Better early osteogenesis of electroconductive hydroxyapatite-calcium titanate composites in a rabbit animal model

In view of the fact that bone healing can be enhanced due to external electric field application, it is important to assess the influence of the implant conductivity on the bone regeneration in vivo. To address this issue, this study reports the in vivo biocompatibility property of multistage spark plasma sintered hydroxyapatite (HA)-80 wt % calcium titanate (CaTiO3) composites and monolithic HA, which have widely different conductivity property (14 orders of magnitude difference). The ability of bone regeneration was assessed by implantation in cylindrical femoral bone defects of rabbit animal model for varying time period of 1, 4, and 12 weeks. The overall assessment of the histology results suggests that the progressive healing of bone defects around HA-80 wt % CaTiO3 is associated with a better efficacy with respect to (w.r.t) early stage neobone formation, which is histomorphometrically around 140% higher than monolithic HA. Overall, this study demonstrates that the in vivo biocompatibility property of HA-80 wt % CaTiO3 with respect to local effects after 12 weeks of implantation is not compromised both qualitatively and quantitatively, and a comparison with control implant (HA) points toward the critical role of electrical conductivity on better early stage bone regeneration. (c) 2013 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 102A: 842-851, 2014.

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.

Europium-doped calcium titanate: Optical and structural evaluations

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural disorder-dependent upconversion in Er3+/Yb3+-doped calcium titanate

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of calcium ion deposition on apatite-inducing ability of porous titanium for biomedical applications

In the present study, the influence of calcium ion deposition on the apatite-inducing ability of porous titanium(Ti) was investigated in a modified simulated body fluid (m-SBF). Calcium hydroxide (Ca(OH)₂) solutions with five degrees of saturation were used to hydrothermally deposit Ca ions on porous Ti with a porosity of 80%. Apatite-inducing ability of the Ca-ion-deposited porous Ti was evaluated by soaking them in m-SBF for up to 14 days. Scanning electron microscopy (SEM) and X-ray diffractometry (XRD) confirmed that a thin layer of calcium titanate (CaTiO₃)/calcium oxide (CaO) mixture with a nanostructured porous network was produced on porous Ti substrates after hydrothermal treatment at 200 °C for 8 h. X-ray photoelectron spectroscopy results demonstrated that the content of the Ca ions deposited on Ti and the thickness of the CaTiO₃/CaO layer increased with increasing saturation degree of the Ca(OH)₂ solution. The thickest (over 10 nm) CaTiO₃/CaO layer with the highest Ca content was achieved on the Ti treated in an oversaturated Ca(OH)₂ solution (0.2 M). SEM, XRD, transmission electron microscopy and Fourier transformed infrared spectroscopy analysis indicated that the porous Ti samples deposited with the highest content of Ca ions exhibited the best apatite-inducing ability, producing a dense and complete carbonated apatite coating after a 14 day soaking in m-SBF. The present study illustrated the validity of using Ca ion deposition as a pre-treatment to endow desirable apatite-inducing ability of porous Ti for bone tissue engineering applications.

Dielectric Studies of laser ablated Ca doped BaTiO3 thin films

Recently, there has been growing interest in Ca modified BaTiO3 structures due to their larger electro-optic coefficients for their use in optical storage of information over conventional BaTiO3 crystals. Barium Calcium Titanate (BCT) shows promising applications in advanced laser systems, optical interconnects and optical storage devices. BaTiO3 thin films of varied Ca (3 at. % - 15 at. %) doping were deposited using pulsed laser ablation (KrF excimer laser) technique over Pt/Si substrates. The stoichiometric and the compositional analysis were carried out using EDAX and SIMS. The dielectric studies were done at the frequency regime of 40 Hz to 100 kHz at different ambient temperatures from 200 K to 600 K. The BCT thin films exhibited diffuse phase transition, which was of a typical non lead relaxor behavior and had high dielectric constant and low dielectric loss. The phase transition for the different compositions of BCT thin films was near the room temperature, showing a marked departure from the bulk phase transition. The C - V and the hysteresis behavior confirmed the ferroelectric nature below the phase transition and paraelectric at the room temperature.

