Role of Fuel on Cation Disorder in Magnesium Aluminate (MgAl2O4) Spinel Prepared by Combustion Synthesis

Magnesium aluminate spinel (MgAl2O4) forms an interesting system having tetrahedral and octahedral voids filled with near similar sized divalent Mg2+ and trivalent Al3+ cations. Structural disorder (e.g., Mg-Al antisite defects) can be tuned by synthetic conditions. This study reports the evolution of Mg/Al disorder in MgAl2O4 prepared by combustion synthesis using different types of fuels. The effect of nature of fuel and the final calcination temperature (600 degrees C-900 degrees C for 9h) on degree of cation ordering has been investigated combining powder X-ray (XRD) and neutron (NPD) diffraction. The results indicate very high degree of inversion in the samples crystallized at low annealing temperature, which on further annealing reduces toward the thermodynamically stable values. Raman spectroscopy, probing MgO4, and AlO4 tetrahedral bonds, confirmed the results at a local level.

Flow Cytometry Analysis of Cytotoxicity In Vitro and Long-Term Toxicity of HA-40wt% BaTiO3 Nanoparticles In Vivo

The development of new implantable biomaterials requires bone-mimicking physical properties together with desired biocompatible property. In continuation to our earlier published research to establish compositional dependent multifunctional bone-like properties and cytocompatibility response of hydroxyapatite (HA)-BaTiO3 composites, the toxicological property evaluation, both invitro and invivo, were conducted on HA-40wt% BaTiO3 and reported in this work. In particular, this work reports invitro cytotoxicity of mouse myoblast cells as well as invivo long-term tissue and nanoparticles interaction of intra-articularly injected HA-40wt% BaTiO3 and BaTiO3 up to the concentration of 25mg/mL in physiological saline over 12weeks in mouse model. The careful analysis of flow cytometry results could not reveal any statistically significant difference in terms of early/late apoptotic cells or necrotic cells over 8d in culture. Extensive histological analysis could not record any signature of cellular level toxicity or pronounced inflammatory response in vital organs as well as at knee joints of Balb/c mice after 12weeks. Taken together, this study establishes nontoxic nature of HA-40wt% BaTiO3 and therefore, HA-40wt% BaTiO3 can be used safely for various biomedical applications.

Investigation of Annealing Induced Yttria Segregation in Sputtered Yttria-Stabilized Zirconia Thin Films

8mol% yttria-stabilized zirconia (8YSZ) is an extensively studied solid electrolyte. But there is no consistency in the reported ionic conductivity values of 8YSZ thin films. Interfacial segregation in YSZ thin films can affect its ionic conductivity by locally altering the surface chemistry. This article presents the effects of annealing temperature and film thickness on free surface yttria segregation behavior in 8YSZ thin film by Angle Resolved XPS and its influence on the ionic conductivity of sputtered 8YSZ thin films. Surface yttria concentration of about 32, 20, and 9mol% have been found in 40nm 8YSZ films annealed at 1273, 1173, and 1073K, respectively. Yttria segregation is found to increase with increase in annealing temperature and film thickness. Ionic conductivities of 0.23, 0.16, and 0.08Scm(-1) are observed at 923K for 40nm 8YSZ films annealed at 1073, 1173, and 1273K, respectively. The decrease in conductivity with increase in annealing temperature is attributed to the increased yttria segregation with annealing. Neither segregation nor film thickness is found to affect the activation energy of oxygen ion conduction. Target purity is found to play a key role in determining free surface yttria segregation in 8YSZ thin films.

Neutron diffraction, Mossbauer effect and Electron Paramagnetic Resonance studies on multiferroic Pb(Fe2/3W1/3)O-3

Multiferroic Pb(Fe2/3W1/3)O-3 ceramics were synthesized via a modified two-stage Columbite method. Single phase formation was confirmed from the analysis of x-ray and neutron diffraction patterns recorded at room temperature. Structural analysis of the diffraction data reveals cubic phase (space group Pm-3m) for the title compound. Magnetic structure of the title compound at room temperature exhibits G-type antiferromagnetic structure. The Mossbauer spectroscopy and Electron Paramagnetic Resonance (EPR) studies were carried out at 300 K. The isomer shift and quadrupole splitting of the Mossbauer spectra confirms the trivalent state of iron (Fe3+). The Mossbauer spectra also suggest that the iron and tungsten are randomly distributed at the octahedral, B site. EPR spectra show a single broad line associated with Fe3+ ions. Both spectra clearly exhibit weak ferromagnetic behaviour of Pb(Fe2/3W1/3)O-3 ceramic at 300 K. Considering neutron diffraction, Mossbauer and EPR results together, it may be stated here that Pb(Fe2/3W1/3)O-3 exhibits antiferromagnetic behavior along with weak ferromagnetism at room temperature.

