j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560

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Short Technical Note

Characterization of mechanically alloyed

Fe100−x Six and Fe83.5 Si13.5 Nb3 nanocrystalline powders

S. Miraghaei, P. Abachi ∗ , H.R. Madaah-Hosseini, A. Bahrami

Materials Science and Engineering Department, Sharif University of Technology, P.O. Box 11365, 9466 Tehran, Iran

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

Article history: In present research, nanocrystalline Fe100−x Six (x = 6.5, 10, 13.5, 20 and 25 at.%) and
Received 25 August 2007 Fe83.5 Si13.5 Nb3 alloy powders were prepared by mechanical alloying using high-energy ball
Received in revised form milling. The resulting powders mainly consist of micron-sized particles with an average
5 November 2007 grain size of less than 20 nm. According to the XRD test results, by increasing the milling time
Accepted 12 November 2007 and/or the Si content the lattice parameter decreases and the internal microstrain increases.
In addition, the specific saturation magnetization diminishes as Si content increases. The
coercive forces of the as-milled nanocrystalline powders are much higher than those of cor-
Keywords: responding Fe–Si bulk alloys with a minimum at 13.5 at.% Si. The presence of Nb retards
Mechanical alloying the crystallite coarsening during annealing but adversely affects the magnetic properties.
Nanostructured Fe–Si powder Annealing of milled powders caused the coercive force to reduce slightly due to reduction
Soft magnetic properties of internal strains.
© 2007 Elsevier B.V. All rights reserved.

1. Introduction electrical resistivity, lower thermal conductivity and superior

The Fe–Si alloys as soft magnetic materials with low coer-
cive force, high magnetic permeability and low core loss
are widely used as magnetic cores in electrical appliances
(Yoshizawa et al., 1994; Ding et al., 2001). The addition of
proper amounts of Si to Fe not only results in decrement of
magnetic anisotropy and coercive force but also increment
of electrical resistivity and, thereby, reduction of eddy cur-
rent loss (O’Handley, 2000; Zhou et al., 1999). Nb has a large
atomic radius in comparison with that of Fe and it seems
that addition of Nb to Fe–Si alloys prevents grain growth
(McHenry and Willard, 1999). Nanostructured or nanocrys-
talline materials have different physical properties from
non-crystalline, single-crystalline and polycrystalline mate-
rials. These materials exhibit often considerably improved
properties, including increased mechanical properties, higher
soft magnetic properties, in comparison with those of conven-
tional coarse grained polycrystalline materials (Anon., 1998).
Mechanical alloying is a convenient and economical method
to completely synthesise nanostructural alloy powders from
elemental powders (Chiriac et al., 1999; Suryanarayana, 2001).
However, the high value of disordered grain boundaries,
extended imperfections, micostresses and internal strain are
characteristics of mechanically alloyed powders. Since these
parameters adversely affect the magnetic properties, espe-
cially coercive force, applying an annealing process at proper
temperature could reduce the internal strain and there-
fore causes magnetic properties’ improvement (Phan et al.,
2005).
In present research, nanocrystalline Fe100−x Six (x = 6.5, 10,
13.5, 20 and 25 at.%) and Fe83.5 Si13.5 Nb3 alloy powders were
prepared by mechanical alloying. The effects of milling time,