Synthesis, characterization, EPR and thermoluminescence properties of CaTiO3 nanophosphor

Calcium titanate (CaTiO3) nanophosphors were synthesized by three different routes namely solution combustion (SC), modified solid-state reaction (MSS) and solid-state (SS) methods. Rietveld refinement studies revealed the presence of an orthorhombic structure with traces of CaCO3. The crystallite sizes were found to be in the 43-45 nm range. TEM studies also confirm the nano size with well crystalline nature. EPR spectrum for SS method exhibits a broad resonance signal at g = 2.027 is attributed to TiO6](9-) center, whereas in MSS sample the resonance signals are attributed to surface electron and hole trapping sites. The TL behavior has been investigated for the first time using gamma-irradiation. TL glow peak at 169 degrees C were recorded in CaTiO3 prepared by SC, MSS and SS methods. The trapping parameters such as activation energy (E) and order of kinetics (b) were estimated using peak shape method and results are discussed in detail. (C) 2013 Elsevier Ltd. All rights reserved.

Substrate conductivity dependent modulation of cell proliferation and differentiation in vitro

In designing and developing various biomaterials, the influence of substrate properties, like surface topography, stiffness and wettability on the cell functionality has been investigated widely. However, such study to probe into the influence of the substrate conductivity on cell fate processes is rather limited. In order to address this issue, spark plasma sintered HA-CaTiO3 (Hydroxyapatite-Calcium titanate) has been used as a model material system to showcase the effect of varying conductivity on cell functionality. Being electroactive in nature, mouse myoblast cells (C2C12) were selected as a model cell line in this study. It was inferred that myoblast adhesion/growth systematically increases with substrate conductivity due to CaTiO3 addition to HA. Importantly, parallel arrangement of myoblast cells on higher CaTiO3 containing substrates indicate that self-adjustable cell patterning can be achieved on conductive biomaterials. Furthermore, enhanced myoblast assembly and myotube formation were recorded after 5 days of serum starvation. Overall, the present study conclusively establishes the positive impact of the substrate conductivity towards cell proliferation and differentiation as well as confirms the efficacy of HA-CaTiO3 biocomposites as conductive platforms to facilitate the growth, orientation and fusion of myoblasts, even when cultured in the absence of external electric field.

Perovskite ceramic nanoparticles in polymer composites for augmenting bone tissue regeneration

There is increasing interest in the use of nanoparticles as fillers in polymer matrices to develop biomaterials which mimic the mechanical, chemical and electrical properties of bone tissue for orthopaedic applications. The objective of this study was to prepare poly(epsilon-caprolactone) (PCL) nanocomposites incorporating three different perovskite ceramic nanoparticles, namely, calcium titanate (CT), strontium titanate (ST) and barium titanate (BT). The tensile strength and modulus of the composites increased with the addition of nanoparticles. Scanning electron microscopy indicated that dispersion of the nanoparticles scaled with the density of the ceramics, which in turn played an important role in determining the enhancement in mechanical properties of the composite. Dielectric spectroscopy revealed improved permittivity and reduced losses in the composites when compared to neat PCL. Nanofibrous scaffolds were fabricated via electrospinning. Induction coupled plasma-optical emission spectroscopy indicated the release of small quantities of Ca+2, Sr+2, Ba+2 ions from the scaffolds. Piezo-force microscopy revealed that BT nanoparticles imparted piezoelectric properties to the scaffolds. In vitro studies revealed that all composites support osteoblast proliferation. Expression of osteogenic genes was enhanced on the nanocomposites in the following order: PCL/CT>PCL/ST>PCL/BT>PCL. This study demonstrates that the use of perovskite nanoparticles could be a promising technique to engineer better polymeric scaffolds for bone tissue engineering.

