Synthesis dependent characteristics of Sr1-xMnxTiO3 (x=0.03, 0.05, 0.07 and 0.09)

Sr1-xMnxTiO3 (where x=0.03, 0.05, 0.07 and 0.09) was synthesized via different routes that include solid-state, oxalate precipitation and freeze drying. In oxalate precipitation technique, compositions corresponding to 3 and 5 mol% doping of Mn were monophasic whereas the higher compositions revealed the presence of the secondary phases such as MnO, Mn3O4 etc., as confirmed by high resolution X-ray diffraction (XRD) studies. The decomposition behavior of the precursors prepared using oxalate precipitation method corresponding to the above mentioned compositions was studied. Nanopowders of compositions pertaining to 5 to 9 mol% of Mn doping were obtained using freeze-drying technique. The average crystallite size of these nanopowders was found to be in the 35 to 65 nm range. The microstructural studies carried out on the sintered ceramics, fabricated using powders synthesized by different routes established the fine grained nature ( < 1 mu m) of the one obtained by freeze drying method. Raman scattering studies were carried out in order to complement the observations made from XRD regarding the phase purity. The dielectric properties of the ceramics obtained by different synthesis routes were studied in the 80-300 K temperature range at 100 kHz and the effect of grain size has been discussed. (C) 2012 Elsevier Inc. All rights reserved.

High Temperature Phase Transition Studies and Dielectric Properties of Sr2SbMnO6

Sr2SbMnO6 (SSMO) ceramics were, fabricated using the nanocrystalline powders obtained via molten salt synthesis (MSS) method. High temperature X-ray diffraction studies confirmed the structural phase transition (room temperature tetragonal (I4/mcm) to the cubic phase (Pm-3m)) temperature to be around 736K. The discontinuity in the phase transition indicated its first order nature reflecting the presence of ferroelectric-like distortions in SSMO prepared from MSS which seemed to be unique as it was not observed so far in the case of SSMO prepared using solid-state reaction method. The dielectric behavior of SSMO was studied in the 300-950 K temperature range at high frequencies (MHz range) in order to suppress the of space charge and related effects that dominate at such higher temperatures and mask the real phase transition.

Hot-pressed TiB2-10 wt.% TiSi2 ceramic with extremely good thermal transport properties at elevated temperatures (up to 1273 K)

This contribution reports and analyses the high thermal transport property of hot-pressed TiB2-10 wt.% TiSi2 ceramics. Depending on the test temperature, the thermal conductivity values of the TiB2 composite (which range from 89 to 122W m(-1) K-1) are determined to be 18-25% higher than that of monolithic TiB2. The thermal transport properties are analyzed in terms of electronic and phonon contributions. The electronic contribution is the major component of the thermal conductivity of TiB2 and comparable contributions from both electronic and phonon components are observed for the TiB2-TiSi2 composite. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

The study of dielectric, pyroelectric and piezoelectric properties on hot pressed PZT-PMN systems

Hot uniaxial pressing technique has been adopted for the densification of PZT-PMN system with an aim to yield dense ceramics and to lower the sintering temperature and time for achieving better and reproducible electronic properties. The ceramics having >97% theoretical density and micron size grains are investigated for their dielectric, pyroelectric and piezoelectric properties. The effect of Li and Mn addition has also been studied. Copyright 2012 Author(s). This article is distributed under a Creative Commons Attribution 3.0 Unported License. http://dx.doi.org/10.1063/1.4769889]

In vitro bioactivity and cytocompatibility properties of spark plasma sintered HA-Ti composites