∗
Corresponding author.
E-mail address: abachi@sharif.edu (P. Abachi).
0924-0136/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2007.11.064
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560
chemical composition and annealing on powder structures
and magnetic properties were investigated.
2. Experimental procedure
2.1. Alloy powder preparation
The high purity Fe, Si and Nb powders with particle size of <200,
<150 and <90 ␮m, respectively were used as starting materials. Starting
mixtures in 20-g batches were loaded into a wear-resistant steel vial
together with steel balls of a 20-mm diameter. Ball to powder weight
ratio (BPR) was 10:1. Therefore, around 40 vol.% of vial capacity was
filled with grinding medium. The mechanical milling continued up to
40 h with running speed of 600 rpm under argon atmosphere. The alloy
powders with different amounts of Si in the form of Fe100−x Six with
x = 6.5, 13.5 and 20 at.% and a sample containing Nb in the form of
Fe83.5 Si13.5 Nb3 were prepared. For stress relief purpose and examina-
tion of annealing effects on microstructure and magnetic properties of
samples, two types of powders, i.e. the Fe86.5 Si13.5 alloy powder with
minimum coercive force and Fe83.5 Si13.5 Nb3 containing Nb and same
amounts of Si, were annealed at 370 and 500 ◦ C for 20 min under vac-
uum. To find out these proper annealing temperatures, the differential
scanning calorimeter (DSC) measurements were conducted with heat-
ing at a rate of 10 ◦ C/min in argon atmosphere.
2.2. XRD, SEM and magnetic properties examinations
To determine lattice parameter, grain size and lattice microstrain of
powders particles, the powder specimens were analyzed by an X-ray
diffractometer (Philips X’Pert) using Cu K␣ radiation. In order to obtain
precise measurements of peak position and half-maximum width a
slow scan rate (time per step: 1 s) were employed. Since peak broad-
ening in X-ray diffraction could be due to instrumental and physical
factors such as crystallite size and lattice strain (Zuo et al., 2004; Zhou et
al., 1996; Vives et al., 2004), the instrumental broadening correction was
provided using a reference powder. The reference powder which should
Fig. 1 – Scanning electron micrographs of (a) starting powders mixture and Fe86.5 Si13.5 powder milled for (b) 20 h and (c) 40 h.
555
be free of physical factors, with Bragg’s peaks near those of the sam-
ple under investigation was the starting Fe powder annealed at 700 ◦ C
for 5 h. The instrumental-broadening-corrected line profile breadth ı
of each reflection 2 was calculated from the parabolic approximation
correction (Klug and Alexander, 1974) given by
 1/2
b2
ı(2) = B 1 − (1)
B2
where B and b are the breadth of the same Bragg’s peak (in rad)
for experimental and reference powders, respectively. Both B and
b were calculated by computer software (X’Manager) as full-width
at half-maximum (FWHM) after background removal and K␣2 strip-
ping. The grain sizes and internal strains were obtained using the
Williamson–Hall plot (Williamson and Hall, 1953) given by
0.9
ı(2)cos 0 = +  sin 0 (2)
L
where  0 is the Bragg’s angle of the analyzed peak,  is the incident X-ray
wave length (1.54060 Å), L is the crystallite size and  is the apparent
strain. The values of ı(2) are obtained from Eq. (1). The first five Fe
reflections were used to construct a linear plot of ı(2) cos  0 against
sin  0 . Then, crystallite size L was obtained from the intercept and the
strain  from the slope.
The morphological and particle size changes were examined using a
Philips XL 30 scanning electron microscope operated at 28 kV. Magnetic
properties were measured using a vibrating sample magnetometer
(VSM) with a maximum applied field of 15 kOe at room temperature.
3. Results and discussion
3.1. Evaluation of morphological changes after milling
Fig. 1 shows scanning electron micrographs of the starting
powders mixture, 20 and 40 h milled Fe86.5 Si13.5 powders. By
556 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560

Fig. 2 – Scanning electron micrographs of (a) Fe86.5 Si13.5 and (b) Fe83.5 Si13.5 Nb3 powders milled for 40 h.

increasing milling time, particles become rounded, smaller

with more homogenous size distribution. Similar behavior
could be seen in the case of Fe83.5 Si13.5 Nb3 powder particles.
However, at a certain milling time, powder particles containing
Nb are finer (Fig. 2). During mechanical alloying, morphol-
ogy, size and size distribution of powder particles have been
changed because of the cold welding and fracturing of the
particles. According to Schaffer and McCormick (Schaffer and
McCormick, 1992), when at least one of the components is duc-
tile, these processes result in a fine lamellar structure. This
lamellar morphology is clearly seen on the edges of the as-
milled powder particles in Fig. 3.

