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15 visualizzazioni7 pagineAjay Shankar,
Rajendra Prasad Pant, Mahesh Chand
, Gounda Abdul Basheed
, Sanjeeve Thakur
EPR
oleic acid
Ferroﬂuid
Ferromagnetic resonance
Spin-glass transition

May 07, 2017

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Ajay Shankar,
Rajendra Prasad Pant, Mahesh Chand
, Gounda Abdul Basheed
, Sanjeeve Thakur
EPR
oleic acid
Ferroﬂuid
Ferromagnetic resonance
Spin-glass transition

© All Rights Reserved

15 visualizzazioni

Ajay Shankar,
Rajendra Prasad Pant, Mahesh Chand
, Gounda Abdul Basheed
, Sanjeeve Thakur
EPR
oleic acid
Ferroﬂuid
Ferromagnetic resonance
Spin-glass transition

© All Rights Reserved

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4 Journal of Magnetism and Magnetic Materials

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

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Low temperature FMR investigations on double surfactant water based

13 ferrouid

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Q1 A. Shankar a,b, M. Chand a, G.A. Basheed a, S. Thakur b, R.P. Pant a,n

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a

17 EPR Spectroscopy Section, CSIR-National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi 110012, India

b

School of Applied Sciences, Netaji Subhas Institute of Technology, University of Delhi, Sector 3, Dwarka, New Delhi 110078, India

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

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Article history: Magnetite nanoparticles were synthesized by coprecipitation of reverse micelles in an aqueous phase.

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Received 24 June 2013 XRD, TEM and VSM results conrm the average particle size 910 nm. The FMR measurements were

24 Received in revised form performed in zero-eld-cooled (ZFC) and eld-cooled (FC) protocol. Raikher and Morais models were

25 10 September 2014

used for interpreting the resonance eld and linewidth results. A value of 2.3 10 2 erg cm 2 for

26 intrinsic surface anisotropy constant is observed as per the Raikher model. The higher melting point of

27 Keywords: water leaves the magnetic particles with a more disordered distribution of anisotropy axes of particles

28 Ferrouid even in FC measurements. The angular variation of resonance eld differentiates the magnetic behavior

29 Ferromagnetic resonance of system in 440 K (region I), 70200 K (region II) and 200260 K (region III). The value of effective

Spin-glass transition

30 magnetic anisotropy constant varied from 4.7 104, 2.1 104 to 0 erg cm 3 through regions I, II to III.

31 Linewidth analysis reveals that system undergoes spin-glass transition 46 K. The tting of linewidth

32 data for region I and II indicate the presence of frozen and unfrozen surface spin states. Moreover, the

33 role of applied magnetic eld i.e. 1 T in eld-cooled FMR spectra is reected in interparticle distance

parameter and magnitude of energy barriers related to the relaxation mechanisms. At 260 K uid melts

34

resulting in minimization of angular dependent anisotropy in resonance lines.

35

& 2014 Published by Elsevier B.V.

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39

1. Introduction temperature determinative for this dynamic phase transition is 69

40

regarded as blocking temperature, TB. 70

41

Ferrouids (FFs) are an important class of magnetic materials In addition, the reduced lattice symmetry of atoms on the 71

42

surface of MNPs gives rise to a disordered surface layer also 72

43 since they have found numerous technological applications. Their

termed as dead layer, which is antiferromagnetic in nature. 73

44 peculiar properties such as superparamagnetism, dipolar interac-

The lower value of saturation magnetization in MNPs has been 74

45 tions, blocking of moments by anisotropy eld and effects of

ascribed to the presence of this non-magnetic surface layer [8]. 75

46 different carrier medium offers intensive research opportunities

This further adds another dimension of complexity when one 76

47 [1]. Among these, superparamagnetic relaxation of magnetic

assumes a coreshell kind of structure in individual MNPs. This 77

48 moments in these nanoparticles resulting from magnetization

structural perspective becomes more evident especially below 78

49

reversal is an important aspect for majority of their applications. 79

50 surface spin-freezing temperature [913]. Below this characteristic

Thus, they have been widely studied by a variety of techniques temperature, a coupling of uniaxial FM core and surface spin glass 80

51

having quite different time scale of measurements (M) viz., DC generates a non-zero exchange anisotropy eld in system. 81