Twinning induced enhancement of fracture toughness in ultrafine grained Hydroxyapatite-Calcium Titanate composites

Despite being highly bioactive and biocompatible, the limitations of monolithic hydroxyapatite (HA) include extremely low fracture toughness, poor electrical conductivity. While addressing these issues, the present study demonstrates how CaTiO3 (CT) addition to HA can be utilized to obtain a combination of long crack fracture toughness (1.7 MPa m(1/2) SEVNB technique) and flexural strength of 98-155 MPa (3-point bending) and a moderate tensile strength (diametral compression) of 17-36 MPa. The enhancement in fracture resistance in spark plasma sintered HA-CT composites has been explained in reference to the observed twin morphology. TEM reveals the presence of twins in CT grains due to 1800 rotation about 101]. The measured properties along with our earlier reports on biocompatibility and electrical properties make HA-CT suitable for bone tissue engineering applications. When compared with other competing HA-based biocomposites, HA-CT composites are found to have a better combination of properties useful for medium load bearing implant applications. (C) 2015 Elsevier Ltd. All rights reserved.

Monoclinic to cubic phase transformation in combustion synthesized gadolinium oxide

Gadolinium oxide, cerium oxide, and 10 mol% gadolinia doped ceria ceramic powders have been synthesized using combustion technique. Though the cubic gadolinia phase is stable at room temperature, single phase monoclinic gadolinia was obtained as a result of combustion synthesis using fuel lean and stoichiometric precursor compositions. This powder was subjected to calcination treatment and ceria doping to study the stability of phases and the rate of phase transformation from monoclinic to cubic gadolinia. It was found that monoclinic gadolinia transforms to cubic gadolinia upon calcination at temperatures less than 1200 degrees C. It was also found that rate of phase transformation is more for powder produced using fuel lean compositions; and the rate is enhanced upon ceria doping. (C) 2015 Elsevier Ltd. All rights reserved.

High frequency millimetre wave absorbers derived from polymeric nanocomposites

The world has dominated by automation, wireless communication and various electronic equipments, which has led to the most undesirable offshoots like electromagnetic (EM) pollution. The rationale is environmental concern and the necessity to develop EM absorbing materials. This paper reviews the state of the art of designing polymer based nanocomposites containing nanoscopic particles with high electrical conductivity and complex microwave properties for enhanced EM attenuation. Given the brevity of this review article, herein we have summarized the high frequency millimetre wave absorbing properties of polymer nanocomposites consisting of various nanoparticles that either reflect or absorb microwave radiation like electrically conducting carbon nanotubes (CNTs) and graphene nanosheets (GNs), high dielectric constant ceramic nanoparticles that show relaxation loss in the microwave frequency and magnetic metal and ferrite nanoparticles that absorb microwave radiation through natural resonance, eddy current and hysteresis losses. Furthermore, we have stressed the necessity and impact of hybrid nanoparticles consisting of magnetic and dielectric nanoparticles along with conducting inclusions like CNT and GNs in this review. Electromagnetic interference (EMI) theory and necessary criterion for attenuation has been briefly discussed. The emphasis is made on various mechanisms towards EM attenuation controlled by these nanoparticles. Various structures developed using polymer nanocomposites like bulk, foam and layered structures and their effect on EM attenuation has been elaborately discussed. In addition, various covalent/non-covalent modifications on nanoparticles have been juxtaposed in context to EM attenuation. In addition, we have highlighted important facets and direction for enhancing the microwave attenuation. (C) 2016 Elsevier Ltd. All rights reserved.

Strength reliability and in vitro degradation of three-dimensional powder printed strontium-substituted magnesium phosphate scaffolds

