Effect of pulse magnetic field on microstructure of austenitic stainless steel during directional so

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Materials Science and Engineering A485 (2008) 403–408Effect of pulse magneticfield on microstructure of austeniticstainless steel during directional solidificationChangjiang Song a,Qiushu Li a,b,Haibin Li a,b,Qijie Zhai a,∗a School of Materials Science and Engineering,Shanghai University,Shanghai200072,Chinab Taiyuan University of Science and Technology,Taiyuan030024,ChinaReceived22June2007;received in revised form31July2007;accepted31July2007AbstractUsing directional solidification via zone melting,we investigated the effect of axial pulse magneticfield on microstructure and inter-face morphology of austenitic stainless steel over a wide range of growth rate(from planar to dendritic growth mode).Experimental results show that during directional solidification,applications of pulse magneticfield destabilize the interface morphology,i.e.it promotes planar–cellular–dendritic–cellular transition of growth mode under the same conditions.Analysis reveals that freezing rate oscillations caused by the pulse magneticfield may be responsible for this phenomenon.© 2007 Elsevier B.V. All rights reserved.Keywords:Pulse magneticfield;Directional solidification;Austenitic stainless steel;Electromagnetic force1.IntroductionApplications of current and magneticfield to material pro-cessing,so-called electromagnetic processing of material(EPM) has been widely studied in last two decades.And EPM has been successfully used to improve quality and properties of materi-als,such as grain refinement,improving interface stability and crystal quality during directional solidification,controlling crys-tal orientation,etc.[1–10].EPM was considered as an effective method to promote efficiency,fabricate high performance mate-rials,and develop advanced material processing technique.Now, the investigations were mainly focused on the applications of alternate currentfield,direct currentfield,pulse current,alternate magneticfield and static magneticfield[8–18].However,appli-cations of pulse magneticfield to material process have been seldom investigated.Directional solidification was frequently observed during melt solidification,and was important in many technological applications.The aim of this paper is to investigate the effect of the axial pulse magneticfield on the microstructure and solid/liquid(S/L)interface stability of austenitic stainless steel during directional solidification.∗Corresponding author.Tel.:+862156331218;fax:+862156331218.E-mail address:qjzhai@(Q.Zhai).2.ExperimentsThe setup used in this work was schematically shown in Fig.1,which mainly consists of generator of pulse magnetic field,heating coil,pulling mechanism,high purity alumina cru-cible and the coolant of liquid Ga–In–Sn alloy.The studied alloy was commercial austenitic stainless steel,whose composi-tion was shown in Table1.Its solidus and liquidus temperature are about1426.66◦C and1461.74◦C,respectively.The studied alloy were melted in an induction furnace and cast into cylinder bars with diameter of3mm and length of150mm.The experimental procedure was as follows:first,the pre-pared cylinder bar was placed in the high purity alumina crucible with inside diameter of3mm;second,the sample was slowly heated and melted to the predetermined temperature(1550◦C); third,holding5–8min for melt homogeneousness,the samples began to be pulled downward at a constant rate,and the pulse magneticfield was synchronously imposed on it;last,the sam-ple was quenched into liquid Ga–In–Sn alloy to observe the solid/liquid(S/L)interfaces at the predetermined time in steady-state growth stages.The frequency of pulse magneticfield was about4–5Hz,and a typical discharge course of power supply of pulsed magneticfield was shown in Fig.2.During the exper-iments,the sample was melted by the heating coil connected with high frequency(400kH)power supply,and the melt length was about15mm.A series of experiments were carried out0921-5093/$–see front matter© 2007 Elsevier B.V. All rights reserved. doi:10.1016/j.msea.2007.07.079404 C.Song et al./Materials Science and Engineering A485 (2008) 403–408Fig.1.Sketch of experimental setup.Table 1Composition of austenitic stainless steel (wt.