Preparation and combustion properties of α-Fe2O3 coated Zr particles

Zirconium particles with irregular morphology and broad size distribution were uniformly coated by spherical α-Fe₂O₃ crystal grain via a facile route without polymer or surfactant as directing agents. The synthesized α-Fe₂O₃/Zr composite particles were characterized by X-ray diffraction, scanning electron microscopy, energy dispersion X-ray, UV-vis spectroscopy and Raman spectroscopy. The synthesis mechanism could be explained by cooperated heterogeneous nucleation and solid state transformation reaction. The combustion properties of α-Fe₂O₃/Zr composite particles were investigated. Compared with Zr particles, the combustion lasting time decreased from 16 s of Zr particles to 0.13 s of α-Fe₂O₃/Zr composite particles, and the top point of temperature reached in combustion increased from 2004 °C of Zr particles to 2378 °C of α-Fe₂O₃/Zr particles.     

Synthesis, crystal structure and thermal decomposition of [La2(CH3CH2COO)6·(H2O)3]·3.5H2O precursor for high-k La2O3 thin films deposition

Lanthanum acetylacetonate La(C₅H₇O₂)₃·xH₂O has been used in the preparation of the precursor solution for the deposition of polycrystalline La₂O₃ thin films on Si(1 1 1) single crystalline substrates. The precursor chemistry of the as-prepared coating solution, precursor powder and precursor single crystal have been investigated by Fourier Transformed Infrared Spectroscopy (FTIR), differential thermal analysis coupled with quadrupole mass spectrometry (TG-DTA-QMS) and X-ray diffraction. The FTIR and X-ray diffraction analyses have revealed the complex nature of the coating solution due to the formation of a lanthanum propionate complex. The La₂O₃ thin films deposited by spin coating on Si(1 1 1) substrate exhibit good morphological and structural properties. The films heat treated at 800 °C crystallize in a hexagonal phase with the lattice parameters a = 3,89 Å and c = 6.33 Å, while at 900 °C the films contain both the hexagonal and cubic La₂O₃ phase.     

Phase stabilization and microstructural studies of lead lanthanum titanate thin films

Thin ferroelectric films of PLTx (Pb_1−xLa_xTi_1−x/4O₃) have been prepared by a sol-gel spin coating process. As deposited films were thermally treated for crystallization and formation of perovskite structure. Characterization of these films by X-ray diffraction (XRD) have been carried out for various concentrations of La (x = 0.04, 0.08 and 0.12) on ITO coated corning glass substrates. For a better understanding of the crystallization mechanism, the investigations were carried out on films annealed at temperatures (350, 450, 550 and 650 °C). Characterization of these films by X-ray diffraction shows that the films annealed at 650 °C exhibit tetragonal phase with perovskite structure. Atomic force microscope (AFM) images are characterized by slight surface roughness with a uniform crack free, densely packed structure. Fourier transform infrared spectra (FTIR) studies of PLTx thin films (x = 0.08) deposited on Si substrates have been carried out to get more information about the phase stabilization.     

α-MoO3 nanocrystals of controlled size on a glass substrate

A procedure to grow α-MoO₃ nanocrystals of rod and belt forms under mild conditions involved deposition onto a glass substrate via vapor transport with a water-soluble precursor. Scanning electron and transmission electron microscopic studies, selected-area electron diffraction and powder X-ray analyses indicate that these α-MoO₃ nanocrystals exhibit rod or belt forms that grow along [0 0 1] and became vertically aligned on the glass substrate. Such deposition is effective to form thin films of controllable size and density of coverage on varying the precursor concentration and the duration of deposition.     

Microwave-assisted synthesis and humidity sensing of nanostructured α-Fe2O3

Nanocrystalline α-Fe₂O₃ has been prepared on a large-scale by a facile microwave-assisted hydrothermal route from a solution of Fe(NO₃)₃·9H₂O and pentaerythritol. A systematic study of the morphology, crystallinity and oxidation state of Fe using different characterization techniques, such as transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy was performed. It reveals that nanostructured α-Fe₂O₃ comprises bundles of nanorods with a rhombohedral crystalline structure. The individual nanorod has 8-10 nm diameter and ∼50 nm length. The as-prepared nanostructured α-Fe₂O₃ (sensor) gives selective response towards humidity. The sensor shows high sensitivity, fast linear response to change in the humidity with almost 100% reproducibility. The sensor works at room temperature and rejuvenates without heat treatment. The as-prepared nanostructured α-Fe₂O₃ appears to be a promising humidity sensing material with the potential for commercialization.     