52

susceptibility measurements (1100 s) and low-frequency AC To study spin dynamics in such a system, the FMR technique 82

53

susceptibility measurements (10 110 5 s), Mossbauer spectro- has been utilized in many instances. A classical ferromagnetic 83

54

scopy (10 710 9 s) and ferromagnetic resonance (FMR) with approach using the LandauLifshitzGilbert equation incorporated 84

55

85

56 M 10 10 s [27]. But, the uctuation of magnetic moments stops with thermal parameters is widely used to understand dynamics

of uctuating moments in these systems [5,1416]. An alternative 86

57 when magnetic anisotropy energy dominates over thermal energy

method to the above approach is proposed by Noginova et al. [17] 87

58 of magnetic nanoparticles (MNPs) and system becomes single-

where iron oxide MNPs were considered as a giant macrospin 88

59 domain ferromagnetic (bulk-like) in nature, and the critical

under quantization model to describe spectral linewidth, reso- 89

60

nance condition and signal intensity. On the other hand, FMR has 90

61

n also been used to study spin-glass transition in mixed and doped 91

62 Corresponding author. Fax: 91 11 4560 9310.

E-mail address: rppant@nplindia.org (R.P. Pant). iron oxide nanoparticles [10,1820]. A sudden decrement in 92

63

93

64 http://dx.doi.org/10.1016/j.jmmm.2014.09.038 94

65 0304-8853/& 2014 Published by Elsevier B.V. 95

66

Please cite this article as: A. Shankar, et al., Journal of Magnetism and Magnetic Materials (2014), http://dx.doi.org/10.1016/j.

jmmm.2014.09.038i

2 A. Shankar et al. / Journal of Magnetism and Magnetic Materials ()

2 linewidth respectively with the decrease in temperature are 68

3 accompanied by this characteristic transition. 69

4 The aim of this work is to describe experimentally observed 70

5 spin-glass transition using the Raikher and Morais models [2127]. 71

6 Later on, freezing effects of carrier medium in double surfactant 72

7 water based ferrouid were also observed. The particles were 73

8 prepared by reverse micelle precipitation in aqueous phase and 74

9 coated twice with oleate group, each in a reverse manner for a 75

10 good dispersion in water. The FMR investigations of water based FF 76

11 are seldom reported due to high microwave absorption tendency 77

12 of water. The aqueous dispersions similar to this double surfactant 78

13 FF are used very frequently in biomedical applications [28]. 79

14 80

15 81

16 2. Synthesis and experimental methods 82

17 83

18 The Fe3O4 nanoparticles (FNPs) were synthesized in two steps 84

19 via chemical route. In rst stage, 13.96 g FeSO4 7H2O and 16.21 g 85

20 FeCl3 were dissolved in 100 mL MilliQ water along with 4 mL oleic Fig. 1. Room temperature X-ray diffraction pattern of Fe3O4 nanoparticles with

86

21 acid. The mixture was ultrasonicated with 2 mL acetone as Rietveld renement. (a) TEM micrograph of as synthesized FNPs. (b) Magnetization 87

22 emulsier for 25 min to form oil-in-water emulsion. It was then curve with t with a comparison of particle size distribution from VSM and TEM 88

23 results. 89

heated to 70 C followed by addition of 60 mL of 25% aq. NH3 in a

24 time span of 35 min. The mixture was subsequently cooled down 90

25 and magnetically separated for washing by MilliQ water. In second shaped particles can be described by following equation [20,30]: 91

26 stage, a 20 mL aqueous solution of sodium oleate (3.8580 g) was 92

27

prepared by heating at 50 C (15 min). The washed precipitate was M= 0 L () f (D) dD i H

(1)

93

28 94

transferred to above solution and heated for further 15 min. The

29

mixture was allowed to cool down and centrifuged at 13,500 rpm where L() is the Langevin function, 95

30 96

for 15 min. The ltrate was separated via pipette and labeled as FF.

