Journal of Alloys and Compoundsniﬁcantly, the size of recrystallization grains was slightly increased and the microstructure became more homogeneous in AZ31 alloy treated by ECAP

Journal of Alloys and Compounds 646 (2015) 1–9

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Journal of Alloys and Compounds

journal homepage: www.elsevier .com/locate / ja lcom

Microstructure, mechanical properties and static recrystallizationbehavior of the rolled ZK60 magnesium alloy sheets processed byelectropulsing treatment

http://dx.doi.org/10.1016/j.jallcom.2015.04.1960925-8388/� 2015 Elsevier B.V. All rights reserved.

⇑ Corresponding author at: Key Laboratory of Interface Science and Engineeringin Advanced Materials, Ministry of Education, Taiyuan University of Technology,Taiyuan 030024, PR China. Tel.: +86 351 6014852; fax: +86 351 6010311.

E-mail address: [email protected] (J. Fan).

Wei Jin a,b,c, Jianfeng Fan a,b,c,⇑, Hua Zhang a,b,c, Yang Liu a,b,c, Hongbiao Dong a,b,c,d, Bingshe Xu a,b,ca Key Laboratory of Interface Science and Engineering in Advanced Materials, Ministry of Education, Taiyuan University of Technology, Taiyuan 030024, PR Chinab Shanxi Research Center of Advanced Materials Science and Technology, Taiyuan 030024, PR Chinac College of Materials Science and Engineering, Taiyuan University of Technology, Taiyuan 030024, PR Chinad Department of Engineering, University of Leicester, Leicester LE1 7RH, UK

a r t i c l e i n f o a b s t r a c t

Article history:Received 20 September 2014Accepted 28 April 2015Available online 21 May 2015

Keywords:Magnesium alloysMicrostructureMechanical propertiesGrain refinementRecrystallization

Influences of electropulsing treatment (EPT) on microstructure, mechanical properties and static recrys-tallization (SRX) behavior of the rolled ZK60 magnesium alloy sheets were investigated. The experimentalresults indicated that the SRX of the rolled ZK60 alloy sheets processed by EPT was liable to occur com-pared with that processed by routine heat treatment (RHT). Furthermore, the recrystallizationmicrostructure was refined and the comprehensive mechanical properties were improved tremendouslyby EPT with a pulse width of 22–25 ls. The grain size was refined from 100 lm to 2 lm, the tensile stressof ZK60 alloy sheets was improved from 210 MPa to 320 MPa and the tensile elongation was increasedfrom 15.7% to 30%. Analyses on measured temperature and theoretical calculation of Fourier heat transfermodel were carried out to discuss the effect of Joule heat induced by EPT on recrystallization behavior.Moreover, the SRX mechanism under EPT was studied based on subgrain coalescence theory. EPT accel-erated the nucleation of strain-free grains by subgrain coalescence mechanism. An additional energy Geinduced by EPT rather than Joule heat increased the driving force of recrystallization.

� 2015 Elsevier B.V. All rights reserved.

1. Introduction

Low density, high specific strength and reasonable cost of mag-nesium alloys have attracted much interest in automotive andaerospace applications [1]. However, the poor mechanical proper-ties [2] have restricted their comprehensive application in thesefields. So how to improve the properties of magnesium alloys hasbecome a hotspot in the past years. Compared with the traditionalreinforcing methods, such as solution strengthening, strain hard-ening and dispersion strengthening, grain refinement is consideredto be one of the most efficient ways to improve both strength andplasticity of magnesium alloys.

