Journal of Magnetism and Magnetic Materials 401 (2016) 425–431

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Journal of Magnetism and Magnetic Materials

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

Structural and magnetic properties of yttrium iron garnet (YIG) and

yttrium aluminum iron garnet (YAIG) nanoferrites prepared by
microemulsion method
Majid Niaz Akhtar a,b,n, Abu Bakar Sulong b, Muhammad Azhar Khan c, Mukhtar Ahmad d,
Ghulam Murtaza e, M.R. Raza b,f, R. Raza a, M. Saleem a, M. Kashif g
a
Department of Physics, COMSATS Institute of Information Technology, Lahore 54000, Pakistan
b
Department of Mechanical and Materials Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600 Bangi,
Selangor, Malaysia
c
Department of Physics, The Islamia University of Bahawalpur, Bahawalpur 63100, Pakistan
d
Department of Physics, COMSATS Institute of Information Technology, Islamabad, Pakistan
e
Centre for Advanced Studies in Physics, G.C. University, Lahore, Pakistanf Department of Mechanical Engineering, COMSATS Institute of Information
Technology Sahiwal Pakistan
f
Department of Mechanical Engineering, COMSATS Institute of Information Technology Sahiwal, Pakistan
g
Department of Physics, Govt. College University Faisalabad, Pakistan

art ic l e i nf o a b s t r a c t

Article history: Yttrium iron garnet (YIG) and yttrium aluminum iron garnet (YAIG) nanoferrite samples were synthe-
Received 5 January 2015 sized by microemulsion method. The effect of sintering was examined by heating the samples at 900,
Received in revised form 1000, and 1100 °C. The YIG and YAIG samples were then characterized using X-ray diffraction and field-
10 June 2015
emission scanning electron microscopy. Static and dynamic magnetic properties were measured by
Accepted 15 October 2015
Available online 17 October 2015
evaluating initial permeability, Q factor, and vibrating sample magnetometry properties of YIG and YAIG
samples. YIG samples sintered at 1100 °C showed higher initial permeability and Q factor compared with
Keywords: YAIG samples. However, hysteresis loops also showed variations in the saturation magnetization, re-
Yttrium iron garnet (YIG) manence, and coercivity of YIG and YAIG samples sintered at 900, 1000, and 1100 °C. The observed
Yttrium aluminum iron garnet (YAIG)
magnetic parameter such as saturation magnetization, coercivity and initial permeability are strongly
XRD (X-ray diffraction)
affected by increasing temperature. The saturation magnetization and coercivity of YIG and YAIG na-
FESEM (field emission scanning electron
microscopy) noferrites were found in the range 11.56–19.92 emu/g and 7.30–87.70 Oe respectively. Furthermore, the
Static and dynamic magnetic measurements decreasing trends in the static and magnetic properties of YAIG samples may be due to the introduction
of Al ions in the YIG crystal lattice. Thus, YIG and YAIG sintered at 1100 °C can be used for wide-ranging
frequency applications.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction
Ferrimagnetic materials (rgarnets) have been widely in-
vestigated because of their potential applications in various fields
[1]. Garnet ferrites with composition (A3B5O12) structure have
unique electromagnetic, magneto-optical, mechanical, and ther-
mal properties [2]. Garnet ferrite have three crystallographic lat-
tice (a, b, and c) sites. Among these lattice sites, the 24Fe3 þ ,
16Fe3 þ , and 24R3 þ ions occupy the [b] tetrahedral, (a) octahedral,
and {c} dodecahedral sites, respectively, whereas oxygen ions are
distributed to the interstitial sites [3]. However, R is the rare earth
n rotation and high saturation magnetization, this ferromagnetic
Corresponding author at: Department of Physics, COMSATS Institute of In-
formation Technology, Lahore 54000, Pakistan.
E-mail address: majidniazakhtar@ciitlahore.edu.pk (M.N. Akhtar).
ions such as Ce, Gd, Y and Nd. The general formula for rare earth
garnets is R3Fe5O12, whereas the ion distribution in rare earth
garnets are [Fe2](Fe3){R3}O12 represented tetrahedral, octahedral
and dodecahedral sites respectively [4].
Yttrium iron garnet (YIG, Y3Fe5O12) is a versatile ceramic ma-
terial with high melting point, large resistivity, high electro-
magnetic properties, high thermal stability, low thermal expan-
sion, high chemical stability, and high thermal conductivity [5].
Y3Fe5O12 is well-known as magnetic garnet and widely applied
in electronics and microwave communication, such as in circula-
tors, optical isolators, phase shifters, and numerous magnetic op-
tical devices. Given that yttrium iron garnet has large Faraday
garnet can be potentially applied in electronic devices, magnetic
bubble domain-type digital memories, etc. [6].