Crystallization kinetics and thermal properties of 20Li2O-80TeO2 glass

In this work, X-ray diffraction, Raman spectroscopy and differential scanning calorimetry techniques were used to understand the crystallization process on 20Li₂O-80TeO₂ glass. X-ray diffraction results reveal the presence of three distinct alpha γ-TeO₂, α-TeO₂ and α-Li₂Te₂O₅ crystalline phases in the glass matrix. The Raman spectroscopy band structure of this glass is similar to the one observed in glassy TeO₂. Raman results clearly reveal the metastable character of the γ-TeO₂ phase in the 20Li₂O-80TeO₂ glass, whose associated vibration modes disappear completely at temperatures higher than 315 °C. On the other hand, the Raman modes associated to α-TeO₂ and α-Li₂Te₂O₅ phases persists up to temperatures close to the final stages of the crystallization in the studied glass (around 420 °C). From DSC measurements, the activation energies 296 ± 3 and 298 ± 1 kJ mol⁻¹ were associated to γ-TeO₂ and α-TeO₂ phases crystallization, indicating that these phases crystallizes at temperatures very close in the studied glass.     

Stress-induced shifting of the morphotropic phase boundary in sol-gel derived Pb(Zr0.5Ti0.5)O3 thin films

The structure evolution of Pb(Zr_0.5Ti_0.5)O₃ thin films with different thicknesses on the Pt(1 1 1)/Ti/SiO₂/Si substrates has been investigated using X-ray diffraction and Raman scattering. Differing from Pb(Zr_0.5Ti_0.5)O₃ bulk ceramic with a tetragonal phase, our results indicate that for PZT thin films with the same composition monoclinic phase with Cm space group coexisting with tetragonal phase can appear. It is suggested that tensile stress plays a role in shifting the morphotropic phase boundary to titanium-rich region in PZT thin films. The deteriorated ferroelectric properties of PZT thin films can be attributed mainly to the presence of thin non-ferroelectric layer and large tensile stress.     

Growth and characterization of electrosynthesized iron selenide thin films

Iron selenide (FeSe) thin films were electrodeposited onto indium doped tin oxide coated conducting glass (ITO) substrates at various bath temperatures from 30 °C to 90 °C in an aqueous electrolytic bath containing FeSO₄ and SeO₂. The deposition mechanism was investigated using cyclic voltammetry. The appropriate potential region where the formation of stoichiometric iron selenide thin films' occurs was found to be −1100 mV versus SCE. X-ray diffraction studies revealed that the deposited films are found to be hexagonal structure with a preferential orientation along (002) plane. The parameters such as crystallite size, strain, dislocation density are calculated from X-ray diffraction studies. Optical absorption measurements were used to estimate the band gap value of iron selenide thin films deposited at various bath temperatures. Scanning electron microscopy (SEM) was used to study the surface morphology. The composition of FeSe thin films was analyzed using an energy dispersive analysis by X-rays (EDX) set up attached with scanning electron microscopy. Preliminary studies for photoelectrochemical solar cells based on iron selenide thin films were carried out and the experimental observations are discussed.     

Thin films of iron oxide by low pressure MOCVD using a novel precursor: tris(t-butyl-3-oxo-butanoato)iron(III)

Deposition of thin films of iron oxide on glass has been carried out using a novel precursor, tris(t-butyl-3-oxo-butanoato)iron(III), in a low-pressure metalorganic chemical vapor deposition (MOCVD) system. The new precursor was characterized for its thermal properties by thermogravimetry and differential thermal analysis. The films were characterized by X-ray diffraction (XRD), transmission electron microscopy, scanning electron microscopy, and by optical measurements. XRD studies reveal that films grown at substrate temperatures below ∼550 °C and at low oxygen flow rates comprise only the phase Fe₃O₄ (magnetite). At higher temperatures and at higher oxygen flow rates, an increasing proportion of α-Fe₂O₃ is formed along with Fe₃O₄. Films of magnetite grown under different reactive ambients—oxygen and nitrous oxide—have very different morphologies, as revealed by scanning electron microscopic studies.     

