Ultrasonochemical coating and characterization of TiO2-coated zirconia fine particles

Zirconia fine particles were prepared by ultrasonic spray pyrolysis (USP) and employed as a substrate for titanium/titania coating by ultrasonochemistry. The effects of several process factors on the characteristics of the prepared particles were investigated and the particles were then characterized by various techniques. This substrate was coated with various titanium concentrations (0.025–0.1 M) for two ultrasonication time periods (30 min, 2 h) by sonochemistry, and finally calcined at 1100 °C. Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), particle size analysis (PSA), Fourier transformation infrared spectroscopy (FT-IR) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) comprised the techniques used to characterize them. The particles were prepared in a monodispersed spherical form with no interior cavity; their average size was shown to be 0.62 μm before calcination and 2.57 μm after calcination. The titania surface coating acted to partially stabilize the particles to a tetragonal phase. Based on the analytical results, the optimum conditions for preparing the particles were shown to be 7.5 wt% of titania as an initial solution concentration and 0.5 h of coating time.     

Microstructure evolution of Ti3SiC2 powder during high-energy ball milling

Ti₃SiC₂ powder was milled by high-energy ball milling under argon atmosphere and subsequently thermally annealed. The microstructure evolution of Ti₃SiC₂ after milling was investigated. It was found that 200 nm particle size Ti₃SiC₂ powder could be achieved by 9 h milling whereas a longer milling time would induce Ti₃SiC₂ decomposition. After 18 h milling, the particle size gradually decreased to 150 nm and TiC appeared in the XRD pattern. It is suggested that the collision of the milling balls triggered the formation of TiC from the amorphous phase which was generated in the milling process.     

Formation of TiC particle during carbothermal reduction of TiO2

Formation of TiC particle during carbothermal reduction of titanium dioxide (TiO₂) was investigated. The mixture with TiO₂ and carbon resin was reacted at 1500 °C for 0–45 min under flowing Argon atmosphere. The powders were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The partially reduced TiO₂ particles were conglomerated in the initial stage of the reduction and the size of this conglomerate ranged from 500 to 1000 nm. After the complete reaction between Ti as a reduction product and C, the large conglomerates separated to homogeneous and fine TiC particles with a size of 80 nm.     

Preparation and microwave absorption properties of Fe-doped SiC powder obtained by combustion synthesis

Fe-doped SiC powders were synthesized via combustion reaction of the Si and C system in a 0.1 MPa nitrogen atmosphere using iron as the dopant. The prepared powders have fine spherical particles and narrow particle size distribution. The electric permittivities of SiC samples were determined in the frequency range of 8.2–12.4 GHz. Results show that the permittivity of SiC increases with the increasing iron contents. The 5% Fe-doped SiC powder with 2 mm or 2.5 mm thickness exhibits the best microwave absorption over the frequencies ranging from 8.2 to 12.4 GHz.     

Synthesis of fine dispersed titanium diboride from nanofibrous carbon

This paper presents the experimental data on the synthesis of titanium diboride (TiB₂) fine dispersed powder carried out in laboratory scale. TiB₂ powder was prepared by the reduction of titanium dioxide with boron carbide and nanofibrous carbon in an argon atmosphere. The powders of TiB₂ were characterized by X-ray diffraction (XRD), elemental analyses, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), low-temperature nitrogen adsorption, particle size analysis, simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC). The resulting material contains a single phase – titanium diboride. The particles of the powder were predominantly aggregated. The average size of the particles and the aggregates were 7.4–8.0 µm with a wide size of distribution. The specific surface values of samples obtained were 2.4–5.8 m²/g. The oxidation of titanium diboride began from the temperature of 450 °C. In this work, the optimal synthesis conditions were estimated: the molar ratio was TiO₂:B₄C:C=2:1:3 (according to stoichiometry), the temperature was 1600 °C, the process duration was 20–30 min.     

