Microstructural Characteristics and Magnetic Properties of Gadolinium-Substituted Cobalt Ferrite Nanocrystals Synthesized by Hydrothermal Processing

Gadolinium substituted cobalt ferrite nanocrystals with composition of CoFe_2?xGd_xO₄ (x = 0–0.04 in a step of 0.01) were prepared by a hydrothermal process and without subsequent annealing. X-ray diffraction, field-emission scanning electron microscopy, and vibrating sample magnetometer were used to investigate the effect of Gd³⁺ cation substitution on structural Characteristics and magnetic properties of cobalt ferrite nanocrystals. The X-ray diffraction analysis demonstrated that single phase spinel ferrites were obtained. The FE-SEM micrographs of the synthesized samples indicated the presence of two distinct groups of grains exhibiting different sizes and, more important, different shapes. The results of magnetic hysteresis at a room temperature showed that with an increase in gadolinium content, the coercive field decreased from 1250 Oe for x = 0 to 450 Oe for x = 0.03. In addition, it was observed that with substitutions of gadolinium cations, the values of saturation magnetization decreased.     

Structural, electrical, and thermal properties in Ca-doped fresnoite ceramics

Polycrystalline ceramic samples of Ca-doped fresnoite of general formula Ba_2?x Ca _x TiSi₂O₈ (x = 0.0, 0.2, 0.4, 0.8, and 1) have been prepared by standard solid state reaction technique using high purity oxides and carbonates. The formation of the single phase compound and its structural parameters were investigated by X-ray diffraction followed by Rietveld refinement using non-centrosymmetric space group P4bm. The bond distances between atoms in a unit cell for all the compounds were also calculated which supports the structural results analyzed by Rietveld analysis. The frequency and temperature dependent dielectric constant and ac conductivity of all the compounds have been measured. The real and imaginary parts of the dielectric constant increases with the increase of temperature. The activation energy (E _a) calculated from ac conductivity increases from x = 0.0 to 0.4 and then decreases from x = 0.8 to 1.0. The modulated differential scanning calorimetry has been used to investigate the effect of substitution on the specific heat, heat flow, and other thermal parameters of the compounds.     

Magnetic Investigation of Various NiFe<Subscript>2−<Emphasis Type="Italic">x</Emphasis></Subscript>Bi<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>O<Subscript>4</Subscript> Ferrite Nanostructures Synthesized by Ball Milling Technique

NiFe_2?x Bi _x O₄ (x = 0, 0.1, 0.2, 0.3) nanoparticles with various grain sizes were synthesized via annealing treatment followed by ball milling of its bulk component materials. Commercially available bismuth, nickel and iron oxide powders were first mixed and then annealed at 1200 °C in an oxygen environment furnace for 4 h. The samples were then milled for 2 h by high-energy ball milling. X-ray diffraction (XRD) pattern indicated that in this stage the samples are single phase. The microstructure investigation was carried out by a scanning electron microscope with maximum magnification of 30,000. The average grain size for different samples was estimated by XRD technique and transmission electron microscopy. Magnetic behavior of the samples at room temperature was studied using an alternating gradient force magnetometry. The Néel temperature of the powders was measured by a Faraday balance. Based on magnetic studies, increase in bismuth content leads to a decrease in the saturation magnetization, coercive field and Néel temperature. This can be attributed to the substitution of Bi³⁺ ion in the ferrite system as a nonmagnetic cation.     

Synthesis,thermal, spectral and biological properties of zinc(II) 4-hydroxybenzoate complexes

New zinc(II) 4-hydroxybenzoate complex compounds with general formula [Zn(4-OHbenz)₂L_n]·xH₂O, where 4-OHbenz = 4-hydroxybenzoate; L = isonicotinamide, N-methylnicotinamide, N,N-diethylnicotinamide, thiourea, urea, phenazone, theophylline, methyl-3-pyridylcarbamate; n = 2, 3; x = 0–3, 5, were synthesized and characterised by elemental analysis, thermal analysis and IR spectroscopy. The thermal behaviour of the prepared compounds was studied by TG/DTG and DTA methods in argon atmosphere. The thermal decomposition of hydrated compounds started with dehydration. During the thermal decomposition, organic ligand, carbon monoxide, carbon dioxide and phenol were evolved. The final solid product of the thermal decomposition was zinc or zinc oxide. The volatile gaseous product, solid intermediate products and the final product of thermal decomposition were identified by IR spectroscopy, mass spectrometry, qualitative chemical analyses and X-ray powder diffraction method. The antimicrobial activity of zinc(II) carboxylate compounds was tested against various strains of bacteria, yeasts and filamentous fungi (S. aureus, E. coli, C. parapsilosis, R. oryzae, A. alternata, M. gypseum). The presence of zinc in complexes led to the increase in their antimicrobial activity in comparison with free 4-hydroxybenzoic acid.     

