Nb2O5 nanoparticles obtained by microwave assisted combustion synthesis under different conditions

The microwave assisted combustion synthesis (MACS) as a new, quick and low cost synthesis method was used for preparation of niobium pentoxide (Nb2O5) powders. The present paper investigated the effect of reactant concentrations (ammonium niobium oxalate, urea and ammonium nitrate) on the characteristics of Nb2O5 nanoparticles. Three samples were synthesized with stoichiometric ratio between the fuel and oxidant (C1), excess of oxidant (C2) and excess of fuel (C3). In all samples, Nb2O5 crystalline nanoparticles with irregular morphology were detected. The synthesis of nanoparticles with smaller diameter in the C2 and C3 samples was confirmed by greater values of band gap energy measured through UV-Visible diffuse reflectance spectroscopy (indicating quantum confinement) and by the Rietveld refinement of X-ray diffraction patterns. The results showed that the amounts of oxidant and fuel can change synthesis temperature, influencing the final characteristics of the particles, such as size and existent phases. In these cases the excess of oxidant and fuel in the C2 and C3 samples, respectively, decreases the average synthesis temperature and decelerates the particle growth and the formation of the monoclinic phase.

Improved thermal stability of SiCf/SiC ceramic matrix composites fabricated by PIP process

Improvement of the thermal stability of continuous SiC fiber reinforced SiC ceramic matrix composites (SiCf/SiC CMC) by the pre-treatment of SiC fillers and the suppression of oxidation during polymer impregnation and pyrolysis (PIP) process were investigated. Dense SiCf/SiC CMCs were fabricated using the slurry infiltration and PIP process under a purified argon atmosphere. Structure and mechanical properties of the SiCf/SiC CMC heated at different temperatures were evaluated. The flexural strength of the SiCf/SiC CMC decreased only 15.3%after heating at 1400 ?C, which exhibited a clear improvement compared with the literature data (49.5% loss), where severe thermal deterioration of SiCf/SiC composite occurred at high temperatures by the crystallization and decomposition of the precursor-derived ceramic matrix. The thermal stability of the SiCf/SiC CMC fabricated by PIP process was improved by the pre-treatment of SiC fillers for removing oxides and the strict atmosphere control to prevent oxidation.

Hydrothermal synthesis of tetragonal barium titanate nanopowders under moderate conditions

Monodispersed tetragonal barium titanate (BaTiO3) nanopowders were synthesized by a convenient hydrothermal route at a low temperature of 200?C in only 24 h. The key point of this method is to promote the generation of ultrafine titanium hydroxide precipitation precursors with the help of absolute ethyl alcohol and ammonia solution during the hydrolysis of Ti(OC4H9)4. The results of X-ray diffraction and Raman spectra show that the as-prepared BaTiO3 nanopowders possess tetragonal-dominant structure. The synthesized tetragonal BaTiO3 nanopowders exhibit relatively uniform size and good dispersity, with the average particle size of 96.1 nm and a tetragonality of 1.0073, which enable broad application prospects in the field of multilayer ceramic capacitors.

Chelating agent and substrate effect on hydrothermal growth of Yb3+/Er3+ doped NaYf4 film

We report simultaneous crystal growth and deposition of upconverting Yb3+/Er3+ doped NaYF4 film (UCF) on conducting and non-conducting substrates by one-step hydrothermal method. The characteristics such as film topography, morphology, crystallographic phase and upconverting luminescence intensity were found to depend both on the chelating agent and nature of the substrate. The characteristics of the prepared films varied interestingly when either the chelating agent or the substrate was changed. The upconversion emission intensities were found to increase with decreasing film roughness. Further, current investigation demonstrated that the NaYF4 films deposited using EDTA or DTPA chelating agents on ITO substrate and EGTA chelating agent on PG substrate were more uniform and resulted in greater upconverted emission intensities. We envision plausible use of current technology in the development of affordable optical platforms for several optoelectronic applications.

Influence of ZnO addition and milling process on structure and conductivity of BaCe0.2Zr0.7Y0.1O3-δ ceramics

Precursor powders for BaCe0.2Zr0.7Y0.1O3-?(BCZY27) ceramics were synthesized by a modified Pechinimethod and calcined at 900?C for 12 h. The calcined BCZY27 powders were milled in eccentric and in high energy mill with the addition of 2 and 4mol% ZnO as sintering aid. The effects of milling and sintering aids on the sinterability and electrical conductivity were studied. The linear shrinkage in thermomechanical analyses started at 1050?C for the BCZY27 with 4mol% ZnO processed in eccentric mill. Theoretical density above of 90%TD was obtained for the BCZY27 milled with 4mol% ZnO and sintered at 1400?C for 4h. X-ray diffraction analysis of the BCZY27 ceramics sintered at 1400?C confirmed the presence of BaCe0.2Zr0.7Y0.1O3-? and Y0.4Ce0.6O1.8 phases. The incorporation of Zn into perovskite lattice leads to the secondary phase formation. SEM and EDS analyses confirmed the presence of Y0.4Ce0.6O1.8 phase. The sintering was assisted by BaO-ZnO eutectic, which was reflected by the increase of activation energy values for grain boundary conduction. The milling processing did not affect the conductivity properties. The obtained BCZY27 dense sample has conductivity of 7.60 ? 10?3 S/cm at 500?C.

