Advances in Science and Technology Vol. 63

Abstract: Niobium and nitrogen co-doped SrTiO3 possessing excellent visible light responsive photocatalytic activity was successfully synthesized by microwave-assisted solvothermal reaction using SrCl2.6H2O, Ti(OC3H7)4, NbCl5 and hexamethylenetetramine in KOH aqueous solution. The photocatalytic activity was determined by DeNOx ability using LED lamps with the wavelengths of 627 nm (red), 530 nm (green), 445 nm (blue) and 390 nm (UV). The photocatalytic activity of SrTiO3 for DeNOx ability in visible light region could be improved by co-doping Nb5+ and N3-. The excellent visible light photocatalytic activity of this substance may be due to the generation of a new band gap that enables to absorb visible light and decrease in the lattice defects which acts as a recombination center of photoinduced electrons and holes.

Abstract: A macro-scale model of spark plasma sintering (SPS) that couples electrical, thermal, stress-strain and densification components is presented. The continuum theory of sintering is incorporated enabling the evolution of the densification based on local conditions, thus a true spatial density distribution could be obtained. Specimen behavior is described through a non-linear viscous constitutive relation. The simulation is based on an FEM computer code. Several examples are shown and results are compared with experimental data available.

Abstract: The densification mechanism during the park-plasma-sintering (SPS) processing was examined in high purity MgAl2O4 spinel. As the density ρt increases, that is, as the effective stress σeff decreases, stress exponent n evaluated from σeff dependence of densification rate varies from n ≥ 4 in the low ρt region, n ≈ 2 in the intermediate ρt region to n ≈ 1 in the high ρt region. TEM observation shows that significant stacking faults caused by partial dislocations are observed in the low ρt region, but limited in the high ρt region. The ρt dependent densification behavior and microstructure suggest that the predominant densification mechanism during the SPS processing changes with ρt from plastic flow by partial dislocation motion for the low ρt region (n ≥ 4) to diffusion-related creep for the high ρt region (n ≈ 1).

Abstract: This study was carried out to produce and characterize B4C - TiB2 ceramics by spark plasma sintering. Initial B4C and TiB2 powders were mixed in ethanol solution with YSZ balls for 1 hour. Sintering was performed with 5, 10, 15 and 20 volume % TiB2 containing mixtures respectively in disc-shaped graphite dies. The applied pressure was 40 MPa at 1760 °C for 5 minute sintering duration. The improvement of low sinterability and low strength of B4C was investigated as well as strength of flexibility, hardness and fracture toughness. The obtained products were characterized by X-ray diffraction and SEM imaging. The hardness values were measured under 1000 g load and the density values were measured with Archimedes' principle. The 3-point bending tests and modulus of elasticity measurements were also conducted.

Abstract: Nanocrystalline alumina (Al2O3) powders were sintered by Spark Plasma Sintering (SPS) method in a vacuum atmosphere to obtain highly dense and fine grained final ceramic products. In the first section of experiments, 0.4 % wt MgO doped and 0.4 wt % Y2O3 doped Al2O3 were sintered at high temperatures and under high pressure with a SPS system. Later sintering procedures were carried out with codoping Y2O3 with the cathodic ratio of 0.4 wt % in order to investigate dopant effects on spark plasma sintered alumina. The microstructures of all samples were observed using scanning electron microscope and the properties such as density, hardness and fracture toughness were examined.

Abstract: The aim of this study was to produce dense and mechanically strong boron carbide ceramics with the help of different oxide additives. Physical properties of two different grades of pure boron carbide powders were analysed and sintered by Spark Plasma Sintering method. Starting powders were prepared by ball milling with the addition of 5 wt. % Y2O3, Al2O3, SiO2 and Y2O3 + Al2O3. In the sintering step, powder mixtures were sintered by SPS method in round-shaped graphite dies under 50 MPa for 5 minutes in the range of 1700-1800oC. In the characterization step, sintered sample compositions and microstructures were characterized by XRD and SEM analysis respectively. The hardness values were measured under 1000 g load and the density values were measured with Archimedes' principle. The fracture toughness analysis were also carried out.

Abstract: Stabilized zirconia shows rather high microwave absorbency at room temperature, and the absorbency become higher with increasing temperature. In this study, stabilized zirconia powder, partially stabilized zirconia powder and zirconia fiber were subjected for microwave absorption measurements at elevated temperature. Microwave absorption measurements were done by using a system consists of a microwave vector network analyzer, a circular wave-guide fixture and a vacuum furnace. Microwave absorbency was evaluated by the reflection power change from the sample in the circular wave-guide fixture under vacuum heating. Microwave absorbency of stabilized zirconia powder, partially stabilized zirconia powder and zirconia fiber gradually increased with the increase of temperature. We supposed that the increase of microwave absorbency is related to the ionic (oxygen) conduction behavior of stabilized zirconia. Stoichiometric composition ZrO2 powder was also subjected for a measurement to consider the relation between microwave absorbency and ion conduction of zirconia. As the result, stoichiometric composition ZrO2 powder was not absorbed microwave power even when the powder was heated up to 900oC because it isn’t an oxygen ion conductor.

Abstract: Mullite- zirconia composites have better mechanical properties than monolithic mullite ceramics and can be produced by reaction sintering of ZrSiO4 and  -Al2O3. The samples were prepared from high-purity (99.9%) α-alumina and fine zircon (ZrO2>65 wt.%) powders using PVA as binder. The powder mixtures were compacted under 80 MPa as coin shaped samples by uniaxial dry pressing and then sintered in a multimode microwave field of 2.45 GHz. The microwave effect on ZrSiO4 dissociation and mullite formation was evaluated by comparing the microwave sintered samples with those sintered conventionally. The as-reacted compacts were characterized by X-ray diffraction and scanning electron microscopy (SEM). The effects of sintering parameters on mullitization and mullite grain growth were investigated.

Abstract: Today chemistry of materials and as such the ceramic field of research are addressed through more and more complex synthetic methodologies in order to optimize final material performances. The notion of complexity in chemical science is illustrated inhere through the concept of integrative chemistry. Particularly the integration between bi-liquid foams, sol-gel process, organo-silane functionnalization, lanthanides complexation and Pd heterogeneous nucleation is proposed as a non-exhaustive synthetic tool box to reach specific advanced ceramics. The first section is dealing with the synthesis of the first series of Si(HIPE) macrocellular foams where the oil volume fraction of the starting emulsion allows a nice tuning of the foams macroporosity. The second section is dealing with Europium complexation of diketone and malonamide hybrid Organo-Si(HIPE) leading to the Eu3+@Organo-Si(HIPE) luminescent foams, while the third part is dedicated to Pd heterogeneous nucleation within host hybrid foams. This last series of macrocellular ceramics are labeled Pd@Organo-Si(HIPE) which demonstrates good turn over number (TON) and turn over frequencies (TOF) when acting as supported catalysts for the Mizoroki-Heck coupling reactions. In the above mentioned foams the HIPE acronym is for High Internal Phase Emulsion.

Abstract: The hybrid materials consisting of plate-like potassium lithium titanate (K0.81Li0.27Ti1.73O4) micro particles coated with calcia-doped ceria (Ce0.8Ca0.2O1.8) nano particles were prepared by the co-precipitation method and sol-gel method. Broad-spectrum UV-shielding composite materials with good comfort and low oxidation catalytic activity were successfully synthesized. The comfort when applied on skin and UV-shielding ability of the composites prepared by the sol-gel method were superior to those by the co-precipitation method.