Structural,morphological and magnetic properties of nano-crystalline zinc substituted cobalt ferrite system

Nano-crystalline zinc-substituted cobalt ferrite powders, Co_1−xZn_xFe₂O₄ (x = 0, 0.25, 0.5, 0.75 and 1), have been synthesized by the combustion route. The structural, morphological and magnetic properties of the products were determined and characterized in detail by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating sample magnetometer (VSM). X-ray analysis showed that the samples were cubic spinel. The increase in zinc concentration resulted in an increase in the lattice constant, unit cell volume, X-ray density, ionic radii, the distance between the magnetic ions and bond lengths on tetrahedral sites and octahedral sites of cubic spinel structure. Opposite behavior was observed for the average crystallite size of the as synthesized solids. The variation of saturation magnetization (M_s) value of the samples was studied. The maximum saturation magnetization value of the Co_o.25Zn_0.75Fe₂O₄ sample reached 76.87 emu/g. The high saturation magnetization of these samples suggests that this method is suitable for preparing high-quality nano-crystalline magnetic ferrites for practical applications.     

Synthesis and characterization of highly preferred orientation polycrystalline Co-doped ZnO thin films prepared by improved sol–gel method

Highly preferred orientation polycrystalline Zn_1?xCo_xO (x = 0, 0.03, 0.06, 0.09) thin films were prepared by improved sol–gel method on quartz glass substrates. The structural, optical and magnetic properties were investigated. The X-ray diffraction patterns show that all the samples have the same structure with one highly oriented c-axis (002) peak. None of the samples showed any signal of impurity phases. The c-axis lattice constant increased linearly with the increase in Co doping content, indicating that the doping of Co ions into the host lattice did not change the wurtzite structure of ZnO. UV–Vis transmittance spectroscopy showed that the average optical transmittance of the films is about 90 % in visible wavelength range. The optical band gap (Eg) decreased with increasing Co content. Also, the results of vibration sample magnetization ascertained the ferromagnetic behavior of Co-doped ZnO, having a Curie temperature higher than room temperature.     

Real and Imaginary Parts of Magnetic Susceptibility of Fine Dispersed Nanoparticles Synthesized by Reverse Micelle: From Superparamagnetic Trend to Ferrimagnetic State

Ni_0.6Zn_0.4Fe_2?xCr_xO₄ (x = 0–0.5) ferrite nanoparticles were prepared using reverse micelle process. X-ray diffraction patterns demonstrated that single phase of spinel ferrites are obtained. TEM micrographs demonstrate the formation of well dispersed nanoparticle with almost spherical morphologies. The EDS analysis proved that the chemical composition has almost uniform distribution in the whole series of samples. Magnetic dynamics of the samples was studied by the measurement of AC magnetic susceptibility versus temperature at different frequencies. The phenomenological Néel–Brown and Vogel–Fulcher models were employed to distinguish between the interacting or non-interacting system. Results exhibited that there is strong interaction between fine particles. The results obtained from vibrating sample magnetometer confirmed that with an increase in chromium content, the saturation magnetization increases. SQUID results at 2 K displayed the ferromagnetic state in nanoparticle and it was found that with an increase in substitution contents, the coercivity decreased.     

The influence of concentration of doping elements on anatase–rutile transformation at the synthesis of rutile pigments (Ti,Cr,Nb)O2 and their pigmentary properties

An analysis of the effects of dopants concentration and different starting titanium compounds on the anatase to rutile phase transformation at the synthesis of rutile pigments Ti_1?3xCr_xNb_2xO_2±δ is presented in this study. The main goal was to analyze reaction mixtures for x = 0.05 (previous study) and 0.30 by simultaneous TG–DTA analysis and to determine the temperature of anatase–rutile transition. For x = 0.05, initial temperatures 760–830 °C are needful for a formation of rutile structure. The temperature is the lowest for the hydrated Na₂Ti₄O₉ paste (760 °C) and similar for other starting compounds of titanium. But for x = 0.30, the anatase–rutile transition begins at higher temperatures 910–1,030 °C because of high-Nb content, which is the inhibitor of this modification change. In addition, we found the influence of calcination temperatures (850, 900, 950, 1000, 1050, 1100, and 1150 °C) on color properties and particle size distribution of these materials prepared from anatase TiO₂ and with x = 0.30. Selected pigments were also analyzed by X-ray powder diffraction.     

