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Journal of Magnetism and Magnetic Materials 374 (2015) 748–754

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Nanoferrites of nickel doped with cobalt: Influence of Co2 þ on the
structural and magnetic properties
A.P.G. Rodrigues a, D.K.S. Gomes b,e,n, J.H. Araújo c, D.M.A. Melo a, N.A.S. Oliveira a,
R.M. Braga d

Federal University of Rio Grande do Norte, Chemical Institute, Natal-RN 59078-970, Brazil
Federal University of Rio Grande do Norte, Graduate Program in Materials Science and Engineering, Laboratory of Catalysis and Materials, Natal-RN
59078-970, Brazil
Federal University of Rio Grande do Norte, Department of Theoretical and Experimental Physics, Laboratory of Magnetism and Magnetic Materials,
Natal-RN 59078-970, Brazil
Federal University of Paraíba, DEER-CEAR, João Pessoa–PB 58051-970, Brazil
Coordination of Improvement of Higher Education Personnel, CAPES/PNPD, Brazil

art ic l e i nf o

a b s t r a c t

Article history:
Received 23 July 2014
Received in revised form
3 September 2014
Available online 27 September 2014

Nanoferrites of nickel substituted with cobalt of composition Ni1  xCoxFe2O4 (0 rx r 0.75), were
synthesized by combustion reaction assisted in microwaves. The influence of the substitution of Ni2 þ by
Co2 þ content and the concentration of Co2 þ in the structural and magnetic properties was investigated.
The powders were prepared by combustion according to the concept of chemical propellants and heated
in a microwave oven with a power of 7000 kW. The synthesized powders were characterized by
absorption spectroscopy in the infrared region (FTIR), X-ray diffraction (XRD) together with Rietveld
refinement, surface area (BET) method, scanning electron microscopy (MEV) and magnetic measurements (MAV). The results indicated that it was possible to obtain nickel ferrite doped with cobalt in all
compositions and that an increase of cobalt concentration caused an increase in particle size (9.78–
21.63 nm), a reduction in surface area, and reduction in magnetic concentrations greater than 50%.
& 2014 Published by Elsevier B.V.

Magnetic propertie

1. Introduction
Results of numerous studies have aided in the establishment of
the laws governing magnetism, allowing for the construction of
more efficient and useful magnetic materials for applications in
various electronic devices. In this context, nickel ferrite is considered one of the most promising and versatile materials. Due to
its high electrical resistivity, low coercivity, moderate saturation
magnetization, and low hysteresis losses, it is located in the class
of soft ferrites [1,2]. This material has been industrially utilized in
radio-requency circuits, high-quality filters, antennas and cores of
transformers, and other devices such as converters, inductors, and
suppressor signals [3,4].

Corresponding author at: Federal University of Rio Grande do Norte, Chemical
Institute. Laboratório de Tecnologia Ambiental (LabTam). Senador Salgado Filho Av.,
3000. Campus Universitário, Lagoa Nova, 59.072-970. Natal - RN, Brazil.
E-mail addresses: (D.K.S. Gomes), (J.H. Araújo), (D.M.A. Melo), (R.M. Braga).
0304-8853/& 2014 Published by Elsevier B.V.

Particularly, the ability of certain materials such as ferrites
doped with cobalt to acquire high magnetic momentum is of great
importance. The applications of these magnetic materials are
varied. In ferrites, the origin of magnetism is due to the presence
of irregular 3d electrons distributed in uneven numbers in the
tetrahedral and octahedral sites [5–8]. Therefore, the magnetic
properties of ferrites depend on the electron spins of the constituent ions and their interactions.
The performance of the ferrite is directly related to the quality
and the technical processing of this material, since the morphology and microstructure of ferrites are critical to its performance.
Factors such as grain size, porosity, density, impurities, constituent
phases, and the structure of the cell unit generate the information
needed to understand the relationship between structure, microstructure, and the inherent magnetic properties of the end product
The need for high performance ferrites led to the need to
develop more appropriate methods for obtaining different compositional possibilities of controlled structure with advanced
magnetic characteristics. Among the existing methods, synthesized combustion reaction has been successfully employed to

