Complex permittivity, complex permeability and microwave absorption properties of ferrite-paraffin polymer composites

We have investigated the electromagnetic (EM) characteristics of Co_xMn_1−xFe₂O₄ spinel ferrite (where x=0.0, 0.5 and 1.0) nanoparticles (NPs)/paraffin nanocomposite material at 8-20 GHz. Co_xMn_1−xFe₂O₄ NPs have been synthesized by cetyltrimethylammonium assisted hydrothermal route using NaOH. A variation in complex dielectric permittivity and magnetic permeability at room temperature with frequency in the range 8-20 GHz has been studied. Particles showed phase purity and crystallinity in powder X-ray diffraction (XRD) analysis. At the same time, Co_xMn_1−xFe₂O₄ NPs demonstrated a spinel cubic structure from XRD results. A reflection loss of −46.60 dB was found at 10.5 GHz for an absorber thickness of 2 mm. Co_xMn_1−xFe₂O₄ may be attractive candidates for EM wave absorption materials.     

Impact of zinc substitution on the structural and magnetic properties of chemically derived nanosized manganese zinc mixed ferrites

Mn_1−xZn_xFe₂O₄ nanoparticles (x=0-1) were synthesized by wet chemical co-precipitation techniques. X-ray diffraction, transmission electron microscopy and high-resolution transmission electron microscopy were effectively utilized to investigate the different structural parameters. The elemental analysis was conducted using energy-dispersive spectrum and inductively coupled plasma analysis. The magnetic properties such as magnetization and coercivity were measured using vibrating sample magnetometer. The observed magnetization values of the nanoparticles were found to be lower compared to the bulk counterpart. The magnetization showed a gradual decrease with zinc substitution except for a small increase from x=0.2 to 0.3. The Curie temperature was found to be enhanced in the case of ferrites in the nanoregime. The variation in lattice constant, reduced magnetization values, variation of magnetization with zinc substitution, the presence of a net magnetic moment for the zinc ferrite and the enhancement in Curie temperature in Mn_1−xZn_xFe₂O₄ all provide evidence to the existence of a metastable cation distribution together with possible surface effects at the nanoregime.     

Structural and magnetic investigations of sub-nano Mn-Mg ferrite prepared by wet method

Manganese-magnesium ferrite nanoparticles Mn_1−xMg_xFe₂O₄; 0≤x≤0.25 were prepared by the co-precipitation route. The samples were characterized by X-ray diffraction (XRD), which confirms the single phase spinel structure. Crystallite size, calculated from the (3 1 1) peak using the Scherrer formula, was found to increase with increasing Mg²⁺ concentrations and was found to be within the range 3-6 nm. TEM was also used to characterize the microstructure of nanosized Mn_1−xMg_xFe₂O₄. Nominal composition of the samples was determined by Atomic Absorption analysis (AA). Hysteresis loops of manganese-magnesium ferrite were obtained at room temperature and revealed lower saturation magnetization values associated with nanocrystalline Mn_1−xMg_xFe₂O₄ particles. This behavior was attributed to structural distortion of surface spins compared to that of the bulk one.     

Magnetic properties and microwave absorption in Ni-Zn and Mn-Zn ferrite nanoparticles synthesized by low-temperature solid-state reaction

In this work, Mn_0.7Zn_0.3Fe₂O₄ and Ni_0.7Zn_0.3Fe₂O₄ nanoparticles with super-paramagnetic properties and size distribution from 10 to 52 nm were investigated. These particles were produced by a low-temperature solid-state reaction method without the ball-milling process. The size and morphology of the nanocrystallites were determined by X-ray diffraction, transmission electron microscopy and scanning tunneling microscopy methods. Magnetic measurements such as alternating gradient field magnetometers were used to justify the super-paramagnetic properties of these nanoparticles. Their microwave absorption in the range of 8-18 GHz was studied by a vector network analyzer. Responses of the device under tests were studied. Also, the percentage of the resin, the size and thickness of the mount were determined. The band width of 2.3 GHz was obtained with reflection-loss/written-loss of −16 dB around 10.4 GHz.     