http://dx.doi.org/10.1016/j.jmmm.2015.10.060
0304-8853/& 2015 Elsevier B.V. All rights reserved.
426 M.N. Akhtar et al. / Journal of Magnetism and Magnetic Materials 401 (2016) 425–431
RF communication devices are important because of their
function in satellites and mobile communication devices. There-
fore, magnetic materials with very low loss with high Q values that
could operate in the microwave range are in demand. Ferrite
materials with garnet structures have impact on the electronic
industry because of their application in diverse technological fields
and devices, such as in isolators, phase shifters, oscillators, IC
fabrications, sensors, antennas, etc. [7,8]. The efficiency and per-
formance of these devices have been improved using the yttrium
iron garnet ferrites [9]. The synthesis techniques may affect the
properties of these ferrite materials that depend on the size,
shape, and morphology of the ferrite samples [10]. Therefore,
controlling the grain size, shape, morphology and homogeneity of
the samples is important to enhance the characteristics of the
ferrite samples at low sintering temperature. Nanocrystalline fer-
rite garnets have recently attracted much attention given their
versatile electromagnetic properties [11]. Nonconventional (che-
mical) methods, such as chemical co-precipitation [12], hydro-
thermal precipitation [13], auto combustion method [14], glass
crystallization method [15], mechanical alloying [16], sol–gel
synthesis [17,18] and self combustion [19], have been used to
synthesize garnet ferrite powder nanoparticles. Akhtar et.al. used
various synthesis routes to prepare garnet nanoparticles for mi-
crowave application [20]. The substitution of metal ions in the
garnet structure has motivated the tune up of the properties of
garnet ferrites. Therefore, these ferrites can be used in the fabri-
cation of devices for a certain frequency range [21]. Al substitution
in the yttrium iron garnet (Al-YIG) by citrate–nitrate gel combus-
tion spray deposition was performed using atmospheric plasma-
spray. The increase in Al content decreased saturation magneti-
zation (MS) and Curie temperature (TC) of the Al-YIG powders [22].
In this study, Al ions were introduced into the YIG crystal
structure to obtain garnet ferrites operated at a wide frequency
range. The effect of sintering temperature on the structural, mor-
phological, and magnetic properties of YIG and yttrium aluminum
iron garnet (YAIG) nanoferrites was also investigated. Most studies
[20,21] have examined YIG and YAIG ferrites through diverse
methods. However, to the best of our knowledge, YIG and YAIG
nanoferrites prepared by microemulsion technique has not been
reported yet. Furthermore, the effect of sintering temperature on
the YIG and YAIG has not been considered yet.
2. Materials and methods
2.1. Materials
Yttrium nitrate [Y3(NO3)3  6H2O], iron nitrate [Fe(NO3)3  9H2O],
aluminum nitrate [Al3(NO3)3  6H2O], and citric acid [C6H8O7  H2O]
with purity 99.99%, as well as cetyltrimethylammonium bromide
(CTAB), methanol, and ammonia (NH3), were used to prepare the
Y3Fe5O12 (YIG) and Al-Y2Fe5O12 (YAIG) nanoparticles.
2.2. Samples preparation
Nitrates and citric acid were used to synthesize YIG and YAIG
nanoferrites. Whereas, CTAB, methanol, and NH3 were used as
surfactant, washing, and precipitating agent respectively. In mi-
croemuslion process, the metallic nitrates such as yttrium nitrates
and iron nitrates with molarities 10.121 and 17.033 mM were used