3.2. Evaluation of lattice parameter, grain size and

lattice microstrain after milling and annealing

The XRD patterns of the powder specimens milled for differ-

ent times give clear indication of the changes occurring in the
powders during milling. As an example, the observed changes
in the Fe86.5 Si13.5 and Fe83.5 Si13.5 Nb3 alloys are discussed here
but the trend is applicable to all compositions. Fig. 4 shows
the X-ray diffraction patterns of starting powders mixture,
Fe86.5 Si13.5 and Fe83.5 Si13.5 Nb3 powders, after different milling
times. The peaks of Fe, Si and Nb exist in the XRD pattern of
the initial mixture. After milling for 20 h, the Si peaks in the
Fe86.5 Si13.5 powder and the Si and Nb peaks in Fe83.5 Si13.5 Nb3
powder are disappeared. This indicates that Si and Nb atoms

Fig. 4 – XRD patterns of starting powders mixture and (a)

Fe86.5 Si13.5 and (b) Fe83.5 Si13.5 Nb3 powders milled for
different times.

have dissolved in the bcc-Fe matrix. Similar results have been

previously reported for mechanically alloyed Fe–Si powders
(Ding et al., 2001; Zhou et al., 1996; Stevulova et al., 1999).
Furthermore, there are measurable shifts in Bragg’s angle, 2,
which have been used to calculate the changes of the lattice
parameter due to milling.
Fig. 5a shows the (1 1 0) Fe peaks of pure Fe and Fe86.5 Si13.5
milled powders. The (1 1 0) Fe peak is shifted to higher angles
due to changes in lattice parameter during solution of small
Fig. 3 – Lamellar structure of Fe86.5 Si13.5 powder particles Si atoms in the Fe. Fig. 5b shows also the first Fe reflections for
milled for 40 h. pure Fe and Fe83.5 Si13.5 Nb3 milled powders. Like the former
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560
Fig. 5 – X-ray diffraction line profile of pure Fe: (a)
Fe86.5 Si13.5 and (b) Fe83.5 Si13.5 Nb3 powders milled for
different times.
case the Fe peaks is shifted to higher angles in Fe83.5 Si13.5 Nb3
alloys but by increasing the milling time from 20 to 40 h it
returns a little to smaller angles. The changes in lattice param-
eter of the alloys confirm the solution of alloying elements
atoms in the Fe lattice. The lattice parameter was calculated
for each of the bcc-Fe diffracting planes, (1 1 0), (2 0 0), (2 1 1),
(2 2 0), and (3 1 0), from the XRD patterns. The actual lattice
parameter was obtained as described by Cullity (1978), by plot-
ting the calculated lattice parameter for each Bragg’s angle on
the y-axis with the corresponding value of cos2 /sin  on the
x-axis and extrapolating to obtain the intercept on the y-axis.
The lattice parameter reported for the pure ␣-Fe is 2.8664 Å
(Anon., 2007). Table 1 shows the lattice parameter and unit
Table 1 – Lattice parameter, a, and unit cell volume, V, of
pure Fe, Fe86.5 Si13.5 , and Fe83.5 Si13.5 Nb3 powders milled
for 20 and 40 h
Sample a (Å)
Pure bcc-Fe 2.8664
Fe86.5 Si13.5
20 h 2.8615
40 h 2.8592
Fe83.5 Si13.5 Nb3
20 h 2.8614
40 h 2.8623
557
Fig. 6 – Lattice parameter of the as-milled Fe–Si powders
with different Si content.
cell volume of pure Fe, Fe86.5 Si13.5 and Fe83.5 Si13.5 Nb3 powders
milled for different times. Since Si has a smaller atomic radius
than Fe, the substitutional Fe–Si solid solution has a smaller
lattice parameter and reduced unit cell volume in comparison
with those of pure bcc-Fe. Milling for longer times causes more
Si to be dissolved in the Fe lattice. Fig. 6 shows also the depen-
dence of the Fe–Si alloys lattice parameter on the Si content. By
increasing the Si content, lattice parameter decreases due to
more Si atoms introduce into the Fe lattice in powders milled
for 40 h. Nb has a large atomic radius than Fe and therefore,
Fe–Nb solid solution should have a greater lattice parameter.
At the early stages of milling of Fe83.5 Si13.5 Nb3 powder the Si
atoms dissolve in the Fe lattice and cause the lattice parame-
ter to reduce but it seems that by increasing time the Nb atoms
introduce into structure and expand the Fe lattice (Table 1).
The increase of the full-width at half-maximum (FWHM)
of Fe peaks in Fig. 5 is also an indication for development
of refined and internally strained grains during mechanical
alloying. This effect is pronounced by increase of milling time
(Fig. 5a). The grain size and internal microstrain obtained from
the Williamson–Hall plots are listed in Table 2 for Fe86.5 Si13.5
and Fe83.5 Si13.5 Nb3 alloy powders milled for different times.
The grain size decreases while the microstrain increases with
milling time. It is worthy to note that although the grain sizes
have been reduced to a nanometer scale, the size of powder
particles are still in the micrometer scale. The results of the
same calculations for Fe–Si alloy powders are listed in Table 3,
which represents the grain size and microstrain for alloy pow-
Table 2 – Grain size and microstrain values of Fe86.5 Si13.5
and Fe83.5 Si13.5 Nb3 alloy powders after 20 and 40 h
V (Å3 ) milling
23.5511 Alloy Grain size (nm) Microstrain (%)
Fe86.5 Si13.5
23.4305 20 h 17.1 0.85
23.3740 40 h 14.4 1.03
Fe83.5 Si13.5 Nb3
23.4280 20 h 16.5 0.91
23.4501 40 h 12.2 1.19
558 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560