31

The structural characterization was performed by a Rigaku

1

L () = Msf coth () ; Msf = Md with =

Md H (1/6) D3 ( ) 97

32 kT 98

powder X-ray diffractometer with Cu-K radiation, 40 kV A and

33 99

30 mA with step size 0.02/s, scan range (2) from 25 to 80. The and f (D) is the log-normal size distribution of MNPs

34 100

morphology of nanoparticles was examined with M/s Tecnai F30

35 1 101

HRTEM. The magnetization measurements were carried out on f (D ) = e { ln (D / Do )2 /2 D2 }

36 2 D D 102

these samples using were carried out using vibrating sample

37 103

magnetometer (VSM) model 7304 from Lakeshore Cryotronics Here, sD is the standard deviation, H is the applied magnetic

38 104

Inc., USA. The ferromagnetic resonance (FMR) measurements were eld, k is the Boltzmann constant, T is the temperature, Msf is the

39 105

40

performed using a M/s Bruker biospin (model A300) using uid magnetization, is the solid volume fraction of FNPs in the 106

41

rectangular resonator cavity having TE102 resonance mode in the FF, Md is domain magnetization, Do is median diameter and iH 107

temperature range 4300 K. Before low temperature measure- represents diamagnetic contribution from surfactants and water in

42 108

ments, the signal channel was calibrated at room temperature sample.

43 109

using 1 mg DPPH standard. The best t of Eq. (1) to the MH curve (shown in inset (b)) is

44 110

45 obtained for Do 9.6(2) nm, Md 3.84 105 A m 1 384 G with s 111

f

46 D 0.23, Ms 1.0(1) emu/g and 0.0129. Further, to estimate 112

47 3. Results and discussion particle concentration (n), the volume fraction can be expressed 113

48 as 114

49 3.1. Structural characterization 115

1

50 = n Do3 116

6 (2)

51 The Rietveld renement of the XRD pattern (Fig. 1) of FNPs was 117

52 performed by the use of FullProf via pseudo-voigt prole method. Using requisite values in Eq. (2) the particle concentration for 118

53 Using the WilliamsonHall equation [29], the calculated average the present sample was found as 2.78 1022/m3. Further, while 119

54 crystallite size (D) and strain () induced in the FNPs were found to assuming that particles are uniformly distributed in the uid, the 120

55 be 9.8(1) nm and 0.0010(1) respectively. The inset in Fig. 1 average core-to-core interparticle distance can be calculated by 121

56 (a) shows the morphological view of the NPs. The average particle (1/n)1/3, which is 32.9 nm. 122

57 size was calculated by counting over 150 NPs, and found to be 123

58 10.9 nm with standard deviation, s 2.8 nm. 3.3. FMR measurement 124

59 125

60 3.2. Magnetic measurement FMR measurements were performed on ten times diluted FF 126

61 sample kept in a ne cylindrical quartz capillary. Thus, average 127

62 The magnetization curve of FF recorded at room temperature is interparticle distance is now 71.1 nm. A typical FMR spectra at 128

63 shown in Fig. 1 (inset (b)). The MH loop showed a low coercive room temperature constitutes a broad ferrimagnetic signal 129

64 eld of 2.5 Oe which indicated that particles exhibit superpara- 3100 Oe superimposed by a sharp signal at 3400 Oe due to a 130

65 magnetic nature. Further while assuming the non-interacting superparamagnetic phase which is similar to the previous reports 131

66 behavior, the magnetic state of such a system with spherical [25,31]. The low temperature FMR measurements were performed 132

Please cite this article as: A. Shankar, et al., Journal of Magnetism and Magnetic Materials (2014), http://dx.doi.org/10.1016/j.

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A. Shankar et al. / Journal of Magnetism and Magnetic Materials () 3

1 onwards. In later part this has been ascribed to the surface spin- 67

2 glass transition taking place due to freezing of surface spins (Fig. 3 68

3 (c)). Region II (50 Ko To200 K) shows the core dominant feature 69

4 i.e. ferromagnetic behavior of FNPs. In region III 70

5 (200 K oT o300 K) the resonance lines gradually loses their 71

6 angular anisotropy with progressive increase in temperature and 72

7 becomes unobservable when uid melts. 73

8 In FC measurements, the applied eld of 1 T is chosen inten- 74

9 tionally so as to create the environment where Hcf c HA, HA is 75

10 anisotropy eld [20,25,33]. This condition works in the favor of 76

11 minimizing orientational distribution of anisotropy axes for 77

12 achieving an excellent texturation in the sample. For the ZFC 78

13 sample having random distribution of anisotropy axes, the reso- 79

14 nance eld of a particle with uniaxial anisotropy is given by 80

15 [24,34] 81

16 82

o

17 HR = HA (P2 cos ) 83

(3)

