CN104583429A - Al-Nb-B master alloy for grain refining - Google Patents

Al-Nb-B master alloy for grain refining Download PDF

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CN104583429A
CN104583429A CN201380043494.5A CN201380043494A CN104583429A CN 104583429 A CN104583429 A CN 104583429A CN 201380043494 A CN201380043494 A CN 201380043494A CN 104583429 A CN104583429 A CN 104583429A
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alloy
grain
mother
melt
mother alloy
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CN104583429B (en
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哈里巴比·内登德拉
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Brunel University London
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C22C21/04—Modified aluminium-silicon alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
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  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)

Abstract

A method of producing a master alloy for refining the grain size of a bulk alloy comprises the step of providing an Al-B alloy and adding Nb in elemental form to form an Al-Nb-B master alloy. The Al-B alloy may be prepared by providing an Al-B alloy with a higher boron content than is required and diluting it with elemental aluminium.

Description

For the Al-Nb-B mother alloy of grain refining
The application relates to the method for the mother alloy (being also referred to as masterbatch alloy) of the grain size for the preparation of fining metal alloy, and relates to the purposes of the grain-refining agent as metal alloy subsequently.Especially, it relates to the preparation of the mother alloy of the grain size for refinement aluminum-silicon alloy and (that comprise aluminium and that do not comprise aluminium two kinds) magnesium alloy.
An important goal in the production of metal alloy is the grain size reducing end product.This is called as " grain refining " and usually solve by adding so-called " grain-refining agent ", and described grain-refining agent is the material being considered to the inoculation promoting metal alloy crystal.In casting technique, bring many benefits by the grain refining of inoculation and on raising mechanical property, there is significant impact.Thin equi-axed crystal tissue gives high yield strength, high toughness, good extrudability, being uniformly distributed and microporosity in fine-scale of second-phase.This causes the machinability of improvement, good surface smoothness and the resistance (and other desirable performances various) to hot tear crack thereupon.
Applicant of the present invention have submitted international patent application no PCT/GB2012/050300 (being disclosed as WO 2012/110788 after the priority date of the application), its relate to refinement (i) comprise aluminium and at least 3%w/w silicon alloy or (ii) comprise the method for the grain size of the alloy of magnesium, described method comprises the following steps:
A () adds enough niobiums and boron to form niobium dioxide or Al in described alloy 3nb or both, or
B () adds niobium dioxide in described alloy, or
C () adds Al in described alloy 3nb, or
(d) their arbitrary combination.
For the industry manufacturing aluminium wrought alloy, adding the Al-Ti-B system grain-refining agent with the form of the mother alloy of the chemical constitution of 94 % by weight Al-5 % by weight Ti-1 % by weight B is general ways.Mother alloy adds avoids corrodibility KBF in casting technique 4the use of salt.Do not advise adding the boron of simple substance form, this is owing to the difficulty in the practice disperseed in the melt, and this is that it is low by the result of the character of liquid Al or Mg alloys wet.The interpolation of mother alloy overcomes these problems.
In WO 2012/110788, disclose: replace salt to add, people can add the niobium dioxide grain-refining agent of little Al-Nb-B mother alloy tinsel form to obtain thin grain size in Al-Si system liquid alloy.Add concentrated Al-Nb-B alloy and guarantee NbB 2dispersed in molten aluminium.
Especially, WO 2012/110788 discloses: in electric furnace, melt commercially pure Al ingot at temperature range 800-850 DEG C and keep 2 hours.By 5 % by weight NbB 2(Nb and KBF 4mixture) add in melt to form NbB 2phase.After stirring and remove scum silica frost, liquid metal is poured in mould, thus produces Al-Nb-B grain-refining agent mother alloy.
In another example, WO 2012/110788 discloses: melt business Al-10Nb mother alloys at 900 DEG C and be added to pure Al to dilute this alloy thus to form Al-2Nb mother alloy.Then in melt, 1 % by weight boron is added to realize the mother alloy composition of Al-2Nb-B.
US 3,933,476 (Union Carbide Corporation) discloses to utilize and adds titanium, aluminium and KBF 4the method for aluminium grain refinement.
GB 1 244 082 (Kawecki Berylco Industries, Inc.) disclose the method for the alloying of silk or strips or grain refining composition being added in major metal, wherein said composition is made up of one or more in aluminium and boron, titanium or zirconium.
According to a first aspect of the invention, provide a kind of method of mother alloy of the grain size for the preparation of refinement bulk alloy, described method comprise Al-B alloy is provided and the Nb adding simple substance form to form the step of Al-Nb-B mother alloy.
Technological merit according to mother alloy of the present invention is: the first, and it can not use corrosive salt as KBF 4when, produces; The second, what in bulk alloy, add that concentrated Al-Nb-B alloy ensure that in the melt in opposite directions of Nb system is dispersed; And the 3rd, it achieves the thinner grain size (in other words, it is more effective grain-refining agent) in final alloy.