Table 3 – Grain size and microstrain values of the Fe–Si Table 4 – Grain size and microstrain values of Fe86.5 Si13.5
alloy powders with different Si content after 40 h milling and Fe83.5 Si13.5 Nb3 alloy powders annealed at different
temperatures
Alloy Grain size (nm) Microstrain (%)
Alloy Annealing Grain Microstrain
Fe93.5 Si6.5 15.9 0.82 at (◦ C) size (nm) (%)
Fe90 Si10 13.5 0.94
Fe86.5 Si13.5 14.4 1.03 370 16.7 0.65.65
Fe86.5 Si13.5
Fe80 Si20 14.8 1.20 500 44.7 0.60
Fe75 Si25 13.2 1.28
370 12.5 0.89
Fe83.5 Si13.5 Nb3
500 16.9 0.40
ders with different Si content. It seems that by increasing the
Si content, the grain size randomly changes but the micros-
train gradually increases.
The decreasing of crystalline size after milling could be
due to formation of new defects such as dislocations that
can appear in different ways: formation of dense regions of
these dislocations into the grains, pile up the grain boundaries
or untidy clusters into the grain. All these possibilities guide
to formation of sub-grain structures into the original grain,
therefore decreasing the effective size in crystalline region
(Schilling et al., 1996). On the other hand, the increasing of
residual strains into the material could be due to stress fields
associate with the multiplication of the dislocations (Gómez
et al., 2006; Oleszak and Matyja, 1995).
Fig. 7 shows the DSC curves of 40 h milled Fe86.5 Si13.5 and
Fig. 8 – The specific saturation magnetization of as-milled
Fe83.5 Si13.5 Nb3 alloy powders. The main exothermic peak of
Fe–Si powders, single-crystal and polycrystalline Fe–Si
both samples appears at temperature ranging between 400
alloys vs. the Si content.
and 470 ◦ C. Since the maximum temperature in Fig. 7 is esti-
mated to be the same as recrystallization temperature of
sample, the annealed powders at 500 ◦ C could be in fully
recrystallized and then in the grain growth state, whereas the the Si content dependence of  s for as-milled (nonstructured)
annealed powders at 370 ◦ C could not experience recrystalliza- powders, single-crystal (Arai et al., 1985) and polycrystalline
tion. Table 4 shows the calculated grain size and internal strain (Bozorth, 1951) Fe–Si alloys. As it can be seen, the Si con-
of powders after annealing at 370 and 500 ◦ C. Obviously, by tent dependence of  s for as-milled powders is similar to both
increasing annealing temperature, grain growth has occurred reported latter cases. Referring to saturation magnetization
and the strain has been reduced. It seems that presence of Nb definition as the number of magnetic moments parallel to
retards the grain coarsening during annealing. the applied field per unit volume of the material, increasing
the Si content of alloys leads to decrement of Fe as a ferro-
magnetic component and thereby reduction of the saturation
3.3. Evaluation of magnetic properties
magnetization. Considering Fig. 8, specific saturation mag-
netization values of the as-milled powders are slightly less
According to the vibrating sample magnetometer test results,
than those of the corresponding bulk Fe–Si alloys. This may be
the specific saturation magnetization,  s , of Fe–Si alloys
explained by the fact that large volume fractions of disordered
depends on both the structure and the Si content. Fig. 8 shows
regions (the grain boundaries) and extended imperfections
(especially point defects and dislocations) exist in the former
case, while no grain boundary or a very small volume frac-
tion of grain boundaries and few imperfections are present in
the two latter cases. As suggested by Ding and Zhou (Ding et
al., 2001; Zhou et al., 1996), both grain boundaries and imper-
fections can reduce  s . Table 5 shows the specific saturation

