CN102294553B - Magnesium alloy brazing filler metal containing rare-earth element Er and preparation method thereof - Google Patents
Magnesium alloy brazing filler metal containing rare-earth element Er and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnesium alloy brazing filler metal containing a rare-earth element Er and a preparation method thereof, and belongs to the technical field of magnesium alloy connection. The magnesium alloy brazing filler metal comprises the following components in percentage by weight: 40-55% of Mg, 39-55% of Zn, 1-5% of Al and 0.1-1.5% of Er, wherein the Er is uniformly distributed.The preparation method comprises the steps of arranging alloy ingots in a preheat crucible, heating under protective atmosphere and mechanical stirring, fishing slag after the alloy ingots are completely fused, stopping heating brazing filler metal, stirring the brazing filler metal, applying ultrasonic waves on the fused brazing filler metal after the brazing filler metal is cooled to 380-600 DEG C, inserting an ultrasonic rod preheated to 300-700 DEG C into a brazing filler metal liquid level with the ultrasonic frequency of 18-22kHz, ultrasonic intensity of 0.5-5W/cm2 and the time of 10-150s, standing still after moving out the ultrasonic rod after ending, pouring the brazing filler metal liquid into a mould and air cooling to room temperature. The number of dendritic crystals of the obtained product is obviously reduced, crystal grains are refined, and the strength and the toughness are improved.
Description
Technical field
The present invention relates to a kind of Mg-Al-Zn-Er magnesium alloy brazing filler metal and technology of preparing thereof that contains rare earth element er, belong to magnesium alloy interconnection technique field.
Background technology
From early 1990s, marked change has occured in the application development of major metal material in the world, the application of the traditional materials such as steel, iron, copper, aluminium, zinc increasess slowly, and the light metal material take magnesium alloy as representative is a dark horse, the speed sustainable growth with annual 20%.The research and development of magnesium alloy are paid much attention in countries in the world, with the grand strategy goods and materials of magnesium resource as 21 century, and have strengthened application and development and the research of magnesium alloy in fields such as automobile, computer, communication and Aero-Space.Therefore, the research of magnesium alloy connection also more and more obtains paying attention to.
American Welding Society (AWS) write " the commercial solder that can be used at present magnesium alloy brazing enumerated of soldering handbook has BMg-1, BMg-2a (U.S. test material association trade mark is respectively AZ92A and AZ125).More than two kinds of solders all be suitable for gas brazing, furnace brazing and dip brazing.But these two kinds of solder fusing points are higher, the brazing flux melting temperature that is equipped with is higher (about 538 ℃) also, the burning-point and the melting temperature that surpass most magnesium alloy, therefore only be suitable for a small amount of several magnesium alloys such as soldering AZ10A, K1A and M1A, be not suitable for that soldering is applied such as magnesium alloys such as Mg-Al-Zn systems.The composition of the MC3 standard magnesium alloy brazing filler metal of Japan is in close proximity to the BMg-1 of the U.S., but the temperature range of this solder is 605～615 ℃, and this brazing temperature is too high.The In-Mg-Zn-Al solder of the new research and development of Japan, its solder fusion temperature scope is at 449～490 ℃.Contain a large amount of precious metal In in this solder, wherein the mass percent of In reaches 65%, has greatly improved the solder cost.Welding society of Chinese Mechanical Engineering Society write " the Mg-Al-Zn solder has only been enumerated in the soldering of relevant magnesium alloy in the welding handbook, and its composition is Al12%, Zn0.5%, Be0.005%, Mg surplus, and other related contents are few.