Structure and magnetic properties of La0.67Sr0.33MnO3 thin films prepared by sol–gel method

La_1?xSr_xMnO₃ (x = 0.33) (LSMO) thin films have been fabricated successfully by sol–gel method on two different types of substrates, Si (111) and SrTiO₃ (STO) (001). Microstructure and magnetic properties of LSMO thin films have been investigated. The X-ray diffraction studies of the films confirm the pure phase of the LSMO thin films. In contrast with LSMO thin films on Si substrate, the performances of LSMO on STO substrate are superior both from structural and magnetic properties. For the samples deposited on STO substrate, highly preferred orientation as well as less strain and grain defects was found; in other aspect, the magnetization, the residual and saturation moment value, tended greater while a decreased coercive field required merely (saturation moment value was about five times and coercive field was only about 13 % of those on Si substrate). The Curie temperature of LSMO thin films on Si and STO substrates is estimated to be about 349.7 and 359 K, respectively.     

单分散NixZn1-xFe2O4纳米颗粒的制备及其磁热效应

以乙酰丙酮金属盐为前驱体,三乙二醇为溶剂,采用多元醇法制备了镍锌不同配比的Ni_xZn_(1-x)Fe_2O_4(x=0,0.3,0.5,0.7和1.0)铁氧体,并通过X射线衍射仪(XRD),透射电子显微镜(TEM)和振动样品磁强计(VSM)等对样品的结构、形貌、磁性能和磁热性能进行了表征。结果表明:Ni_xZn_(1-x)Fe_2O_4铁氧体分散性较好,尺寸均一,形状近似球形,平均粒径为4~5 nm。Ni_xZn_(1-x)Fe_2O_4纳米颗粒在室温下表现出亚铁磁性,饱和磁化强度随着镍含量的增加先增大后减小,当x=0.5时达到最大值29.38 emu·g~(-1)。在382k Hz交变磁场作用下,Ni_(0.5)Zn_(0.5)Fe_2O_4铁氧体温度可升温至313 K,表现出较好的磁热性能。     

Effects of lutetium doping on the X-ray-excited luminescence properties of the tungstate Zn<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Lu<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>WO<Subscript>4</Subscript>

Polycrystalline samples in the lutetium-doped zinc tungstate system Zn_1?x Lu _x WO₄ with 0 ≤ x ≤ 0.08 were synthesized using the coprecipitation method followed by thermal treatment at 1000 °C during 4 h. The polycrystalline samples were characterized by X-ray diffraction analysis, scanning electron microscopy (SEM), infrared spectroscopy, and luminescence analysis under X-ray excitation. Rietveld analyses were performed. The variation of the wolframite structure cell parameters in the range 0 ≤ x ≤ 0.05 were congruent with substitution of Zn²⁺ by Lu³⁺. SEM micrographs of the obtained samples presented improved crystallization with morphology depending on the lutetium fraction. The luminescence spectra obtained under X-ray excitation (E < 40 keV) were in the blue–green region, and their intensity increased with x up to x = 0.05. The differences in the intensities of the X-ray luminescence spectra could be related to additional cation vacancies resulting from substitution of Zn²⁺ by Lu³⁺.     

Ferromagnetism study of Co<Subscript>0.2</Subscript>Mg<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Zn<Subscript>0.8−<Emphasis Type="Italic">x</Emphasis></Subscript>O films prepared by the sol–gel method

Co_0.2Mg _x Zn_0.8−x O films prepared with different molar ratio of magnesium acetate to zinc acetate were deposited on substrates by the sol–gel technique. X-ray diffraction, photoluminescence (PL) and ferromagnetism measurements were used to characterize the Co_0.2Mg _x Zn_0.8−x O diluted magnetic semiconductors. The acceptor-like defects were determined in the PL band and the intensity of the acceptor-related PL increased with increasing Mg concentration. Therefore, an increase in the number of the acceptor-like defects (zinc vacancies especially) in the Co_0.2Mg _x Zn_0.8−x O film may lead to the enhancement of the magnetic properties. It is worth noting that changes in Mg concentration and the number of the acceptor-like defects are important issues for producing strong ferromagnetism Co_0.2Mg _x Zn_0.8−x O films prepared by the sol–gel method.     