In preferred embodiments, described Al-B alloy is prepared in the following manner: the Al-B alloy that has than required higher Boron contents is provided and is diluted with pure aluminum.Such as, in order to prepare 97 % by weight Al-2 % by weight Nb-1 % by weight alloys, dilute commercially available 95 % by weight Al-5 % by weight B alloys to produce 99 % by weight Al-1 % by weight B alloys by adding fine aluminium.Add enough simple substance niobiums afterwards, until obtain 97 % by weight required Al-2 % by weight Nb-1 % by weight B alloys.
According to a second aspect of the invention, provide a kind of by adding mother alloy and the method for the crystal grain of fining metal alloy as defined above.In preferred embodiments, the metal alloy adding mother alloy is wherein Al-Si alloy or (ii) magnesium alloy that (i) comprises at least 3%w/w silicon.
Masterbatch (being also referred to as mother alloy) can comprise the niobium of q.s and boron to form enough niobium dioxides in final alloy product, thus when this mother alloy is added to Al-Si or Mg alloy melt, its grain size refinement of tissue that can will solidify.When representing the formula of alloy, usually omit the weight percentage of most high alloy component.Therefore, the masterbatch alloy for being added to aluminium alloy can have the general formula of Al-X % by weight Nb-Y % by weight B, and wherein X can be 0.01 to 99 and Y can be 0.002 to 25, and the weight percentage of al composition be make summation be 100 surplus.
Now with reference to accompanying drawing, multiple preferred embodiment of the present invention is described, in the accompanying drawings:
Typical microstructures feature in Fig. 1 Al-5B mother alloy.Boride phase particle (AlB 12) be dark contrast.
Fig. 2: Al-4.05Nb-0.9B mother alloy microstructure, display NbB 2phase particle
Fig. 3 Al-2Nb-2B mother alloy microstructure, display NbB 2phase particle
Fig. 4 Al-2Nb-B mother alloy microstructure, display NbB 2phase particle
The photo of the corroded surface of the macroscopic view of the cross section of Fig. 5 .Al-10Si castings sample.The photo on the left side is Al-10Si alloy, and the photo on the right is for the sample prepared after Al-2Nb-2B is added to melt.
The light micrograph of the sample shown in Fig. 6: Fig. 5.A () & (b) is for Al-10Si, and (c) & (d) is for the Al-10Si's with Al-2Nb-2B interpolation.Thinner primary aluminium and thinner eutectic particle can be seen in the sample with Al-2Nb-2B interpolation.
Fig. 7. the photo of the top surface of the A380 ingot bar of the liquid metal casting adding Al-2Nb-B with (b) is not added by (a).
Fig. 8. the schematic diagram of the difference spatially of grain structure in the Al-10Si alloy billet processed when not there is and have Al-2Nb-B mother alloy and adding.
Fig. 9. the photo of the Al-10Si alloy billet prepared when not there is and have Al-2Nb-B mother alloy and adding.
Figure 10. the schematic diagram of the cross section of wedge shape mould.Tl, T2, T3 represent the position of thermopair in mould.Also show the microstructure of the corroded surface at these three different positions places.
Figure 11. the microstructure of the cross section of the tensile bar that the AM50 alloy adding Al-2Nb-B mother alloy with (b) uses Hpdc technique to prepare is not added for (a).
Figure 12. the sketch of the mould used in the experiment of embodiment 7.The typical rate of cooling obtained in these moulds is depicted in these sketches.Along with the thickness of cast structure body increases, rate of cooling reduces.
The cross section of the corrosion of the macroscopic view of Figure 13 alloy A wedge shape and cylinder sample: a) do not add and b) add Al-2Nb-2B mother alloy.
Figure 14. the cross section of the corrosion of the macroscopic view of alloy B wedge shape and cylinder sample: a) do not add and b) add Al-2Nb-2B mother alloy.
Figure 15. the cross section of the corrosion of the macroscopic view of alloy C wedge shape and cylinder sample: a) do not add and b) add Al-2Nb-2B mother alloy.
Figure 16. (a) does not add and (b) adds the microstructure with the alloy D of the mother alloy of Al-2Nb-2B composition being equivalent to the Nb of 0.1 weight.Al-2Nb-2B adds the grain structure of refinement significantly Al crystal grain and the size both eutectic Si pin.
Figure 17. (a) does not add the microstructure of adding the alloy E of Al-2Nb-2B mother alloy with (b).For the size of both Al crystal grain and eutectic Si pin, the obvious refinement of grain structure.
Figure 18. the microstructure of the anodic oxidation treatment of alloy F.The microstructure on the left side is for the cylindrical die sample when not adding grain-refining agent.The microstructure on the right with the addition of Al-2Nb-2B.
The cross section of the corrosion of the macroscopic view of Figure 19 alloy G wedge shape and cylinder sample: a) do not add and b) add Al-2Nb-2B mother alloy.
Figure 20. the un-added alloy G of comparison (a) of the microstructure of cylindrical cast samples.B () has the alloy G that Al-2Nb-2B mother alloy adds.Compared with the large-scale dendritic structure seen in reference sample, the interpolation of the grain-refining agent of Al-2Nb-2B mother alloy form creates the grain structure of very thin (~ 150 microns).It is the particle (dark contrast particle) of thinner primary silicon size after Al-2Nb-2B adds.
