Production and characterization of spodumene dosimetric pellets by prepared by pechini and proteic sol–gel route

Spodumene is an aluminosilicate that has proven suitable for high-dose TL dosimetry of beta or gamma rays. Due to the presence of lithium in its chemical composition (LiAlSi₂O₆ – β-LAS), it has potential as neutron dosimeter as well. This silicate may be obtained naturally or synthetically. The synthetic LAS has been produced by solid state reaction and conventional sol–gel, whose difficulty arises from the need to employ high temperatures and high cost reagents, respectively. Alternative routes like Pechini and proteic sol–gel methods are promising, because they can reduce production costs and the possibility of environmental pollution. This work aimed at producing spodumene with the proteic sol–gel method using edible unflavored gelatin as a precursor and also with the Pechini method. The products were characterized physically and morphologically, and their applicability as TL dosimeter was investigated, comparing the sensitivity of samples produced by different methods. Two sets of samples were produced using different sources of silicon, tetraethyl orthosilicate (TEOS, Si(C₂H₅O)₄) and silica (SiO₂). The materials produced were characterized by X-ray diffraction and by thermal analysis in order to evaluate their structural properties, as well as possible temperature-dependent changes in physical or chemical properties. The syntherized pellets produced with these crystals were irradiated with a ⁹⁰Sr–⁹⁰Y source and their TL glow curves were evaluated. The production of β-LAS was successful by both methods, either using silica or TEOS as a silicon source. The crystals were obtained using much lower temperatures than by methods described in literature. We observed that the method of powder production was critical to develop a radiation detector: the best TL material was the powder produced using silica and the Pechini Method.     

Synthesis and characterizations of new morphological ZnO and Ce-doped ZnO powders by sol–gel process

ZnO micro-tori and cerium-doped hexangulars ZnO have been prepared by the sol–gel method under methanol hypercritical conditions of temperature and pressure. X-ray diffraction (XRD) measurement has revealed the high crystalline quality and the nanometric size of the samples. Scanning electron microscopy (SEM) has shown that the ZnO powder has a torus-like shape while that of ZnO:Ce has a hexangular-like shape, either standing free or inserted into the cores of ZnO tori. Transmission electron microscopy (TEM) has revealed that the ZnO particles have sizes between 25 and 30 nm while Ce-doped ZnO grains have diameters ranging from 75 nm to 100 nm. It is demonstrated from photoluminescence (PL) spectra at room temperature that the introduction of cerium in ZnO reduces the emission intensity lines, particularly the ZnO red and green ones.     

Fabrication and characterization of nanocrystalline Al,Co:ZnO thin films by a sol–gel dip coating

The consequence of annealing on the micro-structural and electrochemical characteristics of Al doped CoZnO thin films deposited by sol–gel dip coating technique are studied. X-ray diffraction indicates that films have a hexagonal wurtzite structure oriented towards the (100). Optical properties of films are recorded by transmission curves utilising a UV–VIS spectrophotometer. The investigation of the optical transmission spectra indicates that the band gap of the films decrease from 3.99 eV to minimum 3.83 eV upon annealing. All films show room temperature ferromagnetism whose magnetization increases with annealing. Dip coated films possess polycrystalline nanosized grains with porous morphology.     

Synthesis and characterization of nanostructured strontium hexaferrite thin films by the sol–gel method

Nanostructured single phase strontium hexaferrite, SrFe₁₂O₁₉, thin films have been synthesized on the (100) silicon substrate using a spin coating sol–gel process. The thin films with various Fe/Sr molar ratios of 8–12 were calcined at different temperatures from 500 to 900 °C. The composition, microstructure and magnetic properties of the SrFe₁₂O₁₉ thin films were characterized using Fourier transform infrared spectroscopy, differential thermal analysis, thermogravimetry, X-ray diffraction, electron microscopy and vibrating sample magnetometer. The results showed that the optimum molar ratio for Fe/Sr was 10 at which the lowest calcination temperature to obtain the single phase strontium hexaferrite thin film was 800 °C. The magnetic measurements revealed that the sample with Fe/Sr molar ratio of 10, exhibited higher saturation magnetization (267.5 emu/cm³) and coercivity (4290 Oe) in comparison with those synthesized under other Fe/Sr molar ratios.     