%)C 0.07Si 0.29Mn 0.70P 0.030S 0.002Ni 9.27Cr 17.47Ti 0.06FeBalancewith different pulling rate and different magnetic intensity under otherwise identical conditions.The temperature gradient at the S/L interfaces was measured by a B-type (Pt-30%Rh/Pt-6%Rh)thermocouple inserted the melt without magnetic field,the thermocouple moved together with samples during the measurement.It is difficult to measure the temperature in 3mm diameter samples,thus we measured the temperature gradient in a 5mm diameter sample under identical conditions,which was about 627K/cm in 5mm diametersampleFig.2.A discharge course of power supply of pulsed magnetic field.under identical conditions.The magnetic intensity was measured by an oersted-meter for strong magnetic field.The quenched samples were removed from the alumina cru-cible,and were cut along the symmetrical axis.The as-polished specimens were etched by the reagent of FeCl 3(18g)+HCl (30ml)+H 2O (100ml)for microstructure examination.The microstructure was examined by an optical microscope.3.ResultsWe mainly investigated the effect of the axial pulse magnetic field on S/L interface morphology at the pulling rate of 12,24,64,and 96␮m/s.The corresponding growth modes are planar,cel-lular,cellular–dendrite,and dendrite front growth,respectively.Fig.3shows the effect of pulse magnetic field on the longitudinal microstructure and interface morphology of austenitic stainless steel at the puling rate of 12␮m/s (grey phase is austenite phase,and black phase is ferritic phase).It indicates that without the pulse magnetic field,the growth mode is planar front growth as shown in Fig.3(a).When 0.50T pulse magnetic field is imposed,the disturbances appear on the growth interface as shown in Fig.3(b),which reveals onset of interface instability.When the magnetic intensity is 0.84T,the growth mode changes into the cellular front growth,as shown in Fig.3(c).And when the mag-netic intensity is 1.00T and 1.54T,the growth mode evolves into complex cellular–dendritic or dendritic front growth as shown in Fig.3(d and e).The above results show that application of the pulse magnetic field makes the growth mode transform from the planar to cellular to dendritic front growth at the pulling rate of 12␮m/s.Fig.4is the longitudinal microstructure and interface mor-phology at the pulling rate of 24␮m/s with different magnetic intensity.It reveals that without the pulse magnetic field,the growth mode is cellular front growth as shown in Fig.4(a).When the pulse magnetic field is applied,the side branch of cellular crystal begins to appear and gradually develop.The growth mode gradually transforms from cellular to dendritic front growth with increasing the magnetic intensity.Moreover,the primary spacing gradually decreases with increasing the magnetic intensity.Fig.5presents the longitudinal microstructures and interface morphology at the pulling rate of 64␮m/s with different mag-netic intensity.It exhibits that without the pulse magnetic field,the growth mode is cellular–dendritic front growth as shown in Fig.5(a).Application of 0.5T and 0.84T pulse magnetic field makes the growth mode evolve into dendritic front growth,as shown in Fig.5(b and c).Further increasing the magnetic inten-sity makes the growth mode evolve again into cellular–dendritic (or cellular)front growth as shown in Fig.5(d and e).And the primary spacing gradually becomes smaller with increasing the magnetic intensity.Fig.6shows the longitudinal microstructure and interface morphology at the pulling rate of 96␮m/s with different