Effect of calcination temperature on structural,vibrational, optical,and rheological properties of zirconia nanoparticles

ZrO₂ nanoparticles (NPs) were prepared by a simple, versatile, and an efficient methodology based on microwave. The synthesized NPs were calcined at temperatures ranging from 100 °C to 600 °C. The samples were characterized by X-ray powder diffraction (XRD), transmission electron microscope (TEM), FT-IR spectroscopy, Far-IR spectroscopy, Raman spectroscopy, and UV-vis absorption spectroscopy. The results clearly showed the presence of purely monoclinic phase of zirconia when the calcination temperature exceeds 400 °C. The experimental results showed that the viscosity of zirconia NPs in ethylene glycol (EG) increases with increasing the particle volume fraction and decreases with increasing temperature.     

Ultrasonic dispersion of nano TiC powders aided by Tween 80 addition

Nano TiC powders were dispersed in aqueous media. Effects of ultrasonic treatment and Tween 80 addition on dispersion of TiC powders were investigated. The results showed that ultrasonic treatment had a large effect on the dispersion of nano TiC powders, and 30 min of ultrasonic treatment was necessary for fine dispersion from TEM images and particle size measurement. Tween 80 was selected as the dispersant. Sedimentation test indicated that 0.5 vol.% was the optimum addition level of Tween 80 in TiC suspension. FTIR spectrum proved the adsorption of Tween 80 on the surface of nano TiC powders. XPS analysis revealed the existence of TiO₂ on the TiC powder surface, which led to a hydroxylated surface during dispersion. In the presence of Tween 80 in the solution, zeta potential values became more negative. Both electrostatic stabilization and steric stabilization were deduced to be the main mechanisms for well dispersion of the nano TiC powders in aqueous media.     

Iron modified titanium–hafnium binary oxides as catalysts in total oxidation of ethyl acetate

Multicomponent iron–titanium–hafnium oxide materials with different compositions were prepared by combination of homogeneous precipitation with urea and incipient wetness impregnation techniques and tested as catalysts for ethyl acetate oxidation as representative VOCs. Nitrogen physisorption, XRD, Raman, UV–Vis, XPS, Mössbauer spectroscopy and TPR analyses reveal co-existence of substituted Fe_xTi_1 − xO₂ oxide, finely dispersed iron oxide species with supper paramagnetic behavior and well crystallized α-Fe₂O₃ particles, which relative part depends on hafnium content in titania lattice. The effect of phase composition on the catalytic behavior of these materials in ethyl acetate oxidation was discussed.     

Production of TiB2 by SHS and HCl leaching at different temperatures: Characterization and investigation of sintering behavior by SPS

Sub-micron sized TiB₂ ceramic powders were prepared via self-propagating high-temperature synthesis (SHS) followed by HCl leaching at different temperatures. Purified powders obtained using optimum process parameters were consolidated by field assisted sintering technology/spark plasma sintering (FAST/SPS) technique. Phase and microstructural analyses of both the powder and sintered samples were carried out by X-ray diffractometer (XRD) and scanning electron microscope (SEM). The chemical analyses and particle size measurements of the specimen were conducted by inductively coupled plasma-mass spectrometry (ICP-MS) and dynamic light scattering (DLS) techniques. The final properties of the sintered sample were determined in terms of density and microhardness. The effects of different HCl leaching temperatures on the formation, microstructure, particle size, purity and sintering behavior of the SHS-produced TiB₂ powders were investigated. The SHS reaction of TiO₂-B₂O₃-Mg powders as a starting mixture yielded MgO, Mg₃(BO₃)₂ and Mg beside the desired phase TiB₂. All three magnesium containing by-products were completely removed by performing hot HCl leaching. TiB₂ powders after SHS reaction and leaching with 9.3 M HCl for 30 min at 80 °C revealed a minimum purity of 98.4% and a homogenous particle size distribution with an average particle size of 536 nm. In the ultimate SPS experiment which was conducted at 1500 °C for 5 min under a pressure of 50 MPa, a relative density of 94.9% and a micro-hardness value of 24.56 GPa were achieved.     