As an instantaneous high energy input method, EPT has beenwidely used for optimizing and modifying the microstructure[3,4]. It has been reported that there was a significant influenceof electropulsing on cold deformed ferroalloys [5]. After EPT,cementite with an average size of 30 nm was prepared in

ferroalloys [5]. This phenomenon appeared not only in some par-ticular locations but throughout the cementite area, which was dif-ferent from the conventional situation. Conrad et al. [6] found thatthe annealing temperature, the recrystallization time and the sizeof recrystallization grains were all decreased when electropulsingwas applied in the recrystallization process of copper. Recently,Du et al. [7] reported that the failure elongation was improved sig-nificantly, the size of recrystallization grains was slightly increasedand the microstructure became more homogeneous in AZ31 alloytreated by ECAP + EPT compared to that treated by ECAP only. Xuet al. [8] and Guan et al. [9,10] have found that the microstructurewas refined and a tilted basal texture was obtained by rolling pro-cess accompanied by electropulsing in AZ31 alloy. The results wereascribed to the enhancement of boundary migration caused byapplied electropulsing during rolling. According to those observa-tions, it has been proposed that EPT greatly affected themicrostructure and properties of metals. Some researchers havebeen devoted to investigating the influence of EPT on solid solutionof magnesium alloys [11]. However, little has been reported on EPTapplied in magnesium alloy sheets before. Furthermore, the effectof EPT on recrystallization behavior of magnesium alloys was still

http://crossmark.crossref.org/dialog/?doi=10.1016/j.jallcom.2015.04.196&domain=pdfhttp://dx.doi.org/10.1016/j.jallcom.2015.04.196mailto:[email protected]://dx.doi.org/10.1016/j.jallcom.2015.04.196http://www.sciencedirect.com/science/journal/09258388http://www.elsevier.com/locate/jalcomhttps://www.researchgate.net/publication/257009116_Mechanical_properties_and_microstructure_of_pure_polycrystalline_magnesium_rolled_by_different_routes?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/251597097_Twinning_effects_in_a_rod-textured_AM30_Magnesium_alloy?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/260606524_Microstructure_properties_and_temperature_evolution_of_electro-pulsing_treated_functionally_graded_Ti-6Al-4V_alloy_strip?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/248481923_Effects_of_electropulse_duration_and_frequency_on_grain_growth_in_cu?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/232019265_Effect_of_the_electropulsing_on_mechanical_properties_and_microstructure_of_an_ECAPed_AZ31_Mg_alloy?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/243162799_The_effect_of_multiple_pulse_treatment_on_the_recrystallization_behavior_of_Mg3Al1Zn_alloy_strip?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/229385473_Texture_evolution_in_cold-rolled_AZ31_magnesium_alloy_during_electropulsing_treatment?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/231867689_Enhancement_of_ductility_in_Mg-3Al-1Zn_alloy_with_tilted_basal_texture_by_electropulsing?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/250343595_The_Influence_of_Electric_Current_Pulses_on_the_Microstructure_of_Magnesium_Alloy_AZ91D?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==

2 W. Jin et al. / Journal of Alloys and Compounds 646 (2015) 1–9

unclear. Therefore, the current work mainly aims at investigatingthe microstructure evolution and recrystallization mechanism ofdeformed magnesium alloy sheets by using EPT.

Fig. 1. Schematic illustration of the typical wave form of electropulsing.

2. Experimental procedure

A commercial ZK60 magnesium alloy ingot was cut into rectangular plates withthe size of 100 � 50 � 3 mm3 and then homogenized by heat treatment (at 613 Kfor 6 h and then warming up to 663 K for 10 h followed by furnace cooling). Therectangular plates with a thickness of 3 mm were rolled to 1.1 mm at 423 K witha total reduction of 63.3%. It should be noted that dynamic recrystallization(DRX) does not happen during rolling process. Then the rolled plates were cut intosamples with the gauge size of 50 � 2 � 1.1 mm3. Finally, the samples were treatedby EPT and routine heat treatment (RHT), respectively. After that, the samples werepolished and etched in nitric acid for optical microscopy (OM) observation andscanning electron microscopy (SEM) observation, and electrolytically polished forelectron back-scattered diffraction (EBSD) analysis. EBSD analysis was performedon an OXFORD-SEM equipped with an HKL-EBSD system. EBSD maps were mea-sured with the scan step length of 0.2 lm. Uniaxial tensile test at room temperaturewas carried out at a rate of 0.5 mm/min.