Synthesis and characterization of silver/lithium cobalt oxide (Ag/LiCoO2) nanofibers via sol–gel electrospinning

We report on the preparation and characterization of Ag/LiCoO₂ nanofibers (NFs) via the sol–gel electrospinning (ES) technique. Ag nanoparticles (NPs) were produced in an aqueous polyvinyl pyrrolidone (PVP) solution by using AgNO₃ precursor. A viscous lithium acetate/cobalt acetate/polyvinylalcohol/water (LiAc/(CoAc)₂/PVA/water) solution was prepared separately. A Ag NPs/PVP/water solution was prepared and added to this viscous solution and magnetically stirred to obtain the final homogeneous electrospinning solution. After establishing the proper electrospinning conditions, as-spun precursor Ag/LiAc/Co(Ac)₂/PVA/PVP NFs were formed and calcined in air at a temperature of 600 °C for 3 h to form well-crystallized porous Ag/LiCoO₂ NFs. Various analytical characterization techniques such as UV–vis, SEM, TEM, TGA, XRD, and XPS were performed to analyze Ag NPs, as-spun and calcined NFs. It was established that Ag NPs in the precursor Ag/LiAc/Co(Ac)₂/PVA/PVP NFs are highly self-aligned as a result of the behavior of Ag in the electric field of the electrospinning setup and the interaction of Ag ions with Li and Co ions in the NF. Ag/LiCoO₂ NFs exhibit a nanoporous structure compared with un-doped LiCoO₂ NFs because the atomic radius of Ag is larger than the radius of Co and Li ion; thus, no substitution between Ag and Li or Ag and Co atoms occurs, and Ag NPs are located at the interlayer of LiCoO₂ while some are left in the fiber.     

Synthesis by sol–gel process,structural and optical properties of nanoparticles of zinc oxide doped vanadium

We report the elaboration of vanadium-doped ZnO nanoparticles prepared by a sol–gel processing technique. In our approach, the water for hydrolysis was slowly released by esterification reaction followed by a supercritical drying in ethyl alcohol. Vanadium doping concentration of 10 at.% has been investigated. After treatment in air at different temperatures, the obtained nanopowder was characterised by various techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence (PL). Analysis by scanning electron microscopy at high resolution shows that the grain size increases with increasing temperature. Thus, in the case of thermal treatment at 500 °C in air, the powder with an average particle size of 25 nm shows a strong luminescence band in the visible range. The intensity and energy position of the obtained PL band depends on the temperature measurement increase. The mechanism of this emission band is discussed.     

Rare-earth doped (Lu0.85Y0.15)2SiO5 nanocrystalline powders obtained by polymer assisted sol–gel synthesis

In the present work we explored the possibility of obtaining nanocrystalline (Lu_0.85Y_0.15)₂SiO₅ (LYSO) powders using polymer assisted sol–gel method. The synthesis started from TEOS as alkoxide precursor while polyethylene glycol with average molecular weight of 4000 was used as fuel. The resulting powders were obtained by firing gels in two ways: in conventional furnace and in microwave oven, with further annealing. This modified sol–gel synthetic route enabled production of pure phase LYSO powders at much lower temperatures (1050 °C) compared to classical, -solid-state methods (1400 °C). Crystallization kinetics are examined using differential thermal analysis, and rather low values of crystallization activation energies (around 12 kJ/mol) were found, revealing good potential of this method for low-temperature production of LYSO powder.     