Application number a kind of Mg-Zn magnesium alloy brazing material that has been 200910092586.8 patented invention, application number a kind of magnesium alloy middle temperature brazing material that has been 200810116505.9 patented invention, its solder main component is Al:1～2.5%, Zn:46～52%, surplus is Mg, application number a kind of Zn-Mg-Al magnesium alloy brazing material that has been 200910092580.0 patented invention, application number a kind of Zn-Mg magnesium alloy brazing material that has been 200910092579.8 patented invention.These several brazing materials are mainly used in the welding of AZ series magnesium alloy, and the shear strength of its welding point is no more than 72MPa, differ far away with the tensile strength (being about 280MPa) of magnesium alloy itself.Application number a kind of magnesium alloy brazing material that contains rare earth Nd that has been 200910092578.3 patented invention, above-mentioned patent solder all is to heat alloy pig in crucible, obtains solder after the condensation.The solder that is made by this method is when the heating alloy pig, heating-up temperature surpasses 30～50 ℃ of liquidus curve, because each element fusing point is different, has when solidifying successively in the cooling procedure, have serious segregation phenomena, there is the problem of brazing quality shakiness in made solder in brazing process.
Er adds in the magnesium alloy, and effectively the as cast condition crystal grain of refinement alloy can improve to some extent alloy microstructure, improve the tensile property under alloy heat endurance and the different conditions, and is meanwhile little on the plasticity impact.
Summary of the invention:
The invention provides a kind of Mg-Zn-Al-Er magnesium alloy brazing filler metal that adds rare earth element er, simultaneously by in the alloy pig melt, applying hyperacoustic method, solved in the crucible that the segregation of preparation magnesium alloy brazing filler metal is serious, coarse grains and trace element problem pockety in solder, prepared the Mg-Zn-Al-Er brazing filler metal that a kind of grain refinement and micro-Er are evenly distributed.
Preparation method provided by the present invention also is applicable to the preparation of other Magnesium Alloys solder, aluminium alloy brazing filler metal.Crucible can be used among the preparation method provided by the present invention, also smelting furnace can be used.
A kind of Mg-Zn-Al-Er brazing filler metal provided by the present invention is characterized in that, its each component and shared percentage by weight are: Mg:40-55%, and Zn:39-55%, Al:1-5%, Er:0.1-1.5, Er is evenly distributed.
In the Mg-Zn-Al-Er magnesium alloy brazing filler metal that contains rare earth element er provided by the present invention, the effect of various elements is as follows:
Zn: the fusing point that significantly reduces magnesium alloy brazing filler metal.Increase the solubility of Al in Mg, improve the solution strengthening effect of Al.
Al:Al and Mg form limit solid solution; Reduce smelting temperature and the pouring temperature of magnesium alloy; Improve the mobile of solder and improve wetability.
Er: add and contain in the magnesium alloy increase magnesium alloy heat endurance and intensity, hardness.Along with Er content increases, keeping under the substantially constant prerequisite of plasticity, alloy strength, hardness improve.Al in Er and the magnesium alloy generates Al
3The Er particle, this nascent Al
3The Er particle as heterogeneous nuclei, improves nucleation rate, thereby makes grain refinement, the Al of small and dispersed when solidifying
3The Er particle crystal boundary and intracrystalline precipitation strength effect, because the refined crystalline strengthening effect that crystal grain thinning produces and the substructure strengthening effect that in deformation and heat treatment process, forms so that alloy strength, hardness intensity increase; The tiny Al that disperse distributes
3The pinning effect that the Er particle has dislocation and sub boundary can the establishment recrystallization, the refinement recrystal grain.
The above-mentioned preparation method who contains the magnesium alloy brazing filler metal of rare earth provided by the present invention is characterized in that, may further comprise the steps:
1, crucible is preheating to 100 ℃～300 ℃.
2, will place crucible through preheating for the alloy pig of preparation soldering.
3, under protective atmosphere and mechanical agitation condition, be heated to 600 ℃～700 ℃.Protective atmosphere is SF
6+ N
2Mist.
4, after alloy pig melts fully, drag for slag, solder is stirred 2～10 minutes after, the stopped heating solder.Continue to stir solder, when treating that solder is cooled to 380 ℃-600 ℃, adopt supersonic generator that the magnesium alloy molten solder is applied ultrasonic wave.The ultrasonic wave bar that is preheating to 300-700 ℃ is inserted 5～100mm under the magnesium alloy molten solder liquid level, and ultrasonic frequency is 18～22kHz, and ultrasonic intensity is 0.5～5W/cm
2, the time is 10～150s.