A laboratory-made electropulsing generator was used to acquire a maximumelectropulsing of 10,000 A. The samples were hold by two copper electrodes con-nected to the generator with a distance of 50 mm. Electropulsing parameters,including pulse width, frequency and amplitude were monitored by an oscilloscope.Different electropulsing parameters are listed in Table 1. The RHT was operated at573 K for 1 h.

A typical wave form used in experiments is shown in Fig. 1. Where td representsthe pulse width, tp is the pulse period. The pulse period was controlled by elec-tropulsing frequency. In this paper, the amplitude of electropulsing was a constantvalue of 10,000 A, so the current density during EPT was about 4.5 � 109 A/m2. Thefrequency of EPT was 100 Hz. The EPT processing time for each sample was 10 min.

3. Results

3.1. Microstructure of different states of ZK60 alloy

Fig. 2 demonstrates the optical micrographs of ZK60 alloy underdifferent states. As shown in Fig. 2a, the as-cast microstructure iscomposed of coarse a-Mg dendrites and Mg–Zn phase is dis-tributed in interdendritic area. The average grain size of as-castsample was 100 lm. After homogenization heat treatment, therewas no obvious change in grain size. However, the dendrites weregranulated and most of the intermetallic compounds were also dis-solved into the matrix (seen in Fig. 2b). For the rolled sample, themicrostructure is mainly composed of deformation twins andshear bands with some un-deformed fractions, as shown inFig. 2c. Fig. 2d and e shows the SRX microstructure of rolled sam-ples after EPT and RHT, respectively. It can be seen that the grainsize of the EPT sample is much finer than that of the RHT sampleand their average grain sizes are 3 lm and 10 lm, respectively.

3.2. Microstructure evolution of the rolled ZK60 alloy during EPT withdifferent pulse widths

Fig. 3 shows the SRX micrographs of the rolled ZK60 alloy underEPT with different pulse widths. As shown in Fig. 3a, after EPT with15 ls, the microstructure is the same as the rolled sample indi-cated in Fig. 2c and there are still a large number of deformationtwins inside the original grains elongated along the rolling direc-tion. As indicated in Fig. 3b, when the pulse width increases to

Table 1Different electropulsing parameters.

Sample number Frequency (Hz) Amplitude (A) Pulse width (ls)

1 100 10,000 152 100 10,000 203 100 10,000 224 100 10,000 255 100 10,000 30

20 ls, the recrystallization appears and most of the deformed areasdisappear. Fig. 4a shows the SEM photograph of sample indicatedin Fig. 3b, it can be seen that the twins are evolving into subgrainswhere the recrystallization occurs. When the pulse width increasesto 22 ls, the deformed microstructure is replaced by the finerecrystallization grains completely, as shown in Fig. 3c. Fig. 4bshows the SEM photograph of sample indicated in Fig. 3c, it isobserved that the microstructure is fine equiaxed grains and theaverage grain size is about 2 lm. When the pulse width increasesto 25 ls, the grains tend to grow up and the average grain size isabout 3 lm, as shown in Fig. 3d. With the further increase of pulsewidth, the growth of grains has become more pronounced and theaverage grain size is about 8 lm, as shown in Fig. 3e. Thus, it isconcluded that the appropriate pulse width is 22–25 ls in the pre-sent work. In other words, the fine and homogeneous microstruc-ture can be obtained by EPT under the pulse width of 22–25 ls.The pulse width represents the energy of a single pulse in EPTexperiments. Therefore, different SRX microstructures are obtainedby adjusting the pulse width during EPT.