Structural studies of Fe2O3-Bi2O3-CdO glass system

xFe₂O₃·(100 − x)[Bi₂O₃·CdO] system with 0 ≤ x ≤ 50 mol% was prepared and investigated by X-ray diffraction, density, FT-IR and Raman spectroscopies. The XRD patterns confirm the formation of a vitreous structure for x < 35 mol% Fe₂O₃. The evolution of density and molar volume with the addition and increasing of iron content indicates structural changes in the structure of Bi₂O₃·CdO glass matrix. The FT-IR spectrum of the glass matrix reveals a structure realized from BiO₃ pyramidal and BiO₆ octahedral units. With the addition of iron the structure proposed by the glass matrix is changing by the appearance of FeO₄ units. Also the existence of FeO₆ units cannot be excluded. The Raman spectra suggest a structure build from BiO₆ octahedral units. By Raman scattering the presence of structural units characteristic to Fe₂O₃ was not directly observed but the evolution of the spectra is dependent of the iron content.     

Electrodeposited nanostructured α-Fe2O3 thin films for solar water splitting: Influence of Pt doping on photoelectrochemical performance

Electrochemically deposited α-Fe₂O₃ thin films, whose composition was tuned by Pt doping, were investigated as photoanode for photoelectrochemical water splitting. Morphological and structural characteristics of the nanostructured α-Fe₂O₃ thin films were studied by scanning electron microscopy and X-ray diffraction techniques. The films were characterized by Raman spectroscopy and X-ray photoelectron spectroscopy to determine the effect of Pt doping on the α-Fe₂O₃ structure. The photoelectrochemical performance of the films was examined by linear sweep voltammetry and electrochemical impedance spectroscopy. Results of these studies showed that Pt doping increased the density of small-sized nanoparticles in α-Fe₂O₃ thin films. The Pt doped films exhibited higher photoelectrochemical activity by a factor of 1.4 over un-doped α-Fe₂O₃ films. The highest photocurrent density of 0.56 mA cm⁻² was registered for 3% pt doped film at 0.4 V versus Ag/AgCl in 1 M NaOH electrolyte and under standard illumination conditions (AM 1.5 G, 100 mW cm⁻²). This high photoactivity can be attributed to the high active surface area and increased donor density caused by Pt doping in the film. Electrochemical impedance analysis also revealed significantly low charge transfer resistance of Pt doped films, indicating its superior electrocatalytic activity for water splitting reaction compared to un-doped α-Fe₂O₃ thin films.     

α-Fe2O3 as an anode material with capacity rise and high rate capability for lithium-ion batteries

We report a simple molten salt method to prepare nanosize α-Fe₂O₃, as well as its electrochemical performance as anode material for lithium ion batteries. The structure and morphology were confirmed by Raman spectroscopy, X-ray diffraction, and transmission electron microscopy. The as-prepared α-Fe₂O₃ is a rhombohedral phase of hematite with crystal size in the range of 20-40 nm. The electrochemical measurements were performed using the as-prepared powders as the active material for a lithium-ion cell. The nanosized α-Fe₂O₃ shows excellent cycling performance and rate capability. It also exhibits the feature of capacity increase upon cycling. The outstanding electrochemical performance of the α-Fe₂O₃ can be related to several factors, namely, the short Li⁺ diffusion length along the porous rhombohedral structures and the nanosized nature of the materials, which decreases the traverse time for electrons and Li⁺ ions, and reduces the volume expansion to some extent during charge/discharge reactions.     

Electrodeposition of As2Se3 thin films

Semiconducting As₂Se₃ thin films have been prepared from an aqueous bath at room temperature onto stainless steel and fluorine-doped tin oxide (F.T.O.)-coated glass substrates using an electrodeposition technique. It has been found that As₂O₃ and SeO₂ in the volumetric proportion as 4:6 and their equimolar solutions of 0.075 M concentration forms good quality films of As₂Se₃. The films are annealed in a nitrogen atmosphere at temperature of 200 °C for 2 h. The films are characterised by scanning electron microscopy, X-ray diffraction and optical absorption techniques. Studies reveal that asdeposited and annealed thin films are polycrystalline in nature. The optical band gap has been found to be 2.15 eV for the above-mentioned composition and concentration of the film.     

Thin film growth of boron nitride on α-Al2O3 (0 0 1) substrates by reactive sputtering

Boron nitride thin films were grown on α-Al₂O₃ (0 0 1) substrates by reactive magnetron sputtering. Infrared attenuated total reflection (ATR) spectra of the films gave an intense signal associated with in-plane B-N stretching TO mode of short range ordered structure of BN hexagonal sheets. X-ray diffraction for the film prepared at a low working pressure (ca. 1 × 10⁻³ Torr) gave a diffraction peak at slightly lower angle than that corresponding to crystal plane h-BN (0 0 2). It is notable that crystal thickness calculated from X-ray peak linewidth (45 nm) was close to film thickness (53 nm), revealing well developed sheet stacking along the direction perpendicular to the substrate surface. When the substrates of MgO (0 0 1) and Si (0 0 1) were used, the short-range ordered structure of h-BN sheet was formed but the films gave no X-ray diffraction. The film showed optical band gap of 5.9 eV, being close to that for bulk crystalline h-BN.     