Table 5 – The specific saturation magnetization and

coercive force values of as-milled and annealed powders
Condition Alloy  s (emu/g) Hc (Oe)

Fe86.5 Si13.5 176.55 65.8

As-milled
Fe83.5 Si13.5 Nb3 160.92 92.1

Fe86.5 Si13.5 175.5 41.7

Fig. 7 – DSC curves of as-milled Fe86.5 Si13.5 and Annealed
Fe83.5 Si13.5 Nb3 145.4 53.6
Fe83.5 Si13.5 Nb3 alloy powders.
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 554–560
Fig. 9 – The coercive force values of as-milled
nanostuctured Fe–Si alloy powders and the corresponding
calculated values vs. Si content.
magnetization of Fe86.5 Si13.5 and Fe83.5 Si13.5 Nb3 alloys in as-
milled and annealed conditions. The milling time has selected
as 40 h and the annealing temperature and time equal 370 ◦ C
and 20 min, respectively. It is clear that the addition of Nb as a
non-magnetic agent reduces  s as mentioned above. Anneal-
ing of as-milled powders has caused the specific saturation
magnetization to reduce slightly.
Considering O’Handley statement (O’Handley, 2000), by
interruption of the exchange interaction between the fer-
romagnetic nanocrystals, the behavior of nanocrystals is
essentially that of single-domain particles, interacting only
by their weak magnetic dipole fields. For as-milled Fe–Si
powders, the average coercive force of randomly oriented
single-domain particles was calculated. The calculation is
based on saturation magnetization values presented in Fig. 8,
the anisotropy constant values, K1 , for conventional Fe–Si
alloys in bulk form (Bozorth, 1951) and average coercive force
of randomly oriented single-domain particles with positive
values of anisotropy constant (K1 > 0) according to the follow-
ing equation (Kittel, 1949):
0.64K1
Hc ave =
0 Ms
where 0 is the vacuum permeability. Fig. 9 shows depen-
dence of experimental and calculated coercive forces of
as-milled nanostructured Fe–Si alloy powders on Si content
of the alloys. As it is shown in Fig. 9, there is a good fitness
between the calculated and the experimental values of Hc for
the as-milled powders with low Si content alloys. By increas-
ing the Si content, coercive force reduces sharply from 197.4
to 65.8 Oe and then increases gradually to 144.7 Oe. It seems
that, increasing the Si content of the alloys causes two coun-
teracting effects, i.e. (a) reduction of the magnetocrystalline
anisotropy and (b) increase of the strain anisotropy. Increasing
the Si content up to 13.5 at.% decreases the magnetocrys-
talline anisotropy and thus reduces Hc . In high Si alloys, the
strain anisotropy could be dominant and by increasing the Si
content the coercive force increases. Obviously, the obtained
values of coercive force are extremely high while Hc values
in single-crystalline and polycrystalline Fe–Si alloys are less
that 1 Oe (Arai et al., 1985; Bozorth, 1951). The high values
559
of Hc have been reported by Ding et al. (2001), Zhou et al.
(1999), Zhou et al. (1996), Manivel Raja et al. (2000). Ding et