Fig. 5 shows the EBSD maps and the corresponding distributionsof the misorientation angle of samples under EPT with differentpulse widths. It is observed that incomplete recrystallizationoccurs in the 20 ls–100 Hz EPT sample, as indicated in Fig. 5a.And its misorientation angle distribution mainly consists of twostrong misorientation angle distribution peaks of 2–10� and 85–90�. The frequencies of the low angle grain boundaries (LAGBs)with misorientation angles below 10� are approximately 42%.When the pulse width increases to 22 ls, the microstructure isfully recrystallized in the sample, as shown in Fig. 5b. The frequen-cies of the LAGBs decrease to 13%. With the further increase ofpulse width, the grains grow up slightly, as shown in Fig. 5c.Furthermore, the frequencies of the LAGBs become 7%.Consequently, with the increase of pulse width, the frequenciesof the LAGBs decrease gradually and the high angle grain bound-aries (HAGBs) with misorientation angles beyond 10� become pre-dominant. It is concluded that EPT enhances the transformation ofdeformed ZK60 alloy from LAGBs to HAGBs.

3.3. Mechanical properties of the rolled ZK60 alloy processed by EPTwith different pulse widths

Fig. 6 shows the engineering stress–strain curves of the samplesand the corresponding values of tensile stress, yield stress and ten-sile elongation are listed in Table 2. The as-rolled sample shows thehighest engineering stress of 353 MPa. The tensile stress decreaseswhile the tensile strain increases with the increase of the pulse

Fig. 2. Optical micrographs of ZK60 alloy under different states: (a) as-cast, (b) after homogenization heat treatment (at 613 K for 6 h and then warming up to 663 K for 10 h),(c) after rolling at 423 K, (d) SRX microstructure by EPT under 25 ls–100 Hz and (e) SRX microstructure by RHT.

W. Jin et al. / Journal of Alloys and Compounds 646 (2015) 1–9 3

width of EPT. When the pulse width is 22–25 ls, the tensile stressof sample is 320 MPa and the average tensile strain is 30%. Whenthe pulse width of EPT increases further to be more than 25 ls,the tensile stress decreases obviously although the tensile strainis still above 30%.

4. Discussions

In this paper, a low rolling temperature of 423 K was chosen inorder to obtain high dislocation density in ZK60 alloy. It has beenreported that there are two methods to increase the dislocationdensity in metals [12]: one is decreasing the deformation temper-ature; the other is increasing the deformation rate. When rolledunder 373 K, ZK60 alloy is much easier to crack due to the poordeformability. On the other hand, when rolling temperature isabove 473 K, dynamic recovery and recrystallization are liable tooccur, which will decrease the density of dislocations [13]. Thus,the rolling temperature between 373 K and 473 K is consideredas the appropriate temperature interval to acquire a high disloca-tion density without resulting in the generation of DRX.Therefore, an intermediate temperature value of 423 K was used

for rolling in the present work. After rolling process, the sufficientdistortion energy has been accumulated in deformed ZK60 alloy.

4.1. Effect of the EPT on microstructure and properties of the rolledZK60 alloy

EPT has a great influence on microstructure and properties ofthe rolled ZK60 alloy. When the pulse width is lower than 22 ls,high tensile stress with poor tensile elongation is obtained due tothe incomplete recrystallization and the work hardening duringrolling process. But when the pulse width is increased to 22–25 ls,the improved comprehensive mechanical properties of ZK60alloy are obtained due to the complete recrystallization and thefine microstructure. With further increase of pulse width toabove 25 ls, the tensile stress decreases obviously due to thegrowth of recrystallization grains. The improved properties ofZK60 alloy is due to the fine recrystallization microstructureobtained by EPT. Consequently, grain refinement induced byEPT is an efficient way to improve the mechanical properties ofZK60 alloy.

https://www.researchgate.net/publication/235698324_Deformation_Behavior_and_Controlling_Mechanisms_for_Plastic_Flow_of_Magnesium_and_Magnesium_Alloy?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/279893721_Dynamic_plastic_deformation_DPD_A_novel_technique_for_synthesizing_bulk_nanostructured_metals?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==

Fig. 3. Optical micrographs of SRX for the rolled ZK60 alloy under EPT with different pulse widths: (a) 15 ls–100 Hz, (b) 20 ls–100 Hz, (c) 22 ls–100 Hz, (d) 25 ls–100 Hzand (e) 30 ls–100 Hz.

Fig. 4. Scanning electron micrographs of SRX for the rolled ZK60 alloy under EPT with different pulse widths: (a) 20 ls–100 Hz and (b) 22 ls–100 Hz.


