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<a href=Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 Contents lists available at S c i V e r s e S c i e n c e D i r e c t Journal of Magnetism and Magnetic Materials journal homepage: w w w . e l s e v i e r . c o m / l o c a t e / j m m m Induction heating studies of combustion synthesized MgFe O nanoparticles for hyperthermia applications V.M. Khot, A.B. Salunkhe, N.D. Thorat, M.R. Phadatare, S.H. Pawar Center for Interdisciplinary Research, D.Y. Patil University, Kolhapur 416006, India article info Article history: Received 30 July 2012 Received in revised form 1 December 2012 Available online 13 December 2012 Keywords: Combustion synthesis Magnetic nanoparticle Biomaterial Induction heating abstract The structural, magnetic and ac magnetically induced heating characteristics of combustion synthe- sized MgFe O nanoparticles have been investigated for application in magnetic particle hyperthermia. As prepared nanoparticles showed ferrimagnetic behavior at room temperature with magnetization of about 33.83 emu/g at 7 15 kOe. The solid state MgFe O nanoparticles exhibited specific absorption rate (SAR) of about 297 W/g at physiological safe range of frequency and amplitude. The increase in SAR and heating temperature in ac magnetic field was thought to be due to enhancement in magnetic hysteresis loss caused by dipole–dipole interactions in combustion synthesized MgFe O nanoparticles. & 2012 Elsevier B.V. All rights reserved. 1. Introduction Magnetic particle hyperthermia (MPH) with magnetic nano- particles (MNPs) has emerged as one of the promising cancer modality either alone or in combination with existing cancer modalities [1 , 2 ]. In MPH, magnetic nanoparticles are used for heating the specific region of body via absorption of radio frequency when subjected to an alternating current (ac) magnetic field [3] . In spite of enormous efforts in this field, clinical appliances of hyperthermia for completely treating cancer were not effective. High heating temperatures and large specific absorption rate (SAR) at small particle concentration are consid- ered as most critical challenge to achieve desirable tumor damage. Especially considering temperature reduction due to circulation and tissue perfusion in in vivo application, bare nanoparticles should produce sufficiently high heating tempera- ture and high SAR in physiological tolerable range of frequencies and magnetic field with their product e H o 5 10 Am s [4] . Ferrimagnetic or superparamagnetic nanoparticles (especially spinel ferrites) have been extensively studied for MPH as they exhibit attractive biotechnical and physiological properties such as: self heating rise due to resonance response to AC magnetic fields excitation, easy coating with biological entities etc [5 , 6 ]. The SAR values of MNPs strongly depend on magnetic moment, anisotropy energy, particle size and distribution which are highly sensitive to synthesis methods [7] . Although chemical Corresponding author. Tel.: þ 91 231 fax: þ 91 231 2601595. 2601202, þ 91 231 2601235; E-mail addresses: wish_khot@yahoo.co.in , pawar_s_h@yahoo.com (S.H. Pawar) . 0304-8853/$ - see front matter & 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.jmmm.2012.12.010 co-precipitation method is suitable for mass production of MNPs, it does require careful adjustment of the pH value of the solution for particles formation. Combustion method is known for its cost effectiveness, low reaction time, large mass production and homogeneity among the products. Also, no further thermal treatment is required for samples prepared by combustion method [8] . Though, magnetic nanoparticles have been studied intensively for MPH in recent years, no distinct report is available for stable and saturated heat rise in physiological tolerable range of frequencies and amplitude. In the present investigation, ferrimagnetic MgFe O nanopar- ticles were prepared by promising combustion method having sizes below 40 nm. The structural and magnetic properties of nanoparticles were explored to understand their self heating mechanism in ac magnetic field. The effectiveness of combustion synthesized MgFe O as potential heating agents for MPH have been investigated. 2. Materials and method Polycrystalline MgFe O nanoparticles were prepared by com- bustion using glycine as a fuel [8] . The detailed process condition for synthesizing MgFe O nanoparticles were reported else- where [9] . The particles were characterized by a Philips PW- 3710 automated X- ray diffractometer (XRD) and Perkin–Elmer FTIR (400–4000 cm ) spectroscope for structure and phase identification. The morphology and particle size were observed by transmission electron microscopy (TEM, JEOL1200). Magnetic measurements were carried out with a vibrating sample magnet- ometer (VSM, Lakeshore model no. 7407). " id="pdf-obj-0-5" src="pdf-obj-0-5.jpg">

