CHAPTER 8 SYNTHESIS AND CHARACTERIZATION OF COPPER DOPED NICKEL-MANGANESE MIXED FERRITE NANOPARTICLES BY CO-PRECIPITATION METHOD

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1 198 CHAPTER 8 SYNTHESIS AND CHARACTERIZATION OF COPPER DOPED NICKEL-MANGANESE MIXED FERRITE NANOPARTICLES BY CO-PRECIPITATION METHOD 8.1 INTRODUCTION Ferrites are hard, brittle and chemically inert ceramic materials. They are commercially important functional materials because of their excellent magnetic and electrical properties (Sugimoto 1999, Kong et al 2007). The properties of ferrites are very much sensitive to the methodology adopted for their synthesis, the preparative parameters, initial ingredients, etc. Any change in cation distribution also results in an unexpected electrical and magnetic behaviour. Most soft ferrites have a cubic spinel structure with the general composition as MeFe 2 O 4, where Me represents one or several of the divalent transition metals (Yi et al 1995, Satyanarayana et al 2003). Many reports have shown that the property of these spinel ferrites can be improved by doping metal elements in MeFe 2 O 4 which will lead to their enhanced crystal anisotropy (Xiao et al 2006). The co-doping of two metal ions in MeFe 2 O 4 has been extensively studied (Han et al 2004, Doh et al 2004, Hallynck et al 2006) but only a few reports involve the co-doping of three metal ions in spinel ferrite (Zhou et al 2004, Zakaria et al 2006, Slam et al 2006, Gama et al 2007). Various preparation techniques have been

2 199 used by researchers for the synthesis of fine particles of ferrites which exhibit novel properties when compared to their bulk counterpart. In the present investigation, an attempt has been made to synthesize copper doped nickel-manganese mixed ferrite (Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 ) nanoparticles by the co-precipitation method and to study their structural, magnetic and dielectric properties. 8.2 MATERIALS AND METHODS Copper doped nickel-manganese mixed ferrite (Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 ) nanoparticles are prepared by co-precipitation method. The desired composition is obtained by taking stoichiometric amounts of nickel chloride [NiCl 2.6H 2 O], manganese(ii)chloride [MnCl 2.4H 2 O], cupric chloride [CuCl 2.2H 2 O] and anhydrous ferric chloride [FeCl 3 ] dissolved in distilled water. The neutralization is carried out with sodium hydroxide solution and the reaction temperature is maintained at 60 C. The ph of the solution is maintained at 8 and it is stirred for 2 hrs. The precipitate is thoroughly washed with distilled water until it is free from impurities. The product is dried at a temperature of 100 C to remove the water contents. The dried powder is annealed at 130 C, 600 C and 900 C. These samples are characterized using FT-IR, XRD, SEM, EDX, TEM, VSM and LCRZ meter and the results are discussed. 8.3 RESULTS AND DISCUSSION FT-IR Spectral Analysis FT-IR spectra of the sample nickel-manganese-copper mixed ferrites of composition Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 sintered at 130 C, 600 C and

3 C respectively recorded at room temperature in the wave number range 4000 cm cm -1 are shown in Figure 8.1. Figure 8.1 FT-IR spectra of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at (a) 130 C (b) 600 C and (c) 900 C It is observed from the spectra that the absorption bands around 589 cm cm -1 are due to the stretching vibrations of tetrahedral complexes and the depth of the band increases as the sample is sintered at 900 C. This may be due to the existence of lower ionic states in that site (i.e) diffusion of Ni 2+ (Pradeep et al 2008) by the replacement of Fe 3+ in the A-site as also reported for nickel-copper system in Chapter 6. Subsidiary bands are observed around 688 cm -1 and 646 cm -1 as reported for pure nickel ferrites in Chapter 4 and nickel-copper mixed ferrites in Chapter 6. These bands disappear as the sample is sintered at 900 C. The band at