18 84

19 where, P2 is Legendre polynomial. For perfectly aligned particles, 85

20 the resonance eld in parallel and perpendicular orientation, i.e. 86

21 for 0 and 90, can be written as HR(0) o/ HA and HR(90) 87

22 Fig. 2. Selected ZFC and FC recorded spectra for FF. o/ HA/2. The simplication yields HR(90) HR(0) (3/2)HA. 88

23 Using values from Fig. 3(a), one nds HA Z340 Oe. The equality 89

24 in two different protocols; zero-eld cooled (ZFC) and eld-cooled is valid for an ideal frozen ferrouid where there is a perfect 90

25 (FC) to investigate the spin dynamics of the system. Fig. 2 shows texturation. However during preparation of real eld frozen 91

26 selected FMR spectra recorded via ZFC and FC procedure with a ferrouid samples, thermal energy tries to disorient the magnetic 92

27 dened 3-dimensional coordinate axis system of FNPs under moments which in turn are bounded to the anisotropy axes of 93

28 study. particle. This affair always results in a nite amount of orienta- 94

29 These measurements were carried out using 9.54 GHz micro- tional disorder affecting the alignment of anisotropy axes in real 95

30 wave frequency with the power of 1.03 mW [32]. Thus reference cases [25,35]. The magnitude of Hcf is one the factors which affects 96

31 resonance eld set for these measurements is o/ 3.404 kOe, this orientational distribution and hence 1 T of eld is chosen 97

32 where is gyromagnetic ratio of free electrons. A 100 kHz intentionally to minimize this effect. 98

33 modulation frequency and 6 G of modulation amplitude was used From Fig. 3(a) it is clear that ZFC and FC resonance lines shifts 99

34 for recording spectra. In ZFC measurements, the sample was isotropically away from reference eld for T o200 K. This behavior 100

35 cooled down from 298 K to 4 K in zero magnetic eld and the has been proposed to have surface origin which has been well 101

36 spectra were recorded while raising the temperature. For the FC conrmed by many researchers [19,20,25]. This isotropic shift is 102

37 measurements, the sample was cooled in magnetic eld (Hcf) of dened by Hiso o/ HR(ZFC), where the shift can be seen as an 103

38 extra unidirectional internal eld always parallel to the magnetiz- 104

1 T to form textured suspension and spectra were recorded during

39 ing eld. The strength of this uniform intrinsic eld is greater for 105

warm up cycle (4298 K) at different angular orientations (i.e. 0,

40 smaller sized particles. Raikher and coworkers extended this FMR 106

30, 60, 90, 120, 150, and 180) at each specied temperature.

41 107

Fig. 3(a) shows variation of resonance eld (HR) in the temperature theory of MNPs where they assumed that at low temperatures the

42 108

range from 4 K to 298 K for ZFC and FC measurements. magnetization is weakly pinned at the particle surface by a

43 109

In ZFC, resonance eld shows a non-monotonic behavior with a unidirectional anisotropy [26]. Under the condition of a weak

44 110

maximum at 200 K. The corresponding FC data with in plane surface pinning, a uniform external radio-frequency eld instead

45 111

angular rotation also retained this behavior but reveal more of the uniform Larmor precession excites in a particle a magneti-

46 112

interesting features. For simplicity we have divided Fig. 3(a) into zation mode that is spatially modulated along the radius. Thus, the

47 113

three regions. Region I shows the temperature region resonance eld value for a single particle can be expressed as a

48 114

(4 KoT o50 K) where a steep rise in HR can be seen from 40 K combination of an internal surface and bulk anisotropy elds as

49 115

50 116

51 117

52 118

53 119

54 120

55 121

56 122

57 123

58 124

59 125

60 126

61 127

62 128

63 129

64 130

65 131

66 Fig. 3. (a) HR vs T for ZFC and FC measurements (4298 K). (b) Variation of isotropic shift and 2/3[HR(90) HR(0)] with temperature. 132

Please cite this article as: A. Shankar, et al., Journal of Magnetism and Magnetic Materials (2014), http://dx.doi.org/10.1016/j.