Fabrication and analysis of the structural phase transition of ZrO2 nanoparticles using modified facile sol–gel route

The synthesis of zirconia nanoparticles is achieved through a modified facile sol–gel route. The as-prepared gel is analyzed thermally using TGA and DTA techniques to spot the crystallization process of zirconia nanoparticles. The prepared gel is then annealed at different temperatures and the structure was found to change between tetragonal and monoclinic crystal systems. The first stable tetragonal phase is achieved after annealing for 2?h at 400°C. The annealed powders between 600°C and 800°C demonstrate mixed tetragonal/monoclinic phases. Annealing at 1000°C and higher temperatures up to 1200°C resulted in pure monoclinic phase. Cubic phase was not detected within the annealing temperature range in this study. The elemental analysis of the annealed powder confirmed the formation of zirconia nanoparticles with the chemical formula ZrO₂. The FTIR spectra of the annealed samples introduced a variation in the vibrational bands especially around the phase transition temperature. HR-TEM images reported the formation of nano-zirconia crystals with apparently large particle sizes. The optical energy gap of zirconia nanoparticles is investigated and determined.     

Synthesis, structure characterization and magnetic properties of nanosize LiCo1 − y Ni y O2 prepared by sol–gel citric acid route

Single phase LiCo_1 − y Ni _y O₂ (y = 0.4 and 0.5) with fine particles and high homogeneity was synthesized by “chimie douce” assisted by citric acid as the polymeric agent and investigated as positive electrodes in rechargeable lithium batteries. The long-range and short-range structural properties are investigated with experiments including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and superconducting quantum interference device magnetometry. The physicochemical properties of the powders (crystallinity, lattice constants, grain size) have been investigated in this composition. The powders adopted the α-NaFeO₂ structure as it appeared from XRD and FTIR results. Magnetic measurements shows signal at low temperature attributed to the magnetic domains in the nanostructure sample from which we estimated that the cation mixing are 3.35 and 4.74% for y = 0.4 and 0.5 in LiCo_1 − y Ni _y O₂, respectively. LiCo_0.5Ni_0.5O₂ cathode yields capacity (135 mAh g⁻¹) compared to LiCo_0.6Ni_0.4O₂ cathode (147 mAh g⁻¹) when discharged to a cutoff voltage of 2.9 V vs. Li/Li⁺. Lower capacity loss and higher discharge efficiency percentage are observed for the cell of LiCo_0.6Ni_0.4O₂ cathode.     

Synthesis and characterization of nanostructured (Pb1− x Sr x )TiO3 thin films by a modified chemical route

The coating solutions of nanostructured (Pb_{1– x} Sr _x )TiO₃ (PST) thin films have been prepared by the sol–gel combined metallo-organic decomposition method. The coating solutions were deposited on Pt/Ti/SiO₂/Si substrates using a spin-coating technique with spinning speed of 4300 rpm and annealed at 650°C. The effect of Sr content in reducing the grain size and tetragonal distortion of PST films has been studied. The optimum conditions for crystalline phase formation in the films have been analyzed by thermogravimetric, differential thermal analysis and Fourier transform infrared spectroscopy. The phase and microstructure of the films were studied by X-ray diffraction (XRD) and atomic force microscopy (AFM). The XRD pattern shows that the PST thin films are crystallized into tetragonal structures without any impurity phase and the distortion ratio reduces with increasing Sr concentration. The AFM results indicate an increase in grain size with increasing annealing temperature of the film and reduction in grain size with increasing Sr concentration.     

Synthesis and characterization of nanoporous silica film via non-surfactant template sol–gel technique

Nanoporous silicon dioxide has received growing interests owing to their peculiar application potentials in conservation and storage energy. Therefore, the development of novel and simple techniques is required for raising these nanoporous materials to industrial level. In this research, we report novel strategy for the synthesis of nanoporous SiO₂ via non-surfactant template sol–gel technique for the first time. The morphology and structure of the as prepared and annealed nanoporous silica films were studied using X-ray diffraction, scanning electron microscope, Fourier transform infrared spectroscopy and nitrogen absorption/desorption technique. The results showed that highly order nanoporous silica film has been obtained at annealing temperature 600 °C with average diameter 5.1 nm and average pore volume 3.6 cm³ g⁻¹.     

