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Materials Today: Proceedings 2 (2015) 3565 – 3574

4th International Conference on Materials Processing and Characterization

Development of Al-Fe3Al Nanocomposite by Powder Metallurgy

Route
Deepankar Panda*, Lailesh Kumar, Syed Nasimul Alam
Metallurgical and Materials Engineering Department, National Institute of Technology Rourkela, Rourkela-769008, Orissa, India

Abstract

The present work investigates the microstructure, sliding wear resistance and hardness of an aluminium MMC reinforced with
different (10,20,30) vol. % of Fe3Al intermetallic developed by powder metallurgy route. Nanocrystalline Al developed by ball
milling was mixed with Fe3Al in different vol. % and compacted under uniaxial load of 222MPa and sintered at 500oC in
Aratmosphere. Wear tests of the various Al-Fe3Al composites showed that the wear resistance of the Al-Fe3Al composites
improved significantly with the increase in vol. % of Fe3Al. The hardness of the compositesalso showed increase with the
increasing vol. % of Fe3Al.

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© 2015 Elsevier Ltd. All rights reserved.
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ProcessingProcessing and Characterization.
and Characterization.

Keywords:Metal Matrix Compoistes(MMC) ;Fe3Al intermetallic; Al-Fe3 Al composites; microstructure; wear

1. Introduction

Aluminium based metal matrix composites (MMC) have gained considerable attention as structural materials in
various areas like aerospace, automotive and transportation industries because of their high specific modulus,
specific strength and superior fatigue and creep resistances. Al is widely used in automotive and aerospace
industries due to its excellent properties such as low density (2.72 gm/cc) and high thermal conductivity (237W.m-
1 -1
K ). However, Al has poor wear resistance behaviour and hardness of 167 MPa.Its modulus is 70 GPa and ultimate
tensile strength 110 MPa.For improved different properties, metal matrix composites with hard particles are gaining

* Corresponding author. Tel.: +91-9861272147 ; fax: +91-661-2462022

E-mail address: deepankar.panda66@gmail.com

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing
and Characterization.
doi:10.1016/j.matpr.2015.07.070
3566 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574

importance. This is why Al is reinforced with hard materials like carbides, borides, nitrides, oxides
andintermetallics. Among the reinforcements that are used in Al based metal matrix composites iron aluminide
(Fe3Al) intermetallic gives superior wear resistance. In recent years, Al based metal matrix composites reinforced
with aluminides like Ni3Al and Fe3Al has gained a great attention specifically in wear based applications. For
tribological application an interest in production of intermetallic composites has grown considerably along with the
development
of MMCs. Intermetallic compounds are not only popular for their hardness and wear resistance but also for their
good compatibility with the metal matrix of the composites which makes them more suitable for the tribological
applications. Among nickel aluminides (Ni3Al, NiAl) and iron aluminides (Fe3Al, FeAl), the latter is found to be
more suitable because of their low cost and abundant availability. Fe3Al intermetallic compound shows unique
physical properties and mechanical properties including high melting point (1540oC), high hardness (338HV), low
density (6.72 g/cc) and good oxidation and corrosion resistance. Fe3Al resists corrosion by the formation of an
adherent surface film of Al2O3.Furthermore the yield strength of these compounds increases with the rise in
temperature up to 600oC.Fe3Al is found to be more ductile than stainless steel. These properties make Fe3Al a
suitable material for several applications.High yield strength and ultimate tensile strength and excellent resistance to
highly oxidizing molten salts as well as good sulfidation resistance at high temperatures makes Fe 3Al an ideal
reinforcement material.Composites with Fe3Al as reinforcement could exhibit strength comparable to many ferritic
and austenitic stainless steels which makes them very attractive as candidate materials for high temperature
applications. However low room temperature ductility has been a major obstacle for mechanical processing of these
materials, as a drop in strength above 600°C limits their applications. The binary phase diagram of Fe-Al system is
given in Fig.1.Fe3Al is an intermetallic compound in the Fe-rich portion of the Fe-Al binary phase diagram. Fe3Al is
an intermetallic compound having 25 at. % Al (13.87 wt. % Al). The melting point of Fe3Al is around 1540oC and it
has an incongruent melting point at around 550oC. Its heat of formation ΔH298 is -16 kcal/mol.Fe3Al occurs in any of
three different kinds of crystal structure depending upon the temperature. An ordered D03 type structure below about
550oC, a defective ordered B2 type structure between 550oC and 750oC and disordered BCC structure also called the
disordered A2 type structure at higher temperature. Fe3Al with the D03 structure has excellent wear and corrosion
resistance, but it has a lower plasticity and higher brittleness at a room temperature as compared to the B2 structure
[1-5].

