Sol–gel synthesis and spectrometric structural evaluation of strontium substituted hydroxyapatite

Investigations of the electronic structures of substituted strontium apatites were carried out by using X-ray photo electron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction technique (XRD) has been used to determine the structural parameters. Electron microprobe microanalysis technique was used to estimate the elemental concentrations in each substituted apatite material. The present work aims at studying the changes in the electronic structure of Sr₅(PO₄)₃OH (Sr-HAP) upon isomorphic substitution by F and Cl at the OH site of apatite and Sr by Na at trans Sr-HAP. The ion exchange between Na⁺ in sodium alginate and aqueous Ca²⁺ was important for the preparation of calcium hydroxyapatite. In contrast, the reaction of sodium alginate with the mixture of Na₄P₂O₇ and aqueous Sr²⁺ afforded strontium hydroxyapatite at the specific ratio. The structure of calcium and strontium phosphates prepared from the sol–gel process evidently depended on the amount of sodium alginate introduced into the mixture of Na₄P₂O₇ and the corresponding divalent cations. The findings have ensured that substitution of Sr-HAP by Na enhances the binding energy of O and Sr core levels. It was also noticed that the same substitution decreases the binding energy of P 2s-level. These observations point out to a decrease in the electron density at P and an increase in the electron density at O in Sr atoms.     

Preparation and magnetic properties of SrFe12O19/Ni0.5Zn0.5Fe2O4 nanocomposite ferrite microfibers via sol–gel process

SrFe₁₂O₁₉/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite ferrite microfibers with diameters of 1–2 μm have been prepared by the sol–gel process. The SrFe₁₂O₁₉/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite ferrites are formed after the precursor calcined at 850 °C for 2 h, fabricating from nanosized particles with a uniform phase distribution. The ferrite grain size increases with the calcination temperature. The magnetic properties for the nanocomposite ferrite microfibers are mainly influenced by the chemical composition and grain size. The nanocomposite ferrite microfibers obtained at 900 °C show the enhanced specific saturation magnetization (M_sh) of 64.8 Am² kg⁻¹, coercivity (H_c) of 146.5 kA m⁻¹ and remanence (M_r) of 33.6 Am² kg⁻¹ owing to the exchange–coupling interaction. This exchange–coupling interaction in the SrFe₁₂O₁₉/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite ferrite microfibers has been discussed.     

Studies of structural and magnetic properties of sol–gel synthesized cobalt substituted Zn–Mn chromites

Cobalt substituted Zn–Mn chromites Zn_1?xCo_xMnCrO₄ (0 ≤ x ≤ 1) were prepared by sol–gel method. The synthesized material was characterized by various physico-chemical methods. The temperature of decomposition, crystallization and phase transformation of the as-prepared powder was studied using TGA–DTA measurement. X-ray diffraction patterns revealed that all compositions are in single phase cubic structure. An infra-red spectral study shows two strong bands, which is attributed to the intrinsic vibrations of tetrahedral sites and the octahedral sites. Formation of spherical particles was revealed by scanning electron microscopy analysis. The elemental analysis as obtained from energy dispersive analysis of X-ray is in close agreement with the expected composition from the stoichiometry of reactant solutions used. Magnetic properties were measured by vibrating sample magnetometer. All the compositions indicated ferrimagnetic nature. The substitution of cobalt ions in the lattice affected the structural as well as magnetic properties of spinel.     

