Journal of Magnetism and Magnetic Materials 449 (2018) 297–303

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Journal of Magnetism and Magnetic Materials

journal homepage: www.elsevier .com/locate / jmmm

Effect of process control agent on the structural and magnetic propertiesof nano/amorphous Fe0.7Nb0.1Zr0.1Ti0.1 powders prepared by high energyball milling

https://doi.org/10.1016/j.jmmm.2017.10.0180304-8853/� 2017 Published by Elsevier B.V.

⇑ Corresponding author at: Department of Nano Technology, Mineral IndustriesResearch Center (MIRC), Shahid Bahonar University of Kerman, 7618868366Kerman, Iran.

E-mail address: m.h.khazaei@eng.uk.ac.ir (M.H. Khazaei Feizabad).

Mohammad Hossein Khazaei Feizabad a,b,⇑, Shahriar Sharafi a,c, Gholam Reza Khayati a,c,Mohammad Ranjbar a,d

aDepartment of Nano Technology, Mineral Industries Research Center (MIRC), Shahid Bahonar University of Kerman, 7618868366 Kerman, IranbYoung Researchers Society, Shahid Bahonar University of Kerman, 7618868366 Kerman, IrancDepartment of Material Science and Engineering, Shahid Bahonar University of Kerman, 7618868366 Kerman, IrandDepartment of Mining Engineering, Shahid Bahonar University of Kerman, 7618868366 Kerman, Iran

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

Article history:Received 31 May 2017Received in revised form 29 September2017Accepted 4 October 2017Available online 14 October 2017

Keywords:Amorphous alloyCrystallinitySoft magnetic propertiesMillingThermal stability

In this study, amorphous Fe0.7Nb0.1Zr0.1Ti0.1 alloy without metalloids was produced by mechanical alloy-ing of pure mixture elements. Miedema’s semi-empirical model was employed to predict the possibilityof amorphous phase formation in proposed alloying system. The effect of Hexane as process control agent(PCA) on the structural, magnetic, morphological and thermal properties of the products was investi-gated. The results showed that the presence of PCA was necessary for the formation of amorphous phaseas well as improved its soft magnetic properties. The PCA addition causes an increase of the saturationmagnetization (about 43%) and decrease of the coercivity (about 50%). Moreover, the sample milledwithout PCA, showed a wide particle size distribution as well as relatively spherical geometry. While,in the presence of PCA the powders were aspherical and Polygon. In addition, the crystallization andCurie temperatures were found to be around 800 �C and 650 �C, respectively which are relatively highvalues for these kinds of alloys.

� 2017 Published by Elsevier B.V.

1. Introduction

Silicon steels are widely used in magnetic components for theirhigh magnetization. On the other hand, these alloys have poor softmagnetic properties in the high frequency ranges and their appli-cations are limited to the low frequency ranges. These materialsdo not have appropriate permeability and core loss. However, theyare challenged by the amorphous and nanocrystalline Fe basedalloys which show much higher permeability, lower core lossand can be used in high frequency applications [1–8].

There are two main routes to produce amorphous alloys [9]:rapid quenching and mechanical alloying. In the rapid quenching,the molten alloy must be solidified rapidly that can be achieved byseveral techniques such as: arc melt casting, suction casting, lowpressure copper mould casting, high pressure die casting, wateratomization, melt spinning and centrifugal casting [3,9–12].In this

route, the existence of metalloids such as Si and B are necessaryfor amorphousphase formation inorder to decrease the critical cool-ing rates [13]. But these atoms may lead to the formation of someintermetallic compounds such as borides that are detrimental forformability and soft magnetic properties [14–19].

Mechanical alloying is an effective method to produce non-equilibrium structures such as nanocrystalline, extended solidsolution and amorphous structures. In this method the particlesare repeatedly cold welded and fractured. These processes leadto the formation of layer structures and crystalline defects and aslight temperature raising, consequently; solid solutions can beformed [9]. With increasing the milling time, destabilization ofthe crystalline phases are thought to occur by the free energyincrease through accumulation of structural defects such as vacan-cies, dislocations, grain and antiphase boundaries. The continuousdecrease in grain size (and consequently increase in grain bound-ary area) and a lattice expansion would also contribute to the freeenergy increase of system to a level higher than that of the amor-phous phase; consequently; the formation of amorphous phase canbe possible [20].