Fig. 5. Electron back-scattered diffraction (EBSD) maps and the corresponding distributions of the misorientation angle of SRX for the rolled ZK60 alloy under EPT withdifferent pulse widths: (a) 20 ls–100 Hz, (b) 22 ls–100 Hz and (c) 30 ls–100 Hz.


Fig. 7. Schematic illustration of the heat transfer model for the rolled ZK60 alloysample during EPT.

Table 3Temperature of different points in the deformed samples measured bythermocouples.

Samplenumber

Temperatureof point A (K)

Temperatureof point B (K)

Temperatureof point C (K)

Temperatureof point D (K)

1 339 315 300 2982 362 328 326 3003 376 358 331 3014 385 367 330 3005 405 373 343 302

Fig. 6. Engineering stress–engineering strain curves of ZK60 alloy samples.


4.2. Effect of the Joule heat induced by EPT on SRX behavior of therolled ZK60 alloy

After EPT, the deformed microstructure gradually disappearsand it is replaced by new strain-free recrystallization grains. Thesimilar result is obtained in deformed sample after RHT.Furthermore, the recrystallization microstructure of ZK60 alloy isstrongly dependent on electropulsing parameters.

During EPT process, the temperature increment of deformedsample is mainly from Joule heat. As shown in Fig. 7, four thermo-couples which were connected to point A, B, C and D were used tomonitor the temperature change of the samples during EPT exper-iment and the corresponding results are listed in Table 3. It isfound that the temperature in point A is the highest one and thetemperature decreases from point A to point D.

After one pulse passes through the sample, the temperatureincrement can be evaluated using the following equation [14]:

DT ¼ qj2tðc � dÞ�1 ð1Þ

where j is the current density, t is the pulse width of electropulsing,q is the electrical resistivity of magnesium alloy, c is the specificheat of magnesium alloy and d is the density of magnesium alloy.In the present experiment, the current density of deformed sampleis about 4.5 � 109 A/m2. After one pulse passes through the sample,the temperature increment is about 14.4 K when the pulse width is22 ls. Furthermore, taking the heat dissipation into account duringEPT process, the Fourier heat transfer model can be used to calcu-late the temperature field of deformed sample and several assump-tions are suggested as follows:

(1) The heat dissipation is realized only by heat conductionwithout regard to radiation and convection.

Table 2The values of tensile stress, yield stress and tensile elongation of ZK60 samples.

Samplestate

Tensile stress(MPa)

Yield stress(MPa)

Tensile elongation(%)

As-received 210 102 15.7As-rolled 353 285 5.0Sample 1 342 256 7.2Sample 2 330 241 15.0Sample 3 323 215 28.5Sample 4 318 209 31.7Sample 5 301 193 32.0

(2) The heat transfer from the sample to the copper electrode isone dimensional. So the temperature in point A is the high-est one due to the longest dissipation distance.

(3) The temperature in point D connected to the copper elec-trode is considered as a constant (298 K, room temperature).

(4) The temperature gradient from point A to point D is linearafter every pulse passes through.

Based on the above prerequisite, the calculation model of ther-mal conduction about the slender rod [15] can be expressed:

ut � a2uxx ¼ 0 ð2Þ

ujx¼0 ¼ 0;uxjx¼l ¼ 0;

�ð3Þ

ujt¼0 ¼ u0x=lð0 < x < lÞ ð4Þ

where x is the length between the test point and the constant tem-perature point, u is the temperature in test point, ux is the partialderivative of u, uxx is the second partial derivative of u, a2 is equalto k/C � d, k is the thermal conductivity of the rod, C is the specificheat capacity of the rod, d is the density of the rod and l is the lengthof the rod. Eq. (3) is a definition that the constant temperature pointof rod is the fixed end and the point at x = l is the free end. The solu-tion of the above differential equation is:

uðx; tÞ ¼ 2u0p2X1k¼0ð�1Þk 1

kþ 12� �2 e�

kþ12ð Þ2p2a2

l2tsin

kþ 12� �

pxl

ð5Þ

In this model, the temperature of the cold end is needed to bezero, but the value in the present experiment is 298 K. To satisfythe conditions of the model, a definition can be done as:

u ¼ T � 298 ð6Þ

where T represents the actual temperature in the present experi-ment. After the first pulse, ujx¼0 ¼ 0; ujx¼l ¼ 14:4. Therefore, thetemperature field of the deformed sample under EPT can be calcu-lated by the iteration of all pulses.