for the fabrication of YIG nanoferrites. However, for the prepara-
tion of YAIG, the molarities of yttrium nitrate, aluminum nitrates
and iron nitrates were 6.804, 3.387 and 17.033 mM respectively.
According to stoichiometric calculations, the aqueous solution was
prepared using distilled water and citric acid. All the nitrates were
dissolves in the aqueous solution and were stirred at 250 rpm with
a magnetic hot plate stirrer at 65 °C to prepare the clear solution.
Precipitates were formed, which were sequentially washed with
de-ionized water and methanol. The precipitates of both YIG and
YAIG samples were dried in an oven at 130 °C for 24 h. The dried
samples were ground for 10 h and then sintered at 900, 1000, and
1100 °C for 4 h.
2.3. Samples characterization
The crystalline structures of the as-prepared samples of
Y3Fe5O12 and Al1Y2Fe5O12were examined by an X-ray dif-
fractometer with CuKα radiation 1.5406 Å (Bruker D8 advance).
Field emission scanning electron microscopy (FESEM; SUPRA 55VP
ZEISS) was used to measure the shape, morphology, and grain size
of the as-prepared nanoparticles. The static magnetic measure-
ments of the prepared samples were conducted using an LCR
meter (Model Agilent 4294A) in the frequency range of 40 Hz–
110 MHz. The dynamic magnetic measurements, such as satura-
tion magnetization (Ms), remanance magnetization (MR), and
coercivity (Hc), were recorded at room temperature using a vi-
brating sample magnetometer (VSM).
3. Results and discussions
3.1. X-ray diffraction (XRD)
The XRD patterns of the YIG- and YAIG-sintered samples syn-
thesized using microemulsion method are presented in Fig. 1a and
b.
The XRD patterns of YIG and YAIG sintered at 900, 1000, and
1100 °C were analyzed using the standard JCPDS cards (43-0507
and 77-1888). The patterns revealed the presence of the spinel
single-phase structure of the YIG and YAIG samples sintered at
1100 °C. The number of peaks increased with sintering tempera-
ture. The broadening of the maximum peak intensity [420] illu-
strated the crystal structure growth in a particular order along the
lattice. Al substitution, instead of yttrium ions, introduced new
diffracted peaks at the dodecahedral site, which may be due to the
preference of Al ions to the tetrahedral and octahedral sites. This
phenomenon may have been caused by the smaller ionic radii of
Al ions compared with that of yttrium ion. The new diffracted
peaks attributed in the represented YIG and YAIG samples at dif-
ferent sintering temperatures also show the phase change from
maghemite (Fe2O3) and perovskite (YFeO3) phase to single phase
of YIG and YAIG respectively. It is also noticed that both YIG and
YAIG patterns sintered at 900 and 1000 °C have incomplete crys-
tallization due to multiphase structures. Similar results were re-
ported by the researchers done by sintering YIG from low to high
temperature [23,24].
No extra peaks were observed at 1100 C sintering temperature,
which confirmed the presence of a single-phase structure at the
sintering temperature. However, the crystallite size measured
from the XRD patterns using Debye–Sherrer formula is given in Eq.
(1), whereas the lattice parameter was also calculated using Eq. (2)
[25]:
Kλ
D=
ω cos θ (1)
(
a = dhkl h 2 + k 2 + l 2 ) (2)
where K is the variation in hkl and the crystallite shape and is
equal to 0.89, λ is the wavelength of the incident radiation, ω is the
full width at half maximum, and θ is Bragg’s angle.
 M.N. Akhtar et al. / Journal of Magnetism and Magnetic Materials 401 (2016) 425–431 427