Effect of surfactant and heat treatment on morphology,surface area and crystallinity in hydroxyapatite nanocrystals

Hydroxyapatite (HA) powders were synthesized by the wet precipitation method, with and without surfactant, under identical processing parameters. These powders were then heat treated at 900 °C for 3 h in air. The detailed characterization of the powders was done by using SEM, dynamic light scattering, nitrogen adsorption, XRD, Raman spectroscopy, and FTIR techniques. The HA phase, identified by well defined PO₄^3? and OH^? ion peaks in Raman and FTIR spectra, was observed in all the powder samples. The addition of surfactant changed the morphology of the particles from spherical to needle/rod-like structure and increased the surface area up to three times (from 33 to 96 m²/g). Also, suppression in the evolution of β-TCP phase was observed along with decrease in the crystal size and crystallinity of the powder due to the addition of surfactant. Synthesized nano-HA crystals were found to have diameters and lengths in the range 10–25 nm and 75–150 nm, respectively. The heat treatment changed the architecture of the particles, increased the crystallinity and reduced the surface area to ≈7 m²/g. However, the relative increase in crystallinity was much higher for the powder synthesized with surfactant. The ratio of the average crystallite size to the crystallinity degree was about 0.53±0.07 for all the powders. The particle size distribution was bimodal and coarser for the powder synthesized without surfactant. The pore size analysis showed transformation of a predominantly mesoporous structure into a meso- plus macroporous one on heat treatment. The intensity of OH^? group peak in Raman spectra was found to be highly sensitive to the crystalline state of the HA powder and may be used to assess crystallinity.     

Phase transformation characterization of olivine subjected to high temperature in air

Olivine is one of the well-suited materials for fluidized bed reactor technology. After calcination at high temperature, olivine undergoes phase transformations resulting in dehydration and oxidation of fayalite to hematite and magnetite. The transformation mechanisms of olivine subjected to a calcination process at 1400 °C for 4 h are studied. Calcined olivine is characterized by X-Ray Diffraction (XRD), in situ XRD at varying temperatures and Raman spectroscopy. This paper explains the contribution of Raman spectroscopy to the study of iron oxide with regard to XRD. The heterogeneous distribution of hematite, magnetite and forsterite in the calcined material is exhibited by Raman mapping.     

Synthesis,calcination and characterization of Nanosized ceria powders by self-propagating room temperature method

Nanometric ceria powders with fluorite-type structure were obtained by applying self-propagating room temperature method. The obtained powders were subsequently thermally treated (calcined) at different temperatures for different times. Powder properties such as specific surface area, crystallite size, particle size and lattice parameter have been studied. Roentgen diffraction analysis (XRD), BET and Raman scattering measurements were used to characterize the as-obtained (uncalcined) powder as well as powders calcined at different temperatures.It was found that the average diameter of the as-obtained crystallites is in the range of 3–5 nm whereas the specific surface area is about 70 m²/g. The subsequent, 15 min long, calcination of as-obtained powder at different temperatures gradually increased crystallite size up to ～60 nm and reduced specific surface down to 6 m²/g. Raman spectra of synthesized CeO_2?y depicts a strong red shift of active triply degenerate F_2 g mode as well as additional peak at 600 cm^?1. The frequency of F_2 g mode increased while its line width decreased with an increase in calcination temperature. Such a behavior is considered to be the result of particle size increase and agglomeration during the calcination. After the heat treatment at 800 °C crystallite size reached value larger than 50 nm. Second order Raman mode, which originates from intrinsic oxygen vacancies, disappeared after calcination.     