Fe3Al

Fig. 1.Binary phase diagram of Fe-Al system.

2. Experimental

Al powder having purity > 99.99 % was procured from Loba Chemie. Al was milled in a high energy Fritsch P5
planetary ball mill for 20 h. The vials and balls were made of hardened chrome steel. The balls were of 10 mm
diameter. Ball milling was done at 300 rpm with ball to powder mass ratio of 10:1 in wet medium using toluene as
the process control agent. Milling was carried out for a period of 20 h. Samples of milled powder were taken out
intermittently from the vial after intervals of 5 h. Fe3Al having purity of 97.5 % and particle size< 53 μm was
procured from Alfa Aesar. A Phillips Pananalytical PW 3040/00 x-ray diffractometer was used to determine the
various phases in the as-milled powder. The formation of any phase during ball milling and heat treatment of the
ball milled powder were studied by XRD using Cu Kα radiation (λ=0.15406 nm). The crystallite size and r.m.s.
 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574 3567

lattice strain was calculated from the broadening of XRD peaks using Williamson-Hall equation. The pellets of Al-
10, 20, 30 vol. % Fe3Al were formed by cold compaction under a uniaxial compressive load of 222 MPa followed
by sintering at 500oC for 2 h in inert atmosphere. The morphology of ball milled and sintered pallets were
characterized using a JEOL JSM-6480LV scanning electron microscope (SEM) equipped with energy-dispersive x-
ray spectroscopy (EDX). EDX was performed in order to identify the composition. The JEOL JSM-6480LV
scanning electron microscope was equipped with an INCAPentaFET-x3 X-ray microanalysis system with a high-
angle ultra-thin window detector and a 30 mm2 Si(Li) crystal. Density of the samples was measured by Archimedes
principle. Dry sliding wear test was carried out using a ball on plate DUCOM tribometer using diamond indenter. A
20 N load was used for 10 minutes for the wear test of the sample.

3. Results and Discussion

Al was milled for 20 h in wet medium using toluene as process control agent in a high energy Fritsch P5 planetary
ball mill. Samples of milled Al were collected at regular intervals of 5 h. The x-ray diffraction plots of Al milled for
various periods of time is shown in Fig. 2(a). No peaks due to contamination from milling media could be found in
the x-ray diffraction plots. Fig. 2(b) shows the variation of crystallite size of Al with milling time. Al shows a
gradual decrease in crystallite size with milling time up to 15 h of milling. Beyond 15 h of milling there was a slight
rise in the crystallite size possibly due to cold welding taking place during milling. Al is a ductile metal and its
crystallite size after 20 h of milling was found to be 54 nm.Al is very ductile and this is why it is not possible to
reduce it’s crystallite size to a very low valueeven after 20 h of milling. Fig. 2(c) shows the variation of strain with
milling time for Al. There is a gradual increase in r.m.s. strain with increase in milling time.Precise lattice parameter
was calculated using the Nelson-Riley parameter.Fig. 2(d) shows the variation of lattice parameter with milling time
for Al. Lattice parameter shows slight decrease upto 15 h of milling but beyond 15 h of milling there is increase in
lattice parameter [6-8].