It enables us to obtain powders with nanometric particles. The combustion method does not involve many steps and produces powders of high purity. we used Ni(NO3)2  6H2O (nickel nitrate hexahydrate. corresponding to stretching of the tetrahedral and octahedral sites of the crystal structure.044). The vibration in the tetrahedral site is more intense than the octahedral site due to the values assigned to the shorter connection length in the tetrahedral towards octahedral [19. 97%). Co(NO3)2  6H2O (Cobalt nitrate hexahydrate. This has caused multiple processes to be based on microwave heating in industrial applications [17].25Fe2O4.75Fe2O4.21]. and NCF75 Region. 2. prepared in accordance with stoichiometric compositions according to the established concepts of propellant chemistry [18]. dispersed with acetone. high specific area. 749 (MAV). Fe(NO3)3  9H2O (Iron nitrate nonahydrate. NCF25. NFC25. The samples were placed directly into the sample port. Rodrigues et al. this paper aims to synthesize nickel ferrite replaced in various proportions with cobalt. and coated with a thin film of gold to ensure adequate electrical conductivity. The method of combustion is self-sustaining after initiating the reaction and reaches high temperatures which ensure the formation and crystallization of powders in a short period of time with the release of a large quantity of gas.75) system involved a mixture containing metal ions such as oxidizing reagents (nitrates) and a fuel (urea) as reducing agent. Micrographs were taken using the equipment Philips XL-30-EMEV. 3. / Journal of Magnetism and Magnetic Materials 374 (2015) 748–754 obtain various types of materials. Specific area measurements were calculated using the BET method using Quantachrome NOVA 2000 model low temperature equipment. In observing the diffraction patterns of the powders in all the compositions evaluated. The magnetic measurements were performed on a vibrating sample magnetometer Fig. Then the solution was introduced to a Panasonic STYLEPANAGRILL microwave oven. Ni0. The samples were dispersed in KBr and pressed into 10 mm in diameter pellets. Material and methods 2. until the occurrence of auto-ignition (combustion).1.02° step. The region in the infrared where absorptions related to metal vibrations (oxygen in ceramic powders). NFC50. with a potential difference of 20 kV. and to evaluate the influence on the structural and magnetic properties of the synthesized compositions. Preparation of ferrite The synthesized combustion reaction for the preparation of Ni1  xCoxFe2O4 (0 rx r0. This tends to minimize the state of agglomeration of the particles formed. The reagents were mixed and subjected to a preheat temperature of 100 °C. NCF50. 1 shows the absorption spectra in the infrared (FTIR) spectrum of the Ni1  xCoxFe2O4 system in the range of 4000–500 cm  1. preprogrammed for the synthesis conditions at a power of 7000 KW for 10 min. The presence of stretches of the intrinsic vibrations of the metal (oxygen in tetrahedral sites at 573 cm  1). from combustible waste (urea) used in the synthesis method [19]. and a high purity. Bands of low intensity that were observed at 1657 cm  1 and 1547 cm  1 are assigned to the angular deformation in the plane N–H. The Rietveld method was used to refine the X-ray diffraction data using MAUD software (version 2. For this redox mixture.25Co0. The data was collected over a range of 2θ angular variation between 10° and 80° with a scan rate of 2° min  1 and 0. since this stretch is commonly observed in the range of 450–385 cm  1 and the equipment has a limitation range of 4000–500 cm  1. The crystalline phases were identified using the International Centre for Diffraction Data (ICDD) database. The primary vibrations of this kind of material usually occur in the range of 600–400 cm  1.2. PA). the most intense stretching is generally observed in the range between 600 and 550 cm  1 and less intensely between 450 and 385 cm  1. The hysteresis curves were obtained at ambient temperature using 30 mg of the powder sample and applying fields of  15000–15000 Oe. NFC50. are generally observed in the range of 1000–400 cm  1. There are several benefits of using microwave energy. a 2. such as reduction in processing times and energy savings. 98%) and CO(NH2)2 (urea. respectively. compositions are named NF. and NFC75.A.5Fe2O4 and Ni0. it was not possible to view the vibration of the metal in the octahedral site. and almost always of the nanometer scale [14–16]. Absorption Spectra in the Infrared compositions NF. Material processing based on heating by means of microwave energy has gained increasing prominence and importance in many industrial applications due to a number of advantages compared to conventional heating methods. and NFC75 compositions. 97%). . employing the methods of synthesis by combustion in a microwave. indicates the formation of the Ni–Co ferrite phase spinel type.G. The X-ray patterns were obtained using a Shimadzu XRD-7000 diffractometer with monochromatic CuKα radiation. For spinel ferrite structures in particular. Results and discussion Fig. Thus. NFC25. Characterization of ferrites The powders resulting from the combustion reaction were characterized by absorption spectroscopy in the infrared spectral range of 4000–500 cm  1 in an ABB Bomem model MB104 spectrometer.P.5°) is apparent. The absorption band at 2346 cm  1 corresponds to the deformation of CO2 molecules arising from the decomposition atmosphere or absorbed from the ambient atmosphere during the handling of the material [19–21].75Co0. For didactic purposes the NiFe2O4. chemical homogeneity. and are usually characterized by vibration of ions in the crystal lattice. Ferrites were identified as ttoheir crystalline structure by standard X-ray diffraction. 1. Fig. the presence of well-defined peaks (2θ ¼35. which corresponds to the intrinsic vibration of the metal in the tetrahedral (Mtetrahedral2O) and octahedral (Moctahedral2O) sites. Ni0. 2 shows the X-ray patterns obtained for the Ni1  xCoxFe2O4 system powders for NF. In the infrared spectra of this work.5Co0.