al. (2001) have proposed that high values of coercive force in
nanostructured Fe–Si powders are due to strains developed
during severe plastic deformation. They have reported that
by applying a proper annealing process, a decrease in Hc of
Fe75 Si25 alloy from 73.5 to 2.4 Oe can be resulted. Zhou et al.
(1999) have calculated effective magnetic anisotropy constant,
Keff , of the milled nanocrystalline Fe–Si alloys and shown that
these values are higher than values of K1 in conventional Fe–Si
alloys. High values of Keff in nanocrystalline alloys prepared
by mechanical alloying has been related to the presence of
large amounts of stress and doping of Si atoms along the
grain boundaries which are pinning the domain walls located
on the grain boundaries and lowering their mobility. Manivel
Raja et al. (2000) have suggested that the higher coercive
force of the mechanically alloyed powders can be attributed
to the presence of grain boundaries instead of amorphous
matrix which exists in alloys prepared by rapid solidifica-
tion. They believe that the absence of the residual amorphous
matrix in nanostuctured alloys prepared by mechanical alloy-
ing weakens the ferromagnetic exchange interaction between
nanocrystals. Considering Table 5, annealing made the coer-
civity to decrease but the remained values are still higher
than those of conventional Fe–Si alloys. Therefore, the pres-
ence of the internal strain in the milled powders cannot be
the main reason for higher Hc values. The high values of
coercive force of the prepared powders seems to be due to
the presence of single-domain condition for the nanocrys-
talline Fe–Si alloys without exchange interaction between the
nanocrystals.
4. Conclusions
Based on the experimental results, the following conclusions
could be drawn:
1. The as-milled powders mainly consist of micron-sized par-
(3) ticles with an average grain size of less than 20 nm.
2. By increasing both the milling time and Si content of
the alloyed powders the lattice parameter reduces but the
internal strain increases.
3. The ␣-Fe(Si) substitutional solid solutions have smaller lat-
tice parameter than pure Fe.
4. Specific saturation magnetization,  s , depends on the
structure and essentially on the chemical composition of
the Fe–Si alloys.
5. Coercive force decreases sharply with Si content from 197
to 66 Oe and then increases gradually to 145 Oe.
6. Nb prevents the grain growth during annealing but its pres-
ence in the Fe–Si alloys has adverse effects on the magnetic
properties.
7. Annealing of milled powders causes the coercive force to
reduce slightly due to reduction of internal strains.
8. The high values of coercive force of the prepared powders
seems to be due to the presence of single-domain condi-
tion for the prepared nanocrystalline Fe–Si alloys without
exchange interaction between the nanocrystals.
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references Oleszak, D., Matyja, H., 1995. Nanocrystalline Fe-based alloys