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298 M.H. Khazaei Feizabad et al. / Journal of Magnetism and Magnetic Materials 449 (2018) 297–303

In the mechanical alloying in contrast to rapid quenching, met-alloid elements are not necessary for amorphous formation. Thereare a few published papers [15,16] about synthesizing amorphousFe based alloys without using metalloids by mechanical alloying. Inthis investigation the Fe0.7Nb0.1Ti0.1Zr0.1 amorphous alloy was pro-duced by mechanical alloying process and the effect of PCA (pro-cess control agent which is an organic substance that reduce thecold welded rate) on the structural and magnetic properties andthermal stability of the alloy was studied.

2. Materials and methods

The Fe0.7Nb0.1Ti0.1Zr0.1 alloy was prepared by mechanical alloy-ing from pure elemental powders. The characteristic of the pow-ders are: Fe (Merck, 99%, 10 lm), Nb (Alfa Aesar, 99.8%,

Fig. 1. The mixing enthalpy of Fe0.7(NbTiZr) (kJ/mol).

Fig. 2. The XRD pattern of unmilled powder mixtures.

M.H. Khazaei Feizabad et al. / Journal of Magnetism and Magnetic Materials 449 (2018) 297–303 299

where P, Q and R are empirical constants and proposed by Miedemaand co-workers. u and n are the work function and electronic den-sity at the boundary of Wigner-Seitz cell, respectively. Also, the con-stant a that is consequent upon experimental volume contractionsin compounds and are equal to 0.14 for alkaline metals; 0.10 fordivalent metals; 0.07 for noble and trivalent metals and 0.04 forall other metals. The applied parameters in present study are takenfrom Ref. [24].

Fig. 1 shows the enthalpy of amorphous phase formation forFe0.7(NbTiZr) alloys. It can be seen that for all of these alloys, theformation enthalpy is negative which indicates that in the studiedcases the formation of amorphous phase with the compositionFe0.7Nb0.1Ti0.1Zr0.1 is thermodynamically possible. The formationenthalpy of proposed composition was calculated to be about –34.42 kJ/mol.

Fig. 3. The XRD patterns of powders milled for different times with and withoutPCA.

3.2. Microstructure characterization

As shown in XRD pattern of unmilled sample (Fig. 2) the inten-sity of Nb element is more than those of the Fe and other elements.The reason of this can be that X-ray does interact with the elec-trons around the atoms. Consequently, the heavier elements suchas Nb that have more electrons, scatter X-rays more strongly. Alsoit can be seen that Ti peaks do not appear in the XRD pattern ofunmilled powder because Ti have low density and its mass valueis also low (about 7 percent).

Fig. 3 shows the XRD patterns of Fe0.7Nb0.1Ti0.1Zr0.1 alloy withand without PCA. From this figure, it can be seen that after 10 hof milling the peaks of all the soluble elements are disappeared,except Zr peaks. It can be deduced that the dissolution of Zr is moredifficult than that of Nb and Ti despite the fact that it has morenegative mixing enthalpy in Fe (�118 kJ/mol) compared withthose of Ti (�74 kJ/mol) and Nb (�70 kJ/mol) in the Fe. The largeratomic radius of Zr is probably responsible for this phenomena.Increasing the milling time up to 20 h leads to formation of singlephase of iron based nanocrystalline solid solution. As can be seenin the figure, increasing the milling time for the sample that havePCA is along with decreasing of the sharpness of the main peakand consequently at the 60 h of milling a halo which is typicalfor amorphous materials is formed. However, in the sample with-out the PCA for all milling times the main peak maintains some of

its sharpness. The sharpness of the peak can be a sign of the crys-talline part of the solid solution phase. It can be concluded that thepresence of the PCA enhances the formation of amorphous phase.Hexane, as PCA, has low boiling temperature (68 �C) and duringthe milling process it can be evaporated and decomposed thatcan damp the energy of ball collision which yields to lower tem-perature raising [26] and prevents the mechanical crystallization.On the other hand, the PCA decomposition produce H and Celements. The H and C can penetrate to the interstitial places inthe alloy structure and act as catalyst for the formation ofamorphous phase [20,27,28].

A closer observation on the main peak changes during themilling process (Fig. 4) reveals the asymmetric shape of both sam-ples at the initial stages of milling. While at the final stages ofmilling, only the samples prepared in the presence of PCA maintainthe symmetric shape of the main peak. It can be concluded thatasymmetric peaks are composed of a sharp peak and a broad peakresponsible for crystalline and amorphous portions, respectively.The deconvolution of the peaks for the samples which were milled

Fig. 4. Deconvolution of the XRD patterns of powder milled for 10 h a) with PCA and b) without PCA.

