 ℃, 97gMg is preheating to 250 ℃ and join in the Al melt fusing and insulation 5min, the Al-9wt%Mg melt of system again.
When 3, treating that the Al-9wt%Mg melt temperature drops to 660 ℃, use the twi-tier blade agitator that this melt is stirred, speed with 15g/min adds the good SiC particle of 121.8g pre-treatment gradually, adds before the temperature of melt drops to 605 ℃, continues to stir 45min again.
4, stop to stir, temperature is elevated to 850 ℃ and be incubated 90min, carries out the Al that reaction in has heterogeneous forming core effect 4C 3, finally obtain the Al-Mg-SiC grain-refining agent.
5,690g magnesium heat fused is superheated to 750 ℃, in melt, adds 22.2gAl-10%Mn master alloy, 5.92gZn, 30.2gAl-Mg-SiC-Al successively 4C 3, grain-refining agent makes and contains the 0.4%SiC magnesium alloy.Insulation 15min is poured in the cavity swage of external diameter 10cm, internal diameter 4cm, high 10cm and obtains magnesium alloy ingot.
6, utilization Image-Pro Plus software measurement grain-size is from the 220 μ m that refine to of original 390 μ m.

Claims (2)

1. the preparation method of a grain refiner containing aluminum magnesium alloy, the chemical ingredients of described grain refiner containing aluminum magnesium alloy and weight percent are: Mg is 5-10%, and SiC is 5-25%, and surplus is A1; With the SiC particle surface clean handle, grind, screening, it is characterized in that: with the A1 heat fused and be superheated to 720-750 ℃, Mg is added in the A1 melt again; When body temperature degree fusion drops to 650-680 °, stir, add the SiC particle gradually simultaneously, before the temperature of melt is reduced to 610-590 ℃, add, continue to stir 30-45min again; Afterwards, temperature is elevated to 850-950 ℃ and be incubated 30-90min.
2. the preparation method of fining agent according to claim 1 is characterized in that grain-size<10 μ m of described SiC.
CN 200910115577 2009-06-24 2009-06-24 Grain refiner containing aluminum magnesium alloy and preparation method thereof Expired - Fee Related CN101597701B (en)

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Publication number Priority date Publication date Assignee Title
CN102492881A (en) * 2011-12-05 2012-06-13 大连理工大学 Method for refining AZ31 magnesium alloy grains
CN104818399A (en) * 2015-05-12 2015-08-05 苏州列治埃盟新材料技术转移有限公司 Magnesium-aluminum-silicon carbide intermediate alloy material and preparation method thereof
KR101895567B1 (en) * 2016-07-12 2018-09-06 한국기계연구원 Grain refiner for magnesium alloy, method of fabricating the same and grain refinement method for magnesium alloy
CN114369741A (en) * 2022-01-04 2022-04-19 湖南化工职业技术学院(湖南工业高级技工学校) SiC inoculation treatment process of Mg-3.0Zn medical magnesium alloy

Citations (1)

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CN101250629A (en) * 2008-04-15 2008-08-27 郑州大学 Refiner containing nitrogen for magnesium alloy as well as preparing and using method thereof

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN101250629A (en) * 2008-04-15 2008-08-27 郑州大学 Refiner containing nitrogen for magnesium alloy as well as preparing and using method thereof

Non-Patent Citations (4)

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Title
TiC/Al和SiC/Al中间合金对Mg-Al系合金晶粒的细化;柳延辉等;《铸造》;20030722;第52卷(第7期);第472-475页,试验方法、分析与讨论 *
岳云龙等.粉末冶金法制备SiC颗粒增强AZ81镁基复合材料性能研究.《稀有金属材料与工程》.2007,第36卷(第3期),第533-536页.
柳延辉等.TiC/Al和SiC/Al中间合金对Mg-Al系合金晶粒的细化.《铸造》.2003,第52卷(第7期),
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