According to the above measurement and theoretical calcula-tion, the temperature in point A of the rod sample is the highestone and the corresponding calculated result in point A of each

Fig. 8. Microstructure of different samples for comparison experiments: (a) as-rolled, (b) after heat treatment at 449 K for 10 min and (c) after 30 ls–100 Hz EPTfor 10 min.


sample is shown in Table 4. It is obvious that both the measuredtemperature and the calculated temperature in point A are muchlower than the static recrystallization temperature (573 K) ofZK60 alloy [16,17]. So, a conclusion can be drawn that the increas-ing temperature resulting from the Joule heat of electropulsing isnot enough to induce the SRX in deformed ZK60 alloy.

Moreover, the temperature increment resulting from the Jouleheat of electropulsing is in proportion to the current density, thepulse width and the frequency of electropulsing. If the pulse widthand frequency are large enough, the temperature in deformed sam-ple will increase to the recrystallization temperature and then theJoule heat will induce the SRX. For a comparison, the rolled samplewas heat treated at 449 K (equal to the maximum value among themeasured temperature and the calculated temperature in Table 4)for 10 min (equal to the processing time of EPT) and the corre-sponding results are shown in Fig. 8. It can be seen that the amountof deformation twins in Fig. 8b is less than that in the as-rolledsample (Fig. 8a) and no new grains are observed in Fig. 8b. It isrevealed that the heat treatment at 449 K for 10 min is not enoughto result in the SRX in the deformed ZK60 alloy. However, as shownin Fig. 8c, the complete recrystallization is acquired in thedeformed ZK60 alloy after EPT, which can also give rise to the tem-perature increasing to 449 K. Why does this phenomenon occur? Itis proposed that there is a new recrystallization mechanism duringEPT and it is different from the conventional recrystallizationmechanism during heating treatment.

4.3. Effect of the additional energy Ge induced by EPT on SRX behaviorof the rolled ZK60 alloy

There is a transformation [18] (deformed state to recrystallizedstate) of ZK60 alloy during EPT and RHT. However, the differencebetween the above two methods is that the SRX induced by EPTis much easier to occur. The above results and analyses demon-strate that the EPT accelerates the static recrystallization processof ZK60 alloy.

It has been reported that when the electropulsing passesthrough metal materials, the system free energy of the metal mate-rials will obtain an additional term Ge in comparison with the sys-tem without electropulsing under the same state, and thisadditional energy is directly proportional to the electric resistanceof metal materials [5]. It is known that the electric resistance indeformed metals with high dislocation density is higher than thatin recrystallized metals with low dislocation density. Therefore,when the electropulsing passes through the deformed metal, thedriving force of recrystallization can be described as [5,19–21]:

DG ¼ DG0 þ DGe ð7Þ

where DG0 is the stored energy in deformed sample and DGe is theenergy change due to the impact of electropulsing.

A theoretical treatment of DG was developed by Qin et al. [5]:

DGe ¼l

8p

ZZj1ðrÞj1ðr0Þ � j2ðrÞj2ðr0Þ

jr � r0j d3rd3r0 ð8Þ

Table 4Measured and calculated results of the temperature in point A.