(a) (c)

(d) (b)

Fig.2. (a) X-ray diffraction of Al milled for various periods of time; (b) Variation of crystallite size; (c) Variation of
strain;(d)Variation oflattice parameterwith milling time for Al.

Figs. 3(a-c) shows the SEM images of as-received Al powder. Most of the powder particles were found to be nearly
spherical. Few particles were also found to be dumbbelled shape or granular. Particles ranging from less than 10 μm
to about 30 μm could be found in the SEM image of the as-received Al powder. Fig. 3(d) is the EDX analysis of the
as-received Al. It shows the composition of the as-received powder as 100 % Al.Fig. 3(e-g) shows the SEM images
3568 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574

of Al milled for 20 h. Milling of Al for 20 h leads to layered structure. There is evidence of welding during
mechanical milling of Al. Large particles having flat surface could be seen due to the ductile nature of Al. The EDX
analysis in Fig. 3(h) shows 100 % Al after 20 h of milling. There is absence of contamination from the vials and
balls. Al is a ductile and soft material and shows very little wear of the vials and balls during milling. Al also does
not show any oxidation during milling as Al is known to highly oxidation resistant.

(a) (b)
cps/eV

(c) 120
(d)
Al

100

80

60

40

20

0
1 2 3 4 5 6 7 8 9 10
keV

(e) (f) (g) (h) Element Weight% Atomic%

Al K 100.00 100.00
Element Weight% Atomic%
Totals 100.00
Al K 100.00 100.00
Totals 100.00

Fig. 3. (a-c) SEM of as-received Al; (d) EDX of as-received Al;. (e-g) SEM of 20 h milled Al; (h) EDX of 20 h milled Al.

Fig.3 shows the morphology of as-received and 20 h milled Al powder. The morphological changes during ball
milling of ductile powders like Al can be considered as a combination of two mechanisms, fracture and cold
welding. Initially during milling undergo size reduction due to fracturing later the ductile Al particles tend to deform
and cold weld. The impact of balls during milling flattens the as-received Al particles. These particle later cold weld
to form bigger disc-shape particles. Plastic deformation during milling makes the particles hard and brittle as a result
fracture mechanism becomes dominant after initial few hours of milling.As a result the big plate-like particles now
fracture to form smaller flake-like particles. During the later part of milling fracture mechanism is dominant over
cold welding and the flake-like particles change to equiaxed ones and particle size of the powder reduces. This is
also evident from the variation of crystallite size with milling time in Fig.2 (b) which shows an initial reduction of
crystallite size upto 15 h of milling followed by a rise in the crystallite size. It should be noted that within 5 h of
milling the rate of reduction in crystallite size is very fast after which the crystallite size reduces gradually up t 15 h.

(a) (b) (c) (220)

(200)
(111)

Fig. 4. (a, b) TEM; (c) SAD pattern of 20 h milled Al powder.

The TEM images in Fig.4 (a, b) show that the 20 h milled Al powder is nanometric in dimension. It is evident from
the TEM images that cold welding of the milled Al has taken place. The ring pattern of the SAD image also
indicates that the 20 h milled Al powder is nanometric in dimension. The rings in the SAD pattern could be indexed
to the (111), (200) and (220) planes of the Al lattice [9-12].
 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574 3569

(a) (b)

(c) (d)

Fig. 5. (a) DSC; (b) TGA of unmilled Al powder;(c) DSC; (d) TGA of 20 h milled Al powder.