4 cm -1 is due to the stretching vibrations of octahedral complexes and the existence of Cu 2+ ions could be confirmed from the position of the band which could also be evidenced from pure copper ferrite as reported in Chapter 4. The band around 3600 cm -1 is due to the presence of hydroxyl group and the bands around 2350 cm -1 and 1530 cm -1 are due to traces of adsorbed or atmospheric CO 2 as reported in Chapter 4 for pure manganese ferrite Structural Analysis The X-ray powder diffraction patterns of copper doped nickelmanganese mixed ferrites of composition Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 synthesized at ph equal to 8 and sintered at 130 C, 600 C and 900 C are shown in Figure 8.2. It is observed that the intensities of all the peaks increase with increase in the sintering temperature. This increase in intensities of all the peaks may be attributed to the increase in grain growth with the increase in the sintering temperature. The peaks could be indexed by comparing with the standard JCDPS card nos , and of nickel ferrite, manganese ferrite and copper ferrite respectively as (111), (220), (311), (222), (400), (422), (511), (440), (533), (622), (551), (711) and (642). The diffraction patterns show amorphous nature for the sample sintered at 130 -Fe 2 O 3 ) is observed in the sample sintered at all temperatures and it is also observed for the samples Ni 0.4 Cu 0.6 Fe 2 O 4 and pure manganese ferrite sintered at 600 C and 900 C as reported in Chapter 6 and Chapter 4 respectively. The formation -Fe 2 O 3 is due to preferential loss of one or more of divalent cations during the washing and drying stages (Mangalaraja et al 2004, Suwalka et al 2007).

5 202 Figure 8.2 XRD pattern of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at (a) 130 C (b) 600 C (c) 900 C The lattice parameter a of Ni-Mn-Cu ferrite system is found to be Å for the most intense diffraction peak (311) of the sample sintered at 900 C. It is observed to be higher than that of Nickel ferrite and lower than that of Manganese ferrite and may be attributed to be due to the larger ionic radii of Mn 2+ ion when compared to that of Ni 2+ ion (Qiangmin Wei et al 2001, Abid Hussain et al 2013, Yüksel 2013). The lattice constant increases from Å to Å for the most prominent plane (311) of the samples sintered at 600 C and 900 C respectively. The crystallite size is calculated using Debye-Scherrer equation and is found to be 12 nm for the sample sintered at 600 C and 27 nm for the sample sintered at 900 C as shown in Table 8.1.

6 203 Table 8.1 Structural parameters of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles Sintering Temp C Lattice Parameter (a) Å Crystallite Size (D) nm The crystallite size increases with increase in sintering temperature as it is observed in Ni-Cu ferrite system and Co-Cu ferrite system. The microstrain is calculated to be , and for the samples sintered at 130 C, 600 C and 900 C respectively. The decrease in microstrain with increase in sintering temperature may be attributed to the reduction in lattice defects at the grain boundary SEM Analysis

7 204 Figure 8.3 SEM micrographs of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 600 C Figure 8.3 shows the micrographs of nickel-manganese-copper mixed ferrite Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 600 C with different magnifications. The micrographs show that the nanoparticles are dense and agglomerated. They are distributed regularly with voids and pores present in them EDX Analysis cps/e V C u Mn N i O F e M n F e N i C u ke V Figure 8.4 EDX spectrum of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 600 C

8 205 EDX analysis gives the qualitative composition of nanoparticles of nickel-manganese-copper mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 as shown in Figure 8.4. It indicates the quantitative presence of Ni, Mn, Cu, Fe and O in the samples. From the EDX spectrum it is clear that no impurities are present in the samples TEM Analysis Figure 8.5 HR-TEM micrographs of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 600 C

9 206 Figure 8.5 shows the HR-TEM images of nanoparticles of nickel-manganese-copper mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 sintered at 600 C. The micrographs indicate the presence of tetragonal shaped particles and also a few elongated sphere like particles. The particle size is found to be around 27 nm and is found to be in good agreement with XRD results SAED Analysis Figure 8.6 SAED pattern of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 600 C Figure 8.6 shows the electron diffraction pattern of nanoparticles of nickel-manganese-copper mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 sintered at 600 C. The position and intensities of lines in the diffraction pattern confirm the spinel structure. The nanoparticles are found to be in crystalline form as shown by the SAED analysis.

10 Magnetic Measurements using VSM Figure 8.7 (a, b & c) show the typical magnetic hysteresis loops obtained from room temperature VSM measurement for nanoparticles of copper substituted nickel-manganese mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 sintered at 130 C, 600 C and 900 C respectively. (a) (b) (c) Figure 8.7 VSM measurements for Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at (a) 130 C (b) 600 C (c) 900 C