5, apply and shift out the ultrasonic wave bar after ultrasonic wave finishes, aluminium alloy is left standstill 5～50s.
6, the molten solder liquid castable is entered in the stainless steel mould, air cooling to room temperature obtains solder.
Pass through its cavitation, fragmentation when ultrasonic wave is propagated in melt, cross cold forming core effect, can play the effect that increases the forming core particle, increases equiax crystal quantity, inhibiting grain growth, impurity screening and degasification.The present invention utilizes hyperacoustic this characteristic, in the magnesium alloy brazing filler metal melt, apply ultrasonic energy, by hyperacoustic fragmentation, prepared compact grained Mg-Zn-Al-Er brazing filler metal, when containing trace rare-earth in the Mg-Zn-Al-Er brazing filler metal, also can promote the even distribution of rare earth element, further improve soldered fitting intensity.
Compared with prior art, the present invention has following beneficial effect:
1, compare with the Mg-Zn-Al solder that does not apply ultrasonic processing and do not add element Er, alloy branch crystal quantity obviously reduces, and crystal grain obtains refinement, and toughness improves, and solder institute soldering lap joint shear strength improves about 5%～25%.
2, compare with the Mg-Zn-Al solder that does not apply ultrasonic processing and do not add element Er, add on a small quantity the elements such as element such as Ar and distribute more even.
3, compare with the Mg-Zn-Al solder that does not apply ultrasonic processing and do not add element Er, trace additives Er distributes more even in solder, can not be deposited on the bottom of solder.
4, compare with the Mg-Zn-Al solder that does not apply ultrasonic processing and do not add element Er, adopt the magnesium alloy brazing filler metal time of repose after the ultrasonic processing to greatly reduce, need not carry out homogenising and process the solder that also can obtain even tissue.
The specific embodiment:
Employed crucible electrical resistance furnace is the SG2A7.5-10 crucible electrical resistance furnace among the following embodiment.
Comparative Examples:
Crucible is preheating to 150 ℃.In crucible, add the 290g magnesium ingot, 306g zinc ingot metal, 20g aluminium ingot, 20g magnesium-erbium alloy ingot.It is 30% that magnesium-erbium alloy ingot contains the erbium amount.Insulation after being heated to 700 ℃ under protective atmosphere and the mechanical agitation condition.Melt rear stirring 3 minutes fully until alloy, leave standstill after 10 minutes and come out of the stove, drag for slag, cast in stainless steel mould, cast temperature is 660 ℃.Air cooling to room temperature obtains adding the Mg-Zn-Al solder of element Er.In whole process, all use SF
6+ N
2Mist is protected molten solder.
Embodiment 1
Crucible is preheating to 100 ℃.In crucible, put into the 270g magnesium ingot, 295g zinc ingot metal, 15g aluminium ingot, 28g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 700 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 2 minutes, melt temperature is incubated after being down to 600 ℃, the ultrasonic wave bar that is preheating to 300 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 5mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 18kHz, and ultrasonic intensity is 0.5W/cm
2, the time is 10s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 5s, casts in stainless steel mould, and cast temperature is 600 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al solder of element Er.
Embodiment 2
Crucible is preheating to 150 ℃.In crucible, put into 260g magnesium ingot and 320g zinc ingot metal, 15g aluminium ingot, 28g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 650 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 4 minutes, melt temperature is incubated after being down to 550 ℃, the ultrasonic bar that is preheating to 500 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 20mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 20kHz, and ultrasonic intensity is 1W/cm
2, the time is 20s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 40s, casts in stainless steel mould, and cast temperature is 550 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al solder of element Er.