mag-netic intensity.It indicates that without the pulse magnetic field,the growth mode is dendritic front growth as shown in Fig.6(a).When 0.50T and 0.84T pulse magnetic field is applied,the growth mode transforms from dendritic to cellular front growth as shown in Fig.6(b and c).With further increasing magneticC.Song et al./Materials Science and Engineering A 485 (2008) 403–408405Fig.3.Longitudinal microstructure at the pulling rate of12␮m/s with different magnetic intensity:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and(e)1.50T.intensity,the microstructure exhibits complex morphology as shown in Fig.6(d and e).That may enter the band-microstructure zone from the dendritic to planar transition at high growth rate,as observed by many researches[19–21].On the other hand,increase of the magnetic intensity does not make the pri-mary spacing decrease at the pulling rate of96␮m/s,inversely increase as shown in Fig.6(b and e).In the directional solidi-fication of Al–0.52wt.%Mn near the absolute stability[20,21], increasing freezing rate also makes primary spacings increase when growth mode transforms from the dendritic to planar front growth at high growth rate.Our experiments are similar to their experimental results.4.DiscussionsAccording to Trivedi and Kurz[19],microstructure of directional solidification exhibits planar–cellular–dendritic–cellular–planar transition due to the competition between differ-ent physical process(the convection effect is not considered). The solute diffusion length is defined as l D=D/V,the ther-mal diffusion length l T= T0/G,and the capillarity length d0=Γ/ T0(for an alloy),where D is the solute diffusion coef-ficients,V the growth rate, T0the equilibrium freezing range of the alloy,G the temperature gradient at the S/L interface and Γis the Gibbs–Thomson coefficient.For directionalsolidifica-Fig.4.Longitudinal microstructure at the pulling rate of24␮m/s with different magnetic intensity:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and(e)1.50T.406 C.Song et al./Materials Science and Engineering A485 (2008) 403–408Fig.5.Longitudinal microstructure at the pulling rate of 64␮m/s with different magnetic intensity:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and (e)1.50T.tion of the alloy,the transition growth rate can be expressed as follows:V c =DG T 0=DGkmC 0(k −1)for planar–cellular transition (1)V tr =DG k T 0=DGmC 0(k −1)for cellular–dendrite transition(2)V trh =D T 0aΓ=DmC 0(k −1)akΓfor dendrite–cellular(high rate)transition(3)where k is the equilibrium distribution coefficient,m the liquidus slope,C 0the initial alloy composition and a a constant.The equations show that transition velocity of growth mode increases with increasing the temperature gradient.The primary spacing is also a function of the growth rate and the temperature gradient.At low growth rate,the primary spacing decreases with increase of temperature gradient for constant growth rate and increase of growth rate for constant temperature gradient [12,22].The experimental results indicate that applications of the pulse magnetic field reduce the interface stability and promote planar–cellular–dendritic–cellular transition of growth mode,i.e.application of pulse magnetic field makes the transition velocity lower under otherwise identical conditions.Accord-ing to Eqs.(1)and (2),decrease of transition velocity may result from decrease of the temperature gradient at the S/L inter-face.However decrease of temperature gradient should result in increasing of primary spacing at low growth rate [12,22],which differs from the experimental results.Thus the experi-ment results cannot be explained by the changes of temperature gradient.When the pulse magnetic field is applied,it would produce the induction current in the melt.Interaction between pulse mag-netic field and the induction current gives rise to electromagnetic force toward the center of the melt.On the other