11 208 The saturation magnetization (M s ), remanent magnetization (M r ), coercivity (H c ) and squareness ratio values are listed in Table 8.2. Table 8.2 The saturation magnetization (M s ), remanent magnetization (M r ), coercivity (H c ) and squareness ratio values of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles Saturation Remanent Coercivity Sintering Squareness Magnetization Magnetization (H c ) Temp C Ratio (M s ) emu/g (M r ) emu/g G It is observed that the saturation magnetization (M s ) and remanent magnetization (M r ) increase on sintering the samples at 600 C and 900 C but the coercivity (H c ) decreases on sintering. The increase in saturation magnetization may be explained by the formation of some agglomerates which could also be evidenced from SEM micrographs and also may be due to the extensive degree of particle coarsening at higher sintering temperatures, which in turn decreases the surface defect with respect to the volume of the particle (Chen et al 1996, Muroi et al 2001, Mendoza-Suarez et al 2001, Iqbal et al 2008, Mozaffari et al 2010). However, in comparison with the cobalt-nickel-copper mixed ferrites (Co 0.4 Ni 0.4 Cu 0.2 Fe 2 O 4 ) as reported in Chapter 7, the value of saturation magnetization is found to decrease. This may be due to the decrease in the particle size of Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 system (27 nm) when compared to that of Co 0.4 Ni 0.4 Cu 0.2 Fe 2 O 4 (32 nm). The decrease in coercivity on sintering the samples at 600 C and 900 C may be due to the transition of

12 209 the magnetic single-domain to the magnetic multi-domain during growth of the particles. The squareness ratio (R) as observed from the Table 8.2 exhibits magnetostatic interaction for the nickel-manganese-copper ferrite system sintered at 130 C and 900 C but coherent rotations for the sample sintered at 600 C due to randomly oriented non-interacting particles as observed from the value of R as Dielectric Properties frequency (f) in the frequency range 100 Hz - 5 MHz for nanoparticles of copper doped nickel-manganese mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 sintered at 130 C, 600 C and 900 C is shown in Figure 8.8. Figure 8.8 Variation of dielectric constant with respect to log frequency for Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles It is observed from the Figure 8.8 that the dielectric constant decreases with increase in frequency and reaches a constant value at higher

13 210 frequencies for the sample sintered at 130 C. The value of dielectric constant is found to be very high and of the order of 10 5 for the sample due to its ultrafine size. In this ultrafine state, the number of grains and grain boundaries are large compared to its bulk state. The surface area of the individual nanosize grain is also large; thereby the surface polarization is large. Hence in the lower frequency region, the contribution of surface polarization is large compared to its electronic or ionic polarization in determining the dielectric properties of the sample (Maxwell 1973, Gawas et al 2013). The decrease in dielectric constant with increasing frequency is a normal behaviour observed in most of the ferromagnetic materials. But the value of dielectric constant is very low and reaches a constant value for the samples sintered at 600 C and 900 C for all the frequencies which may be due to lower concentration of Fe 2+ ions in these samples. The variation of dissipation factor as a function of frequency in the range from 100 Hz - 5 MHz at room temperature for copper doped nickel- manganese mixed ferrites Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles sintered at 130 C, 600 C and 900 C is shown in Figure 8.9. Figure 8.9 Variation of dissipation factor with respect to log frequency for Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 nanoparticles

14 211 The dissipation factor decreases with increase in frequency followed by the relaxation peak for the frequency range between 200 KHz - 5 MHz for the sample sintered at 130 C. The appearance of relaxation peak can be explained according to Debye relaxation theory as explained in previous chapters. It is also observed that the dissipation factor decreases and reaches a very low value for the samples sintered at 600 C and 900 C. The absence of the relaxation peak for these samples ensures that the samples possess high resistivity. 8.4 CONCLUSION Copper doped nickel-manganese mixed ferrites (Ni 0.4 Mn 0.4 Cu 0.2 Fe 2 O 4 ) nanoparticles are prepared by co-precipitation method and sintered at 130 C, 600 C and 900 C. FT-IR spectra confirm the characteristic absorption bands of ferrites around 589 cm -1 and 549 cm -1 for the tetrahedral site and around 419 cm -1 for the octahedral sites. The XRD spectra reveal the average crystallite size to be in the range 12 nm - 27 nm and this is found to be in agreement with the TEM results. SEM micrographs show that the nanoparticles are dense and agglomerated with voids and pores present in them. EDX analysis confirms the presence of Ni, Mn, Cu, Fe and O in the samples without any impurities. The saturation magnetization (M s ) and remanent magnetization (M r ) increase with increase in sintering temperature but coercivity (H c ) decreases with increase in sintering temperature. The dielectric constant decreases with increase in frequency and reaches a constant value at higher frequencies. The highest value of dielectric constant is found for this mixed ferrite system. As the co-doping of three metal ions decreases the crystallite size and enhances the properties, these nanoparticles can be tested for various applications.

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