Samplenumber

The measured temperature ofpoint A (K)

The calculated temperature ofpoint A (K)

1 339 3832 362 4113 376 4234 385 4395 405 449

where l is the magnetic permeability, j is the density of electric cur-rent, and the sub-index 1 and 2 represent the deformed state andrecrystallized state of ZK60 alloy, respectively. jr � r0j is the distancebetween the two positions of space at r(x,y,z) and r0(x0,y0,z0). Usingthe specific mathematical methods and relative typical physicalparameters, Eq. (8) may be simplified as follows [5,22–24]:

DGe ¼ Kfðr2;r1ÞDVj2 ð9Þ

where DV is the volume of a recrystallization nucleus and K is a pos-itive constant which is related to the material. K can be described by[5,22–24]:

https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/226062082_Electropulse-induced_cementite_nanoparticle_formation_in_deformed_pearlitic_steels?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/232017708_Grain_refinement_and_formation_of_ultrafine-grained_microstructure_in_a_low-carbon_steel_under_electropulsing?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/237076155_Influence_of_electropulsing_on_nucleation_during_phase_transformation?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/231799181_Ultrafine-grained_microstructure_in_a_Cu-Zn_alloy_produced_by_electropulsing_treatment?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/279714716_Effect_of_electric_current_pulses_on_grain_size_in_castings_J?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/279714716_Effect_of_electric_current_pulses_on_grain_size_in_castings_J?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/234935805_Segregation_of_lead_in_Cu-Zn_alloy_under_electric_current_pulses?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/234935805_Segregation_of_lead_in_Cu-Zn_alloy_under_electric_current_pulses?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/222249490_Influence_of_an_Electric_or_Magnetic_Field_on_the_Liquid-Solid_Transformation_in_Materials_and_on_the_Microstructure_of_the_Solid?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==https://www.researchgate.net/publication/222249490_Influence_of_an_Electric_or_Magnetic_Field_on_the_Liquid-Solid_Transformation_in_Materials_and_on_the_Microstructure_of_the_Solid?el=1_x_8&enrichId=rgreq-ead7e6b6-c0e4-4e53-8ef5-bc2ea205d4a1&enrichSource=Y292ZXJQYWdlOzI3Nzk0MDI3NjtBUzoyNDc3Nzg3MjcxNjU5NTJAMTQzNjA4NjQ2MDM3Ng==


K ¼ 32

lnba

� �� 65

48� 5

48f

� �lb2 ð10Þ

r1 is the electrical conductivity of the deformed metal and r2 isthe electrical conductivity of the recrystallized metal:

fðr2;r1Þ ¼ ðr1 � r2Þ=ðr2 þ 2r1Þ ð11Þ

Due to the existence of large numbers of deformed microstruc-ture and interfaces within deformed metal where r1 < r2, so thevalue of f(r2,r1) is negative. Furthermore, K is a positive constant.Therefore it can be determined that the value of DGe is negative. Itmeans that the increment of free energy induced by EPT in thedeformed state is higher than that in the recrystallized state.

In order to illustrate the recrystallization mechanism of thedeformed alloy processed by EPT, the schematic diagram of Gibbsfree energy change induced by EPT for ZK60 alloy sample is shownin Fig. 9. The state 1 and state 2 represent the deformed state andthe recrystallized state of ZK60 alloy, respectively. The curve 1 rep-resents the Gibbs free energy of the sample without electropulsing.The free energy of the state 1 (denoted by E) is higher than that ofthe state 2 (denoted by F) because there are a large number ofdeformation twins and interfaces within the deformed sample.The driving force of recrystallization can be described as:

DG0 ¼ GF0 � GE0 < 0 ð12Þ

As shown in curve 2 in Fig. 9, when the electropulsing passesthrough the sample, the free energy of the state 1 and the state 2increase to the positions denoted by E0 and F0, respectively. Thedriving force of recrystallization can be described as:

DG ¼ GF0� GE

0< 0 ð13Þ

In addition, according to the above analysis, jDGj � jDG0j ¼ DGe,which is shown in Fig. 9.