Fabrication and characterization of Fe3O4 thin films deposited by reactive magnetron sputtering

Fe-O thin films with different atomic ratio of iron to oxygen were deposited on glass and thermally oxidized silicon substrates at temperatures of 300, 473 and 593 K, by reactive magnetron sputtering in Ar+O₂ atmosphere. The composition and structure of the thin films were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and electrical resistivity. It was found from XRD that with increasing the oxygen partial pressure in the working gas, the crystalline structure of the Fe-O films deposited at the substrate temperature of 473 K gradually changed from α-Fe, amorphous Fe-O, Fe₃O₄, γ-Fe₂O₃ to Fe_21.34O₃₂. The structure and chemical valence of the Fe₃O₄ films were analyzed by electron microscopy and XPS, respectively.     

Chemical vapor deposition growth of Fe3O4 thin films and Fe/Fe3O4 bi-layers for their integration in magnetic tunnel junctions

A possible route for the synthesis of Fe₃O₄, Fe, and Fe/Fe₃O₄ bi-layers with chemical vapor deposition by employing the same Fe₃(CO)₁₂ carbonyl precursor is presented. The comprehensive structural, chemical, and morphological investigation of the as-deposited thin single films and bi-layers is performed by X-ray diffraction, X-ray reflectivity, Raman spectroscopy, and time-of-flight secondary ion mass spectrometry depth profiling. We present the possibility of performing the deposition of pure metallic Fe and Fe₃O₄/γ-Fe₂O₃ by adjusting the deposition pressure from 10^- 3/^- 4 Pa to 1 Pa, respectively. The integration of Fe₃O₄ thin films in a magnetic tunnel junction stack fully synthesized by in situ atomic layer and chemical vapor deposition processes is also presented, showing good stack stability and marginal interdiffusion.     

A photochemical method for the preparation of indium oxide and indium-cobalt oxides thin films

Indium oxide and indium-cobalt oxide thin films have been successfully prepared by direct UV irradiation of amorphous films of β-diketonate complexes on Si(1 0 0) substrates. Deposited films were characterized by X-ray diffraction, Auger electron spectroscopy and X-ray photoelectron spectroscopy. The surface morphology of the films, examined by atomic force microscopy and scanning electron microscopy, revealed that mixed indium-cobalt oxide films are much smoother than In₂O₃ films, with rms surface roughness of 7.24 and 26.1 nm, respectively.     

A mild solvothermal route to α-Fe2O3 nanoparticles

A mild solvothermal route has been developed to synthesize α-Fe₂O₃ nanoparticles using Fe(NO₃)₃ as a starting material. The results from XRD and TEM indicate the α-Fe₂O₃ powders possess a rhombohedrally centered hexagonal structure, and the size of particles from alcohothermal method at 160 °C is about 50-100 nm.     

Dip coated 12CaO·7Al2O3 thin films through sol-gel process using metal alkoxide

Transparent nanostructured 12CaO·7Al₂O₃ thin films with cubic structure have been prepared on soda lime glass substrates via the sol-gel dip coating using the precursor sol solution at low temperature. The structural, compositional, morphological and optical properties of the 12CaO·7Al₂O₃ films and powder were studied using X-ray diffractometry (XRD), X-ray photoelectron spectroscopy, scanning electron microscopy (SEM) and atomic force microscopy. Optical properties of 12CaO·7Al₂O₃ films have been investigated using UV-visible spectroscopy. Two different precursor sols were prepared using calcium-2-ethyl hexonate and aluminium isopropoxide as precursor materials in isopropanol and ethylene glycol monomethyl ether solvents. Dip coated gel like films were dried at 120 °C for 15 min and subsequently heat-treated at 450 °C for 1 h in air atmosphere. The influence of films thickness and optical transparency with use of different solvent and sol concentration on microstructure of the films were established. In addition, XRD patterns revealed that 12CaO·7Al₂O₃ films have been composed of cubic phase. SEM observations exhibited that the films structure becomes more homogeneous using isopropanol as compared to ethylene glycol monomethyl ether solvent. The 12CaO·7Al₂O₃ films prepared using 2 (wt.%) sol in isopropanol had high transparency nearly 88% in wide visible range with maximum of 90% at 600 nm wavelength.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.