Strontium ions (Sr2+) are known to prevent osteoporosis and also encourage bone formation. Such twin requirements have motivated researchers to develop Sr-substituted biomaterials for orthopaedic applications. The present study demonstrates a new concept of developing Sr-substituted Mg-3(PO4)(2) - based biodegradable scaffolds. In particular, this work reports the fabrication, mechanical properties with an emphasis on strength reliability as well as in vitro degradation of highly biodegradable strontium-incorporated magnesium phosphate cements. These implantable scaffolds were fabricated using three-dimensional powder printing, followed by high temperature sintering and/or chemical conversion, a technique adaptable to develop patient-specific implants. A moderate combination of strength properties of 36.7 MPa (compression), 242 MPa (bending) and 10.7 MPa (tension) were measured. A reasonably modest Weibull modulus of up to 8.8 was recorded after uniaxial compression or diametral tensile tests on 3D printed scaffolds. A comparison among scaffolds with varying compositions or among sintered or chemically hardened scaffolds reveals that the strength reliability is not compromised in Sr-substituted scaffolds compared to baseline Mg-3(PO4)(2). The micro-computed tomography analysis reveals the presence of highly interconnected porous architecture in three-dimension with lognormal pore size distribution having median in the range of 17.74-26.29 mu m for the investigated scaffolds. The results of extensive in vitro ion release study revealed passive degradation with a reduced Mg2+ release and slow but sustained release of Sr2+ from strontium-substituted magnesium phosphate scaffolds. Taken together, the present study unequivocally illustrates that the newly designed Sr-substituted magnesium phosphate scaffolds with good strength reliability could be used for biomedical applications requiring consistent Sr2+-release, while the scaffold degrades in physiological medium. Statement of significance The study investigates the additive manufacturing of scaffolds based on different strontium-substituted magnesium phosphate bone cements by means of three-dimensional powder printing technique (3DPP). Magnesium phosphates were chosen due to their higher biodegradability compared to calcium phosphates, which is due to both a higher solubility as well as the absence of phase changes (to low soluble hydroxyapatite) in vivo. Since strontium ions are known to promote bone formation by stimulating osteoblast growth, we aimed to establish such a highly degradable magnesium phosphate ceramic with an enhanced bioactivity for new bone ingrowth. After post-processing, mechanical strengths of up to 36.7 MPa (compression), 24.2 MPa (bending) and 10.7 MPa (tension) could be achieved. Simultaneously, the failure reliability of those bioceramic implant materials, measured by Weibull modulus calculations, were in the range of 4.3-8.8. Passive dissolution studies in vitro proved an ion release of Mg2+ and PO43- as well as Sr2+, which is fundamental for in vivo degradation and a bone growth promoting effect. In our opinion, this work broadens the range of bioceramic bone replacement materials suitable for additive manufacturing processing. The high biodegradability of MPC ceramics together with the anticipated promoting effect on osseointegration opens up the way for a patient-specific treatment with the prospect of a fast and complete healing of bone fractures. (C) 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Structural, Optical, and Piezoelectric Response of Lead-Free Ba0.95Mg0.05Zr0.1Ti0.9O3 Nanocrystalline Powder

Nanocrystalline powders of Ba1-xMgxZr0.1Ti0.9O3 (x = 0.025-0.1) were synthesized via citrate assisted sol-gel method. Interestingly, the one with x = 0.05 in the system Ba1-xMgxZr0.1Ti0.9O3 exhibited fairly good piezoelectric response aside from the other physical properties. The phase and structural confirmation of synthesized powder was established by X-ray powder diffraction (XRD) and Raman Spectroscopic techniques. Two distinct Raman bands i.e., 303 and 723 cm(-1) characteristic of tetragonal phase were observed. Thermogravimetric analysis (TGA) was performed to evaluate the phase decomposition of the as-synthesized Ba0.95Mg0.05Zr0.1Ti0.9O3 sample as a function of temperature. The average crystallite size associated with Ba0.95Mg0.05Zr0.1Ti0.9O3 was calculated using Scherrer formula based on the XRD data and was found to be 25 nm. However, Scanning and Transmission Electron Microscopy studies revealed the average crystallite size to be in the range of 30-40 nm, respectively. Kubelka-Munk function was employed to determine the optical band gap of these nanocrystallites. A piezoelectric response of 26 pm/V was observed for Ba0.95Mg0.05Zr0.1Ti0.9O3 nanocrystal by Piezoresponse Force Microscopy (PFM) technique. Photoluminescence (PL) study carried out on these nanocrystals exhibited a blue emission (470 nm) at room temperature.