Embodiment 3
Crucible is preheating to 180 ℃.In crucible, put into the 240g magnesium ingot, 340g zinc ingot metal, 20g aluminium ingot, 40g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 650 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 4 minutes, melt temperature is incubated after being down to 550 ℃, the ultrasonic bar that is preheating to 550 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 20mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 20kHz, and ultrasonic intensity is 1W/cm
2, the time is 40s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 30s, casts in stainless steel mould, and cast temperature is 550 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al solder of element Er.
Embodiment 4
Crucible is preheating to 250 ℃.In crucible, put into the 240g magnesium ingot, 340g zinc ingot metal, 20g aluminium ingot, 40g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 600 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 7 minutes, melt temperature is incubated after being down to 450 ℃, the ultrasonic bar that is preheating to 680 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 30mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 22kHz, and ultrasonic intensity is 2W/cm
2, the time is 60s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 50s, casts in stainless steel mould, and cast temperature is 450 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al magnesium alloy brazing filler metal of element Er.
Embodiment 5
Crucible is preheating to 300 ℃.In crucible, put into the 230g magnesium ingot, 300g zinc ingot metal, 23g aluminium ingot, 80g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 700 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 8 minutes, melt temperature is incubated after being down to 400 ℃, the ultrasonic bar that is preheating to 400 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 60mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 21kHz, and ultrasonic intensity is 3W/cm
2, the time is 100s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 50s, casts in stainless steel mould, and cast temperature is 400 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al magnesium alloy brazing filler metal of element Er.
Embodiment 6
Crucible is preheating to 300 ℃.In crucible, put into the 220g magnesium ingot, 310g zinc ingot metal, 25g aluminium ingot, 100g magnesium-erbium alloy ingot.The erbium amount that contains of magnesium-erbium alloy ingot is 30%.Insulation after being heated to 700 ℃ under protective atmosphere and the mechanical agitation condition.After melting fully, alloy drags for slag, stir cooling after 10 minutes, melt temperature is incubated after being down to 380 ℃, the ultrasonic bar that is preheating to 300 ℃ is inserted in the magnesium alloy molten solder, the ultrasonic wave bar immerses about 100mm under the alloy liquid level, then apply ultrasonic wave, ultrasonic frequency is 22kHz, and ultrasonic intensity is 5W/cm
2, the time is 150s.Processing is shifted out the ultrasonic wave bar after finishing, and aluminium alloy is left standstill 50s, casts in stainless steel mould, and cast temperature is 380 ℃.In whole process, all use SF
6+ N
2Mist is protected molten solder.After being poured, air cooling to room temperature obtains adding the Mg-Zn-Al magnesium alloy brazing filler metal of element Er.
Utilize the DSC200PC differential thermal analyzer to measure the fusing point of solder.Test parameters: pure argon protection, gas flow Ar=15ml/min; Programming rate is 10.0K/min; Al2O3 is reference; Sample is solder fine particle or the powder of 10～15mg.Table 1 has been listed the solder fusing point of Comparative Examples and embodiment.
Be bulk with the solder machine cuts of Comparative Examples and embodiment 1-6 preparation, the AZ31B magnesium alloy sheet thick to 3mm carries out induction brazing.Magnesium alloy workpiece is through sand papering before the soldering, and acetone cleans to remove greasy dirt and the oxide-film on surface, and the step brazing flux is spread at the soldered fitting place, and solder places the joint, and the work that assembly is good is put into argon protective device and carried out soldering.Argon flow amount is 10L/min in the brazing process, and programming rate is 2.5 ℃/s, 380 ℃ of brazing temperatures, insulation 35s.After the soldering, soldered fitting is carried out the shear strength test; Its result is as shown in table 1.
As can be seen from Table 1, after the prepared solder of employing the present invention carried out induction brazing, the shear strength of soldered fitting was improved, and average grain size reduces.