Li0.5Fe2.5−xMnxO4 ferrite sintered from microwave-induced combustion

Li_0.5Fe_2.5−xMn_xO₄ (0≦x≦1.0) powders with small and uniformly sized particles were successfully synthesized by microwave-induced combustion, using lithium nitrate, ferric nitrate, manganese nitrate and carbohydrazide as the starting materials. The process takes only a few minutes to obtain as-received Mn-substituted lithium ferrite powders. The resultant powders annealed at 650 ^°C for 2 h and were investigated by thermogravimeter/differential thermal analyzer (TG/DTA), X-ray diffractometer (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), and thermomagnetic analysis (TMA). The results revealed that the Mn content were strongly influenced the magnetic properties and Curie temperature of Mn-substituted lithium ferrite powder. As for sintered Li_0.5Fe_2.5−xMn_xO₄ specimens, substituting an appropriate amount of Mn for Fe in the Li_0.5Fe_2.5−xMn_xO₄ specimens markedly improved the complex permeability and loss tangent.     

Structural, chemical and magnetic investigations of polycrystalline Zn1−xMnxO

Present study reports the detailed structural and magnetic, as well as chemical analysis of polycrystalline Zn_1−xMn_xO (where x=0, 0.005, 0.01, 0.03, 0.05 and 0.1) samples synthesized by the high-temperature solid state reaction route. X-ray diffraction studies reveal the presence of secondary phase for higher Mn-doping concentrations (x≥0.03). Secondary phase formation having spinel structure is confirmed and reported as an evidence for the first time using transmission electron microscopy study. Chemical investigations using X-ray photoelectron spectroscopy showed the presence of Mn in two valence states. From the observed results we are of the opinion that Zn²⁺ ions, mainly present at or near grain boundaries, diffuse into manganese oxide to form a stable spinel phase Zn_xMn_3−xO₄ at or near the grain boundaries of ZnO/Zn_1−xMn_xO. Magnetization measurements did not show any magnetic transition down to 5 K.     

Influence of manganese substitution and annealing temperature on the formation,microstructure and magnetic properties of Mn–Zn ferrites

The effects of annealing temperature and manganese substitution on the formation, microstructure and magnetic properties of Mn_xZn_1−xFe₂O₄ (with x varying from 0.3 to 0.9) through a solid-state method have been investigated. The correlation of the microstructure and the grain size with the magnetic properties of Mn–Zn ferrite powders was also reported. X-ray diffraction (XRD), a scanning electron microscope (SEM) and a vibrating sample magnetometer (VSM) were utilized in order to study the effect of variation of manganese substitution and its impact on crystal structure, crystalline size, microstructure and magnetic properties of the ferrite powders formed. The XRD analysis showed that pure single phases of Mn–Zn ferrites were obtained by increasing the annealing temperature to 1200–1300 °C. Increasing the annealing temperature to ?1300 °C led to abnormal grain growth with inter-granular pores and this led to a decrease in the saturation magnetization. Moreover, an increase in the Mn²⁺ ion substitution up to x=0.8 increased the lattice parameter of the formed powders due to the high ionic radii of the Mn²⁺ ion. Mn–Zn ferrites phases were formed and the positions of peaks were shifted by substituting manganese. The average crystalline size was increased by increasing the annealing temperature and decreased by increasing the substitution by manganese up to 0.8. The average crystalline size was in the range 95–137.3 nm. The saturation magnetization of the Mn–Zn-substituted ferrite powders increased continuously with an increase in the Mn concentration up to 0.8 at annealing temperatures of 1200–1300 °C. Further increase of Mn substitution up to 0.9 led to a decrease of saturation magnetization. The saturation magnetization increased from 17.3 emu/g for the Mn_0.3Zn_0.7Fe₂O₄ phase particles produced to 59.08 emu/g for Mn_0.8Mn_0.2Fe₂O₄ particles.     