hand,interaction between pulse magnetic field and the induction current caused by the high frequency current of heating coil also gives rise to electromagnetic force in the radial direction.The electromag-netic force periodically squeezes the melt,and result in melt flow.During the directional solidification,the melt flow can promote solution transmission,thus can decrease the solution build-up ahead of the interface,promote S/L interface stability and delay the transition from planar to cellular growth mode [23,24]and from cellular to dendritic growth mode [24,25].Therefore,the promotion of solution transmission by melt flow can’t also explain the reason for interface instability caused by application of pulse magnetic field.Application of magnetic field gives rise to change of Gibbs free energy of the liquid and solid.At constant pressure,the change of Gibbs free energy due to magnetic field can be written as [26,27]:d G =−S d T −μM d H(4)where G is Gibbs free energy,S the entropy,T the temperature,μthe magnetic permeability,M the magnetization intensity and H is the magnetic intensity.Due to difference of the magneti-zation intensity between the liquid and solid,application of the magnetic field can affect the liquidus and solidus temperature of the alloy.For example,Li et al.[28,29]found that the peritec-tic phase transformation temperature of Mn–Bi alloy increases about 20◦C in 10T magnetic field.The experimental results also suggest that application of pulse magnetic field can increasesC.Song et al./Materials Science and Engineering A 485 (2008) 403–408407Fig.6.Longitudinal microstructure at the pulling rate of96␮m/s with different magnetic intensity:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and(e)1.50T.the liquidus and solidus temperature of austenitic stainless steel [30].Pulse magneticfield is periodic action of magneticfield on the melt.During action time of magneticfield,increase of the liquidus temperature would lead to greater constitutional super-cooling ahead of the S/L interface at the same melt temperature, which makes the advance rate of the interface increase,and the interface becomes instability.However,weakening and disap-pearance of the magneticfield make the liquidus temperature decrease and return to equilibrium state in absence of magnetic field.Consequently constitutional supercooling decreases,even overheating occurs at the interface.And the interface advance rate would decreases,even interface move backward due to remelting.Therefore,application of pulse magneticfield would causefluctuation of freezing rate.On the other hand,meltflow produced by electromagnetic force of pulse magneticfield can give rise to composition and temperaturefluctuation ahead of the S/L interface,which also can result in freezing ratefluc-tuation.The freezing ratefluctuation can lead to instability of interface and promote planar–cellular–dendritic–cellular tran-sition of growth mode.Moreover,the formed striations are clearly seen in the lower magnification microstructure in the steady-state growth stages of the samples with applied pulsed magneticfield,as shown in Figs.7(d and e)and8(d and e). The formed striations usually are caused by growth rate oscilla-tions of interface during the directional solidification.Increase of advance rate can make new cellular(or dendritic)crystal form either by branching or by nucleation.And decrease of advance rate can make the cellular(or dendritic)crystal ter-minate by overgrowth of other cellular(of dendritic)crystal. If there exists kinetic difference between formation and ter-mination of cellular(or dendritic)crystal.Thefluctuation of freezing rate can cause the average primary spacing to deviate (increase or decrease)from that at steady freezing rate[31,32]. It was theoretically and experimentally testified by Regel et al.in MnBi–Bi eutectic alloy[31,32].Consequently,thefreez-Fig.7.Longitudinal microstructure in the steady-state