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4 A. Shankar et al. / Journal of Magnetism and Magnetic Materials ()

1 follows: textured form. Thus, one needs to consider the magnitude of this 67

2 disorder in calculation. In addition, the usage of Eqs. (6)(8) for 68

o 6KS

3 HR () = Ha (P2 cos ) determining KS has been found reliable but the same is not true for 69

ID (4)

4 Ha [25,27]. 70

5 where, I is the magnetization of dispersed MNPs, D is the particle Fig. 4 shows angular variation of FC resonance eld values. The 71

6 diameter, Ha is the bulk anisotropy eld, KS is effective intrinsic characteristic behavior of resonance eld values with maxima 72

7 anisotropy constant due to surface anisotropy, is the angle around 90 and minima around 0 and 180 proves that particles 73

8 between n^ and applied sweeping eld and P2 is associated have uniaxial kind of anisotropy [17,20,25,33]. To explain angular 74

9 Legendre polynomial. For ZFC samples, the isotropic angular variation of three different regions we use model developed by 75

10 averaging of the pertinent uniaxial anisotropy is valid and hence Morais and coworkers [22,23]. In this model, the effective mag- 76

11 an angular independent relation can be written as netic eld (HEFF) acting on MNPs at resonance condition is 77

12 proposed to constitute three main components, viz., external 78

13 o 6KS 79

Hiso = HR (ZFC) = sweeping eld (HE), exchange anisotropy eld (HX), and effective

14 DI (5) 80

uniaxial anisotropy eld (HEK). At resonance, the external eld

15 81

Fig. 3(b) shows the variation of Hiso with temperature. Using becomes equal to resonance eld and the resonance condition can

16 82

I 384 G and D 9.6 nm, one obtains KS 2.3 10 2 erg cm 2 at be expressed mathematically as follows:

17 83

4 K, which is consistent with other reports [25,26]. For a textured

18 HR = HEFF HX HEK (9) 84

suspension, Eq. (5) can be further resolved for two general cases,

19 85

20 where the orientation of anisotropy axis to the external eld can with, HEK = (KEFF/I)(3 cos2 1) and KEFF = K V + (6/D) KS where, KV 86

21 be parallel or perpendicular whose resonance conditions can be and KS both are anisotropy constants having volume and surface 87

22 written as origin respectively [36]. Employing Eq. (9) and using I 384 G the 88

23 theoretical t is performed on the experimental data in order to 89

o 6KS

24 HR (0) = Ha obtain effective magnetic anisotropy of particles. The KEFF values 90

DI (6) obtained after tting angular variation data of Fig. 4 is shown in

25 91

26 and Fig. 5. The behavior of magnetic anisotropy shows that its 92

27 magnitude decreases with increase in temperature, which is 93

o 3KS H consistent with previous reports [22]. Though, effective anisotropy

28 HR (90) = + + a 94

DI 2 (7) in lowest temperature regime (region I; 440 K) is highest, but is

29 95

30 still smaller than the bulk value of Fe3O4 i.e. 1.1 105 erg cm 3 96

Simplifying Eqs. (6) and (7), one obtains

31 [37]. This observation is directly related to the nite size effects 97

32 2 6KS and larger interparticle distances in the matrix. It should be 98

[HR (90) HR (0)] = + Ha

3 DI (8) remarked that the thermal variation of effective anisotropy is

33 99

34 clearly visible in Fig. 5 with three distinct regions, as already 100

By using observed resonance eld values in left hand side of Eq.

35 marked in Fig. 3(a). The red lines are the linear ts to different 101

(8), the thermal variation of the same is plotted in Fig. 3(b). regions. The extrapolation of linear t to the y-axis, where (1000/

36 Though if one uses Eqs. (5) and (8), to determine Ha, then one can 102

37 T)-0, yields characteristic value of KEFF for the corresponding 103

observe positive and negative values at different temperatures. region. For regions I and II, the KEFF values are 4.7 104 and 2.1

38 104

39

This can be further explained as follows. As discussed above, in a 104 erg cm 3 respectively, whereas region III shows its value near 105

magnetic uid there is no opportunity to achieve a perfect to zero due to melting of carrier liquid. Here, it is conspicuous that

40 106

texturation. In fact, the carrier medium employed here, i.e. water the rise in KEFF is more than 50% from regions II to I. Though KEFF is