Study of structural and magnetic properties of (Co–Cu)Fe2O4/PANI composites

The nanocomposites of the polyaniline and Co_1−xCu_xFe₂O₄ (PANI/CoCuFe) were prepared by in-situ oxidative polymerization of aniline. Prepared nanocomposites samples were characterized by using various experimental techniques like X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), field emission scanning electron microscope (FE-SEM), vibrating sample magnetometer (VSM), Mössbauer spectroscopy and ultraviolet–visible spectrophotometry (UV–VIS). The elemental analysis as obtained from the energy dispersive X-ray spectroscopy (EDAX) measurement is in close agreement with the expected composition from the stoichiometry of the reactant solutions. XRD result confirms that all the samples have the single phase cubic spinel structure. Unit cell parameter ‘a’ is found to decrease with the increase in copper ion substitution. The crystallite size was investigated by using the Debye–Scherer formula and it was found in the range of ∼28–37 nm. FE-SEM confirmed the homogeneous and well defined surface morphology of the synthesized samples. FT-IR study showed the main absorption bands corresponding to the spinel structure those arose due to the tetrahedral and octahedral stretching vibrations. Cation distribution was estimated using XRD data. Hysteresis measurements revealed that the saturation magnetization decreased with increase in Cu²⁺ substitution. Magnetic environment of ⁵⁷Fe in Cu-doped cobalt ferrite was investigated by using Mössbauer spectroscopy. Mössbauer study evidenced the ferrimagnetic behavior of the synthesized samples.     

Synthesis and properties of magnetic solid superacid: SO4/ZrO2–B2O3–Fe3O4

A magnetic SO₄²⁻/ZrO₂–B₂O₃–Fe₃O₄ solid superacid catalyst is prepared via a simple chemical co-precipitation approach. The obtained materials were characterized in detailed by X-ray powder diffraction, thermogravimetric analysis–different scanning calorimetry, Fourier transform infrared spectroscopy (FTIR), electron microscopy (SEM and TEM), and Mossbauer spectra. Powder X-ray diffraction patterns show that in this composite oxide the transformation temperature of ZrO₂ from tetragonal to monoclinic phase is higher compared to the pristine SO₄²⁻/ZrO₂ material. The introduction of Fe₃O₄ endows the superacid with a super-paramagnetic property while in a ferromagnetic state after calcination. The superacid exhibits high catalytic activity in forming ethyl acetate by esterification.     

Structural,dielectric and electrical properties of Sol–gel auto-combustion technic of CuFeCr0.5Ni0.5O4 ferrite

Journal of Materials Science - The CuFeCr0.5Ni0.5O4 (CFO) compound was synthesized using sol–gel reaction combustion technic. The structural analysis showed that the obtained composites have...     

Sol–gel auto-combustion synthesis of PVP/CoFe2O4 nanocomposite and its magnetic characterization

Poly(vinyl pyrrolidone)/CoFe₂O₄ nanocomposite has been fabricated by a sol–gel auto-combustion method. Poly(vinyl pyrrolidone) was used as a reducing agent as well as a surface capping agent to prevent particle aggregation and stabilize the particles. The average crystallite size estimated from X-ray line profile fitting was found to be 20 ± 7 nm. The high field irreversibility and unsaturated magnetization behaviours indicate the presence of the core–shell structure in the sample. The exchange bias effect observed at 10 K suggests the existence of the magnetically aligned core surrounded by spin-disordered surface layer. The reduced remanent magnetization value of 0.6 at 10 K (higher than the theoretical value of 0.5) shows the PVP/CoFe₂O₄ nanocomposite to have cubic magnetocrystalline anisotropy according to the Stoner–Wohlfarth model.     

Sol–gel synthesis and spark plasma sintering of Ba0.5Sr0.5TiO3

Ultrafine Ba_0.5Sr_0.5TiO₃ powders were prepared by using barium nitrate, strontium nitrate, tetrabutyl titanate, and ammonia via citrate–nitrate combustion process at low temperature (500 °C), along with the X-ray diffraction (XRD), differential scanning calorimetry (DSC)/thermogravimetry analysis (TGA) and scanning electron microscopy (SEM) analytic reports. Spark plasma sintering was carried out to obtain the ultrafine crystalline BST and to improve the dielectric properity. It was found that the sintered BST showed ultrafine crystalline microstructure. At 25 °C, the dielectric constant and dissipation factor of the sintered sample were 1533 and 0.0063 at 10 kHz.     

