Synthesis of narrow band gap (V2O5)x-(TiO2)1−x nano-structured layers via micro arc oxidation

V₂O₅-TiO₂ layers with a sheet-like morphology were synthesized by micro arc oxidation process for the first time. Surface morphology and topography of the layers were investigated by scanning electron microscope (SEM) and atomic force microscope (AFM). Phase structure and chemical composition of the layers were also studied by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques. It was revealed that the composite layers had a sheet-like structure average thickness of which was about 100 nm depending on the applied voltage. The layers consisted of anatase, rutile, and vanadium pentoxide phases fractions of which varied with the applied voltage. The optical properties of the layers were also examined employing a UV-vis spectrophotometer. It was found that the absorption edge of the grown composite layers shifted toward the visible wavelengths when compared to MAO-synthesized pure titania layers. The band gap energy of the composite layers was calculated as 2.58 eV. Furthermore, photo-catalytic performance of the layers was examined by measuring the decomposition rate of methylene blue under ultraviolet and visible irradiations. The results demonstrated that about 90% and 68% of methylene blue solution was decomposed after 120 min ultraviolet and visible irradiations over the composite layers, respectively.     

Synthesis and electronic behaviors of TiO2/carbon clusters/Cr2O3 composite materials

Nano-structured TiO₂/carbon clusters/Cr₂O₃ composite material has been successfully obtained by the microwave treatment of a TiO(acac)/Cr(acac)₃/epoxy resin complex. The compositions of the composite materials were determined using ICP, elemental analysis and surface characterization by SEM-EDX, TEM and XRD. ESR spectral examinations suggest the possibility of an electron transfer in the process of TiO₂ → carbon clusters → Cr₂O₃ with an oxidation site at TiO₂ particles and a reduction site at Cr₂O₃ particles. The preliminary experimental results show that the calcined materials could decompose methylene blue under visible-light irradiation.     

Hollow glass microspheres coated with CoFe2O4 and its microwave absorption property

Spinel CoFe₂O₄ coating on the surface of hollow glass microspheres of low density was synthesized by co-precipitation method. The phase structures, morphologies, particle size, shell thickness, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and energy dispersive X-ray spectroscopy (EDS). The results show that CoFe₂O₄ coating on hollow glass microspheres can be achieved, and the coating layers are constituted by CoFe₂O₄ nanoparticles of mean size ca. 10 nm. The as-synthesized powder materials were uniformly dispersed into the phenolic cement, then the mixture was pasted on metal plate with the area of 200 mm×200 mm as the test plate. The test of microwave absorption was carried out by the radar-absorbing materials (RAM) reflectivity far field radar cross-section (RCS) method. The results indicate that the coated CoFe₂O₄/hollow glass microspheres composites can be applied in lightweight and strong absorption microwave absorbers.     

In vitro evaluation of bioactivity of CaO-SiO2-P2O5-Na2O-Fe2O3 glasses

Glasses with compositions 41CaO(52 − x)SiO₂4P₂O₅·xFe₂O₃3Na₂O (2 ≤ x ≤ 10 mol.%) were prepared by melt quenching method. Bioactivity of the different glass compositions was studied in vitro by treating them with simulated body fluid (SBF). The glasses treated for various time periods in SBF were evaluated by examining apatite formation on their surface using grazing incidence X-ray diffraction, Fourier transform infrared reflection spectroscopy, scanning electron microscopy and energy dispersive spectroscopy techniques. Increase in bioactivity with increasing iron oxide content was observed. The results have been used to understand the evolution of the apatite surface layer as a function of immersion time in SBF and glass composition.     