41 107

freezes around 260 K, which is high enough so that a good amount combination of both volume and surface terms but we relate such

42 108

43 of orientational disorder of anisotropy axes is present in the an enhancement to the dominance of surface effects present at 109

44 110

45 111

46 112

47 113

48 114

49 115

50 116

51 117

52 118

53 119

54 120

55 121

56 122

57 123

58 124

59 125

60 126

61 127

62 128

63 129

64 130

65 131

66 Fig. 4. HR vs T for FC measurements (a) 440 K and (b) 70270 K. Solid lines are t to Eq. (9). 132

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A. Shankar et al. / Journal of Magnetism and Magnetic Materials () 5

1 67

2 68

3 69

4 70

5 71

6 72

7 73

8 74

9 75

10 76

11 77

12 78

13 79

14 80

15 81

16 82

17 83

18 84

19 85

20 86

Fig. 5. Thermal variation of effective magnetic anisotropy energy constant. Inset

21 Q2 87

shows the schematic diagram of a nanoparticle with frozen surface spin state. (For

22 interpretation of the references to colour in this gure legend, the reader is referred 88

23 to the web version of this article.) 89

24 90

25 91

26 nanometer scale where contributions from volume are negligible. Fig. 6. (a) ZFC, (b) FC || and (c) FC linewidth data with complete region t. (d) FC 92

27 At lower temperatures, the MNPs are proposed to have a core- , (e) FC || and (f) ZFC linewidth data with two-region t. Green region shows the 93

28 temperature region where the onset of freezing of surface spins takes place. (For 94

shell structure whose surface spins freeze at a characteristic interpretation of the references to colour in this gure legend, the reader is referred

29 temperature called surface spin-glass transition temperature 95

to the web version of this article.)

30 (TSG) [19,20,3840]. In FC protocol, the surface spins freeze in 96

31 the direction of Hcf below this characteristic temperature. Before 97

32 linewidth behavior in different MNP systems [39,47,48]. According 98

recording FC spectra when Hcf is removed, the core experiences a to the model, line broadening can be described by

33 nite amount of magnetic eld generated intrinsically by eld 99

34 frozen surface spins which in turn further enhances the anisotropy E 100

35 Hpp = L tanh

101

of system in T oTSG temperature region. When T 4TSG, aligned 2kT (10)

36 frozen surface spins melts and anisotropy is observed alone due to 102

37 with E = EA + Emd + EH + EB + EC + Eed and 103

ordered ferromagnetic core in the system (region II;

38 70oT o200 K). Perhaps, this freezing of surface spins could be 5gSn 104

39 L= 105

the probable cause for the system to exhibit a slight deviation from R3

40 uniaxial anisotropy in region I (Fig. 4(a)). However, using current 106

41 model on ZFC and FC spectra, an exact estimate of surface and where, g is the g-factor, is the Bohr magneton, S is the effective 107

42 exchange anisotropy is possible if one performs measurements on spin of magnetic center, n is the number of magnetic centers inside 108

43 variable sized particles [23]. each grain, R is the average interparticle distance, E is the energy 109

44 In region III at 260 K, the effective magnetic anisotropy gets barrier through which MNPs relaxes, EA is the magnetocrystalline 110

45 minimized with the evolution of a small peak around 3400 Oe anisotropy energy term, Emd is the magnetic dipoledipole inter- 111

46 action, EH is the interaction between moment of particle and 112

along with earlier broad FMR signal. At 265 K and 270 K, the

47 external eld, EB represents the Brownian motion energy, EC is the 113

intensity of this small peak is enhanced without angular depen-

48 electrical Coulomb energy, Eed is the electric dipole energy, k is the 114

dency of main FMR signal. We explained this as the melting of

49 Boltzmann constant and T is temperature. 115

carrier liquid 260 K which rather facilitates the physical rotation

50 The pre-factor, L is related to the magnetic moment of particles 116

of FNPs via Brownian relaxation process in a liquid state. This

51 and their average interparticle distance. Thus, L is a parameter 117

relaxation process is well known to result in insensitivity of

52 which depends upon the sample under investigation. In frozen 118

resonance with respect to angular rotations. The choice of water

53 ferrouids, the reorientational mechanism of particle magnetic 119

54 as a carrier medium offers a higher melting stage (273 K for water) moments via Brownian relaxation is infeasible. Moreover, by 120