Maintaining local displacive disorders in Na0.5Bi0.5TiO3 piezoceramics by K0.5Bi0.5TiO3 substitution

A comprehensive global and local structural characterization using X-ray and neutron diffraction, and EXAFS have been performed to investigate the effect of electrical poling on the structure of (1-x)Na0.5Bi0.5TiO3-(x)K0.5Bi0.5TiO3 compositions. While the annealed samples showed definite indication of presence of local displacive disorders in all the compositions studied (0

Formation and structure of composite coating of HDA and micro-plasma oxidation on A3 steel

Composite coatings were obtained on A3 steel by hot dipping aluminum(HDA) at 720 ℃ for 6 min and micro-plasma oxidation(MPO) in alkali electrolyte. The surface morphology, element distribution and interface structure of composite coatings were studied by means of XRD, SEM and EDS. The results show that the composite coatings obtained through HDA/MPO on A3 steel consist of four layers. From the surface to the substrate, the layer is loose Al2O3 ceramic, compact Al2O3 ceramic, Al and FeAl intermetallic compound layer in turn. The adhesions among all the layers are strengthened because the ceramic layer formed at the Al surface originally, FeAl intermetallic compound layer and substrate are combined in metallurgical form through mutual diffusion during HDA process.Initial experiment results disclose that the anti-corrosion performance and wear resistance of composite coating are obviously improved through HDA/MPO treatment.

Analysis of strip electric saturation model of crack problem in piezoelectric materials

This paper presents a fully anisotropic analysis of strip electric saturation model proposed by Gao et al. (1997) (Gao, H.J., Zhang, T.Y., Tong, P., 1997. Local and global energy release rates for an electrically yielded crack in a piezoelectric ceramic. J. Mech. Phys. Solids, 45, 491-510) for piezoelectric materials. The relationship between the size of the strip saturation zone ahead of a crack tip and the applied electric displacement field is established. It is revealed that the critical fracture stresses for a crack perpendicular to the poling axis is linearly decreased with the increase of the positive applied electric field and increases linearly with the increase of the negative applied electric field. For a crack parallel to the poring axis, the failure stress is not effected by the parallel applied electric field. In order to analyse the existed experimental results, the stress fields ahead of the tip of an elliptic notch in an infinite piezoelectric solid are calculated. The critical maximum stress criterion is adopted for determining the fracture stresses under different remote electric displacement fields. The present analysis indicates that the crack initiation and propagation from the tip of a sharp elliptic notch could be aided or impeded by an electric displacement field depending on the field direction. The fracture stress predicted by the present analysis is consistent with the experimental data given by Park and Sun (1995) (Park, S., Sun, C.T., 1995. Fracture criteria for piezoelectric materials. J. Am. Ceram. Soc 78, 1475-1480).

Correlation between Discharging Property and Coatings Microstructure during Plasma Electrolytic Oxidation

The voltage-current properties during plasma electrolytic discharge were determined by measuring the current density and cell voltage as functions of processing time and then by mathematical transformation. Correlation between discharge I-V property and the coatings microstructure on aluminum alloy during plasma electrolfic oxidation was determined by comparing the voltage-current properties at different process stages with SEM results of the corresponding coatings. The results show that the uniform passive film corresponds to a I-V property with one critical voltage, and a compound of porous layer and shred ceramic particles corresponds to a I-Vproperty with two critical voltages. The growth regularity of PEO cermet coatings was also studied.

The Interaction Between Shock Waves and Foam in a Shock Tube

An experimental study and a numerical simulation were conducted to investigate the mechanical and thermodynamic processes involved in the interaction between shock waves and low density foam. The experiment was done in a stainless shock tube (80mm in inner diameter, 10mm in wall thickness and 5360mm in length). The velocities of the incident and reflected compression waves in the foam were measured by using piezo-ceramic pressure sensors. The end-wall peak pressure behind the reflected wave in the foam was measured by using a crystal piezoelectric sensor. It is suggested that the high end-wall pressure may be caused by a rapid contact between the foam and the end-wall surface. Both open-cell and closed-cell foams with different length and density were tested. Through comparing the numerical and experimental end-wall pressure, the permeability coefficients a and 0 are quantitatively determined.

Influence of the Processing Conditions on the Characteristics of the Clad Layers Produced with Laminar Plasma Technology

Laminar plasma technology was used to produce ceramic hardened layers of Al2O3-40% mass Ni composite powders on stainless steel substrates. In order to investigate the influences of processing conditions on the morphologies of the surface modified layers, two different powder-feeding methods were tested, one with carrier gas called the powder injection method, and the other without carrier gas called powder transfers method. The microscopic investigations demonstrate that the cross-section of the clad layers consists of two distinct microstructural regions, in which the Al2O3 phases exhibit different growth mechanisms. When the powder transfers method is adopted, the number density and volume fraction of the Al2O3 particles increase considerably and their distributions exhibit zonal periodical characteristics. When the powder-feeding rate increases, the microstructure of the Al2O3 phases changes from a small globular to a long needle shape. Finite element simulations show that the transient thermo-physical features of the pool substances, such as solidification rate and cooling rate, influence strongly the mechanisms of the nucleation and the directional growth of the Al2O3 phases in the thermal processing.