obtained by mechanical alloying. Nanostruct. Mater. 6 (1–4),
425–428.
Phan, M.H., Pengillard, H.X., Wisnom, M.R., Yu, S.C., Chau, N.,
Anon., 1998. ASM Handbook, Powder Metal Technologies and
2005. Effect of annealing on the microstructure and magnetic
Applications, vol. 7. ASM International, USA.
properties of Fe-based nanocomposite materials. Composites
Anon., 2007. Joint Committee for Powder Diffraction Standard
A 37, 191–196.
(JCPDS). File no. 60696.
Schaffer, G.B., McCormick, P.G., 1992. Mechanical alloying. Mater.
Arai, K.I., Ohmori, K., Miura, H., Tsuya, N., 1985. Effect of
Forum 16, 91–97.
order–disorder transition on magnetic properties of high
Schilling, P.J., He, J.H., Cheng, J., Ma, E., 1996. Extended X-ray
silicon–iron single crystals. J. Appl. Phys. 57, 460–464.
Absorption fine structure of metastable bcc and fcc phases in
Bozorth, R.M., 1951. Ferromagnetism (England), 77–85.
mechanically alloyed Fe–Cu. Appl. Phys. Lett. 68 (6), 767–769.
Chiriac, H., Mog, A.E., Urse, M., Necula, F., 1999. Formation and
Stevulova, N., Buchal, A., Petrovic, P., Tkacova, K., Sepelak, V.,
magnetic properties of mechanically alloyed Fe–Cu–Nb–Zr–B
1999. Structural investigation of the high energy milled Fe–Si
nanocrystalline powders. J. Magn. Magn. Mater. 203, 159–161.
system. J. Magn. Magn. Mater. 203, 190–192.
Cullity, B.D., 1978. Elements of X-ray Diffraction, second ed.
Suryanarayana, C., 2001. Mechanical alloying and milling. Prog.
Addison Wesley, London, UK.
Mater. Sci. 46, 1–184.
Ding, J., Li, Y., Chen, L.F., 2001. Microstructure and magnetic
Vives, S., Gaffet, E., Meunier, C., 2004. X-ray diffraction line profile
properties of nanocrystalline Fe–Si powders. J. Alloys Compd.
analysis of iron ball milled powders. Mater. Sci. Eng. A 366,
314, 262–267.
229–238.
Gómez, B., Gordo, E., Torralba, J.M., 2006. Influence of milling time
Williamson, G.K., Hall, W.H., 1953. X-ray line broadening from
on the processing of Fe–TiCN composites. Mater. Sci. Eng. A
field aluminum and wolfram. Acta Metall. 1, 22–31.
430 (1/2), 59–63.
Yoshizawa, Y., Bizen, Y., Arakawa, S., 1994. Magnetic properties of
Kittel, C., 1949. Physical theory of ferromagnetic domains. Rev.
Fe–Cu–Nb–Si–B nanocrystalline alloys with low
Mod. Phys. 21, 541–583.
magnetostriction. Mater. Sci. Eng. A 181/182, 871–875.
Klug, H.P., Alexander, L.E., 1974. X-ray Diffraction Procedures for
Zhou, T., Zhang, J., Xu, J., Yu, Z., Gu, G., et al., 1996. Preparation of
Polycrystalline and Amorphous Materials. John Wiley & Sons,
nanocrystalline Fe–Si alloys and their magnetic properties. J.
New York, USA.
Magn. Magn. Mater. 164, 219–224.
Manivel Raja, M., Chattopadhyay, K., Majumdar, B., 2000.
Zhou, T., Yu, Z., Du, Y.W., 1999. The effective magnetic anisotropy
Structure and soft magnetic properties of finemet alloys. J.
in nanocrystalline Fe–Si alloys. J. Magn. Magn Mater. 202,
Alloys Compd. 297, 199–205.
354–358.
McHenry, M.E., Willard, M.A., 1999. Amorphous and
Zuo, B., Saraswati, N., Shitharan, T., 2004. Production and
nanocrystalline materials for applications as soft magnets.
annealing of Fe–Si and Fe–Si–Al alloy powders. Mater. Sci. Eng.
Prog. Mater. Sci. 44, 291–297.
A 371, 210–216.
O’Handley, R.C., 2000. Modern Magnetic Materials. John Wiley &
Sons, New York, USA.