55 to the uid but a current depression in melting point (i.e. 260 K) ignoring the weaker electrical contributions in such uids, the 121

56 can be explained by colligative properties of solutions, since the FF expression describing energy barrier reduces to E EA Emd EH 122

57 under study is a many component system comprising FNPs, free [43]. 123

58 ions (Fe2 /3 , Na etc.), free surfactants in water. The complete range of linewidth data of ZFC and FC (|| and ) 124

59 Fig. 6 shows variation of peak-to-peak linewidth (Hpp) with i.e. 4 KoT o300 K does not yield a good t to Eq. (6); especially 125

60 temperature for ZFC, || and ongurations. However, Hpp does for T o100 K, as can be seen in Fig. 6(a)(c). Thus, it again seems 126

61 not show any signicant angular variation in FC measurements that it is a crossover of two regions i.e. I and II. This further point 127

62 which is consistent with other reports [25,41]. Instead, a consis- towards the occurrence of a magnetic phase transition in the 128

63 tent temperature dependent decrease is observed for both ZFC and system. Recently, Upadhyay et al. [39] observed similar linewidth 129

64 FC measurements. Such behavior of Hpp in MNPs can be well behavior in Gd3 doped Mn0.5Zn0.5Fe2O4 due to surface anisotropy 130

65 described by the model developed by Morais and coworkers effects. Thus, in view of above points, we divided the linewidth 131

66 [21,4246]. The same has been successfully utilized for describing data in further two parts viz., To 50 K and T 450 K for tting Eq. 132

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6 A. Shankar et al. / Journal of Magnetism and Magnetic Materials ()

2 Fitted parameters derived from Fig. 6(d)(f). TEM and VSM are in good agreement with each other. The low 68

3 temperature FMR measurements performed in ZFC and FC proto- 69

Measurement type Frozen surface spin state Unfrozen surface spin state

4 (T o 46 K ) (T 446 K) col reveal interesting features. By applying Raikher and Morais 70

5 models, the dominance of surface effects over volume effects is 71

6 L (Oe) E 1021 (J) L (Oe) E 1021 (J) seen in resonance eld behavior. The higher melting stage of 72

7 carrier medium limits the perfect texturation of frozen uid in FC 73

ZFC 1503.7 2.09 1396.4 5.30

8 FC || 1571.7 2.19 1440.9 5.41 measurements. Linewidth analysis using Morais model of FC and 74

9 FC 1629.4 2.12 1491.6 5.38 ZFC spectra gives 46 K as the critical temperature for spin glass 75

10 transition. The formation of chain-like structure and existence of 76

11 surface spin-glass in FC is reected in tted parameters. The 77

12 (10). Thus tting procedure is performed again, but now by energy barrier for relaxation of nanoparticles is different in frozen 78

13 assuming that the system is separated by two different energy and unfrozen surface spin states of magnetic nanoparticles. 79

14 barriers due to frozen and unfrozen surface spin states. The 80

15 parameters L and E obtained after tting are listed in Table 1. 81

16 From Fig. 6(d)(f), it can be seen that the critical temperature for Acknowledgment 82

17 the occurrence of spin-glass transition in our system is around 83

18 46 K, which is well in agreement for similar studied systems This work was supported by Department of Science and Q3

84

19 [10,19,20,38,39,49]. Technology, Ministry of Science and Technology (DST), Govern- 85

20 In Table 1, it can be seen that the L and E values for both ment of India, (Project no. GAP 123532). Authors would like to

86

21 regions are greater in FCs as compared to ZFC. This explains the 87

thank Dr. Michael Golosovsky, The Racah Institute of Physics, Israel

22 possible role of Hcf in forming chain-like structure of FNPs in FC 88

for fruitful discussion. One of the authors, A. Shankar is also

23 cases. Thus, interparticle distances will decrease with such mor- 89

thankful to CSIR for his grant of research fellowship (NET). Q4 Q5

24 phological transformation and consequent increments in pre- 90

25 factor L values are observed, since L1/R3. The following calculated 91

26 values gives a further insight to the above raised points. Using 92

27 L 1396.4 Oe, R7.11 10 6 cm, S 4, g 2 and 9.27 References 93

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