Table 1 shows the lattice parameters and crystallite size.5% 4. and Ni0 have been identified. NFC50. respectively. The spinel phase.25% 5. with NFC25 composition being the most significant. The Nickel ferrite is an inverse spinel. By treatment of the X-ray data by Rietveld refinement technique. By observing Table 1.5% 0% 0% 0% 0% 7. NFC25. peaks relating to the phases α-Fe2O3.5% 2. is a phase which tends to appear when the material is subjected to a temperature above 500 °C and an atmosphere rich in oxygen. Therefore. in which the ions of Fe3 þ are evenly distributed in tetrahedral and octahedral positions of the network. 2. it can also be seen that increasing the level of Co2 þ in the structure caused a narrowing of the diffraction peaks which characterizes a more accentuated degree of crystalinity. and NFC75.375 9. whose cell unit is represented by the formula (Fe1  x) [NiFe1 þ x]O4. That is. they can be forming (tetrahedral sites) or modifying (octahedral sites). the values in mass%.24]. however. A means of controlling the onset of this stage is to control the heating atmosphere and temperature [23. Rodrigues et al. kept cubic symmetry for all compositions.20 Sig 1.366 8. On the other hand.357 8.06 1.357–8.19 1. NFC50. This behavior leads to a segregation of nickel ions forming in the metallic nickel phase. Note that increasing the concentration of cobalt changed the parameter of the network of 8. (FeCo)O. the precipitation of the metallic nickel phase in the ferrite suggests that nickel ions which typically occupy octahedral positions (network modifier) compete with iron ions which also occupy these modified network positions. and NFC75 compositions. / Journal of Magnetism and Magnetic Materials 374 (2015) 748–754 Fig.78 nm to 21. the addition of Co prevents the formation of α-Fe2O3.09 Phases (mass %) spinel α-Fe2O3 FeO (FeCo)O Ni° 72. due to the positioning of the ions in the crystal lattice.19 1. NFC25.357 8. and 87% for NF. Furthermore. (b) NFC25. Composition Ni1  xCoxFe2O4 NF NFC25 NFC50 NFC75 RW 18. it was possible to extract detailed information about the parameters of the crystal structure obtained. The structure has characteristics of inversed and partly-inversed spinels.36 17. In the X-ray patterns.96 21. The Rietveld analysis confirmed the formation of the spinel type phase for all compositions.4% 0% 0% 0% 9. and decreases the Table 1 Data analysis of the Rietveld refinement of the system Ni1  xCoxFe2O4 for NF. it was also realized that the addition of Co leads to an increased formation of the spinel phase.G.3 nm with increasing concentration of cobalt. It was also observed that the average crystallite size increased from 9.78 20. However. FeO.23 18. the precipitation of the Ni0 phase evidenced in all prepared systems is justified.42% 12% 2. shown only in the NF composition. and (d) NFC75.79 19.33% Lattice Parameter (Å) Dc (nm) 8. 94%.5% 8. (c) NFC50. characteristic of cubic ferrites belonging to the spatial group Fd3m:1 [22]. 90%.375 Å with increasing Co.P.02% 94% 90% 87.750 A. Patterns of X-ray diffraction of Ni1  xCoxFe2O4 system for compositions (a) NF. Hematite (α-Fe2O3).58% 3.63 . The FeO and (FeCo) stages indicate the volatilization of metals resulting in compositional shifts favoring the precipitation of secondary phases [25–27].09 19. corresponding to 72%.