Titania ultrafiltration membrane: Preparation,characterization and photocatalytic activity

A mesoporous photocatalytic titania (TiO₂) membrane on alumina support is successfully fabricated via the sol–gel processing method. Several techniques such as dynamic light scattering, X-ray diffraction (XRD), TGA, N₂-sorption, and SEM are utilized to investigate the optimized processing parameters and their influence on the final properties of the developed membrane. The prepared titania sol containing organic additives (HPC and PVA) has an average particle size of 55.6 nm with a narrow distribution. The resulting TiO₂ membrane with thickness of 1 μm exhibits homogeneity with no cracks or pinholes. It also maintains small pore size (4.7 nm), large specific surface area (75 m²/g), and small crystallite size (8.3 nm).The permeability and photocatalytic properties of the titania membrane were measured. The permeability coefficient of the fabricated membrane is 30.09 cm³ min^?1 bar^?1 cm^?2. These measurements indicate an optimum processing condition for the preparation of the membrane. The prepared titania membrane has a great potential in developing high efficient water treatment and reuse systems because of its multifunctional capability such as decomposition of organic pollutants and physical separation of contaminants.     

Pb(Zr0.95Ti0.05)O3 powders and porous ceramics prepared by one-step pyrolysis process using non-aqueous Pechini method

Using non-aqueous Pechini method, Pb(Zr_0.95Ti_0.05)O₃ powders were prepared at low temperature by one-step pyrolysis process. The polymeric gels and powders were characterized using a range of techniques, such as DTG, XRD, SEM, Raman spectroscopy, and laser particle size distribution. The perovskite phase was formed at about 350–400 °C and some oxocarbonate impurities can be detected in all samples after calcining at 400–850 °C by one-step pyrolysis process. Phase pure and porous Pb(Zr_0.95Ti_0.05)O₃ ceramics were obtained without pore formers from the powders by one-step pyrolysis process at 500 °C for 4 h. The relative densities were 87%, 91% and 94% for the ceramics sintered at 1100, 1150 and 1200 °C for 2 h, respectively. The porous ceramics sintered at 1200 °C for 2 h have homogeneously dispersed pores and fine-grain structures with an individual grain size of 0.7–2 μm.     

In-situ fabrication of TiC-Fe3Al cermet

Titanium carbide has high hardness, resistance to oxidation and abrasion while iron aluminide has proper ductility as well as good strength and excellent oxidation resistance up to high temperatures. Therefore, it can be expected TiC-iron aluminide cermet to have excellent mechanical properties as a cutting tool and a wear-resistance material. In this study, mechanical milling and hot press sintering processes were used to manufacture in-situ TiC-Fe₃Al cermet, whose microstructure and mechanical properties were examined according to the changes in volume fraction of TiC and milling time. After 48 h of milling each mechanically alloyed powder crystallized in a TiC and Fe₃Al biphasic material. The milled powder was hot-pressed at 1250 ℃ and 50 MPa for 30 min to obtain sintered bodies also consisting of only TiC and Fe₃Al phases. The hard phase, TiC, had a size of 100–300 nm with overall uniform distribution decreasing as the volume fraction of TiC increased. The hardness of each sintered body showed a linearly increasing tendency according to the increase in TiC content, the hardness for 90 vol% TiC cermet being as high as 1813Hv. On the other hand, the bending strength was 1800 MPa and 1780 MPa when TiC volume fraction was 50% and 70%, respectively, while it showed an abrupt decrease up to 580 MPa at 90% TiC volume fraction. Fe₃Al phase is effective to toughening of TiC-Fe₃Al cermet and the volume fraction of Fe₃Al phase significantly influences the bending strength of the cermet.     