The DSC plot of unmilled Al in Fig. 5(a) shows an endothermic peak at around 660oC which is the melting point of
pure Al (660.2oC). On the other hand the DSC plot of 20 h milled Al in Fig. 5(c) shows a sharp exothermic peak at
around 650oC with the disappearance of the endothermic peak which was seen in the DSC plot of unmilled Al. The
exothermic peak here is due to the ordering transition in milled Al. The TGA curve of unmilled Al in Fig. 5(b)
shows no decrease in initial mass and there was a continuous increase in mass with rise in temperature. On the other
hand the TGA curve of 20 h milled powder in Fig. 5(d) shows a slight decrease in mass initially. Milling was done
in wet medium of toluene. The initial decrease in mass was due to the evaporation of residual toulene present in the
20 h milled powder. Beyond 400oC there was a continuous rise in the mass with the rise in temperature. Comparison
of the TGA plots of unmilledand milled Al in Figs. 5(b) and Fig. 5(d) respectively shows that the increase in mass
due to oxidation of Al was very less in the case of unmilled Al but a large increase in mass was seen in the case of
20 h milled Al as it could be oxidized to a higher extent due to the large surface area of the milled powder [13-16].
(220)

(422)

(311) (400)
(200)

Fig. 6. X-ray diffraction of Fe3Al.

The phase evolution of Fe3Al was characterized by the X-ray diffractometer using Cu Kα radiation (λ=1.5406 Å).
Fig. 6shows the x-ray diffraction pattern of as-received Fe3Al.The strong noticeable peaks which can be seen in the
x-ray diffraction plot of Fe3Al in Fig. 6 are at 2θ values of 44.186o, 52o, 64.256o, 81.286o. They are indicated as the
characteristic peaks of Fe3Al and are noted to (220), (311), (400) and (422) planes respectively. The appearanceof a
low intensity peak at the d-value of 2.89 Ǻ (2θ=27.8o)present in the XRD spectrum of the bulk sample, corresponds
to the (200) superlattice peaks of Fe3Al. The profile corresponding to the (200) superlattice peak confirms that the
as-received powder has D03-crystal structure. Ordered Fe3Alwith D03structure are considered to be very good
structural intermetallics for high temperature applications, due to their high temperature strength and excellent
3570 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574

creepresistance. Fig.7 (a, b) are the SEM images of as-received Fe3Al powder. The SEM images suggest that the
Fe3Al particles have an irregular morphology. The EDX analysis of the as-received Fe3Al powder in Fig 7(c) shows
only Fe (83.84 at. %) and Al (16.16 at. %) in the powder [5, 16, 17].

(a) (b) (c) Element Weight% Atomic%

Al K 8.52 16.16

Fe K 91.48 83.84

Totals 100.00

Fig. 7. (a, b) SEM; (c) EDX of Fe3Al as-received powder.

Fig. 8(b) and(c) show the elemental maps of Fe and d Al respectively in the as-received Fe3Al powder. Fig.8 (a) is
the SEM image of the particle used for the elemental maps. The elemental maps of Fe and Al suggest that there is a
higher concentration of Fe in the powder. Fe is densely distributed in the powder whereas Al is found to be in
slightly lesser concentration although the both Fe and Al show similar distribution and are found to be present
together in the same region. The EDX analyse in Fig. 8(d) gives almost similar concentration of Fe (81.58 at. %) and
Al (18.42 at. %) as had been seen earlier in the EDX analysis in Fig.7(c).

(a) (b) (c) (d)

Element Weight% Atomic%
Al K 9.83 18.42
Fe K 90.17 81.58
Totals 100.00

Fig. 8. (a) SEM of as-received Fe3 Al powder; Elemental map of (b) Fe; (c) Al in the region shown in the SEM image in (a);(d) EDX of the
sample.

(a) (b)
Peak at 758oC

Fig. 9. (a) DSC; (b) TGA of as-received Fe3Al.