395 2. (b) NFC25. . which favored the formation of soft agglomerates.3 are favorable [28. particle size (DBET). (c) NFC50. prepared by combustion reaction.P. A morphology with non-uniform particle size and irregular formation of agglomerates with a large number of pores can be seen in the micrographs.37 2.A. From the data of BET. and the relationship between the particle diameter and the crystallite size DBET/DDRX are shown in Table 2.51 3. and the Ni as a modifier of the network. 751 The results of specific area (SBET). it is possible that Co stabilizes the Fe forming the network. According to DBET/DDRX. wherein small particles are distributed between 1 μm and 2 μm. the Sig includes the number of variables under refinement whose Sig values r 1. It was generally noticed that the increase of cobalt content led to a decrease of the ratio values DBET/DDRX. 3.G.78 20. with irregular porous (not dense) block formats with soft or fragile characteristics (consisting of weak bonds) of easy disagglomeration. it appears that the values are consistent with those published in the literature. indicating that the particles are polycrystalline and easily agglomerate due to high surface tension. crystallite size (DDRX). Calculated by Rietyeld.049 33 50 51 35 9. The Rw (indicator of numerical convergence) and Sig (optimization refinement) parameters are related to the accuracy of the refinement and the agreement between the observed and calculated profile. 3.222 2. According to the literature.58 1. it is observed that the increase of Co2 þ concentration in Ni1  xCoxFe2O4 system caused a decrease in specific surface area and hence increased particle size.79 21.29]. The compositions exhibit different degrees of agglomeration. formation of FeO and Ni0. indicating that the powders tend to form smaller clusters. Fig. note the formation of a microstructure with grains of irregular size. it was found that all samples have a value greater than 1.47 2. 3 shows the morphology of the powders of Ni1  xCoxFe2O4 system obtained by scanning (MEV) electron microscopy.206 3. It is known that the Fig. which arise due to the release of gases during combustion. Sample SBET(m2 g  1) DBET(nm)a DDRX(nm)b DBET/DDRX NFC NFC25 NFC50 NFC75 3. Rodrigues et al. Also based on the micrographs shown in Fig. / Journal of Magnetism and Magnetic Materials 374 (2015) 748–754 Table 2 Specific area and particle size of the Ni1  xCoxFe2O4 system. Observing the values obtained from the Sig in Table 1 for the XRD patterns of the prepared compositions.23 19. Thus.63 Theoretical density¼ 5373 g/cm3 a b Calculated by BET. Scanning electron microscopy (MEV) of Ni1  xCoxFe2O4 system for compositions (a) NF. and (d) NFC75.