The present study reports the results of the detailed in vitro bioactivity and cytocompatibility properties of the hydroxyapatite (HA) and the HA-titanium (HA-Ti) composite with varying amount of Ti (5, 10, and 20 wt %), densified using spark plasma sintering process (SPS). Using this technique and tailoring suitable processing parameters, it has been possible to retain both HA and Ti in the sintered ceramics. Importantly, the uniquely designed SPS processing with suitably chosen parameters enables in achieving better mechanical properties, such as higher indentation fracture toughness (similar to 1.5 MPa m1/2) in HA-Ti composites compared with HA. X-ray diffraction and scanning electron microscopic (SEM) observations reveal good bioactivity of the HA-Ti composites with the formation of thick, flaky, and porous apatite layer when immersed in simulated body fluid at 37 degrees C and pH of 7.4. Atomic absorption spectroscopic analysis of the simulated body fluid solution reveals dynamic changes in Ca+2 ion concentration with more dissolution of Ca+2 ion from the HA-20Ti composite. However, the measurements with inductively coupled plasma spectrometer do not record dissolution of Ti+4 ions. Transmission electron microscopic analysis indicates weak crystalline nature of the apatite and confirms the formation of fine-scale apatite crystals. MTT assay, fluorescence, and SEM study demonstrate good cell viability and cell adhesion/proliferation of the Saos -2 cells, cultured on the developed composites under standard culture condition, and the difference in cell viability has been discussed in reference to substrate composition and roughness. Overall, HA-Ti composites exhibit comparable and even better in vitro bioactivity and cytocompatibility properties than HA. (c) 2012 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2013.

Temperature dependent structural and dielectric investigations of PbZr0.5Ti0.5O3 solid solution at the morphotropic phase boundary

PbZr1-xTixO3 ceramics synthesised by low temperature calcination followed by sintering at 1280 degrees C show a Morphotropic Phase Boundary (MPB) for compositions of x=0.44-0.51. The morphotropic phase boundary is wider for samples with smaller grain sizes due to the synthesis route. A Rietveld analysis is performed on a composition of x=0.5 composition to quantify the phase fractions of the tetragonal and monoclinic phases present in the PZT system. Temperature dependent X-ray diffraction and dielectric studies of PbZr0.5Ti0.5O3 composition demonstrated a phase transformation from monoclinic to tetragonal at 270 degrees C followed by a ferroelectric tetragonal to a paraelectric cubic transition at 370 degrees C. Thus, the poling of these ceramics should be performed below 270 degrees C to benefit from the presence of a monoclinic phase. (C) 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Rapid synthesis and characterization of an oxygen-deficient defect perovskite La4BaCu5O13+d phase

Oxygen-deficient defect perovskite La4BaCu5O13+d phase has been synthesized by the nitrate-citrate gel combustion method at 950 C for 2 h. Structural parameters were refined by the Rietveld refinement method using room-temperature powder XRD data. The La4BaCu5O13+d crystallizes in the tetragonal structure with space group P4/m (no. 83) and having the lattice parameters a=8.6508 c=3.8606 (1) Å and (2) Å, respectively. Oxygen content was determined by the iodometric titration. Low-temperature resistivity result reveals that La4BaCu5O13+d compound exhibit metallic behavior up to 15 K.

Fabrication and characterization of micro-arc oxidized fluoride containing titania films on Cp Ti

The present study is focussed at establishing an appropriate electrolyte system for developing electrochemically stable and fluorine (F) containing titania (F-TiO2) films on Cp Ti by micro-arc oxidation (MAO) technique. To fabricate the F-TiO2 films on Cp Ti, different electrolyte solutions of chosen concentrations of tri-sodium orthophosphate (TSOP, Na3PO4 center dot I2H2O), potassium hydroxide (KOH) and various F-containing compounds such as ammonium fluoride (NH4F), potassium fluoride (KF), sodium fluoride (NaF) and potassium fluorotitanate (K2TiF6) are employed. The structural and morphological characteristics, thickness and elemental composition of the developed films have been assessed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) techniques. The in-vitro electrochemical corrosion behavior of the films was studied under Kokubo simulated body fluid (SBF) environment by potentiodynamic polarization, long term potential measurement and electrochemical impedance spectroscopy (EIS) methods. The XRD and SEM-EDS results show that the rutile content in the films vary in the range of 15-37 wt% and the F and P contents in the films is found to be in the range of 2-3 at% and 2.9-4.7 at% respectively, suggesting that the anatase to rutile phase transformation and the incorporation of F and P into the films are significantly controlled by the respective electrolyte solution. The SEM elemental mapping results show that the electrolyte borne F and P elements are incorporated and distributed uniformly in all the films. Among all the films under study, the film developed with 5 g TSOP+2 g KOH+3 g K2TiF6 electrolyte system exhibits considerably improved in-vitro corrosion resistance and therefore best suited for biomedical applications. (C) 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