The DSC plot in Fig. 9(a) suggests that the as-received Fe3Al powder has high thermal stability. Iron aluminides
exhibit order-disorder transformations and large concentrations of defects that depend on temperature and
composition. Fe3Al has ordered cubic D03 crystal structure. It is known that Fe3Al transforms from D03 structure to
a defective ordered cubic B2 crystal structure at temperatures above the critical ordering temperature of 541 oC. Here
also we see an exothermic peak at 758oC in the DSC plot shown in Fig. 9(a). This peak corresponds to the
transformation of Fe3Al from a D03 structure to a defective ordered cubic B2 crystal structure (D03යB2 transition).
The TGA plot of as-received Fe3Al powder in Fig. 9(b) showed only a slight oxidation up to a temperature of 550oC.
It should be noted that there almost negligible mass increase up to 550oC. A higher weight gain due to oxidation was
found in the temperature range of 550-800°C. Fe3Al is known to have very good corrosion resistance [14, 18].
 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574 3571

Fig. 10 shows the optical micrographs for Al-10, 20, 30, vol. % Fe3Al sintered composites. Al-10, 20, 30 vol. %
Fe3Al composites were developed by uniaxial cold compaction of the pellets undera load(d)of 222 MPa followed by
sintering at 500oC for 2 h in Ar atmosphere. The optical images of the various composites in Fig.10 (a-d) show
white coloured Fe3Al dispersed homogeneously in the Al matrix. The Fe3Al particles are found to be irregular in
shape. The micrographs indicate that the composite was compact and uniform.It can be concluded from the optical
micrographs that the Fe3Al particles are randomly distributed in the Al matrix and there is no segregation of the
Fe3Al particulates in the sintered composites. Absence of segregation in Al-Fe3Al sintered composites can be
attributed to the uniform mixing of the powders.The sintered Al-Fe3Al composites exhibit better homogenous and
compact microstructure with the increase of Fe3Al content in the Al matrix. It can be seen in Fig.13 that there is an
improvement in the relative density of the Al-Fe3Al sintered composites with the increase in Fe3Al content [19-22].

(a) (b) (c) (d)

Fig.10. Optical images of (a) pure Al; (b) Al-10 vol. % Fe3Al composite; (c) Al-20 vol. % Fe3 Al composite; (d) Al-30 vol. % Fe3Al composite.

The EDX analysis of sintered pure Al sample in Fig, 11(c) shows the presence of oxygen apart from Al. This is
possibly due to the oxidation of Al by the unavoidable oxygen present during sintering. Sintering was done at 500oC
for 2 h in Ar atmosphere. In all the Al-10, 20, 30 vol. % Fe3Al composites shown in Fig. 11 large Fe3Al particles
having size between 30-40μm could be seen in the sintered composites. Elemental maps of Al and Fe suggests that
the Fe3Al particles are surrounded by finer Al particles.The sintered Al-Fe3Al composites exhibited homogenous
and compact microstructure.

(a) (b) (c) Element Weight% Atomic%

OK 35.59 48.24
Al K 64.41 51.76

Totals 100.00
SEM Image

(d) (e) (g) (h)

(f)

O Al Fe
SEM Image
3572 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574

(i) (j) (k) (l) (m)

O Al Fe
SEM Image

(n) (p) (q) (r)

SEM Image
(s) (t)
(o)

Fe Al

Fig.11. (a-c) SEM image and EDX of pure sintered Al; SEM image and elemental map of O, Al, Fe in (d-h) Al-10 vol. % Fe3 Al; (i-m) Al-20 vol.
% Fe3 Al; (n-t) Al-30 vol. % Fe3 Al sintered composites.

The x-ray diffraction plot in Fig.12 shows the presence of Al2O3 in the sintered composites. Al2O3 peaks are seen
due to the oxiadtion of Al by unavoidable oxygen present during sintering of the composites. No new reaction
product between Fe3Al and Al could be found in the compoistes. The (200) superlattice peak of Fe3Al could be seen
in x-ray diffraction plots of Al-20, 30 vol. % Fe3Al sintered composites.

Fig.12. X-ray diffraction plot of pure Al, pure Fe3Al and Al-10,20,30 vol.% Fe3 Al sintered composites.