growth stages of the samples at the pulling rate of12␮m/s:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and(e) 1.50T.408 C.Song et al./Materials Science and Engineering A485 (2008) 403–408Fig.8.Longitudinal microstructure in the steady-state growth stages of the samples at the pulling rate of 24␮m/s:(a)0T,(b)0.50T,(c)0.84T,(d)1.00T,and (e)1.50T.ing rate oscillations caused by pulsed magnetic field should be the origin of change of primary spacing in the experiments.It should be noted that further research is needed to well under-stand the action mechanism of pulsed magnetic field on the microstructure and interface morphology during the directional solidification.5.ConclusionsUsing directional solidification via zone melting,we inves-tigated the effect of axial pulse magnetic field on the microstructure and interface morphology of austenitic stain-less steel.Experimental results show that application of the pulse magnetic field reduces the interface stability and pro-motes planar–cellular–dendritic–cellular transition.Increasing magnetic intensity makes the primary spacing decrease at the pulling rate of 12,24and 64␮m/s.But increasing magnetic intensity makes the primary spacing increase at the pulling rate of 96␮m/s.Analysis reveals that freezing rate oscillations caused by the pulse magnetic field may be responsible for above phenomenon.AcknowledgementsThis work was supported by National Natural Science Foun-dation of China (No.:50274050),973Program of China (No.:2004CCA07000)and China Postdoctoral Science Foundation (No.:20070410716).We expressed our sincere thanks for their financial support.References[1]P.Lehmann,R.Moreau,D.Camel,R.Bolcato,Acta Mater.46(1998)4067–4079.[2]S.Asai,Sci.Technol.Adv.Mater.1(2000)191–200.[3]H.Conrad,Mater.Sci.Eng.A 287(2000)205–212.[4]A.Radjai,K.Miwa,T.Nishio,Metall.Mater.Trans.A 29(1998)1477–1484.[5]Y .-G.Sha,C.-H.Su,S.L.Lehoczky,J.Crystal Growth 173(1997)88–96.[6]O.P¨a tzold,I.Grants,U.Wunderwald,K.Jenkner,A.Cr¨o ll,G.Gerbeth,J.Crystal Growth 245(2002)237–246.[7]S.Asai,K.-S.Sassa,M.Tahashi,Sci.Technol.Adv.Mater.4(2003)455–460.[8]B.Ganapathysubramanian,N.Zabaras,J.Crystal Growth 276(2005)299–316.[9]Y .Wang,K.Kudo,Y .Inatomi,R.Ji,T.Motegi,J.Crystal Growth 284(2005)406–411.[10]B.A.Legrand,D.Chateigner,R.P.de la Bathie,R.Tournier,J.Magn.Magn.Mater.173(1997)20–28.[11]S.R.Coriell,G.B.McFadden,B.Billia,H.Nguyen Thi,Y .Dabo,J.CrystalGrowth 216(2000)495–500.[12]M.G¨u nd¨u z,E.C ¸adırlı,Mater.Sci.Eng.A 327(2002)167–185.[13]T.V .Savina,A.A.Nepomnyashchy,S.Brandon,A.A.Golovin,D.R.Lewin,J.Crystal Growth 237–239(2002)178–180.[14]O.Fornaro,H.A.Palacio,Scripta Mater.36(1997)439–445.[15]C.Song,Z.Xu,X.Liu,G.Liang,J.Li,Mater.Sci.Eng.A 393(2005)164–169.[16]C.-J.Song,Z.-M.Xu,G.Liang,J.-G.Li,Mater.Sci.Eng.A 424(2006)6–16.[17]C.Song,G.Liang,Z.Xu,J.Shen,J.Li,J.Mater.Process.Technol.180(2006)179–184.[18]C.Song,Z.Xu,J.Li,Mater.Sci.Forum 475–479(2005)281–284.[19]R.Trivedi,W.Kurz,Int.Mater.Rev.39(1994)49–74.[20]X.Geng,H.Fu,Sci.Technol.Adv.Mater.2(2001)209–212.[21]A.Ludwig,W.Kurz,Acta Mater.44(1996)3643–4654.[22]C.T.Rios,R.Caram,J.Crystal Growth 174(1997)65–69.[23]B.Kauerauf,G.Zimmermann,L.Murmann,S.Rex,J.Crystal Growth 193(1998)701–711.[24]R.Trivedi,H.Miyahara,P.Mazumder,E.Simsek,S.N.Tewari,J.CrystalGrowth 222(2001)365–379.[25]G.Grange,J.Gastaldi,C.Jourdan,B.Billia,J.Crystal Growth 151(1995)192–199.[26]J.-K.Choi,H.Ohtsuka,Y .Xu,W.Y .Choo,Scripta Mater.43(2000)221–226.[27]H.Wang,Effects of a High Magnetic Field on the Behavior of PrecipitatePhases in Alloys,Ph.D.thesis,Shanghai University,Shanghai,2002,pp.109–112.[28]X.Li,Z.M.Ren,Y .Fautrelle,Mater.Lett.60(2006)3379–3384.[29]Z.Ren,X.Li,Y .Sun,Y .Gao,K.Deng,Y .Zhong,Comp.Coupl.PhaseDiagrams Thermochem.30(2006)277–285.[30]Q.-S.Li,H.-B.Li,Q.-J.Zhai,J.Iron Steel Res.13(2006)69–72.[31]L.L.Regel,W.R.Wilcox,D.Popov,F.Li,Acta Astronaut.48(2001)101–108.[32]F.Li,L.L.Regel,W.R.Wilcox,J.Crystal Growth 223(2001)251–264.。