Bioactivity of SiO2-CaO-P2O5-Na2O glasses containing zinc-iron oxide

Glasses with composition x(ZnO,Fe₂O₃)(65 − x)SiO₂20(CaO,P₂O₅)15Na₂O (6 ≤ x ≤ 21 mol%) were prepared by melt-quenching technique. Bioactivity of the glasses was investigated in vitro by examining apatite formation on the surface of glasses treated in acellular simulated body fluid (SBF) with ion concentrations nearly equal to those in human blood plasma. Formation of bioactive apatite layer on the samples treated in SBF was confirmed by using Fourier transform infrared reflection (FTIR) spectroscopy, grazing incidence X-ray diffraction (GI-XRD) and scanning electron microscope (SEM) equipped with energy dispersive X-ray spectrometer. Development of an apatite structure on the surface of the SBF treated glass samples as functions of composition and time could be established using the GI-XRD data. FTIR spectra of the glasses treated in SBF show features at characteristic vibration frequencies of apatite after 1-day of immersion in SBF. SEM observations revealed that the spherical particles formed on the glass surface were made of calcium and phosphorus with the Ca/P molar ratio being close to 1.67, corresponding to the value in crystalline apatite. Increase in bioactivity with increasing zinc-iron oxide content was observed. The results have been used to understand the evolution of the apatite surface layer as a function of glass composition and immersion time in SBF.     

Microstructure and interfacial properties of HfO2-Al2O3 nanolaminate films

High-k HfO₂-Al₂O₃ composite gate dielectric thin films on Si(1 0 0) have been deposited by means of magnetron sputtering. The microstructure and interfacial characteristics of the HfO₂-Al₂O₃ films have been investigated by using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and spectroscopic ellipsometry (SE). Analysis by XRD has confirmed that an amorphous structure of the HfO₂-Al₂O₃ composite films is maintained up to an annealing temperature of 800 °C, which is much higher than that of pure HfO₂ thin films. FTIR characterization indicates that the growth of the interfacial SiO₂ layer is effectively suppressed when the annealing temperature is as low as 800 °C, which is also confirmed by spectroscopy ellipsometry measurement. These results clearly show that the crystallization temperature of the nanolaminate HfO₂-Al₂O₃ composite films has been increased compared to pure HfO₂ films. Al₂O₃ as a passivation barrier for HfO₂ high-k dielectrics prevents oxygen diffusion and the interfacial layer growth effectively.     

Surface functionalization, morphology and thermal properties of polyamide6/O-MMT composite nanofibers by Fe2O3 sputter coating

In the present work, the pure polyamide6 (PA6) nanofiber and PA6/organically modified montmorillonite (O-MMT) composite nanofiber were firstly prepared by a facile compounding process with electrospinning, and then coated by nanosize Fe₂O₃ using magnetron sputter technique. The effects of Fe₂O₃ sputter coating on structures, surface morphology and thermal stability were characterized by scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX), atomic force microscope (AFM) and thermogravimetric analyses (TGA), respectively. The SEM images showed that the diameters of composite nanofiber were decreased with the loadings of O-MMT and the nanosize Fe₂O₃ is well coated on the surface of the homogeneous and cylindrical nanofibers. The XPS spectra reflected the chemical features of the deposited nanostructures. The EDX confirmed the presence of the O-MMT and Fe₂O₃ in the fibers. The AFM observation revealed that there was a remarkable difference in the surface morphology of composite nanofiber before and after sputter coating. The TGA analysis indicated the barrier effects of silicate clay layers and catalysis effects of Fe₂O₃ improved thermal stability properties of the composite nanofiber.     

Structure and electronic properties calculation of ultrathin α-Al2O3 films on (0 0 0 1) α-Cr2O3 templates