formation of precipitated phases observed in X-ray diffraction is clear. Hysteresis cycles of Ni1  xCoxFe2O4 system for compositions (a) NF.6 96 363 512 657 0.38 0. and NFC75. NFC50.5 15. In this case.41 0. NF. and NFC75 compositions. As already noted. there is the segregation of metallic components with subsequent volatilization.30 4. indicating a higher amount of energy to reverse the magnetic field of this ferrite.P. By MEV analysis. NFC25. it affects the behavior (low coercive field. and 21.41 29. which is only considered the average size of the crystals (Tc) [31]. and NFC75 compositions. the crystallite size varied between 9. it can be noted that the curves do not saturate even at high field strength. The increase in the cobalt concentration reduced the saturation magnetization and the coercive field increased.63 nm for NF. The NFC25 composition had the highest saturation magnetization and remanence in relation to NF. 20. (c) NFC50 and (d) NFC75. the larger crystal size has the largest resulting magnetization. since the NFC75 composition showed higher crystallite size compared to the other compositions. The magnetic parameters (coercive field. According to the literature.752 A. Observing the hysteresis loop for the four compositions.75 41. being higher for the NFC75 composition. NFC50. the order of magnetization obtained did not follow this criterion.4 12. The magnetic Table 3 Magnetic Parameters of the Ni1  xCoxFe2O4 system for compositions. and within all compositions. 18. and NFC75 compositions.78. In this case. it is possible to observe that the increase in CO concentration caused a broadening of the hysteresis loop and by reducing the saturation magnetization.96. with an increase in hysteresis loss and high coercive field indicating a material with longer-lasting characteristics (intermediates). / Journal of Magnetism and Magnetic Materials 374 (2015) 748–754 Fig. Fig. remanent magnetization. Moreover. The low losses in the reverse magnetic field indicate that it is a soft magnetic material releasing little energy to reverse the magnetic momentum. which is not well defined at around 100 nm. 4 displays the dependence of the magnetization as a function of applied magnetic field through the hysteresis loop for the ferrite powders of NF. respectively. According to the Rietveld refinement.43 field varied from 657 Oe to 96 Oe. saturation magnetization. and higher values of magnetization). indicating that the phenomenon may be occurring in super paramagnetism. very small particles below the critical size of Dc.23. smaller the particle size. Rodrigues et al. However.13 0. (b) NFC25. NFC50. 4. NFC25. there was no formation of magnetic domains.18 32. the NFC25 composition had . NFC25.8 13. Hysteresis curves show a tendency s  H hysteresis with low energy losses. Sample (combustion) MS (emu/g) MR (emu/g) HC (Oe) MR/MS NF NFC25 NFC50 NFC75 35. low loss for hysteresis. which generates driving force to promote the increase of the state of agglomeration and/or aggregation [30]. the greater the surface tension. NFC50. and hysteresis loss) obtained from the curves s  H are shown in Table 3. the magnetization is explained by coherent rotation of magnetic momentum.G.