Effect of composition on structural and magnetic properties of nanocrystalline Ni0.8−xZn0.2MgxFe2O4 ferrite

Nanocrystalline magnetic particles of Ni_0.8−xZn_0.2Mg_xFe₂O₄ ferrites with x lying between 0.0 and 0.8 were synthesized using metal nitrates and freshly extracted egg-white. The synthesized powders were characterized using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and transmission electron microscopy (TEM). With increasing magnesium concentration, the lattice constant increases while X-ray density decreases. The average crystallite size determined from XRD data using Scherrer formula lie in the range of 35–59 nm. TEM image shows spherically agglomerated particles with average crystallite size agreed well with that obtained from XRD. Magnetic properties measured at room temperature by vibrating sample magnetometer (VSM) reveal a decrease in saturation magnetization up to Mg content of 0.6. In agreement with FT-IR results, the unexpected increase in the magnetization at Mg content of 0.8 can be attributed to the tendency of Mg²⁺ ions to occupy the tetrahedral site. The decrease in the value of coercivity with increasing magnesium content can be explained based on the magneto-crystalline anisotropy.     

A zinc(II) amidine complex: tandem synthesis,structure, and self assembly

A five-coordinate zinc(II) amidine complex, [Zn(DEP)(N₃)₂] (DEP = N′-(2-(diethylamino)ethyl)picolinamidine), has been synthesized with 2-cyanopyridine and sodium azide in the presence of zinc(II) acetate dihydrate. The structure of the complex is confirmed by single-crystal X-ray diffraction analysis. The complex crystallizes in triclinic space group P-1 with cell dimensions a = 7.486(5) Å, b = 7.678(5) Å, c = 14.480(5) Å, α?=?96.697(5)°, β = 90.282(5)°, and γ?=?95.716(5)°. The hydrogen bonding interactions in the complex lead to the formation of a 2-D supramolecular network. The complex shows fluorescence with lifetime ~4 ns.     

Cu-doping effect on structural, optical and photoluminescence properties of Zn0.96−xFe0.04CuxO (x = 0, 0.02, 0.04, 0.06, 0.08 and 0.1) nanopowders by sol–gel method

Zn_0.96?xFe_0.04Cu_xO (x = 0, 0.02, 0.04, 0.06, 0.08, 0.10) nanopowders have been synthesized by sol–gel method. The synthesized samples have been characterized by powder X-ray diffraction, energy dispersive X-ray spectra, X-ray photoelectron spectroscopy, UV–visible spectrophotometer and Fourier transform infrared spectroscopy. The XRD measurement reveals that the prepared nanopowders have different microstructure without changing a hexagonal wurtzite structure. The calculated average crystalline size increases from 20.9 to 22.1 nm for x = 0 to 0.02 then gradually decreases to 18.2 nm for x = 0.10 which were confirmed by SEM and TEM micrographs. The change in lattice parameters, micro-strain, and shift of X-ray diffraction peaks towards lower angles and increase of energy gap reveal the substitution of Cu²⁺ ions into Zn–Fe–O matrix. X-ray photoelectron spectroscopy study described the increase of oxygen vacancies with increase of Cu concentrations, which was found to enhance the green emission. The presence of functional groups and the chemical bonding is confirmed by FTIR spectra. Photoluminescence spectra of Zn_0.96?xFe_0.04Cu_xO system shows that the blue shift in NBE ultraviolet emission from 389 to 369 nm and the same blue shift in green band emission from 552 to 535 nm with enhancing intensity confirms the substitution of Cu into the Zn–Fe–O lattice. Cu-doped Zn_0.96?xFe_0.04Cu_xO system is appreciable for the fabrication of nano-optoelectronic devices like tunable light emitting diode in the near future.     

Impact of Pb substitution on the formation of high <Emphasis Type="Italic">T</Emphasis><Subscript>c</Subscript> superconducting phase in BSCCO system derived through sol-gel process

Sol-gel process was employed to synthesize the Pb-BSCCO system having general composition Bi_2−xPb_xSr₂Ca₂Cu₃O_10−δ, where x=0.2, 0.4 and 0.8. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), dilatometry and vibrating sample magnetometer (VSM) were employed to study the materials produced at different stages. Two-stage heating firstly at 300 and then 800°C was adopted in order to avoid the burning of the materials and formation of carbonates. The carbonate formation was avoided by heating the materials firstly at 300°C for 2 h and without intermediate cooling moved to the furnace having temperature 800°C and hold for 2 h. The sintering behaviour of samples was studied by dilatometry and the results revealed that the sample having x=0.4 was stabled up to a temperature of 700°C while samples having x=0.2 and 0.8 to a temperature of 625°C. The maximum shrinkage was observed at 850°C in all the samples. On the basis of dilatometry results, the samples were sintered at 845°C for 60 h to observe the superconducting phases. The highest volume fraction of high superconducting phase (2223) was noticed in the sample containing x=0.4 having onset T _c=110 K.     