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<a href=Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 Contents lists available at S c i V e r s e S c i e n c e D i r e c t Journal of Magnetism and Magnetic Materials journal homepage: w w w . e l s e v i e r . c o m / l o c a t e / j m m m Induction heating studies of combustion synthesized MgFe O nanoparticles for hyperthermia applications V.M. Khot, A.B. Salunkhe, N.D. Thorat, M.R. Phadatare, S.H. Pawar Center for Interdisciplinary Research, D.Y. Patil University, Kolhapur 416006, India article info Article history: Received 30 July 2012 Received in revised form 1 December 2012 Available online 13 December 2012 Keywords: Combustion synthesis Magnetic nanoparticle Biomaterial Induction heating abstract The structural, magnetic and ac magnetically induced heating characteristics of combustion synthe- sized MgFe O nanoparticles have been investigated for application in magnetic particle hyperthermia. As prepared nanoparticles showed ferrimagnetic behavior at room temperature with magnetization of about 33.83 emu/g at 7 15 kOe. The solid state MgFe O nanoparticles exhibited specific absorption rate (SAR) of about 297 W/g at physiological safe range of frequency and amplitude. The increase in SAR and heating temperature in ac magnetic field was thought to be due to enhancement in magnetic hysteresis loss caused by dipole–dipole interactions in combustion synthesized MgFe O nanoparticles. & 2012 Elsevier B.V. All rights reserved. 1. Introduction Magnetic particle hyperthermia (MPH) with magnetic nano- particles (MNPs) has emerged as one of the promising cancer modality either alone or in combination with existing cancer modalities [1 , 2 ]. In MPH, magnetic nanoparticles are used for heating the specific region of body via absorption of radio frequency when subjected to an alternating current (ac) magnetic field [3] . In spite of enormous efforts in this field, clinical appliances of hyperthermia for completely treating cancer were not effective. High heating temperatures and large specific absorption rate (SAR) at small particle concentration are consid- ered as most critical challenge to achieve desirable tumor damage. Especially considering temperature reduction due to circulation and tissue perfusion in in vivo application, bare nanoparticles should produce sufficiently high heating tempera- ture and high SAR in physiological tolerable range of frequencies and magnetic field with their product e H o 5 10 Am s [4] . Ferrimagnetic or superparamagnetic nanoparticles (especially spinel ferrites) have been extensively studied for MPH as they exhibit attractive biotechnical and physiological properties such as: self heating rise due to resonance response to AC magnetic fields excitation, easy coating with biological entities etc [5 , 6 ]. The SAR values of MNPs strongly depend on magnetic moment, anisotropy energy, particle size and distribution which are highly sensitive to synthesis methods [7] . Although chemical Corresponding author. Tel.: þ 91 231 fax: þ 91 231 2601595. 2601202, þ 91 231 2601235; E-mail addresses: wish_khot@yahoo.co.in , pawar_s_h@yahoo.com (S.H. Pawar) . 0304-8853/$ - see front matter & 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.jmmm.2012.12.010 co-precipitation method is suitable for mass production of MNPs, it does require careful adjustment of the pH value of the solution for particles formation. Combustion method is known for its cost effectiveness, low reaction time, large mass production and homogeneity among the products. Also, no further thermal treatment is required for samples prepared by combustion method [8] . Though, magnetic nanoparticles have been studied intensively for MPH in recent years, no distinct report is available for stable and saturated heat rise in physiological tolerable range of frequencies and amplitude. In the present investigation, ferrimagnetic MgFe O nanopar- ticles were prepared by promising combustion method having sizes below 40 nm. The structural and magnetic properties of nanoparticles were explored to understand their self heating mechanism in ac magnetic field. The effectiveness of combustion synthesized MgFe O as potential heating agents for MPH have been investigated. 2. Materials and method Polycrystalline MgFe O nanoparticles were prepared by com- bustion using glycine as a fuel [8] . The detailed process condition for synthesizing MgFe O nanoparticles were reported else- where [9] . The particles were characterized by a Philips PW- 3710 automated X- ray diffractometer (XRD) and Perkin–Elmer FTIR (400–4000 cm ) spectroscope for structure and phase identification. The morphology and particle size were observed by transmission electron microscopy (TEM, JEOL1200). Magnetic measurements were carried out with a vibrating sample magnet- ometer (VSM, Lakeshore model no. 7407). " id="pdf-obj-0-63" src="pdf-obj-0-63.jpg">