Fig. 1. XRD of YIG samples prepared by microemulsion method at 900, 1000, and
1100 °C.
Fig. 2. XRD of YAIG samples prepared by microemulsion method at 900, 1000, and
1100 °C.
Table 1
XRD data of Y3Fe5O12 (YIG) and YAIG prepared at 900, 1000, and 1100 °C using
microemulsion method. YAIG as calculated from the FESEM images was 180–200 nm. The
grain size was approximately 148.35% higher than the crystallite
Sample d-Spacing Crystallite size Lattice para- Volume Cell
size given by the XRD data. Thus, YAIG had larger grain size
(Å) (nm) meter (Å)
compared with the YIG garnet nanoferrite. Fig. 2
YIG 900 °C 2.745 78 12.276 1.850  10  27
YIG 1000 °C 2.751 103 12.303 1.862  10  27 3.3. Magnetic measurements of YIG and YAIG samples by micro-
YIG 1100 °C 2.764 156 12.362 1.889  10  27 emulsion method
YAIG 900 °C 2.675 52 11.964 1.712  10  27
YAIG 1000 °C 2.698 63 12.069 1.758  10  27
YAIG 1100 °C 2.760 112 12.343 1.880  10  27 The magnetic properties are strongly dependent on the doping,
sintering, and synthesis methods. Therefore, static and dynamic
magnetic properties are evaluated for YIG and YAIG nanoferrite
The crystallite size of the YIG and YAIG samples increased with samples.
sintering temperature (Table 1). The crystallite size, lattice para-
meter, and volume cell of the YAIG samples decreased with in- 3.3.1. Static measurements (initial permeability and Q factor)
creasing Al contents in the YIG structure. This phenomenon was The inductance Ls and Q values were measured from the im-
due to the fact that the Al3 þ ions could not locate to the dode- pedance vector network analyzer. Figs. 4 and 5 shows the initial
cahedral site, but they preferred to go to the octahedral B- site. The permeabilities and Q factors of the YIG and YAIG ferrites synthe-
other reason may have been the smaller ionic radii of Al3 þ (0.56 Å) sized using microemulsion method. The ferrimagnetic materials
compared with that of Fe3 þ (0.67 Å). Moreover, the shrinkage of had large grain size with bulk density that resulted in higher initial
the unit cell because of Al3 þ introduction may be attributed to the permeability and large Q factor [28,29]. The bulk density of the
higher bond strength and binding energy between Al and oxygen ferrite materials produced the rotational spin, which enhanced the
in the crystal lattice [26]. Furthermore, the slight change in the initial permeability of the nanoferrites [30]. The initial perme-
position of the diffraction peaks at the [420] plane was also ob- ability of YIG was found to increase with frequency from lower to
served after Al3 þ contents were introduced. This characteristic resonance frequency. Initial permeability in YAIG increased in-
was due to the reduction in the yttrium contents from the dode- itially up to 90 MHz but suddenly decreased (Figs. 4 and 5). This
cahedral sites and increased Al3 þ contents in the octahedron lat- phenomenon could be attributed to the contribution of the Al ions
tice sites. Furthermore, the increased Al contents and decreased in the YIG lattice. However, surface morphology, porosity, density,
yttrium contents were responsible for the distortion and peak grain size, single phase structure, and Fe contents also played
intensities of the major peaks in the YAIG samples. important roles for the variation in the initial permeabilities and Q
factors of YIG and YAIG [31]. The initial permeability of YIG sin-
3.2. Microstructural analysis tered at 1100 °C exhibited the highest initial permeability and
largest Q factor compared with those of YIG. These results could be
Fig. 3 shows the FESEM images of the YIG and YAIG samples attributed to the fact that sintering temperature, morphology, and
prepared by microemulsion method and sintered at 1000 and grain size affect the magnetic properties of YIG. However, the in-
1100 °C. Fig. 3a–c shows the micrographs of YIG at 900, 1000, and itial permeability and Q factor of YAIG shows lower values com-
1100 °C. The average grain size of the YIG nanoparticles obtained pared with YIG sintered at the same temperature. This condition
from the FESEM images was 100 nm to 120 nm. Grain size was may have been caused by the nonmagnetic Al ions in the YIG
approximately 94.62% higher than the crystallite size calculated crystal lattice. The significant increase in initial permeability and Q
from the XRD results. The morphology of the YIG sample sintered factor may have resulted from the decrease in internal stress,
at 1100 °C showed spherical YIG nanoparticles (Fig. 3a). The sur- magnetic anisotropy, and less domain wall interruptions [32].
face morphology of the Y3Fe5O12 sample sintered at 1100 °C Initial permeabilities and Q factors of YIG and YAIG sintered at
showed well-crystallite grains with relatively homogenous grain 900, 1000, and 1100 °C were calculated from the series of in-
distribution (Fig. 3b). The grain size depended on various factors ductance (Ls) values using an LCR impedance analyzer. The initial
such as sintering temperature, porosity, and grain boundary [27]. permeability increased with frequency, whereas the Q factor also
Representative FESEM images of Al-doped YIG (YAIG) at 900, 1000, increased until resonance as shown in Figs. 4 and 5. However,
and 1100 °C are presented in Fig. 3d–f. The average grain size of when the grain size was less than 5 μm and the cut off frequency
428 M.N. Akhtar et al. / Journal of Magnetism and Magnetic Materials 401 (2016) 425–431