Sol–gel synthesis,characterization and luminescent properties of Tb doped MLa2O4 (M = Sr or Ba) nanophosphors

Tb³⁺ doped SrLa₂O₄ and BaLa₂O₄ nanophosphors were successfully synthesized via tartaric acid assisted sol–gel method and their luminescent properties were investigated. The crystal structure and morphology of SrLa₂O₄:Tb³⁺ and BaLa₂O₄:Tb³⁺ was studied by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). Thermal decomposition behavior of the dried gels was investigated by thermogravimetry (TG) and differential thermal analysis (TGA). Photoluminescence (PL) behaviors of these nanophosphors were checked by the excitation and emission spectra. These SrLa₂O₄ and BaLa₂O₄ nanophosphors displayed green color under a UV source due to characteristic transition of Tb³⁺ from ⁵D₄ → ⁷F₅ at 544 nm. The dependence of photoluminescence intensity on Tb³⁺ ion concentration, tartaric acid concentration and annealing temperature were also studied in detail. In addition, the optimum doping concentration and time-resolved luminescence spectroscopy were also investigated.     

Sol–gel derived CaO–B2O3–SiO2 glass/CaSiO3 ceramic composites: processing and electrical properties

The CaO–B₂O₃–SiO₂ glass/CaSiO₃ ceramic (CBS/CS) composites were fabricated via sol–gel processing routes. Their densification behavior, structures and dielectric properties were investigated. The precursors of CBS glass and CS ceramic filler were firstly obtained via individual soft chemical route and then mixed together in various proportions. The results indicated that the structures of CBS/CS composites are characteristic of CS and CaB₂O₄ (CB) ceramic phases distributed in the matrix of glass phase at 800–950 °C. The CS ceramic phase not only acts as fillers, but nuclei for the crystallization of CBS glass as well such that the CS content exhibits an effect on the densification and dielectric properties of the composites. The CBS/CS composites with 10% CS sintered at 850 °C own dielectric properties of ε_r < 5 and tanδ = 6.4 × 10⁻⁴ at 1 MHz.     

Sol–gel formation,Mössbauer studies,optical absorption and impedance characteristics of Ba0.5Sr0.5Zn0.2Fe0.8O3−ξ powder

ABO_3−ξ-type oxides have gained prominence because of their usefulness in gas separation, solid oxide fuel cell, gas sensor, etc. Of particular interest is barium and zinc substituted strontium ferrite – an alternative cathode material due to its high structural stability, accommodation of considerable anion deficiency, and good oxygen permeability. An attempt has therefore been made to synthesize Ba_0.5Sr_0.5Zn_0.2Fe_0.8O_3−ξ powder by a novel oxalate sol–gel route to investigate its formation, nature of iron species, optical absorption, and impedance behaviour. The synthesis process involves gel formation, digestion for 6 h, drying at 150 °C for 24 h, and decomposition of oxalate at 950 °C for 15 h in air. The product is shown to exhibit (i) a perovskite-type cubic phase with a = 3.975 ± 0.002 Å, Z = 1, and space group Pm3m, (ii) Fe³⁺_0.5 and Fe⁴⁺_0.3 ions, (iii) oxygen deficiency parameter ξ ∼ 0.45, and (iv) optical absorption at ∼370 nm (∼3.4 eV) and ∼797 nm (∼1.56 eV) – arising due to charge transfer transition from O²⁻(2p) to Fe³⁺(3d) and octahedral crystal field splitting of iron t_2g and e_g orbitals, respectively. Moreover, the high impedance values observed below 10 kHz over a temperature range of 303–413 K have been attributed to space charge polarization; activation energy of the relaxation process being 0.2 eV. The motion of induced polarons is possibly responsible for the decrease of impedance with increase of temperature in the range 303–413 K.     

Effect of co-dopant proportion on the structural,optical and magnetic properties of pristine NiO nanoparticles synthesized by Sol–gel method

Journal of Materials Science: Materials in Electronics - In this present work, the pristine and the different percentages of co-doped NiO nanoparticles have been successfully synthesized through...     