The relative densities of pure Al and Al-10, 20, 30 vol. % Fe3Al sintered composites shown in Fig. 13 were
measured by the Archimedes’ method. The relative density of these sintered composites increase with the increasing
Fe3Al content. The highest relative density of about 67% was achieved in the case of Al-30 vol. % Fe3Al sintered
composite. Addition of higher vol. % of Fe3Al to the Al-Fe3Al composite led to higher densification of the
composite. It should be noted that Al has a melting point of 660oC and Fe3Al has a melting point of 1540oC. At
500oC solid state sintering takes place. Hardness of the composites also increases with the increase in hard Fe3Al
particle content in the composites. Fe3Al has high hardness of nearly 338HV[3,21-24].
 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574 3573

Fig.13. Varition of relative desnity of pure Al and Al-10, 20,30 vol.% Fe3Al sintered composites.

Fig.14. Varition of hardness of various Al-Fe3Al sintered composites.

Fig. 14 shows the variation of microhardness in pure Al and Al-10, 20, 30 vol. % Fe3Al sintered composites. From
the microhardness results it can be concluded that hardness of the sinteredpellets improved with the increasing Fe3Al
content in the respective sintered composites.Fe3Al is harder than Al so the microhardness of the Al-10, 20, 30 vol.
% Fe3Al sintered composites increasedwith the increasing Fe3Al content. It should be noted that the sintered
composite has reached highest hardness value when therelative density of the composite reached maximum
valuethat is in the case of Al-30 vol. % Fe3Al sintered composite. So the hardness value typically depends on the
hard Fe3Al particle content in the sintered composite and the sintering condition.Wear studies done on the powder
metallurgy routebased Almetal matrix composites, reinforced with Fe3Al particles under dry sliding conditions
exhibitenhanced wear resistance of the sintered composites.In Fig.15 it can be seen that the wear depth of sintered
composites decreases significantly with increasing Fe3Al content in the Al-Fe3Al sintered composites. From Fig.15
it is evident that Fe3Al particles providesuperior wear resistance to the Al matrix.This enhancement in wear
resistance can be attributed to the high hardness of Fe3Al particles (338HV) as compared to soft and ductile
unreinforced sintered A. The SEM images in Fig. 16(a-d) show the wear track of pure Al and Al-10, 20, 30
vol.%Fe3Al sintered composites. It can be seen that the width of the wear track reduces significantly with the
increase in Fe3Al content in the sintered composites [25-28].

Fig.15. Varition of wear depth of pure Al and Al-10, 20,30 vol.% Fe3Al sintered composites.
3574 Deepankar Panda et al. / Materials Today: Proceedings 2 (2015) 3565 – 3574

(a) (b) (c) (d)

291 μm
219.5 μm
433 μm

212 μm

Fig.16. SEM image of the wear track of of (a) pure Al (b) Al-10 vol.% Fe3 Al (c) Al-20 vol.% Fe3 Al and (d)Al-30vol.% Fe3Al sintered
composites.
Conclusions
Al-Fe3Al composites could be successfully developed by powder metallurgy route. These composites show
significant imporvement in wear resistance with the increase in content of Fe3Al in the Al-Fe3Al composites.
Hardness of the composites was also found to increse with the increase in Fe3Al content. Realative density of the
sintered samples of Al-Fe3Al composites showed slight increase with increae in Fe3Al content. No new pahse was
formed between Al and Fe3Al in the sintered composites although Al showed a higher tendency of oxdiation
leading to the formation of Al2O3.

Acknowledgments We gratefully acknowledge the

support provided by XRD, SEM and Thermal analysis Laboratory of Metallurgical and Materials Engineering
Department, NIT Rourkela and the FESEM laboratory of the Ceramic Engineering Department of NIT Rourkela.
We also thank the support provided by the Central Research Facility, IIT Kharagpur.

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