the processing of embodiment 1:Al-Nb-B mother alloy
In the present embodiment, boron source is commercially available Al-5 % by weight B mother alloy.Nb is the form of elemental powders, obtains the company Alfa Aesar under Johnson Matthey.Fig. 1 shows the microstructure of Al-B mother alloy.Dark contrast and for spherical particle be the boride of aluminium.This mother alloy with desired content is melted and keeps 2 hours together with commercially pure Al ingot in electric furnace at temperature range 800-850 DEG C, there is the concentration be applicable to listed in table 1.Melt is stirred with non-reacted ceramic rod.The Nb metal-powder of compacted form or discrete particle form is introduced in melt by we afterwards.Be important to note that, in the melt except NbB 2the formation of phase, also may form (Al, Nb) B according to position chemical concentrations 2, Al 3nb phase inclusion.Melt is poured in mould.The metal of casting is called as Al-Nb-B mother alloy.The microstructure of various mother alloy has been shown in Fig. 2,3 and 4.These are molecular by the thin Nb system grain distributed in Al matrix.
embodiment 2:Al-2Nb-2B mother alloy is to the application of Al-10Si alloy
Al-10Si alloy is melted in electric furnace at 800 DEG C and keeps 2 hours.Reference sample is cast in taper die.Mould is preheated to 250 DEG C, and the temperature of melt is remained on 740 DEG C being poured onto before in taper die.Fritter Al-2Nb-2B mother alloy (is equivalent to 0.05 % by weight NbB 2, the weight relative to Al in Al-10Si alloy) be added in remaining melt.After 15 minutes, Melt Stirring about 1 minute is poured in taper die.The grain size of the Al-10Si alloy of Al-2Nb-1B mother alloy is not added and is added in Fig. 5 display.The grain structure of refinement is obtained by adding Al-Nb-B mother alloy.With all kinds mother alloy, castingprocesses is repeated to Al-Si, and show their corresponding grain sizes in Table 1.Confirm the grain size of Al-Si alloy of all mother alloy refinements with the composition shown in table 1.Except thinner grain size, as shown in Fig. 6 (c) & (d), observe thinner eutectic Si.
The mother alloy composition of table 1 in Al-10Si alloy, Pitch-based sphere and corresponding average crystal grain size
embodiment 3:Al-2Nb-1B mother alloy is to the application of A380 alloy
The A380 alloy of 3Kg is melted in electric furnace at 750 DEG C and keeps 1 hour and be poured in steel die.By another batch of fusing of 3Kg, and by fritter Al-2Nb-B femalealloy (is equivalent to 0.05 % by weight NbB 2, the weight relative to A380 alloy) be added in melt.After 15 minutes, Melt Stirring about 1 minute is poured in mould.Fig. 7 (a) shows the grain size of this alloy, and Fig. 7 (b) display is added with the alloy of Al-Nb-B mother alloy.Grain size is reduced to 0.4mm from 1cm by the interpolation of the detailed analysis display Al-Nb-B mother alloy of ingot bar.Also macroporosity is significantly reduced.
embodiment 4: the processing (simulation of direct chill casting method) being added with the Al-10Si blank of Al-2Nb-B
In plumbago crucible, Al-10Si alloy melt is prepared with resistance furnace.Melt temperature is remained on 800 DEG C.The cylindrical steel mould of both ends open is placed in vertical tube furnace.The hot-zone of this stove is controlled by three district's heating systems to maintain uniform temperature along the longitudinal direction of pipe.Temperature along the axle of steel die remains on 720 DEG C.The bottom of steel pipe is closed with Cu block.Melt temperature be reduced to 740 DEG C and afterwards melt be poured onto in steel die.Before toppling over melt, by the water jet standpipe of the flow with 4 l/ minutes, Cu block is cooled.With filling melt steel tube place cost time be ~ 5 seconds.Because provided cooling is water jet standpipe, melt solidifies from bottom.Complete topple over after ten seconds, Cu block is removed and water jet standpipe is directly placed in the bottom of Al-Si alloy graining block.As a result, from melt, one direction extracts heat.Cooling conditions is in a longitudinal direction similar to the cooling conditions of horizontal direction in plant-scale direct chill casting method in this experiment.The schematic diagram of the blank that Fig. 8 (a) display is produced by this method.Huge columnar grain is organized and is formed in the melt.The schematic diagram of the blank that Fig. 8 (b) display is prepared by the melt of NbB2 added with Al-2Nb-B form being added with 0.05 % by weight.After Al-Nb-B adds, there is not columnar grain tissue and only can see thin equi-axed crystal tissue.Figure 9 illustrates with the corroded surface of the macroscopic view of the cylinder blank of one direction solidified cast.The elimination of the columnar growth be sought after is achieved by adding Al-Nb-B mother alloy.
embodiment 5:Al-2Nb-B mother alloy is to the application of magnesium (AM50) alloy
AM50 alloy is melted in electric furnace at 690 DEG C and keeps 2 hours.Use SF 6+ N 2gaseous mixture avoids oxidation to protect melt.Relative to the weight of AM50, the Al-2Nb-B mother alloy of about 0.1 % by weight to be added in melt and to stir 1 minute with rod iron.Will containing NbB 2melt be poured onto in wedge shape mould.For comparison purposes, also carry out without any NbB 2the experiment added.According to the thickness of casting, this wedge shape mould provides the rate of cooling of wide region.Rate of cooling between position T1 and tip, the scope of rate of cooling can between 80 DEG C/s to 1000 DEG C/s.By the polishing of two kinds of castings samples and chemical corrosion.Compare the microstructure at various position (T1, T2 and T3) place in Fig. 10.As shown in Figure 10, when being added in melt by Al-2Nb-B, observe grain refining.
