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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 ()
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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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
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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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
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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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
A. Shankar et al. / Journal of Magnetism and Magnetic Materials () 7
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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