Fig. 5. The crystallinity percent variation of samples milled up to 60 h.

Fig. 6. TEM bright field image and selected area electron diffraction patterncorresponding to the sample milled for 60 h with PCA.

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for 10 h are presented in Fig. 4. The area under these peaks can beused for the estimation of the percent of crystallinity in the sampleduring the milling process. For this purpose the Eq. (14) can beused:

Percent of Crystallinity ¼ Ac=ðAc þ AaÞ � 100 ð14ÞIn this equation Aa and Ac are the area under the amorphous and

crystalline peak, respectively. Fig. 5 shows crystallinity of the sam-ples as a function of milling time. It can be pointed out that in thecase of sample with PCA, crystallinity decreases with increasingmilling time up to 60 h. On the other hand, in the sample that ismilled without PCA, the decreasing of crystallinity continues upto 30 h of milling, but further milling leads to a higher crystallinity.

Fig. 6 shows the TEM analysis including the bright field imageand standard area electron diffraction (SAED) pattern of samplemilled for 60 h with PCA. The diffused halo pattern of SAED verifiesthe formation of amorphous phase.

3.3. Magnetic properties

Coercivity and permeability as the two main magnetic proper-ties of soft magnetic materials are a function of microstructure,chemical composition, history and grain size (D). The coercivityincreases with decreasing grain size. But in a certain grain size,called exchange length, the relation between the coercivity and

grain size changes. The basic exchange length for iron is about40 nm [13]. For the smaller grain size the relation between coerciv-ity and grain size follows the D6 relation. This behavior can bedescribed by random anisotropy model [13,29]. Permeabilityshows inversely behavior with grain size [13].

Fig. 7 shows the coercivity changes of samples versus themillingtime. Accordingly, the coercivity decreases continuously in the pres-ence of PCA. There are two factors that can affect the coercivity: thefirst factor is crystal defects that increase alongwithmilling processleads to increase the coercivity. Second factor is the crystallite sizethat if it was in the range lower than exchange length, the decreaseof the crystallite size leads to decrease of coercivity. From the coer-civity changes of sample with PCA, it is obvious that the crystallitesize is lower than the exchange length after 10 h ofmilling andwithincreasing the milling time up to 60 h the coercivity decreases withreductionof grain sizebasedon the randomanisotropymodel. Theseresults are verified with change of the crystallinity, calculated bydeconvolution of themain XRD peak. The coercivity of samplewith-out PCA showsaminimumafter about 30 hmilling. Basedon the cal-culated crystallinity, it can be concluded that after 30 h milling, themechanical crystallization results an increase of the crystallite sizeand consequently the coercivity.

Fig. 7. The coercivity variation of samples milled up to 60 h.

Fig. 8. The saturation magnetization variation of samples milled up to 60 h.

Fig. 9. SEM images of the samples milled

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Fig. 8 shows the variation of saturation magnetization of thealloy as a function of milling time with and without PCA. Accordingto these results, the saturation magnetization of the samples (withand without PCA) decreases rapidly up to 20 h of milling. In thisstage of milling the formation of solid solution has been occurredthat causes the diffusion of nonmagnetic elements (Nb, Zr and Ti)into the magnetic structure of Fe and changing the nearest neigh-bor atoms of the magnetic element (Fe), which leads to lower sat-uration magnetization. This reduction of magnetization is less inthe case of the sample with PCA at longer milling time and isalmost constant after 50 h milling. The decrease of the magneticsaturation in this stage may be the result of defects and internalstresses induced by mechanical alloying. Finally, using of PCA leadsto raise the saturation magnetization up to 43% in this work. Pilaret al. have reported similar results in Fe-Zr based alloy [30].

3.4. Morphological changes

The morphology of particles have a great effect on the greendensity, green pore size as well as compaction pressure of powders.In compaction process the particles transmit the compressivestress to their nearest neighbors. The spherical particles have min-imal contact points with each other and consequently, are very dif-ficult to compact [21]. Fig. 9 shows the morphology of the mixedpowders after 60 h of milling. Accordingly (Fig. 9a), the samplewithout PCA, shows a wide particle size distribution as well as rel-atively spherical geometry. While, in the presence of PCA the pow-ders are aspherical and Polygon (Fig. 9b). The lubricating effect ofthe PCA decreases the friction coefficient between the constituentsof milling environment, thereby tending to deform the powderparticles into thin flake geometry [21]. By continuing the millingprocess, these flaky particles become fine with non-sphericalshapes. The TEM observations confirmed these results.