Two kinds of energy (e.g. the Joule heat energy and the addi-tional energy Ge) are introduced into the deformed sample whenthe electropulsing passes through. As a result, the Gibbs freeenergy of the deformed sample will increase during EPT. The addi-tional energy Ge rather than Joule heat will increase the drivingforce of recrystallization, DG. According to the theory suggestedby Conrad et al. [25,26], the recrystallization nucleation mainlydepends on the formation and consolidation of sub-grain.Moreover, the dislocation gliding and climbing have a great influ-ence on the recrystallization nucleation [14,27,28]. The electronwind force induced by electropulsing will promote the dislocation

Fig. 9. Schematic diagram of Gibbs free energy change induced by electropulsingfor the deformed state (state 1) and the recrystallized state (state 2) of ZK60 alloy.

motion and open the tangles of dislocations [14,28,29], whichenhances the nucleation of strain-free grains by the subgrain coa-lescence mechanism.

The size of recrystallization grains depends on the driving forceof recrystallization and the temperature. The larger the drivingforce is, the larger the nucleation rate in the early stage of recrys-tallization will be. Meanwhile, the subsequent rate of grain growthdecreases with the decrease of temperature. Therefore, it can bederived that the EPT can enhance the nucleation rate of recrystal-lization and retard the subsequent rate of grain growth. Based onthe above analyses, the value of DGe is proportional to the squareof the current density and the temperature is related to the currentdensity, the duty ratio and the time of EPT. Thus, the fine recrystal-lization grains can be obtained by EPT with high current densityand low duty ratio.

5. Conclusions

Static recrystallization behavior, microstructure and mechani-cal properties of the rolled ZK60 magnesium alloy sheets duringEPT were investigated and the conclusions can be drawn asfollows:

(1) SRX occurs when the EPT is performed on the rolled ZK60magnesium alloy sheets with a high rolling reduction ofabove 60%, which is similar to that processed by the RHT.However, the difference between the above two methodsis that the much finer recrystallization grains are obtainedby EPT.

(2) The fine grain microstructure and improved mechanicalproperties of ZK60 magnesium alloy sheets are obtained byEPT with a pulse width of 22–25 ls. The grain size of ZK60alloy sheets was refined from 100 lm to 2 lm, the tensilestress was improved from 210 MPa to 320 MPa and the ten-sile elongation was increased from 15.7% to 30%.

(3) The Joule heat induced by EPT has some impact on therecrystallization microstructure of the rolled ZK60 alloy.However, it is obvious that SRX cannot occur only dependson the Joule heat in the present experimental conditions.

(4) The additional energy Ge induced by EPT enhances the driv-ing force of recrystallization, which results in the occurrenceof SRX. Furthermore, it can be derived that the finer recrys-tallization grains can be obtained by using electropulsingwith enough high current density and low duty ratio.

Acknowledgements

The authors thank Program for New Century Excellent Talentsin University (NCET-12-1040), National Natural ScienceFoundation of China (50901048 and 51174143), Key Project ofChinese Ministry of Education (2012017), China ScholarshipCouncil (201308140098), Natural Science Foundation of ShanxiProvince (2015011033), Shanxi Province Science Foundation forYouths (2015021073), Scientific Activities of Selected ReturnedOverseas Professionals in Shanxi Province and Scientific andTechnological Innovation Programs of Higher EducationInstitutions in Shanxi (2014118) for their financial supports.

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Microstructure, mechanical properties and static recrystallization behavior of the rolled ZK60 magnesium alloy sheets processed by electropulsing treatment1 Introduction2 Experimental procedure3 Results3.1 Microstructure of different states of ZK60 alloy3.2 Microstructure evolution of the rolled ZK60 alloy during EPT with different pulse widths3.3 Mechanical properties of the rolled ZK60 alloy processed by EPT with different pulse widths

4 Discussions4.1 Effect of the EPT on microstructure and properties of the rolled ZK60 alloy4.2 Effect of the Joule heat induced by EPT on SRX behavior of the rolled ZK60 alloy4.3 Effect of the additional energy Ge induced by EPT on SRX behavior of the rolled ZK60 alloy

5 ConclusionsAcknowledgementsReferences

Documents

Journal of Alloys and Compoundsniﬁcantly, the size of recrystallization grains was slightly increased and the microstructure became more homogeneous in AZ31 alloy treated by ECAP