On the mechanism and the length scales involved in the ductile fracture of a bulk metallic glass

Some bulk metallic glasses (BMGs) exhibit high crack initiation toughness due to shear band mediated plastic flow at the crack tip and yet do not display additional resistance to crack growth due to the lack of a microstructure. Thus, at crack initiation, the fracture behavior of BMGs transits from that of ductile alloys to that of brittle ceramics. In this paper, we attempt to understand the physics behind the characteristic length from the notch root at which this transition occurs, through testing of four-point bend specimens made of a nominally ductile Zr-based BMG in three different structural states. In the as-cast state, both symmetric (mode I) and asymmetric (mixed mode) bend specimens are tested. The process of shear band mediated plastic flow followed by crack initiation at the notch root was monitored through in situ imaging. Results show that stable crack growth occurs inside a dominant shear band through a distance of, similar to 60 mu m, irrespective of the structural state and mode mixity, before attaining criticality. Detailed finite element simulations show that this length corresponds to the distance from the notch root over which a positive hydrostatic stress gradient prevails. The mean ridge heights on fractured surfaces are found to correlate with the toughness of the BMG. The Argon and Salama model, which is based on the meniscus instability phenomenon at the notch root, is modified to explain the experimentally observed physics of fracture in ductile BMGs. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Synthesis, microstructure and thermal expansion studies on Ca0 center dot 5+x/2Sr0 center dot 5+x/2Zr4P6-2x Si-2x O-24 system prepared by co-precipitation method

We report on the synthesis, microstructure and thermal expansion studies on Ca0 center dot 5 + x/2Sr0 center dot 5 + x/2Zr4P6 -aEuro parts per thousand 2x Si-2x O-24 (x = 0 center dot 00 to 1 center dot 00) system which belongs to NZP family of low thermal expansion ceramics. The ceramics synthesized by co-precipitation method at lower calcination and the sintering temperatures were in pure NZP phase up to x = 0 center dot 37. For x a parts per thousand yen 0 center dot 5, in addition to NZP phase, ZrSiO4 and Ca2P2O7 form as secondary phases after sintering. The bulk thermal expansion behaviour of the members of this system was studied from 30 to 850 A degrees C. The thermal expansion coefficient increases from a negative value to a positive value with the silicon substitution in place of phosphorous and a near zero thermal expansion was observed at x = 0 center dot 75. The amount of hysteresis between heating and cooling curves increases progressively from x = 0 center dot 00 to 0 center dot 37 and then decreases for x > 0 center dot 37. The results were analysed on the basis of formation of the silicon based glassy phase and increase in thermal expansion anisotropy with silicon substitution.

Reactive hot pressing of Ti-B-C and Ti-C at 1200 degrees C

Stoichiometric and non-stoichiometric powder mixtures of Ti-B4C and Ti-C with 1 wt% Ni were reactively hot pressed at 40 MPa, 1200 degrees C for 30 min. In both systems, the combined presence of Ni and non-stoichiometry enabled complete densification. While in Ti-C, non-stoichiometry by itself plays a significant role in promoting densification, the formation of intermediate borides in Ti-B4C powder mixtures requires the additional presence of Ni which promotes full reaction through the formation of a transient liquid as established previously in Ti-BN powder mixtures.