Induction heating studies of combustion synthesized MgFe 2 O 4 nanoparticles for hyperthermia applications

V.M. Khot, A.B. Salunkhe, N.D. Thorat, M.R. Phadatare, S.H. Pawar n

Center for Interdisciplinary Research, D.Y. Patil University, Kolhapur 416006, India

article info

Article history:

Received 30 July 2012 Received in revised form 1 December 2012 Available online 13 December 2012

Keywords:

Combustion synthesis

Magnetic nanoparticle

Biomaterial

Induction heating

abstract

The structural, magnetic and ac magnetically induced heating characteristics of combustion synthe- sized MgFe 2 O 4 nanoparticles have been investigated for application in magnetic particle hyperthermia. As prepared nanoparticles showed ferrimagnetic behavior at room temperature with magnetization of about 33.83 emu/g at 7 15 kOe. The solid state MgFe 2 O 4 nanoparticles exhibited specific absorption

rate (SAR) of about 297 W/g at physiological safe range of frequency and amplitude. The increase in SAR and heating temperature in ac magnetic field was thought to be due to enhancement in magnetic hysteresis loss caused by dipole–dipole interactions in combustion synthesized MgFe 2 O 4 nanoparticles. & 2012 Elsevier B.V. All rights reserved.

1. Introduction

Magnetic particle hyperthermia (MPH) with magnetic nano- particles (MNPs) has emerged as one of the promising cancer modality either alone or in combination with existing cancer modalities [1,2]. In MPH, magnetic nanoparticles are used for heating the specific region of body via absorption of radio frequency when subjected to an alternating current (ac) magnetic field [3]. In spite of enormous efforts in this field, clinical appliances of hyperthermia for completely treating cancer were not effective. High heating temperatures and large specific absorption rate (SAR) at small particle concentration are consid- ered as most critical challenge to achieve desirable tumor damage. Especially considering temperature reduction due to circulation and tissue perfusion in in vivo application, bare nanoparticles should produce sufficiently high heating tempera- ture and high SAR in physiological tolerable range of frequencies and magnetic field with their product e n H o 5 10 9 Am 1 s 1 [4]. Ferrimagnetic or superparamagnetic nanoparticles (especially spinel ferrites) have been extensively studied for MPH as they exhibit attractive biotechnical and physiological properties such as: self heating rise due to resonance response to AC magnetic fields excitation, easy coating with biological entities etc [5,6]. The SAR values of MNPs strongly depend on magnetic moment, anisotropy energy, particle size and distribution which are highly sensitive to synthesis methods [7]. Although chemical

n Corresponding author. Tel.: þ 91 231 fax: þ 91 231 2601595.