Table 1 soldered fitting shear strength, crystallite dimension and inclusion size statistics
| The solder fusing point (℃) | Average shear intensity (MPa) | Average grain size (μ m) | |
| Comparative Examples | 380 | 49.2 | 58 |
| Embodiment 1 | 348 | 56.6 | 45.6 |
| Embodiment 2 | 353.2 | 51.7 | 41.9 |
| Embodiment 3 | 345.7 | 58.3 | 42.3 |
| Embodiment 4 | 345.7 | 61.5 | 40.1 |
| Embodiment 5 | 344.5 | 56.1 | 41.6 |
| Embodiment 6 | 340.5 | 58.9 | 44.5 |
Claims (1)
1. a preparation method who contains the magnesium alloy brazing filler metal of rare earth element er is characterized in that, its each component and shared percentage by weight are: Mg:40-55%, and Zn:39-55%, Al:1-5%, Er:0.1-1.5, Er is evenly distributed; May further comprise the steps:
(1) crucible is preheating to 100 ℃～300 ℃;
(2) will place crucible through preheating for the alloy pig of preparation solder;
(3) be heated to 600 ℃～700 ℃ under protective atmosphere and mechanical agitation condition, protective atmosphere is SF
6+ N
2Mist;
(4) after alloy pig melts fully, drag for slag, after 2～10 minutes, the stopped heating solder continues to stir solder to the solder stirring, when treating that solder is cooled to 380 ℃-600 ℃, adopts supersonic generator that the magnesium alloy molten solder is applied ultrasonic wave; The ultrasonic wave bar that is preheating to 300-700 ℃ is inserted 5～100mm under the magnesium alloy molten solder liquid level, and ultrasonic frequency is 18～22kHz, and ultrasonic intensity is 0.5～5W/cm
2, the time is 10～150s;
(5) apply and shift out the ultrasonic wave bar after ultrasonic wave finishes, aluminium alloy is left standstill 5～50s;
(6) the molten solder liquid castable is entered in the stainless steel mould, air cooling to room temperature obtains solder.
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| CN 201110205638 CN102294553B (en) | 2011-07-21 | 2011-07-21 | Magnesium alloy brazing filler metal containing rare-earth element Er and preparation method thereof |
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| CN103769761A (en) * | 2012-10-23 | 2014-05-07 | 石瑛 | Brazing filler alloy and preparing method thereof |
| CN103769763A (en) * | 2012-10-23 | 2014-05-07 | 石瑛 | Brazing filler alloy and preparing method thereof |
| CN103769762A (en) * | 2012-10-23 | 2014-05-07 | 石瑛 | Brazing filler alloy and preparing method thereof |
| CN103394546B (en) * | 2013-08-21 | 2015-06-03 | 武汉钢铁(集团)公司 | Production method for longitudinal welded pipe |
| CN104018049B (en) * | 2014-06-04 | 2016-11-02 | 北京工业大学 | A kind of superplasticity magnesium alloy and preparation method thereof |
| CN104004979B (en) * | 2014-06-04 | 2016-08-24 | 北京工业大学 | A kind of microstructure thinning method improving magnesium alloy temperature-room type plasticity |
| CN104191103B (en) * | 2014-08-15 | 2017-01-18 | 郑州机械研究所 | Medium-temperature magnesium alloy solder containing rare earth element La and preparing method thereof |
| CN104759783B (en) * | 2015-03-24 | 2017-02-01 | 广东工业大学 | Low-silver lead-free solder and preparation method thereof |
| RU2615930C1 (en) * | 2016-06-16 | 2017-04-11 | Юлия Алексеевна Щепочкина | Magnesium solder |
| CN107283085A (en) * | 2017-06-23 | 2017-10-24 | 洛阳理工学院 | A kind of magnesium alloy brazing filler metal containing Sm and preparation method thereof, application |
| CN107116315A (en) * | 2017-06-23 | 2017-09-01 | 洛阳理工学院 | A kind of magnesium alloy brazing solder and preparation method thereof |
| CN113999997A (en) * | 2021-11-18 | 2022-02-01 | 魏敏 | Grain refinement method of biodegradable Zn-1Mg-0.5Ca casting alloy |
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