Dielectric and electrical conductivity properties of multi-stage spark plasma sintered HA-CaTiO3 composites and comparison with conventionally sintered materials

One of the different issues limiting the wider application of monolithic hydroxyapatite (HA) as an ideal bone replacement material is the lack of reasonably good electrical transport properties. The comprehensive electrical property characterization to evaluate the efficacy of processing parameters in achieving the desired combination of electroactive properties is considered as an important aspect in the development of HA-based bioactive material. In this perspective, the present work reports the temperature (RT-200 degrees C) and frequency (100 Hz-1 MHz) dependent dielectric properties and AC conductivity for a range of HA-CaTiO3 (HA-CT) composites, densified using both conventional pressureless sintering in air as well as spark plasma sintering in vacuum. Importantly, the AC conductivity of spark plasma sintered ceramics similar to upto 10(-5) (Omega cm)(-1)] are found to be considerably higher than the corresponding pressureless sintered ceramics similar to upto 10(-8) (Omega cm)(-1)]. Overall, the results indicate the processing route dependent functional properties of HA-CaTiO3 composites as well as related advantages of spark plasma sintering route. (C) 2013 Elsevier Ltd. All rights reserved.

Early osseointegration of a strontium containing glass ceramic in a rabbit model

The most important property of a bone cement or a bone substitute in load bearing orthopaedic implants is good integration with host bone with reduced bone resorption and increased bone regeneration at the implant interface. Long term implantation of metal-based joint replacements often results in corrosion and particle release, initiating chronic inflammation leading onto osteoporosis of host bone. An alternative solution is the coating of metal implants with hydroxyapatite (HA) or bioglass or the use of bulk bioglass or HA-based composites. In the above perspective, the present study reports the in vivo biocompatibility and bone healing of the strontium (Sr)-stabilized bulk glass ceramics with the nominal composition of 4.5SiO(2)-3Al(2)O(3)-1.5P(2)O(5)-3SrO-2SrF(2) during short term implantation of up to 12 weeks in rabbit animal model. The progression of healing and bone regeneration was qualitatively and quantitatively assessed using fluorescence microscopy, histological analysis and micro-computed tomography. The overall assessment of the present study establishes that the investigated glass ceramic is biocompatible in vivo with regards to local effects after short term implantation in rabbit animal model. Excellent healing was observed, which is comparable to that seen in response to a commercially available implant of HA-based bioglass alone. (C) 2013 Elsevier Ltd. All rights reserved.

Long ranged structural modulation in the pre-morphotropic phase boundary cubic-like state of the lead-free piezoelectric Na1/2Bi1/2TiO3-BaTiO3

The nature of the pre-morphotropic phase boundary (MPB) cubic-like state in the lead-free piezoelectric ceramics (1-x)Na1/2Bi1/2TiO3-(x)BaTiO3 at x similar to 0.06 has been examined in detail by electric field and temperature dependent neutron diffraction, x-ray diffraction, dielectric and ferroelectric characterization. The superlattice reflections in the neutron diffraction patterns cannot be explained with the tetragonal P4bm and the rhombohedral (R3c) phase coexistence model. The cubic like state is rather a result of long ranged modulated complex octahedral tilt. This modulated structure exhibits anomalously large dielectric dispersion. The modulated structure transforms to a MPB state on poling. The field-stabilized MPB state is destroyed and the modulated structure is restored on heating the poled specimen above the Vogel-Fulcher freezing temperature. The results show the predominant role of competing octahedral tilts in determining the nature of structural and polar states in Na1/2Bi1/2TiO3-based ferroelectrics. (C) 2013 AIP Publishing LLC.

Optimization of rheological properties of photopolymerizable alumina suspensions for ceramic microstereolithography

Microstereolithography (MSL) is a rapid prototyping technique to fabricate complex three-dimensional (3D) structure in the microdomain involving different materials such as polymers and ceramics. The present effort is to fabricate microdimensional ceramics by the MSL system from a non-aqueous colloidal slurry of alumina. This slurry predominantly consists of two phases i.e. sub-micrometer solid alumina particles and non-aqueous reactive difunctional and trifunctional acrylates with inert diluent. The first part of the work involves the study of the stability and viscosity of the slurry using different concentrations of trioctyl phosphine oxide (TOPO) as a dispersant. Based on the optimization, the highest achievable solid loadings of alumina has been determined for this particular colloidal suspension. The second part of the study highlights the fabrication of several micro-dimensional alumina structures by the MSL system. (C) 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.