Ab initio total energy Hartree-Fock calculations of ultrathin films of α-Al₂O₃ on (0 0 0 1) α-Cr₂O₃ templates are presented. The surface relaxation, the in-plane reconstruction and the surface and strain energies of the slabs are studied as a function of alumina film thickness. The surface Al layer is found to relax inwards considerably, with the magnitude of the inwards relaxation depending on the thickness of the ultrathin alumina film in a non-linear manner. The calculations also reveal that ultrathin films of alumina lower the surface energy of (0 0 0 1) α-chromia substrates. This indicates that the (0 0 0 1) α-chromia surface provides favourable conditions for the templated growth of α-alumina. However, increasing the alumina film thickness is found to give rise to a significant increase in strain energy. Finally, the electronic properties at the surface of the (0 0 0 1) α-Al₂O₃/α-Cr₂O₃ slabs are investigated. Here it is found that the alumina coating gives rise to an increase in the covalency of the bonds at the surface of the slabs. In contrast, the influence of an alumina layer on the electrostatic potential at the surface of the chromia slab is relatively minor, which should also be beneficial for the templated growth of α-alumina on (0 0 0 1) α-chromia substrates.     

Features of the local structural disorder in Li2O-CaF2-P2O5 glass-ceramics with Cr2O3 as nucleating agent

Li₂O-CaF₂-P₂O₅ glasses mixed with different concentrations of Cr₂O₃ (ranging from 0 to 1.0 mol%) were crystallized. The samples were characterized by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy (EDS), differential thermal analysis and conventional spectroscopic techniques. The X-ray diffraction and scanning electron microscopic studies reveal the presence of lithium phosphate, calcium phosphate and chromium phosphate (complexes of Cr³⁺, Cr⁵⁺ and Cr⁶⁺ ions) crystal phases. The study on DTA suggests that the crystallization is predominantly due to the surface crystallization when the concentration of nucleating agent Cr₂O₃ is around 0.8 mol%. The IR and Raman spectral studies of these samples indicate that the sample crystallized with 0.8 mol% Cr₂O₃ is more compact and possesses high rigidity due to the presence of chromium ions largely in tetrahedral positions.     

Chemical synthesis of spinel nickel ferrite (NiFe2O4) nano-sheets

The present investigation is related to the deposition of single-phase nano-sheets spinel nickel ferrite (NiFe₂O₄) thin films onto glass substrates using a chemical method. Nano-sheets nickel ferrite films were deposited from an alkaline bath containing Ni²⁺ and Fe²⁺ ions. The films were characterized for their structural, surface morphological and electrical properties by means of X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and two-point probe electrical resistivity techniques. The X-ray diffraction pattern showed that NiFe₂O₄ nano-sheets are oriented along (3 1 1) plane. The FT-IR spectra of NiFe₂O₄ films showed strong absorption peaks around 600 and 400 cm⁻¹ which are typical for cubic spinel crystal structure. Microstructural study of NiFe₂O₄ film revealed nano-sheet like morphology with average sheet thickness of 30 nm. The room temperature electrical resistivity of the NiFe₂O₄ nano-sheets was 10⁷ Ω cm.     

Preparation and characterization of the electrodeposited Cr-Al2O3/SiC composite coating

To increase the SiC content in Cr-based coatings, Cr-Al₂O₃/SiC composite coatings were plated in Cr(VI) baths which contained Al₂O₃-coated SiC powders. The Al₂O₃-coated SiC composite particles were synthesized by calcining the precursor prepared by heterogeneous deposition method. The transmission electron microscopy analysis of the particles showed that the nano-SiC particle was packaged by alumina. The zeta potential of the particles collected from the bath was up to +23 mV, a favorable condition for the co-deposition of the particles and chromium. Pulse current was used during the electrodeposition. Scanning Electron Microscopy (SEM) indicated that the coating was compact and combined well with the substrate. Energy dispersive X-ray analysis of Cr-Al₂O₃/SiC coatings demonstrated that the concentration of SiC in the coating reached about 2.5 wt.%. The corrosion behavior of the composite coating was studied by potentiodynamic polarization and electrochemical impedance spectroscopy techniques. The data obtained suggested that the Al₂O₃/SiC particles significantly enhanced the corrosion resistance of the composite coating in 0.05 M HCl solution.     