Synthesis and characterization of nickel–manganese oxide via the hydrothermal route for electrochemical capacitors

Nano-sized and well dispersed manganese oxide and nickel–manganese oxide (Ni–Mn–O) powders are synthesized via the hydrothermal route. The addition of nickel ions significantly affects the morphology, particle size and the electrochemical properties of the obtained powders. Adding nickel ions results in a significant change in the shape of the powders from rod-like to plate-like. The electrochemical analysis of the electrode reveals that the specific capacitance of the synthesized powders is greatly increased with the addition of nickel ions. When the hydrothermal temperature is increased to 125 °C, the specific capacitance also increases to 284 F/g and decreases by about 4% after 1500 cycles of charge and recharge. Ni–Mn–O is considered to be a promising material for the electrodes used in electrochemical capacitors.     

Study of NiCuZn ferrite powders and films prepared by sol gel method

This paper reports that a series of NiCuZn ferrite powders and films are prepared by using sol-gel method.The effects of raw material composition and the calcinate temperature on magnetic properties of them are investigated.The NiCuZn ferrite powders are prepared by the self-propagating high-temperature synthesis method and subsequently heated at 700 C～1000 C.The results show that NiCuZn ferrite powders with single spinel phase can be formed after heat-treating at 750 C.Powders obtained from Ni 0.4 Cu 0.2 Zn 0.4 Fe 1.9 O 4 gel have better magnetic properties than those from gels with other composition.After heat-treating at 900 C for 3 h,coercivity H c and saturation magnetization M s are 9.7 Oe (1 Oe=80 A/m) and 72.4 emu/g,respectively.Different from the powders,NiCuZn films produced on Si (100) from the Ni 0.4 Cu 0.2 Zn 0.4 Fe 2 O 4 gel formed at room temperature possess high properties.When heat-treating condition is around 600 C for 6 min,samples with low H c and high M s will be obtained.The minimal H c is 16.7 Oe and M s is about 300 emu/cm 3.In comparison with the films prepared through long-time heat treating,the films prepared through short heat-treating time exhibits better soft magnetic properties.     

Synthesis and characterization of highly-ordered barium-strontium titanate nanotube arrays fabricated by sol—gel method

Highly uniformed barium-strontium titanate nanotube arrays were fabricated using a porous anodic aluminum oxide template from a barium-strontium titanate sol--gel solution. Electron microscope results showed that nanotubes with uniform length and diameter were obtained. The diameters and lengths of these nanotubes were dependent on the pore diameter and the thickness of the applied anodic aluminum oxide template. High resolution transmission electron microscopy and the selected-area electron diffraction pattern investigations demonstrated the perovskite structure and the polycrystalline of the fabricated barium-strontium titanate nanotubes. The characterization of the electrical and dielectric properties had also been made. Compared to thin film material, the intrinsic leakage current density is almost the same. Besides, at 30~℃, the dielectric constant and dielectric loss of the fabricated nanotube is 80 and 0.027 at 1~MHz respectively.     

Thermoluminescence (TL) of europium-doped ZrO2 obtained by sol–gel method

This article reports the preparation and characterization of europium-doped zirconium oxide (ZrO₂:Eu³⁺) formed by homogeneous precipitation from propoxyde of zirconium [Zr(OC₃H₇)₄]. The alkoxide sol gel process is an efficient method to prepare the zirconium oxide matrix by the hydrolysis of alkoxide precursors followed by condensation to yield a polymeric oxo-bridged ZrO₂ network. All compounds were characterized by thermal analysis and the X-ray diffractometry method. The thermoluminescence (TL) emission properties of ZrO₂:Eu³⁺ under beta radiation effects are studied. The europium-doped sintered zirconia powder presents a TL glow curve with two peaks (Tmax) centered at around 204 and around 292 ^°C, respectively. TL response of ZrO₂:Eu³⁺ as a function of beta-absorbed dose was linear from 2 Gy up to 90 Gy. The europium ion (Eu³⁺)-doped ZrO₂ was found to be more sensitive to beta radiation than undoped ZrO₂ obtained by the same method and presented a little fading of the TL signal compared with undoped zirconium oxide.     