Structural,spectral, dielectric,and magnetic properties of indium substituted Cu0.5Zn0.5Fe2−xO4 magnetic oxides

Journal of Materials Science: Materials in Electronics - The influence of indium on the properties of Cu0.5Zn0.5Fe2O4 nano ferrites synthesized by sol–gel auto-combustion technique was...     

Structural and dielectric properties of Li2O–ZnO–BaO–B2O3–CuO glasses

Glass samples of the system (15Li₂O–30ZnO–10BaO–(45 − x)B₂O₃–xCuO where x = 0, 5, 10 and 15 mol%) were prepared by using the melt quenching technique. A number of studies, viz. density, differential thermal analysis, FT-IR spectra, a.c. conductivity and dielectric properties (constant εφ, loss tan δ, a.c. conductivity, σ_ac, over a wide range of frequency and temperature) of these glasses were carried out as a function of copper ion concentration. The analysis of the results indicate that the density increases while molar volume decreases with increasing of copper content indicates structural changes of the glass matrix. The glass transition temperature, T _g, and crystallization temperature, T _c, increase with the variation of concentration of CuO referred to the growth in the network connectivity in this concentration range, while glass-forming ability parameter (T _c − T _g) decreases with increasing CuO content, indicates an increasing concentration of copper ions that take part in the network-modifying positions. The FT-IR spectra evidenced that the main structural units are BO₃, BO₄, and ZnO₄. The structural changes observed by varying the CuO content in these glasses and evidenced by FTIR investigation suggest that the CuO plays a network modifier role in these glasses while ZnO plays the role of network formers. The dielectric constant decreased with increase in temperature and CuO content. The variation of a.c. conductivity with the concentration of CuO passes through a maximum at 5 mol%. In the high temperature region, the a.c. conduction seems to be connected with the mixed conduction viz., electronic conduction and ionic conduction.     

Crystallization and magnetic properties of a 10Li2O–9MnO2–16Fe2O3–25CaO–5P2O5–35SiO2 glass

The crystallization behavior and magnetic properties of 10Li₂O–9MnO₂–16Fe₂O₃–25CaO–5P₂O₅–35SiO₂ (10LFS) glass have been studied using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) to observe the crystallization behavior and a superconducting quantum interference device (SQUID) for measurements of the magnetic properties. The DTA shows that the 10LFS glass has one broad exothermic peak at approximately 674 °C and one sharp (the highest) exothermic peak at 764 °C. When the 10LFS glass crystallized at 850 °C for 4 h, the crystalline phases identified by XRD were lithium silicate (Li₂SiO₃), β-wollastonite (β-CaSiO₃), lithium orthophosphate (Li₃PO₄), magnetite (FeFe₂O₄) and triphylite (Li(Mn_0.5Fe_0.5)PO₄). The SEM surface analysis revealed that the β-wollastonite and lithium silicate have a lath morphology. The TEM microstructure examination showed that the largest FeFe₂O₃ particles have a size of approximately 0.3 μm. When the 10LFS glass was heat treated at 850 °C for 16 h and a magnetic field of 1000 Oe was applied, a very small remnant magnetic induction of 0.01 emu g⁻¹ and a coercive force of 50 Oe were obtained, which revealed an inverse spinel structure.     

Highlighting of structural units of B2O3–Li2O–P2O5 system under heat treatment

As technology evolves towards the design of small size – high efficiency devices there is a necessity for the development of solid, stable electrolytes that can be fabricated in various shapes. Accordingly, a glass system of xB₂O₃·0.4Li₂O·(0.6 − x)P₂O₅ with 0 ≤ x ≤ 0.6 mol%, was prepared by melting the raw materials at 1200 °C and rapidly cooling the melts at room temperature. The samples were afterwards heat treated to develop crystalline structures, for better identification of the units that build up the network.