Synthesis of nanocrystalline Zn0.5Mn0.5Fe2O4 via in situ polymerization technique

Nanocrystalline Zn_0.5Mn_0.5Fe₂O₄ was synthesized through the pyrolysis of polyacrylate salt precursors prepared via in situ polymerization of the metal salts and acrylic acid. The pyrolysis behavior of the polymeric precursors was studied by use of thermal analysis. The as-obtained product was characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), electron diffraction (ED) pattern, scanning electron microscopy (SEM) and electron dispersive X-ray (EDX) analysis. The results revealed that the particle size is in the range of 15–25 nm for Zn-Mn ferrites with good crystallinity. Magnetic properties of the sample at 300 K were measured using a vibrating sample magnetometer, which showed that the sample exhibited characteristics of superparamagnetism.     

Study of magnetic and structural properties of ferrofluids based on cobalt-zinc ferrite nanoparticles

Ferrofluids are colloidal systems composed of a single domain of magnetic nanoparticles with a mean diameter around 30 nm, dispersed in a liquid carrier. Magnetic Co_(1−x)Zn_xFe₂O₄ (x=0.25, 0.50, 0.75) ferrite nanoparticles were prepared via co-precipitation method from aqueous salt solutions in an alkaline medium. The composition and structure of the samples were characterized through Energy Dispersive X-ray Spectroscopy and X-ray diffraction, respectively. Transmission Electron Microscopy (TEM) studies permitted determining nanoparticle size; grain size of nanoparticle conglomerates was established via Atomic Force Microscopy. The magnetic behavior of ferrofluids was characterized by Vibrating Sample Magnetometer (VSM); and finally, a magnetic force microscope was used to visualize the magnetic domains of Co_(1−x)Zn_xFe₂O₄ nanoparticles. X-ray diffraction patterns of Co_(1−x)Zn_xFe₂O₄ show the presence of the most intense peak corresponding to the (311) crystallographic orientation of the spinel phase of CoFe₂O₄. Fourier Transform Infrared Spectroscopy confirmed the presence of the bonds associated to the spinel structures; particularly for ferrites. The mean size of the crystallite of nanoparticles determined from the full-width at half maximum of the strongest reflection of the (311) peak by using the Scherrer approximation diminished from (9.5±0.3) nm to (5.4±0.2) nm when the Zn concentration increases from 0.21 to 0.75. The size of the Co-Zn ferrite nanoparticles obtained by TEM is in good agreement with the crystallite size calculated from X-ray diffraction patterns, using Scherer's formula. The magnetic properties investigated with the aid of a VSM at room temperature presented super-paramagnetic behavior, determined by the shape of the hysteresis loop. In this study, we established that the coercive field of Co_(1−x)Zn_xFe₂O₄ magnetic nanoparticles, the crystal and nanoparticle sizes determined by X-ray Diffraction and TEM, respectively, decrease with the increase of the Zn at%. Finally, our magnetic nanoparticles are not very hard magnetic materials given that the hysteresis loop is small and for this reason Co_(1−x)Zn_xFe₂O₄ nanoparticles are considered as soft magnetic material.     

Preparation and magnetic properties of the conductive Co(1−x)NixFe2O4/polyaniline microsphere composites

Core-shell Co_(1−x)Ni_xFe₂O₄/polyaniline nanoparticles, where the core was Co_(1−x)Ni_xFe₂O₄ and the shell was polyaniline, were prepared by the combination of sol-gel process and in-situ polymerization methods. Nanoparticles were investigated by Fourier transform spectrometer, X-ray diffraction diffractometer, Scanning electron microscope, Differential thermal analysis and Superconductor quantum interference device. The results showed that the saturation magnetization of pure Co_(1−x)Ni_xFe₂O₄ nanoparticles were 57.57 emu/g, but Co_(1−x)Ni_xFe₂O₄/polyaniline composites were 37.36 emu/g. It was attributed to the lower content (15 wt%), smaller size and their uneven distribution of Co_(1−x)Ni_xFe₂O₄ nanoparticles in the final microsphere composites. Both Co_(1−x)Ni_xFe₂O₄ and PANI/Co_(1−x)Ni_xFe₂O₄ showed superparamagnetism.     