Cyclic fatigue behaviour of hydrothermally aged 3Y-TZP ceramics in 4-point bending tests

Fatigue is one of the most important properties to be considered in ceramic dental implants due to cyclic mechanical stresses arising from the chewing process. In this work, the fatigue behaviour of hydrothermally degraded ZrO2-based ceramics stabilized with 3mol% Y2O3 (3Y-TZP) was studied in 4-point bending tests. Samples of 3Y-TZP were compacted (100MPa), sintered at 1475 ?C for 2 h, polished and hydrothermally degraded in an autoclave as described in the ISO-13356 standard. The samples were characterized by their relative density, crystalline phase composition, microstructure and surface roughness. The highly dense (>99.6%TD) sintered 3Y-TZP ceramics has only tetragonal t-ZrO2 phase, even after hydrothermal ageing. Furthermore, the ceramic materials presented a Vickers hardness of 12.7?0.2GPa, a fracture toughness of 7.1?0.3MPa?m1/2 and a 4-point bending strength of 940.1?67MPa. Based on the bending test results 5 different stress levels for the fatigue tests were selected and conducted by cyclic 4-point bending obtaining the S-N curve. Weibull statistics was used for the statistical analysis. The fatigue tests indicate that the limit of fatigue resistance of this 3Y-TZP ceramics is around 550MPa, i.e. higher than the limits established in the ISO-13356 standard for the use of Y-TZP ceramics for the manufacture of implants. The fatigue behaviour of the investigated 3Y-TZP ceramics was related to the toughening mechanisms acting in Y-TZP ceramics, such as transformation toughening related to t?m phase transformation and microcracking.

Effects of oxidation of SiC aggregates on the sintering behaviour and microstructures of SiC-CaAl12O19 composite refractories

In order to develop chrome-free refractory materials applicable in coal slurry gasification, SiC-CaAl12O19 (SiC-CA6) composite refractories were developed and prepared by using SiC aggregates and CA6 powders as main raw materials. The sintering behaviour of the composites was investigated. After firing at different temperatures under CO atmosphere, the effects of oxidation of SiC aggregates on the sintering behaviour and microstructures of SiC-CA6 composite refractorieswere investigated. SiC-CA6 composites could not be sintered when firing temperature was lower than 1500?C. SiC had a passive oxidation and the oxidation components were able to react with CA6 to form CaAl2Si2O8. The CaAl2Si2O8 melted into liquid when sintering temperature was in the range of 1500-1600?C, which promoted the sintering process of the SiC-CA6 composites. At temperatures above 1600 ?C, an active oxidation of SiC occurred. Simultaneously, SiC could also reacted with the SiO2(s,l) to form SiO, leading to the precipitation of Al2O3 and CaO in the liquid to generate plate-like CA6. Above this temperature, the sintering of the SiC-CA6 composite refractories was affected by the growth of CA6 and oxidation of SiC. This work demonstrates that the optimal sintering temperature for the SiC-CA6 composite refractories was 1600?C.

Facile preparation of ZrO2 whiskers by LiF-KCl molten salts synthesis

Monoclinic zirconia (ZrO2) whiskers were made via the molten salt method using zirconyl chloride octahydrate (ZrOCl2 ? 8H2O) as zirconium source, potassium chloride (KCl) as molten salt and lithium fluoride (LiF) as a mineraliser. DSC-TG, XRD, FE-SEM, Raman and TEM were performed to study the effects of heat treatment temperature, holding time and heating rate on the synthesis of zirconia whiskers. The results indicate that zirconia whiskers with diameters of 50-80 nm and aspect ratios of 10-30 can be obtained by heating the precursor at slow rate (3?C/min) to 718?C for 1 h and then at faster rate (7?C/min) to 950?C for 3 h. The whiskers have a smooth surface and grow in [001] direction. The key to the ZrO2 whiskers growth is the controlled dissolution and precipitation of the ZrO2 in a LiF-KCl molten salt solution environment.

Effect of particle size of Y2O3-Al2O3 additives on microstructure and mechanical properties of Si3N4 ceramic balls for bearing applications

Si3N4 ceramic balls were prepared by gas pressure sintering with Y2O3 and Al2O3 as sintering additives. The effects of particle size of Y2O3-Al2O3 additives on densification, microstructure and mechanical properties of Si3N4 ceramic balls were investigated. The reliability of Si3N4 ceramic balls was evaluated through the Weibull modulus. The results showed that Si3N4 ceramic balls containing nanosized Y2O3-Al2O3 additives have a higher relative density and better comprehensivemechanical properties compared with the samples containing microsized additives, with relative density of 98.9 ? 0.2%TD, Vickers hardness of 14.7 ? 0.1GPa, indentation fracture toughness of 6.5 ? 0.1MPa?m1/2 and crushing strength of 254 ? 8.5MPa. The more homogeneous and extensive dispersion of the nanosized sintering additives in the Si3N4 matrix is the main reason for the enhancement in density and mechanical properties of the Si3N4 ceramic balls.

Molten salt synthesis of TiB2 nanopowder by reduction of TiO2 with MgB2

This research work presents the preparation of TiB2 nanopowders by molten-salt synthesis (MSS) technique from TiO2 and MgB2 as starting active materials and MgCl2 as a molten salt. The pure TiB2 nanopowders were finally prepared using 2M HCl aqueous solution to leach the synthesized samples. The effects of the firing temperature, firing time and reactants to salt ratio on the TiB2 nanopowders formation were examined. The results demonstrated that the TiB2 formation was completed even with reactants to salt mass ratio of 1:2 at 1000 ?C for 4 h. The TiB2 nanopowders synthesized with 1:2, 1:5 and 1:10 reactants to salt mass ratios have different particle sizes. Thus, the average particle sizes estimated from BET surface areas were 59, 55 and 46 nm for the samples synthesized with 1:2, 1:5 and 1:10 reactants to salts mass ratios, respectively. These results illustrated that the high concentration of MgCl2 plays a key role in the particles? size reduction. The above results assured that this research study presents a new low-temperature synthesis route for nano-sized metal diboride powders.