embodiment 6: the Hpdc being added with magnesium (AMS0) alloy of Al-2Nb-B mother alloy
Hpdc (HPDC) is the conventional process of the various large structure/assemblies produced for the application of automobile, electronics and building field.It is a kind of mass production techniques.It provides higher rate of cooling for melt and during process of setting, obtains thinner grain structure.As described in example 5 above, AM50 alloy melt is prepared.The melt of the Al-2Nb-B adding and do not add 0.1 % by weight is fed to the shot sleeve (shot-sleeve) of Hpdc machine, then melt is injected to and has in the permanent mold of stamping, and make it solidify afterwards under stress.Produce at least 15 foundry goods.Each cast structure body is made up of three cylindrical bar and three flat bars.The microstructure of the cross section of representative cylindrical sample has been shown in Figure 11.Because the rate of cooling in HPDC process is ~ 1000 DEG C/s, expection forms very thin grain structure.But, toppling over period, when melt contacts with the cold wall of shot sleeve, there is heterogeneous nucleus on these walls and they grow in melt.In the literature, these crystal are called as " premature coagulation crystal " (early solidified crystal, ESC).Measure ESC and be of a size of ~ the size of 250 μm.When adding grain-refining agent, as shown in Figure 11 (b), the size of these crystal obviously reduces and whole grain sizes in whole sample are similar.Separately tension test is carried out at least 40 cylindrical samples.Statistically, when adding Al-2Nb-B, observing elongation and improving 11%.
embodiment 7:Al-2Nb-2B mother alloy is to the application of the Al-Si alloy of various commercial source
Give the alloy composition of the research of the impact for carrying out Al-2Nb-2B mother alloy in table 2.These alloys are nearly eutectic (alloy A); Hypoeutectic alloy (alloy B-F) and hypereutectic (alloy G) business alloy.
the list of the alloy that table 2. is studied
Alloy Si Mg Mn Cu Ni Zn Fe
Alloy A 11-12 0.1 0.5 0.1 0.1 0.1 0.6
Alloy B 7.5-9.5 3 0.5 3.0 0.5 3 1.3
Alloy C 6.5-7.5 0.4 0.3 0.2 0.1 0.1 0.5
Alloy D 9.99 0.005 0.005 0.0017 0.0044 0.005 0.09
Alloy E 10.98 0.268 0.21 2.134 0.068 0.778 0.83
Alloy F 6.06 0.275 0.265 2.725 0.0257 0.305 0.356
Alloy G 13.0 0.4 0.5 0.7 1.5 0.1 1
Alloy is placed in clay-graphite crucible, fusing, and before casting, remains under the processing temperature of 790 DEG C at least 1 hour.Now, reference alloy is left standstill be cooled to about 740 (± 3) DEG C and in the cylindrical die being poured into preheating at 250 DEG C and wedge shape copper mould.These moulds are steel die and the copper wedge shape mould of 30mm diameter.In wedge shape mould, as what see in the sketch that can provide at Figure 12, by the scope of the rate of cooling of this tectonic cycle period between 2 DEG C/s to 150 DEG C/s.
When the grain-refining agent of the form of adding (adding rate of 0.1 % by weight Nb and 0.1 % by weight B) with Al-2Nb-2B mother alloy adds, at melt is remained on 790 DEG C after 60 minutes, mother alloy is added in melt and in order to new grain refining and leaves standstill the time of minimum 30 minutes to dissolve in melt inside, thus guarantee being uniformly distributed of grain refining phase.By glazed surface being immersed in graph card (Tucker) solution (25ml H2O+15ml HF+15ml HNO3+45ml HCl) 20 to 30 seconds, carry out the chemical corrosion for showing micropetrological unit.
The cross section of the corrosion of the macroscopic view of the alloy A wedge shape shape sample not adding and add Al-2Nb-2B has been shown in Figure 13, wherein can see, the feature of the alloy A not having grain-refining agent to add is the important difference spatially of the grain size of primary α-Al crystal grain, because its scope is rise at almost 1mm (top of sample) from about 200 μm (tips).From Figure 13 b it is possible to note that the interpolation of mother alloy significantly reduces average primary α-Al grain size and difference spatially, this latter is decreased between 100 μm and 200 μm.Similarly, final primary α-Al grain size is more insensitive to rate of cooling, and therefore, large-scale casting technique can be utilized to obtain based on having industrial components that the is thin and alloy A of grain size uniformly.
The cross section of the corrosion of the macroscopic view of the alloy A cylindrical sample of not adding and adding Al-2Nb-2B mother alloy is also show in figure (right side).Can find out, as when wedge shaped sample, the microstructure of reference material is made up of thick primary α-Al crystal grain, and there is the difference spatially of size aspect.Especially, in external diameter, grain size is thin, and this corresponds to the material solidified with contacting dies, and obviously increases afterwards, and final center in cylindrical sample reduces a little.The interpolation of mother alloy causes much thin primary α-Al crystal grain and level.Alloy microscopic structure is also more insensitive to the local difference of rate of cooling, and this is very important when manufacturing and having the cast article of different wall degree.
For other alloys whole listed in table 2, observe similar refinement.Macroscopic view or microstructure is given in Figure 14 to 20.