The structure and magnetic properties of Zn1−xNixFe2O4 ferrite nanoparticles prepared by sol–gel auto-combustion

Zn_1−xNi_xFe₂O₄ ferrite nanoparticles were prepared by sol–gel auto-combustion and then annealed at 700 °C for 4 h. The results of differential thermal analysis indicate that the thermal decomposition temperature is about 210 °C and Ni–Zn ferrite nanoparticles could be synthesized in the self-propagating combustion process. The microstructure and magnetic properties were investigated by means of X-ray diffraction, scanning electron microscope, and Vibrating sample magnetometer. It is observed that all the spherical nanoparticles with an average grain size of about 35 nm are of pure spinel cubic structure. The crystal lattice constant declines gradually with increasing x from 0.8435 nm (x=0.20) to 0.8352 nm (x=1.00). Different from the composition of Zn_0.5Ni_0.5Fe₂O₄ for the bulk, the maximum M_s is found in the composition of Zn_0.3Ni_0.7Fe₂O₄ for nanoparticles. The H_c of samples is much larger than the bulk ferrites and increases with the enlarging x. The results of Zn_0.3Ni_0.7Fe₂O₄ annealed at different temperatures indicate that the maximum M_s (83.2 emu/g) appears in the sample annealed at 900 °C. The H_c of Zn_0.3Ni_0.7Fe₂O₄ firstly increases slightly as the grain size increases, and presents a maximum value of 115 Oe when the grains grow up to about 30 nm, and then declines rapidly with the grains further growing. The critical diameter (under the critical diameter, the grain is of single domain) of Zn_0.3Ni_0.7Fe₂O₄ nanoparticles is found to be about 30 nm.     

Electrochemical behaviour of nano-sized spinel LiMn2O4 and LiAlxMn2−xO4 (x=Al: 0.00-0.40) synthesized via fumaric acid-assisted sol-gel synthesis for use in lithium rechargeable batteries

Pristine spinel LiMn₂O₄ and LiAl_xMn_2−xO₄ (x=Al: 0.00-0.40) with sub-micron sized particles have been synthesized using fumaric acid as chelating agent by sol-gel method. The synthesized samples were subjected to thermogravimetric analysis (TGA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and cyclic voltammetry (CV) and galvanostatic cycling studies. The TGA curve of the gel shows several weight-loss regions stepwise amounting to 55% till 800 °C attributed to the decomposition of the precursors. Calcination to higher temperatures (800 °C) yields pure-phase spinel (LiAl_xMn_2−xO₄), as it is evident from the high-intensity XRD reflections matching to the standard pattern. SEM and TEM studies confirm that the synthesized grains are of uniform regular surface morphology. FT-IR studies show stretching and bending vibration bands of Li-O, Li-Al-Mn-O. LiAl_0.1Mn_1.90O₄ spinel was found to deliver discharge capacity of 139 mA h/g during the first cycle with columbic efficiency of 97%. LiAl_0.1Mn_1.90O₄ spinel exhibits the high cathodic peak current indicating better electrochemical performance. Low doping (x=0.1) of Al is found to be beneficial in stabilizing the spinel structure.     

Production of bulk dilute ferromagnetic semiconductor by mechanical milling

We tried to prepare the bulk dilute ferromagnetic semiconductor (DMS) by mechanical milling (MM). Experimental results were as following: (1) The observation of X-ray diffraction and transmitting electron microscopy showed that the particle diameter of host ZnO powder were reduced to about 10 nm by MM. (2) The MM for the mixtures of V₂O₅/ZnO or γ-Fe₂O₃/ZnO realizes the V- or Fe-doped ZnO nano-powders. (3) The values of magnetization under the field of 5 kOe were nearly saturated to 0.8×10⁻³ to 3×10⁻³ μ_B/V-ion for V_xZn_1−xO (x=0.05, 0.1 and 0.2), and 0.2–0.3 μ_B/Fe-ion for Fe_xZn_1−xO (x=0.05 and 0.1) at room temperature. The above results show that the ferromagnetic DMS powder of V_xZn_1−xO and Fe_xZn_1−xO were successfully prepared by MM method.     