C. Rusanov.M. Magn. 5 shows the saturation magnetization as a function of the concentration of the cobalt ferrite Ni1  xCoxFe2O4. References [1] M. The variation of saturation magnetization. NFC50. CAPES/PNPD. likely due to the crystal field organization. Variation of saturation magnetization as a function of the concentration of cobalt.C. Petkov. Conclusions Fig.79 μB.P. Considering the strong preference of the ion Co2 þ . V. Andre. 183 (1998) 163. Matter 405 (2010) 1532–1540. Blaskov. the maximum value is due to the smaller contribution of anti-magnetic iron phases FeO and Ni° present in the structure. Table 4 Ionic radius. thus reducing net magnetic momentum. 2.X. and NFC75 as 2. . J. The ions contribute to the magnetization of the material according to their magnetic momentum. Rahman. Ishaque. that is. and NFC75 composition showed that the concentration of Co2 þ caused a linear decrease of the magnetization and increase in the coercive field.J. Condens. Magn. the magnetization decreases linearly with the increase in the concentration of cobalt. In this work.A.95 μB. D. The dependence of the magnetization as a function of applied magnetic field through the hysteresis loop s  H to the ferrite powders of NF. The XRD patterns do not show monophasic systems however the desired spniel phase was dominant at all compositions.L.F. Gouveia. NFC25. with respect to the magnetization. the octahedral position of the spinel network [21]. A. On the other hand. and an increase in the coercive field. and magnetic momentum of the metal ions [32]. 5. Ms. H. indicating that the particles are polycrystalline and agglomerate easily due to high surface tension.34 μB. M. Opt. 4. and NFC75 compositions were obtained by combustion reaction assisted by microwave.P. NFC50. NFC25. D. 3. The estimated values for the total theoretical Ferrites of Ni1  xCoxFe2O4 system for NF. [2] M. I. Salgueiro. Paiva. Technol. S. Costa. In other compositions. Phys. J. the number of unpaired spins. which indicated that the intrinsic characteristic prevailed. characteristic of combustion reaction assisted in microwaves. Nitianova. where the Fe3 þ ions are evenly distributed in the tetrahedral and octahedral positions of the network. M. On the other hand. L. Mater. NFC50. Grigorova. with cycles of relatively narrow hysteresis. C. 49 (2007) 53–60.6 μB. As explained in Table 4. DBET/DDRX ratio decreased. Structural parameters showed that increasing the amount of Co2 þ caused an increase in crystallite size and hence a reduction in specific surface area. [3] C. Metalic ion Preferred site 3þ Fe Ni2 þ Co2 þ Tetrahedral/octahedral (modifier /forming) octahedral (modifier) octahedral (modifier) Magnetic moment (μB) 5 2 3 higher magnetization compared to the other three compositions. increasing the contribution of the magnetic momentum of the iron in the B site. Structural. A. Blythe. P. as shown by BET analysis. Since in concentrations greater than 25% cobalt this will also go to site A. Hampshire. we observed a linear decrease.P. Genson.M. it became evident that there was a significant influence of cobalt substitution for nickel ions in the nickel ferrite network in synthesis. The magnetic characteristics of ferrites obtained allow for the use of these materials as soft magnetic (permeable) and intermediate (medium magnetic recording). and 1. V. whose cell unit is represented by the formula (Fe1  x) [NiFe1 þ x]O4. Acknowledgements The authors would like to thank the Coordination of Improvement of Higher Education Personnel. Azhar Khan.S. Mǔ noz. however. Islam. since it takes a large amount of spinel phase at all compositions and nano-sized particles with suitable structural properties for use as magnetic materials. preferred site.A. V. we found that the concentration of cobalt led to an increase of particle size. it is known that the extrinsic features such as grain size and/or particle area influence the magnetic field and can contribute to increasing the magnetization because the larger the particle size and/or grain. Nunes. J. electrical and dielectric properties of yttrium substituted nickel ferrites. Rodrigues et al.U. Masheva. the smaller the number of barriers. The laboratory of Magnetism and Magnetic Materials from Department of Theoretical and Experimental Physics (DFTE) of Federal University of Rio Grande do Norte (UFRN) for the magnetic measurements development. This fact can be explained because it presents higher remnant magnetization compared to the other compositions. B: Phys. V.G. and assuming that cobalt partially replaces Ni2 þ ions in this position.Z. . The combustion reaction method can be recommended as a promising method. the ions Ni2 þ and Co2 þ have a preference for octahedral positions. / Journal of Magnetism and Magnetic Materials 374 (2015) 748–754 753 magnetization of each ferrite was calculated based on the magnetic contribution and the stoichiometric amount of each ion in the structure. Rubinger. F. L. a reduction in the magnetic properties is expected when the simultaneous substitution of nickel for cobalt occurs in the spinel ferrite network of nickel. J. NFC25. Therefore. The all compositions showed the non-uniform morphology with irregular-sized particles and the formation of clusters with lots of pores. The Ni2 þ has 3d8 configuration with two unpaired electrons. depends on the distribution of the cations in the spinel network. the PPGCEM/ UFRN and Labtam for facilities.C. It can be seen that the NFC25 composition had an increased saturation magnetization. Mikhov. Microwave dielectric properties of NiFe2O4 nanoparticles ferrites. Microw. respectively. Grac. Martinez. It is known that nickel ferrite is an inverse spinel. Lett.M. as morphological and magnetic characteristics of nanopowders were synthesized in a microwave. we will have the theoretical magnetization (intrinsic characteristic) calculated in the network of the spinels NF. . Fig. M. Thus. since the Co2 þ has 3d7 configuration with three unpaired electrons and the ion Fe3 þ has 3d5 configuration with 5 unpaired electrons. thus achieving greater magnetization.

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