Pressure-induced electrical and structural anomalies in Pb(1-x)Ca(x)TiO(3) thin films grown at various oxygen pressures by chemical solution route

Lead calcium titanate (Pb(1-x)Ca(x)TiO(3) or PCT) thin films have been thermally treated under different oxygen pressures, 10, 40 and 80 bar, by using the so-called chemical solution deposition method. The structural, morphological, dielectric and ferroelectric properties were characterized by x-ray diffraction, FT-infrared and Raman spectroscopy, atomic force microscopy and polarization-electric-field hysteresis loop measurements. By annealing at a controlled pressure of around 10 and 40 bar, well-crystallized PCT thin films were successfully prepared. For the sample submitted to 80 bar, the x-ray diffraction, Fourier transformed-infrared and Raman data indicated deviation from the tetragonal symmetry. The most interesting feature in the Raman spectra is the occurrence of intense vibrational modes at frequencies of around 747 and 820 cm(-1), whose presence depends strongly on the amount of the pyrochlore phase. In addition, the Raman spectrum indicates the presence of symmetry-breaking disorder, which would be expected for an amorphous (disorder) and mixed pyrochlore-perovskite phase. During the high-pressure annealing process, the crystallinity and the grain size of the annealed film decreased. This process effectively suppressed both the dielectric and ferroelectric behaviour. Ferroelectric hysteresis loop measurements performed on these PCT films exhibited a clear decrease in the remanent polarization with increasing oxygen pressure.

Electrophoretic deposition of Ba0.77Ca0.23TiO3 nanopowders

Ba0.77Ca0.23TiO3 (BCT23) nanometric powders, synthesized by the modified Pechini method, were used as precursor to produce thick films (50-130 mu m) employing the electrophoretic deposition (EPD) technique. The BCT23 powder presented a single crystalline phase with an average particle size and a crystallite size of similar to 60 nm and similar to 20 nm, respectively, when calcined at 800 degrees C/2h. BCT23 thick films were deposited on platinum substrates starting from different suspensions prepared by dispersion of the powder into: isopropyl alcohol (IPA) or a mixture of acetylacetone (Acac) and ethanol (EtOH) (1:1, volumetric ratio). A milling process was used to deagglomerate the powders in order to increase the suspension stability and improving the deposition. Dense and crack free thick films with uniform microstructure were obtained after sintering at 1300 degrees C/2 h from Acac+EtOH solution. (C) 2007 Elsevier B.V. All rights reserved.

Pressure-induced electrical and structural anomalies in Pb1-xCaxTiO3 thin films grown at various oxygen pressures by chemical solution route

Lead calcium titanate (Pb1-xCaxTiO3 or PCT) thin films have been thermally treated under different oxygen pressures, 10, 40 and 80 bar, by using the so-called chemical solution deposition method. The structural, morphological, dielectric and ferroelectric properties were characterized by x-ray diffraction, FT-infrared and Raman spectroscopy, atomic force microscopy and polarization-electric-field hysteresis loop measurements. By annealing at a controlled pressure of around 10 and 40 bar, well-crystallized PCT thin films were successfully prepared. For the sample submitted to 80 bar, the x-ray diffraction, Fourier transformed-infrared and Raman data indicated deviation from the tetragonal symmetry. The most interesting feature in the Raman spectra is the occurrence of intense vibrational modes at frequencies of around 747 and 820 cm(-1), whose presence depends strongly on the amount of the pyrochlore phase. In addition, the Raman spectrum indicates the presence of symmetry-breaking disorder, which would be expected for an amorphous (disorder) and mixed pyrochlore-perovskite phase. During the high-pressure annealing process, the crystallinity and the grain size of the annealed film decreased. This process effectively suppressed both the dielectric and ferroelectric behaviour. Ferroelectric hysteresis loop measurements performed on these PCT films exhibited a clear decrease in the remanent polarization with increasing oxygen pressure.

Synthesis of (Ca,Nd)TiO3 powders by complex polymerization, Rietveld refinement and optical properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Room temperature photoluminescence of BCT prepared by Complex Polymerization Method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of microwave energy on structural and photoluminescent behavior of CaTiO3 powders

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)