Magnetic properties of nanostructured MnZn ferrite

Mn_0.5Zn_0.5Fe₂O₄ nanoparticles (10-30 nm) have been prepared via mechanochemical processing, using a mixture of two single-phase ferrites, MnFe₂O₄ and ZnFe₂O₄. SQUID measurements (field-cooled magnetization curves and hysteresis loops) were performed to follow the mechanically induced evolution of the MnFe₂O₄/ZnFe₂O₄ mixture submitted to the high-energy milling process. The resulting single MnZn nanoferrite phase was characterized by SQUID (M-H curve), Faraday balance (M-T curve) and transmission electron microscopy. The magnetic characteristics of the mechanosynthesized material were compared with those of bulk Mn_0.5Zn_0.5Fe₂O₄. It was found that the saturation magnetization of nanostructured Mn_0.5Zn_0.5Fe₂O₄ (87.2 emu/g) is lower than that of the bulk Mn_0.5Zn_0.5Fe₂O₄, but, the Néel temperature of the sample (583 K) is higher than that of the bulk Mn_0.5Zn_0.5Fe₂O₄.     

Magnetic,electronic and structural properties of ZnxFe3−xO4

A series of samples Zn_xFe_3−xO₄ have been prepared by the chemical coprecipitation technique and characterized by X-ray diffraction (XRD), vibrating sample magnetometry (VSM) and X-ray photoelectron spectroscopy (XPS). XRD demonstrates all the samples of Zn_xFe_3−xO₄ have a spinel structure same as Fe₃O₄. The magnetic hysteresis loops of Zn_xFe_3−xO₄ obtained from VSM indicate that the saturation magnetization has a maximum when x is ∼1/3. The chemical states of Fe atoms and Zn atoms in zinc ferrites have been measured using XPS and Auger electron spectroscopy (AES). The Fe 2p core-level XPS spectra and Zn L₃M₄₅M₄₅ Auger peaks have been analyzed and the results have been discussed in correlation with the samples’ magnetic properties. These results suggest most of Zn atoms occupy the tetrahedral sites and a small amount of them occupy the octahedral sites.     

Influence of Fe-doping on the structural,optical and magnetic properties of ZnO nanoparticles

Zn_1–xFe_xO (x=0–0.05) nanoparticles were synthesized without a catalyst by a two-step method. Fe was doped into ZnO by a source of metallic Fe sheets in a solid–liquid system at 80 °C, and the Zn_1−xFe_xO nanoparticles were obtained by annealing at 300 °C. X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy were used to characterize the structural properties of the as-grown Zn_1−xFe_xO. The optical properties were determined by Infrared and Ultraviolet–visible spectroscopy. The results confirm that the crystallinity of the ZnO is deteriorated due to Fe-doping. XPS results show that there is a mixture of Fe⁰⁺ and the Fe³⁺ in the representative Zn_0.95Fe_0.05O sample. The optical band gap of Zn_1−xFe_xO is enhanced with increasing of Fe-doping. Room temperature ferromagnetism was observed in all the Fe-doped ZnO samples.     