Claims (8)

1. for the preparation of a method for the mother alloy of the grain size of refinement bulk alloy, described method comprise Al-B alloy is provided and the Nb adding simple substance form to form the step of Al-Nb-B mother alloy.
2. method according to claim 1, wherein prepares described Al-B alloy: provide the Al-B alloy that has than required higher Boron contents and diluted with pure aluminum in the following manner.
3. method according to claim 2, the wherein said Al-B alloy with higher Boron contents is Al-5B.
4. the mother alloy obtained by the method according to the aforementioned claim of any one.
5. one kind is carried out the method for the crystal grain of fining metal alloy by adding masterbatch alloy according to claim 4.
6. method according to claim 5, wherein said metal alloy comprises:
I () comprises the Al-Si alloy of at least 3%w/w silicon, or
(ii) magnesium alloy.
7. method according to claim 6, wherein said metal alloy is Mg-Al alloy.
8. method according to claim 6, wherein said metal alloy is the Al-Si alloy comprising 3 to 25 % by weight silicon.
CN201380043494.5A 2012-08-16 2013-08-09 Al Nb B foundry alloy for crystal grain refinement Active CN104583429B (en)

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GBGB1214650.2A GB201214650D0 (en) 2012-08-16 2012-08-16 Master alloys for grain refining
PCT/GB2013/052135 WO2014027184A1 (en) 2012-08-16 2013-08-09 Al-nb-b master alloy for grain refining

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CN109022931A (en) * 2018-08-14 2018-12-18 南京云开合金有限公司 A kind of aluminium niobium boron intermediate alloy, preparation method and its application
CN109385542A (en) * 2018-09-17 2019-02-26 上海大学 The preparation method of aluminium niobium B alloy rod for crystal grain refinement

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