Photocatalytic activities of N-doped nano-titanias and titanium nitride

TiO₂ doped with various loadings of nitrogen was prepared by nitridation of a nano-TiO₂ powder in an ammonia/argon atmosphere at a range of temperatures from 400 to 1100 °C. The nano-TiO₂ starting powder was produced in a continuous hydrothermal flow synthesis (CHFS) process involving reaction between a flow of supercritical water and an aqueous solution of a titanium salt. The structures of the resulting nanocatalysts were investigated using powder X-ray diffraction (XRD) and Raman spectroscopy. Products ranging from N-doped anatase TiO₂ to phase-pure titanium nitride (TiN) were obtained depending on post-synthesis heat-treatment temperature. The results suggest that TiN started forming when the TiO₂ was heat-treated at 800 °C, and that pure phase TiN was obtained at 1000 °C after 5 h nitridation. The amounts and nature of the Ti, O and N at the surface were determined by X-ray photoelectron spectroscopy (XPS). A shift of the band-gap to lower energy and increasing absorption in the visible light region, were observed by increasing the heat-treatment temperature from 400 to 700 °C.     

Synthesis of HfB2 powders by mechanically activated borothermal reduction of HfCl4

HfB₂ powders were synthesized via a borothermal reduction route from mechanically activated HfCl₄ and B powder blends. Mechanical activation of the powder blends was carried out for 1 h in a high-energy ball mill using hardened steel vial and balls. Mechanically activated powders were subsequently annealed at 1100 °C for 1 h under Ar atmosphere. Then, purification processes such as washing with distilled water and leaching in HCl solution were applied for the elimination of the undesired boron oxide (B₂O₃) phase and the probable Fe impurity. The effect of boron amount on the microstructure of the resultant powders was investigated. The boron amount in the starting blends plays an important role in the formation of the HfO₂ phase. HfB₂ powders without any detectable HfO₂ were prepared by adding 20 wt% excess amount of boron. Microstructural analyses of the mechanically activated, annealed and purified powders were performed using X-ray diffractometer (XRD), particle size analyzer (PSA), stereomicroscope (SM), scanning electron microscope/energy dispersive spectrometer (SEM/EDS) and transmission electron microscope (TEM).     

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO₃ (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO₃ structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal–oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses.     

Influence of CeO2 addition on crystal growth behavior of CeO2–Y2O3–ZrO2 solid solution

Nanopowders with cubic fluorite-type structure as well as uniform distribution in particle size were synthesized by hydrothermal method in the ternary oxide zirconia–yttria–ceria system with ceria content of 0–25 mol%. X-ray diffraction (XRD), thermogravimetric analysis/differential scanning calorimeter (TG/DSC), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy (Raman), specific surface area (S_BET) and high resolution transmission electron microscopy (HRTEM) were applied to characterize the structure, thermal decomposition, morphological characteristic and crystal growth of the produced powders. Qualitative analyses indicate that the as-synthesized nanoparticles are single-phase crystallites with an average particle size of 4–9 nm. The specific surface area, lattice parameter and microstrain are closely related to Ce⁴⁺ concentration. Moreover, activation energy of crystal growth is significantly dependent on the dopant (CeO₂) concentration. It firstly increased and then decreased with increasing dopant concentration, and the maximum value was observed at the dopant concentration of 5 mol%.     

Dense fine-grained biphasic calcium phosphate (BCP) bioceramics designed by two-step sintering

In this study, dense, fine-grained biphasic calcium phosphate bioceramics were designed via the two-step sintering method. The starting powder was nanosized calcium-deficient hydroxyapatite, whose phase composition, average particle size and morphology were characterized by XRD, FTIR, Raman spectroscopy, laser diffraction and FE-SEM. The phase transformations of the initial powder during heating up to 1200 °C were examined using TG/DSC. At first, conventional sintering was performed and the recorded shrinkage/densification data were used to find out the appropriate experimental conditions for two-step sintering. The obtained results show that two-step sintering yields BCP ceramics, consisting of hydroxyapatite and β-TCP, with full dense, homogeneous structure with average grain size of 375 nm. Furthermore, BCP ceramics obtained by the two-step sintering method exhibit improved mechanical properties, compared to conventionally sintered BCP.