2601202, þ 91 231 2601235;

0304-8853/$ - see front matter & 2012 Elsevier B.V. All rights reserved.

co-precipitation method is suitable for mass production of MNPs, it does require careful adjustment of the pH value of the solution for particles formation. Combustion method is known for its cost effectiveness, low reaction time, large mass production and homogeneity among the products. Also, no further thermal treatment is required for samples prepared by combustion method [8]. Though, magnetic nanoparticles have been studied intensively for MPH in recent years, no distinct report is available for stable and saturated heat rise in physiological tolerable range of frequencies and amplitude. In the present investigation, ferrimagnetic MgFe 2 O 4 nanopar- ticles were prepared by promising combustion method having sizes below 40 nm. The structural and magnetic properties of nanoparticles were explored to understand their self heating mechanism in ac magnetic field. The effectiveness of combustion synthesized MgFe 2 O 4 as potential heating agents for MPH have been investigated.

  • 2. Materials and method

Polycrystalline MgFe 2 O 4 nanoparticles were prepared by com- bustion using glycine as a fuel [8]. The detailed process condition for synthesizing MgFe 2 O 4 nanoparticles were reported else- where [9]. The particles were characterized by a Philips PW- 3710 automated X- ray diffractometer (XRD) and Perkin–Elmer FTIR (400–4000 cm 1 ) spectroscope for structure and phase identification. The morphology and particle size were observed by transmission electron microscopy (TEM, JEOL1200). Magnetic measurements were carried out with a vibrating sample magnet- ometer (VSM, Lakeshore model no. 7407).

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51

49

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 49 Fig.

Fig. 1. Typical XRD pattern (a) and FTIR spectra and (b) for as prepared MgFe 2 O 4 powder.

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 49 Fig.

Fig. 2. TEM image and SAED pattern (inset picture) of as prepared MgFe 2 O 4 powder.

Induction heating of as synthesized MgFe 2 O 4 nanoparticles was performed in a plastic microcentrifuge tube (1.5 ml) using an instrument (Easy Heat 8310, Ambrell, UK) with 6 cm diameter coil (4 turns). Samples (2–5 mg/mL of distilled water) were placed at the center of the coil and the applied frequency was 265 kHz and field amplitude varied [10].

  • 3. Results and discussion

The crystal structure of combusted MgFe 2 O 4 nanoparticles was elucidated by XRD (Fig. 1a). Particles obtained in this case are nanocrystallites with lattice parameter of 0.8385 nm with single phase of spinel MgFe 2 O 4 [11]. The formation of cubic spinel was also supported by FTIR spectra (Fig. 1b). The observed values illustrate that frequency bands appeared at 561 and 451 cm 1 are responsible for the formation of spinel MgFe 2 O 4 [9,12,13]. On the basis of this data it can be suggested that the MgFe 2 O 4 spinel phase is formed with cation distribution,

2

ðFe 1 x 3 þ Mg x 2 þ Þ A ½Mg 1 x 2 þ Fe 1 þ x 3 þ B O 4

ð1Þ

where x is inversion parameter (x ¼ 0 for inverse spinel and x ¼ 1 for normal spinel) while A and B are tetrahedral and octahedral sites in spinel structure respectively. TEM image (Fig. 2) of as prepared powder shows the formation of quasi-spherical

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 49 Fig.

Fig. 3. M–H curve and low field hysteresis (upper inset) for as prepared MgFe 2 O 4 nanoparticles at different temperatures (lower inset shows magnified image for M–H at origin).

MgFe 2 O 4 nanoparticles with sizes ranging 10–40 nm ( 7 2 nm). The selected area electron diffraction pattern (inset of Fig. 2) is consistent with XRD pattern. The M–H measurements of as prepared MNPs are performed at

two different temperatures at 10 K and 300 K (Fig. 3) in order to investigate the effect of temperature on magnetization and coercivity. From the figure, it can be observed that magnetization of sample is about 33.83 emu/g at 300 K and 41.60 emu/g at 10 K respectively. This increase in magnetization at lower temperature was attributed to frustration effects in ferrites below the blocking temperature of the materials [14]. The combustion synthesized MgFe 2 O 4 nanoparticles showed typical characteristics of ferri- magnetism at room temperature with minor hysteresis ( 53 Oe). The rise in temperature versus time for sample with varying field amplitude is shown in Fig. 4 a, b. Heat dissipation by magnetic nanoparticles under ac magnetic field is measured as SAR (W/g) and it can be expressed as:

SAR ¼ C

dT

dt

m

s

m

m

ð2Þ

where C is the specific heat capacity of suspension ¼ 4.186 J/(g.1C),

(dT/dt is the initial slope of temperature versus time graph, m s is the mass of suspension and m m is the mass of the magnetic material in suspension. This value should be as high as possible to minimize the amount of magnetic material applied for hyperthermia. The magnetic induction heating of ferrite materials is originated from their power loss in alternating magnetic field. The total power loss (P)

  • 50 V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51

50 V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 Fig.

Fig. 4. Temperature versus time curves for 2 mg/mL (a) and 5 mg/mL (b) MgFe 2 O 4 nanoparticles at applied field, 167.6 Oe–335.2 Oe (dotted line indicates the hyperthermia temperature region).

is composed of three parts, hysteresis loss, eddy current loss and

residual loss [10,14].

 

The hysteresis loss in an ac magnetic field can be expressed

as [12],

A ¼ Z

-H max

 

m 0 M ðH ÞdH

ð3Þ

-H min

And thus the specific absorption rate is,

 

SAR ¼ Af

 

ð4Þ

where e is frequency of ac magnetic field and it is expressed as

e ¼ o /2p, M is magnetization and H is applied magnetic field. Thus

one has to take into account the SAR dependence on frequency and

amplitude. The heat loss is considered to be due to Brownian

relaxation (when the particle spins to align itself with the magnetic

moment) and Ne´ el relaxation (when the magnetic moment spins

within the crystal structure of the nanoparticle). Neel relaxation (t N )

time can be expressed as,

t N ¼ t 0 exp KV =k b T

and Brownian relaxations (t B ) as,

t B ¼

3ZV H

k b T

ð5Þ

ð6Þ

where the relaxation time constant t 0 is of the order of 10 9 s, V H is

the hydrodynamic volume which is the effective volume (including

that of the nanoparticle and coating or surfactant attached to the

nanoparticle), Z is the viscosity of the medium, T is the temperature

and k b is the Boltzmann constant [15].

The effective relaxation time is given by,

t eff ¼

1

þ

1

t N t B

ð7Þ

The power loss corresponding to Brown or Neel relaxations is

approximately given by,

P ¼ m 0 pw 00 f H 2

ð8Þ

where m 0 ¼ 4p 10 7 H/m and w 00 is the imaginary part of

magnetic susceptibility which can be expressed as,

w 00

¼

ot eff

1 þ ð

ot eff

Þ 2 w

ð9Þ

Though the heating power is directly proportional to square of

the amplitude (Eq. 8), the enhancement of heating power of

magnetic nanoparticles is forbidden by simply increasing field

and frequency [14,15].

From Fig. 4a and b, it is clear that the temperature increases with

increase in field amplitude and concentration of nanoparticles. The

dotted region in figure denotes the hyperthermia threshold tem-

perature. It is observed that for particle concentration 2 mg/mL, the

fields 167.6 and 209.5 Oe are not sufficient to reach hyperthermia

threshold temperature while for concentration 5 mg/mL, hyperther-

mia temperature is reached for all values of applied fields. The

physical nature of the rapid temperature rise in the initial stage can

be thought to be primarily due to the magnetic hysteresis loss, Neel

rotation, Brownian and Eddy current losses of each ferrimagnetic

nanoparticle activated by ac magnetic field [5,15]. However in

present study, Brownian losses are negligible as samples are mea-

sured in powder state in water. Since MgFe 2 O 4 exhibit very low

conductivity (10 7 S/cm), contribution from eddy current losses is

negligible. Therefore heat loss in case of MgFe 2 O 4 may be due to

hysteresis and relaxation losses. The later is more prominent in

single domain magnetic nanoparticles. The heat dissipation by

magnetic nanoparticles in AC magnetic field is also strongly affected

by size distribution [16,17].