Moreover, the particle size distribution (PSD) of samplemilled inthe presence of PCA (Fig. 10) shows a narrow PSD with a Gaussianlike profile due to the balance between the coldwelding and fractur-ing phenomena. It is necessary to note that the Gaussian profile canbe useful in future compaction process of the powders [9].

3.5. Thermal stability

Fig. 11 shows DTA curve for the sample milled for 60 h. Thisthermal analysis was performed under Ar atmosphere. From theresults presented in this figure, it can be seen that TG curve does

for 60 h a) without PCA b) with PCA.

Fig. 10. Particle size distribution of the sample milled for 60 h with PCA.

Fig. 11. The heating DTA/TG curve corresponding to the sample milled for 60 hwith PCA.

Table 1The magnetic properties of the as-milled and stress relived samples.

Ms. (A.m2/kg) Hc (kA/m)

As-milled 59 2.05Annealed 87 1.78

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not show any mass changes. The first exothermic peak in the DTAcurve which is speared over about 200 �C is related to the strainrelaxation, recovery and structural relaxation. The second exother-mic reaction, started at 800 �C, can be related to crystallization ofamorphous phase. This crystallization peak shows that the thermalstability of this alloy have a remarkable increase compared withalloys that used metalloid elements [9,14,17,31,32]. Crystallizationprocess is known to be based on the diffusion of the atoms. How-ever, the diffusion of large solvent atoms such as Nb, Zr and Ti in Felattice is more difficult and consequently higher temperature areneeded for such crystallization process. Also, from the slope changeof this alloy heating curve (Fig. 11), it can be pointed out that theCurie temperature is about 650 �C which is much higher than thatof alloys containing metalloid [9,14].

3.6. Stress reliving

In soft magnetic materials, the presence of external field is nec-essary to move domain walls within the substances. The amount ofthis field may be from tens to hundreds of Oersteds due to thebarrier effects of imperfections in front of domain walls motion.

Inclusions and residual stress in microstructure are the main typeof imperfection within the soft magnetic materials [33]. Residualmicrostress acts as domain wall motion barrier due to magne-tostriction effects. Wall motion changed the direction of magneti-zation by volume swept out. Due to magnetostriction effects, anelastic deformation is created and interacted with local stress dis-tribution in a way that to maintain the domain wall in its first sit-uation. Moreover, the domain wall energy is effected by localmicrostress by adding the stress anisotropy to crystal anisotropy[33].

To reduce the residual stress, the amorphous sample wasannealed for 40 min at heating rate of 5 �C (based on the DTAresult). Table 1 present the magnetic properties of the as milledand stress relived of Fe0.7Nb0.1Ti0.1Zr0.1 samples. It can be seen thatthe coercivity was decreased after heat treatment due to the recov-ery and the strain relaxation of the microstructure. Moreover,increasing of saturation magnetization can be related to the stressrelaxation and removing of Hexane (i.e. absorbed on the surface ofproducts) [31].

4. Conclusions

The amorphous Fe based alloy was produced by mechanicalalloying without using the metalloid elements. The XRD and TEMresults confirmed the formation of Fe0.7Nb0.1Zr0.1Ti0.1 amorphouspowder as dominant phase after 60 h of milling in the presenceof Hexane as PCA. In comparison with the sample milled withoutPCA, the presence of PCA increased the saturation magnetizationas well as decreased the coercivity. The structural and magneticstudies of this alloy proved that the presence of PCA is necessaryto produce nano/amorphous Fe0.7Nb0.1Zr0.1Ti0.1 powders bymechanical alloying method with enhanced magnetic properties.The VSM and XRD results showed that the metalloids are not nec-essary to produce amorphous phase for improving magnetic prop-erties. Moreover, the crystallization and Curie temperatures ofmilled sample with PCA were determined to be about 800 �C and650 �C, respectively. Both of these characteristics are higher thanthe reported values for alloys containing the metalloids elements.

Acknowledgments

The authors gratefully acknowledge INSF for the funding of thisproject (Grant agreement number 95850011).

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Effect of process control agent on the structural and magnetic properties of nano/amorphous Fe0.7Nb0.1Zr0.1Ti0.1 powders prepared by high energy ball milling1 Introduction2 Materials and methods3 Results and discussion3.1 Thermodynamic prediction3.2 Microstructure characterization3.3 Magnetic properties3.4 Morphological changes3.5 Thermal stability3.6 Stress reliving

4 ConclusionsAcknowledgmentsReferences