Fig. 3. FESEM images of YIG at (a) 900 °C, (b) 1000 °C, and (c) 1100 °C, and YAIG at (d) 900 °C, (e) 1000 °C, and (f) 1100 °C prepared by microemulsion method.

was less than 40 MHz, then the domain wall motion was dominant
and contributed to magnetism [33]. The high initial permeability
and Q factor indicated low loss factor values that confirmed the
high purity of the prepared samples obtained by microemulsion
method [34,35]. These materials could be used in various com-
ponents for different frequency applications.
YIG exhibited the highest initial permeability and largest Q
factor compared with YAIG sintered at, 1000, and 1100 °C. These
results could be attributed to the single phase structure, enhanced
morphology, and large grain size through microemulsion method
compared with those of other preparation methods.
3.3.2. Dynamic magnetic measurements [magnetic hysteresis (MH)
loops]
Dynamic magnetic measurements, such as hysteresis loops, of
the YIG and YAIG were performed at room temperature using a
VSM. Fig. 6 shows the typical plots of the prepared YIG and YAIG
samples. The Hc, Ms, and MR values were also calculated from the
hysteresis loops. The calculated Ms, Hc, and MR are depicted in
Table 2. The MH loops revealed that variation occurred in the
magnetic behavior by introducing Al ions in the YIG lattice. YIG
exhibited high MS value but low Hc value compared with YAIG
sintered at 1000 and 1100 °C. This phenomenon was due to the
strong magnetism of YIG compared with that of YAIG. From the
MH loops, YIG and YAIG sintered at 1000 and 1100 °C had Ms
values of 13.98 and 19.92 emu/g, with MR values of 10.36 to
18.05 emu/g, respectively. These values decreased with the in-
crease in temperature in YIG and YAIG. However, the Hc values
decreased due to the increase in the YIG and YAIG grain sizes as
depicted in Tables I and II. Both parameters are inversely
 M.N. Akhtar et al. / Journal of Magnetism and Magnetic Materials 401 (2016) 425–431 429

120 proportional to each other (Hcα1/r) [36]. The Hc values depended

YIG at 1000 C
YIG at 900 C on the extrinsic and intrinsic characteristics of the nanoferrites.
YIG at 1100 C The extrinsic characteristics depended on the grain size, porosity,
100
YAIG at 900 C morphology, and defects in the nanoferrites, whereas intrinsic
YAIG at 1000 C
characteristics depended on the type of structure, composition,
80 YAIG at 1100 C
Initial Permeability

and synthesis method [37].

YIG and YAIG showed weak magnetic behavior at 1000 °C,
60 whereas significant increase in magnetic characteristics was
achieved after sintering at 1100 °C. Moreover, YAIG has larger Hc
40 than YIG because it had more grain boundaries and pinning sites.
Furthermore, YIG and YAIG samples with smaller grain size ex-
hibited lower magnetization compared with those with larger
20
grain size. The inset in Fig. 6 shows the magnified part from the Hc
study. YAIG had larger Hc than YIG primarily because of the Al ions
0
in the YIG lattice. The magnetic domain walls and moments played
0.00E+000 2.00E+007 4.00E+007 6.00E+007 8.00E+007 1.00E+008 1.20E+008
Frequency (Hz) an important role in the variation in Ms, MR, and Hc [38]. In this
study, YIG had higher Ms and lower Hc compared with YAIG. This
Fig. 4. Initial permeabilities of YIG and YAIG samples prepared by microemulsion
condition may have been caused by the better morphology, in-
method and sintered at 900, 1000, and 1100 °C.
creased magnetic moments, and domain wall migration of YIG and
YAIG. Table II also depicts the magnetic squareness ratio of  1,
70 which confirms the superparamagnetic behavior [39]. Moreover,
YIG at 1000 C Hc is found to be less than a hundred oersteds, which revealed the
60
YIG at 900 C soft character of the YIG and YAIG nanoferrites [40]. The variation
YIG at 1100 C in Ms, MR, and Hc for YIG and YAIG samples synthesized by mi-
50
YAIG at 900 C croemulsion method are shown in Fig. 7a and b. However, spin-
YAIG at 1000 C canting effect and colinearity are the main factors that caused the
40
YAIG at 1100 C
variation in the dynamic magnetic characteristics [41]. In addition,
Ms and MR also decreased with Al3 þ nonmagnetic substitution in
Q-factor