Growth and characterization of Y2O3 thin films

Y₂O₃ thin films were grown on silicon (1 0 0) substrates by pulsed-laser deposition at different substrate temperatures and O₂ pressures. The structure and composition of films are studied by using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The Y₂O₃ thin films deposited in vacuum strongly oriented their [1 1 1] axis of the cubic structure and the film quality depended on the substrate temperature. The magnitude of O₂ pressure obviously influences the film structure and quality. Due to the silicon diffusion and interface reaction during the deposition, yttrium silicate and SiO₂ were formed. The strong relationship between composition and growth condition was discussed.     

A study on the luminescence properties of CaAl2B2O7:Eu phosphor

The blue-emitting CaAl₂B₂O₇:Eu²⁺ phosphor was prepared at 800 °C by a modified solid-state reaction. The results of X-ray powder diffraction (XRD) analysis confirmed the formation of CaAl₂B₂O₇:Eu²⁺. Photoluminescence (PL) spectroscopy showed that the phosphor could be excited efficiently by UV-vis light from 250 to 410 nm, and exhibit blue emission (460 nm). The emission intensity of CaAl₂B₂O₇:Eu²⁺ phosphor varies with the increase of Eu²⁺concentration. The mechanism of resonance-type energy transfer from Eu²⁺ to Eu²⁺ was established to be electric multipole-multipole interaction. TEM images showed that the grain size of CaAl₂B₂O₇:Eu²⁺ is about 45 nm, which is in full agreement with the theoretical calculation data from the XRD patterns.     

Surface chemistry and catalytic activity of Ni/Al2O3 irradiated with high-energy electron beam

The radiation effects induced effects by electron beam (EB) treatment on the catalytic activity of Ni/γ-Al₂O₃ were studied for the carbon dioxide reforming of methane with different EB energy and absorbed radiation dose. Transmission electron microscope (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to determine the change in structure and surface states of Ni/γ-Al₂O₃ catalyst before and after the EB treatment. Higher energy EB treatment is useful for increasing the proportion of the active sites (such as Ni⁰ and NiAl₂O₄-phase) on the surface. The increase of Ni/Al-ratio indicates that the Ni dispersion on the surface increased with the EB-treatment, resulting in an increase of the active sites, which leads to improving the catalytic activity. XPS measurement also showed a decrease of the surface carbon with EB dose. The maximum 20% increase in the conversion of CO₂/CH₄-mixture into CO/H₂ gas was observed for the catalyst treated with 2 MeV energy and 600 kGy dose of EB relative to untreated.     

Influence of postdeposition annealing on structural properties and electrical characteristics of thin Tm2O3 and Tm2Ti2O7 dielectrics

We describe the structural properties and electrical characteristics of thin thulium oxide (Tm₂O₃) and thulium titanium oxide (Tm₂Ti₂O₇) as gate dielectrics deposited on silicon substrates through reactive sputtering. The structural and morphological features of these films were explored by X-ray diffraction, X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and atomic force microscopy, measurements. It is found that the Tm₂Ti₂O₇ film annealed at 800 °C exhibited a thinner capacitance equivalent thickness of 19.8 Å, a lower interface trap density of 8.37 × 10¹¹ eV⁻¹ cm⁻², and a smaller hysteresis voltage of ∼4 mV than the other conditions. We attribute this behavior to the Ti incorporated into the Tm₂O₃ film improving the interfacial layer and the surface roughness. This film also shows negligible degrees of charge trapping at high electric field stress.     

Photocatalytic property of TiO2 thin films sputtered-deposited on unheated substrates

TiO₂ films deposited on unheated substrates of alumina silicate glass by rf. (13.56 MHz) magnetron sputtering in the mixture of O₂ and Ar gases have been studied with X-ray diffraction (XRD), Atomic Force Microscopy (AFM) and optical spectroscopy. Structural and optical properties of TiO₂ films deposited at different O₂ concentrations and total pressures have been analyzed. Photocatalytic properties of TiO₂ films were characterized by following the degradation of methylene blue molecules under UV irradiation. It was found that the rate of methylene blue decomposition strongly depends on morphology and crystallinity of the deposited films, namely on the content of the anatase phase and on the size of the anatase grains. The best photocatalytic activity was found on TiO₂ films consisting of pure anatase phase with the size of grains of about 450 Å. With the help of those films a thin film reactor for water purification has been designed and tested.     