Synthesis and characterization of Ni-Zn ferrite nanoparticles

Nickel zinc ferrite nanoparticles Ni_xZn_1−xFe₂O₄ (x=0.1, 0.3, 0.5) have been synthesized by a chemical co-precipitation method. The samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, electron paramagnetic resonance, dc magnetization and ac susceptibility measurements. The X-ray diffraction patterns confirm the synthesis of single crystalline Ni_xZn_1−xFe₂O₄ nanoparticles. The lattice parameter decreases with increase in Ni content resulting in a reduction in lattice strain. Similarly crystallite size increases with the concentration of Ni. The magnetic measurements show the superparamagnetic nature of the samples for x=0.1 and 0.3 whereas for x=0.5 the material is ferromagnetic. The saturation magnetization is 23.95 emu/g and increases with increase in Ni content. The superparamagnetic nature of the samples is supported by the EPR and ac susceptibility measurement studies. The blocking temperature increases with Ni concentration. The increase in blocking temperature is explained by the redistribution of the cations on tetrahedral (A) and octahedral (B) sites.     

Reentrant spin glass behavior and large initial permeability of Co0.5−xMnxZn0.5Fe2O4

A series of polycrystalline ferrites having nominal chemical composition Co_0.50−xMn_xZn_0.5Fe₂O₄ (0<x<0.4) have been synthesized by the solid-state reaction technique. The XRD analysis confirms single phase cubic spinel structure for all compositions. Lattice constant increases from 0.84195 to 0.84429 nm with the increasing Mn content and obeys Vegard's law. The average grain size increases by increasing both Mn content and sintering temperatures. Room temperature saturation magnetization increases for x=0.1 and decreases for increasing Mn content. The coercivity decreases with increasing Mn content due to the decrease of anisotropy constant. A reentrant spin glass behavior of these samples is observed from the zero field cooled magnetization measurements. The real part of the initial permeability increases by increasing both Mn content and sintering temperatures. This is due to the homogeneous grain growth and densification of the ferrites. The highest initial permeability 137 is observed for x=0.4 sintered at 1573 K on the other hand, the highest relative quality factor (2522) is obtained for the sample Co_0.2Mn_0.3Zn_0.5Fe₂O₄ sintered at 1523 K. The Mn substituted Co_0.50−xMn_xZn_0.5Fe₂O₄ ferrites showed improved magnetic properties.     

No room temperature ferromagnetism in Mn over-doped Zn1−xMnxO (x>0.02)

Mn-doped ZnO samples having composition Zn_1−xMn_xO (x=0.02, 0.04 and 0.05) were synthesized by solid state reaction technique with varying concentration of Mn from 0.02 to 0.05. Evidence of room temperature ferromagnetism was observed only in the composition Zn_0.98Mn_0.02O sintered at 500 °C. Our XRD pattern confirms the presence of Mn₃O₄ impurity phase in all the Zn_1−xMn_xO samples with the exception of Zn_0.98Mn_0.02O. We emphasize that the appearance of Mn₃O₄ phase in the system forbids the exchange type of interaction between the Mn ions and suppresses the ferromagnetism in all the Mn over-doped Zn_1−xMn_xO (x>0.02) system. SEM microstructure study also supports the interruption of exchange type of interaction inside the system with the increase in Mn concentration in the sample. Interestingly, for this particular composition, Zn_0.98Mn_0.02O sintered at 500 °C, glassy ferromagnetism type of transition is observed at low temperature. This type of transition is attributed to the formation of the oxides of Mn clusters at low temperature.     

Structural, thermal and magnetic properties of Ni1−xMnxFe2O4 nanoferrites

In this paper, the structural, thermal and magnetic properties of Ni_1−xMn_xFe₂O₄ are presented. It is observed that high concentration of Mn²⁺ ions into NiFe₂O₄ tends to reduce the particle size. Calcination at 500 °C has resulted in the growth of Ni_1−xMn_xFe₂O₄ nanoparticles, but the calcination at 900 °C has led to the evaporation of the majorities of the polyvinyl alcohol. After calcination at 900 °C, crystallographically oriented NiMnFe₂O₄ nanoparticles are formed. These Ni_1−xMn_xFe₂O₄ nanoparticles show hysteresis behaviour upon magnetization. On the other hand, saturation magnetization (Ms) values decreases with increasing Mn content in ferrite due to the influence of Mn²⁺ ion in the sub lattice.