Synthesis and thermal properties of NiSbS–As doped phase

The substitution of Sb with As in the NiSbS intermetallic compound was studied in the framework of evaluating a possible increase of the thermoelectric properties. Different NiSb_1?xAs_xS samples were synthesized with increasing amounts of As (0 < x < 0.66) employing a simple synthetic route using a muffle furnace. Scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy was used to investigate the microstructure. X-ray powder diffraction techniques were employed in order to study the possible existence of a solid solution between NiSbS and NiAsS compounds, as well as to identify the crystal structure and determine the lattice parameters. All compounds were found to crystallise with the NiSbS prototype (cP12-P2₁3), with lattice parameters varying from a = 0.59341(7) nm (x = 0) to a = 0.56849(6) nm (x = 1). Good agreement with Vegard’s law was evidenced. Thermal measurements on NiSb_1?xAs_xS samples were carried out using DTA instruments to evaluate the thermal stability and the melting temperatures.     

Redistribution of cations and enhancement in magnetic properties of sol–gel synthesized Cu0.7?xCoxZn0.3Fe2O4 (0?≤?x?≤?0.5)

Cu_{0.7− x} Co _x Zn_0.3Fe₂O₄ (0 ≤ x ≤ 0.5) nanoparticles are prepared by sol–gel auto combustion method, using copper nitrate, zinc nitrate, ferric nitrate, cobalt nitrate, and citric acid as the starting materials. The process takes only a few minutes to obtain as-received Co-substituted Cu–Zn ferrite powders. X-ray diffraction (XRD), vibrational sample magnetometer and thermo gravimetric analysis are utilized in order to study the effect of variation in the Co substitution and its impact on particle size, lattice constant, density, cation distribution and magnetic properties like magnetization, coercivity, remanent magnetization, ferritization temperature and associated water content. Lattice parameter found to increase with increasing Co content, whereas X-ray density, bulk density, particle size showed decreasing trend with the Co content. Cation distribution indicates that the Co and Cu ion show preference towards octahedral [B] site, Zn occupy tetrahedral (A) site whereas Fe occupy both tetrahedral (A) and octahedral [B] site. Redistribution of cations takes place for x > 0.3. Saturation magnetization (Ms) increases from 52.99 to 79.62 emu/g (x ≤ 0.3), for x > 0.3 Ms decreases with increase in Co content x. However, coercivity, magnetocrystalline anisotropy and remanent magnetization increases with the Co²⁺ substitution.     

Synthesis and neel temperature determination of ferrites from the MO−ZnO−Fe2O3 systems (M=Cu,Co and Ni)

The Curie (Neel) temperature is successfully determined by means of a simple magnetic device attached to the Q Derivatograph (MOM, Hungary), which is widely used in many laboratories. This possibility is demonstrated by a study of ferrite materials with general formula M_xZn_1?xFe₂O₄ (M=Cu, Co and Ni;x=0.0; 0.2; 0.4; 0.5; 0.6; 0.8; 1.0). X-ray phase analysis, Mössbauer spectroscopy and microscopic examinations revealed that the obtained ferrites are monophase samples. The mixed ferrites possess more strongly expressed magnetic properties than those of the individual ferrites; the maximum magnetic interaction in these ferrites is observed at different zinc contents.     

Synthesis, electrical and thermal properties of Bi4V2−xMexO11 (x = 0.0 and 0.02) ceramics

Polycrystalline ceramic samples of Bi₄V_2?xMe_xO₁₁ (Me = Nb, Zr, Y and Cu and x = 0.0 and 0.02) have been synthesized by standard solid state reaction method using high purity oxides. The formation of the compounds have been analysed by X-ray diffraction method. The dielectric constant, dielectric loss and AC conductivity as a function of frequency and temperature have been measured. The dielectric studies indicate that the material is highly lossy and hence its AC conductivity increases with the increase of temperature. The DC conductivity of material has been measured as a function of temperature from room temperature to 380 °C and its activation energy was calculated using the relation σ = σ ₀exp (?E _a/kT). The modulated differential scanning calorimetry has been used to investigate the effect of substitution on the heat capacity and heat flow of the compounds. The results are discussed in detail.