One-dimensional structures of Bi2O3 synthesized via metalorganic chemical vapor deposition process

We have demonstrated the synthesis of one-dimensional (1D) structures of bismuth oxide (Bi₂O₃) by a reaction of a trimethylbismuth (TMBi) and oxygen (O₂) mixture at 450 °C. Scanning electron microscopy showed that the product consisted of 1D materials with width or diameters less than 1 μm and lengths up to several tens of micrometers. The X-ray energy dispersive spectroscopy revealed that the materials contained elements of Bi and O. The results of X-ray diffraction and selected area electron diffraction pattern indicated that the obtained Bi₂O₃ were crystalline with monoclinic structure.     

Microwave assisted combustion synthesis of CdFe2O4: Magnetic and electrical properties

CdFe₂O₄ particles were synthesized by the microwave assisted combustion method using two different fuels—glycine and urea. Microwave heating provides higher chemical yield within a minute. The synthesized particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), ac impedance spectroscopy, vibrating sample magnetometry (VSM) and electron spin resonance (ESR) methods. XRD analysis shows the cubic structure of CdFe₂O₄. The high and low frequency absorption bands of CdFe₂O₄ were found using FTIR analysis. Spherical morphology was revealed from the SEM images. ESR and VSM measurements reveal the antiferromagnetic behavior of CdFe₂O₄. The electrical conductivities of CdFe₂O₄ synthesized using glycine and urea are 6.5×10⁻⁷ S cm⁻¹ and 4.7×10⁻⁸ S cm⁻¹ respectively at 240 ^oC. At elevated temperatures an occurrence of increase in conductivity was observed, which indicates the semiconducting behavior of CdFe₂O₄. The dielectric spectral analysis reveals that dielectric constant of CdFe₂O₄ decreases with frequency and increases with temperature.     

Structure and electrical properties of CdIn2O4 thin films prepared by DC reactive magnetron sputtering

CdIn₂O₄ thin films were prepared by direct-current (DC) reactive magnetron sputtering. The structure, surface morphology and the chemical composition of the thin films were analyzed by X-ray diffraction (XRD), atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS), respectively. The electrical properties of the films prepared in different oxygen concentration and annealing treatment were determined, and the effects of the preparing conditions on the structure and electrical properties were also explored. It indicates that the CdIn₂O₄ thin films with uniform and dense surface morphology contain mainly CdIn₂O₄, In₂O₃ phases, and CdO phase is also observed. The XPS analysis confirms the films are in oxygen-deficient state. The electrical properties of these films significantly depend on the preparing conditions, the resistivity of the films with the oxygen concentration of 4.29% is 2.95 × 10⁻⁴ Ω cm and the Hall mobility is as high as 60.32 cm²/V s. Annealing treatment can improve the electrical performance of the films.     

Low-temperature synthesis and growth of superparamagnetic Zn0.5Ni0.5Fe2O4 nanosized particles

Mono-disperse spinel Ni_0.5Zn_0.5Fe₂O₄ nanosized particles have been synthesized via a hydrothermal method at low temperature. X-ray diffraction (XRD), transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM) analysis indicated that the synthesized nanocrystals were of pure cubic spinel structure with the size about 6-20 nm. The activation energy of grain growth is 35.06 kJ/mol experimented by the Arrhenius equation. A primary experimental model was put forward to shed light on the growth mechanism of crystallined spinel Ni-Zn ferrite nanosized particles under hydrothermal conditions. The magnetic measurements shows that the prepared Ni_0.5Zn_0.5Fe₂O₄ nanoparticle possess good superparamagnetic behavior.