30
the YIG crystal structure which is due to the decrement of super
20 exchange interactions in the crystal [41]. Furthermore, the mag-
netic losses and magnetic field in YIG were larger compared with
10 those of YAIG. This phenomenon can also be explained on the
basis of the static magnetic characteristics of YIG samples. The
0
initial permeability and large Q factor indicated low magnetic
losses whereas MH loops of YAIG also depicted large Hc, which
-10
1000000 1E7 1E8 confirmed the low magnetic losses in YIG. The present investiga-
log f (Hz) tions suggested the magnetic properties of YIG. The comparison of
Fig. 5. Q factors of YIG and YAIG samples prepared by microemulsion method and saturation magnetization and coercivity in this work and reported
sintered at 900, 1000, and 1100 °C. by some other researchers for YIG and YAIG prepared by various
methods are also shown in Table 2 [42,43].

o
YIG at 1100 C 20
o
YIG at 1000 C
o
YAIG at 1000 C
o
YAIG at 1100 C
10
emu/g

0
-8000 -6000 -4000 -2000 0 2000 4000 6000 8000

-10

-20

Applied field (Oe)

Fig. 6. M–H loops of YIG and YAIG samples prepared by microemulsion method and sintered synthesized at 900, 1000, and 1100 °C.
430 M.N. Akhtar et al. / Journal of Magnetism and Magnetic Materials 401 (2016) 425–431

Table 2
Magnetic parameters of YIG and YAIG synthesized using microemulsion method.

Samples Method MR (emu/g) Ms (emu/g) MR /Ms Hc (Oe) References

YIG at 1000 °C Microemulsion 12.53 13.98 0.89 10.6 This work

YIG at 1100 °C Microemulsion 18.05 19.92 0.89 7.30 This work
YAIG at 1000 °C Microemulsion 10.36 11.56 0.90 87.7 This work
YAIG at 1100 °C Microemulsion 15.99 17.58 0.90 61.2 This work
YIG at 1350 °C Modified conventional metal Oxide (MCMO) 0.39 0.35 1.10 2.26 [20]
YIG at 1150 °C self combustion 0.93 0.90 1.03 0.17 [20]
YIG at 1150 °C sol gel 0.92 0.91 1.01 0.10 [20]
Y3Fe5  xAlxO12 at 1300 °C for x¼ 1 Mechanochemcial – 0.88 – – [41]
YIG at 1200 °C Solid state with 48 h milling time – 1.27 – 79.0 [42]
YIG at 800 °C/2 min Sol gel hot pressing – 2.80 – 100 [43]
YIG at 800 °C/3 min Sol gel hot pressing – 7.40 – 80 [43]
YIG at 800 °C/4 min Sol gel hot pressing – 10.0 – 45 [43]
YIG at 800 C/6 min Sol gel hot pressing – 14.7 – 40 [43]

exchange interactions. Thus, YAIG nanoferrites decreased the static

19
and dynamic properties. Therefore, the prepared YIG and YAIG
nanoferrites could be used for a wide range of operated fre-
20
18 Mr quencies applications. Furthermore, these nanoferrites may be
Ms suitable for electromagnetic wave absorbers, switching and sen-
17
18
sors applications.
16

15
Mr (emu/g)

Acknowledgment
Ms (emu/g)

16
14

The authors acknowledge the financial support of the Higher

13 14
Education Commission, Pakistan under Grant no. IPFP/HRD/HEC/
12 2013/1937.
12
11

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