Fe-doped SnO 2 nanopowders obtained by sol–gel and mechanochemical alloying with and without thermal treatment

The present work is aimed to compare the physical properties of $\mbox{Sn}_{1-x} \mbox{Fe}_x \mbox{O}_{2-\delta } $ (x?=?0, and 0.05) nanopowders obtained by sol–gel method, mechanochemical alloying, and mechanochemical alloying followed by thermal treatment. The X-ray diffraction of $\mbox{Sn}_{1-x} \mbox{Fe}_x \mbox{O}_{2-\delta } $ samples prepared by sol–gel showed peaks due to the cassiterite phase of SnO₂ and thier Mössbauer spectra showed ferromagnetic and paramagnetic signals. The samples obtained by the milling process of SnO₂ mixed with $\upalpha $ -Fe showed Bragg peaks due to SnO₂ (rutile) with a line broadening caused by the reduction of grain sizes and the presence of microstrains. Mössbauer spectra for these samples revealed the presence of Fe^3?+? as well as unreacted $\upalpha $ -Fe. In the case of mechanochemical alloying with thermal treatment, the incorporation of Fe^3?+? in the SnO₂ structure with the presence of impurities was observed.     

Structural,optical and photocatalytic properties of (Mg,Al)-codoped ZnO powders prepared by sol–gel method

Structural and optical properties of 1 at % Al-doped Zn_1−xMg_xO (x=0–8%) powders prepared by sol–gel method were systematically investigated by means of X-ray diffraction, scanning electron microscopy, ultraviolet–visible absorbance measurement, photoluminescence and Raman scattering spectra. All the powders retained the hexagonal wurtzite structure of ZnO. The band gap and near band emission energies determined from absorbance and photoluminescence spectra increased linearly with increasing Mg content, respectively, which implied that the Mg worked effectively on ZnO band gap engineering, irrespective of Al codoping. However, according to the PL and Raman scattering studies, for the sample of x=8%, the Al doping efficiency was decreased by higher Mg codoping. On the other hand, the effect of Mg codoping on photocatalytic degradation of methylene orange was explored experimentally. The substitution of Mg ions at Zn sites shifted the conduction band toward higher energies and then enhanced the photocatalytic activity, while the incorporation of interstitial Mg ions and decreased Al doping efficiency for higher Mg doping sample (x=8%) reduced the photocatalytic activity.     

Synthesis and magnetic properties of barium–calcium hexaferrite particles prepared by sol–gel and microemulsion techniques

The preparation of W-type hexaferrite particles with the composition BaCa₂Fe₁₆O₂₇ by microemulsion and a stearic acid sol–gel method with and without surfactant has been investigated at various sintering temperatures. The structural and magnetic characteristics have been studied by X-ray diffraction (XRD), a vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetric (DSC) and Fourier transform infrared (FTIR) techniques. The effect of sintering temperature on the properties of BaCa₂Fe₁₆O₂₇ hexaferrites has been studied. The value of saturation magnetization (M_s) depends on types of surfactant used. The sample prepared in the presence of polyoxyethylene (20) sorbitan monooleat (Tween 80) shows low saturation magnetization (M_s=15.10 emu/g), whereas the other sample prepared in the presence of a surfactant cetyltrimethylammonium bromide (CTAB) exhibits high saturation magnetization (M_s=24.60 emu/g) compared to the normal sample.     

Synthesis of Ag–ZnO powders by means of a mechanochemical process

Nowadays, Ag–CdO alloys are widely used in electrical contact applications, because of their good electrical and thermal conductivity is as well as high resistance to arc erosion and contact welding. Considering the restricted use of Cd due to its toxicity, it is necessary to find a material that can replace those alloys. The objective of this work was to study the possibility of obtaining an Ag–ZnO alloy from an Ag–Zn solid solution powders by means of a mechanochemical method. The mechanochemical process was carried out in a SPEX 8000D mill, under air and with ethanol as a reaction agent. Based on the results obtained, it can be concluded that an Ag–ZnO alloy with a fine and uniform ZnO distribution in the Ag matrix can be obtained by applying the mechanochemical process for 25 h.