The broad particle size distribution increases dipole–dipole inter-

actions which affects the induction heating properties of material.

This holds true only if the particles were uniform with narrow size

distribution. If the particles exhibit broad distribution, both super-

paramagnetic and ferrimagnetic nanoparticle may co-exist and the

particle size being optimal for large heating power in hyperthermia

may be found in this size range [14,16]. Thus broader size distribu-

tion may be favorable to get large heat output for hyperthermia. The

reason is that in case of narrow size distribution, large particle gap

created between adjacent nanoparticles results low particle interac-

tion energy and small coupling exchange energy. If the size distribu-

tion is broad, this interparticle gap would possibly fill up with

smaller particles resulting in increased particle interaction energy

and coupling exchange energy [18,19]. This additionally increased

coupling exchange energy results in enhancement of magnetic

moment as well as magnetic susceptibility. As a consequence of this,

there is enhanced hysteresis loss and enhanced ac magnetically

induced heating characteristics.

Fig. 3 (upper inset) show low field M–H loops measured at the

applied magnetic field of 7 600 Oe. As can be clearly confirmed,

particle–particle interaction in present system corresponding to

‘‘minor hysteresis area loss’’ was observed. This directly demon-

strates that particle dipole interaction affects the magnetic hysteresis

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51

51

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 51 Fig.

Fig. 5. SAR values for MgFe 2 O 4 nanoparticles (2 mg/mL and 5 mg/mL) at applied field, 167.6 Oe–335.2 Oe.

V.M. Khot et al. / Journal of Magnetism and Magnetic Materials 332 (2013) 48–51 51 Fig.

Fig. 6. Rise in temperature for MgFe 2 O 4 nanoparticles (2 mg/mL and 5 mg/mL) at applied field, 167.6 Oe–335.2 Oe.

loss, which is the main physical reason for the remarkably increased

temperature [19]. SAR values are calculated by Eq. (2) for nanopar-

ticles dispersed in distilled water (1 mL) at different fields varying

from 167.6 Oe–335.2 Oe at 265 kHz (Fig. 5). The overall SAR value is

found to increase from 38 W/g to 297.5 W/g with increase in field

from 167.6 Oe to 335.2 Oe. Thus the observed high SAR values may

be considered due to Neel relaxation of MgFe 2 O 4 nanoparticle

induced by hysteresis losses as particle size distribution is broad.

The observed sufficiently high temperature rise, around 14.98 1C and

22.25 1C (Fig. 6) of MgFe 2 O 4 nanoparticles at 2 mg/mL and 5 mg/mL,

respectively in the physiologically tolerable range of the magnetic

field (251.4 Oe or 20 kA m 1 and 265 kHz) are considered as

promising AC magnetically induced heating characteristics for an

in vivo hyperthermia application. Also the concentration used here to

achieve the required temperature is reasonably low (2 mg/ml and

5 mg/ml) that compared to literature values [16].

4. Conclusions

MgFe 2 O 4 nanoparticles with sizes around 10–40 nm and good

dispersibility were successfully prepared by combustion method.

Combustion synthesis was found more advantageous over con-

ventional methods for preparing MgFe 2 O 4 nanoparticles as it does

not require any pH control or intermediate calcination step. The

enhancement in SAR from 38 W/g to 297.45 W/g is primarily

thought to be due to hysteresis loss as particles do exhibit low

coercivity and broad size distribution. Thus, combustion synthe-

sized MgFe 2 O 4 nanoparticles with large enough SAR at low

particle concentration, suitable magnetic properties can be a

promising heating agent for MPH.

Acknowledgments

Author Mr. V.M. Khot acknowledges the Council of Scientific and

Industrial Research, India for the award of senior research fellowship

File No.: 09/1077/(0001)/2012/EMR-1. Authors are thankful to

Dr. D. Das, Dr. R. S. Ningthoujam and Dr. R. K. Vatsa, BARC for

availability of induction heating studies.

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