Cristina Caparrós

Effect of filler size and concentration on the structure and properties of poly(vinylidene fluoride)/BaTiO3 nanocomposites

The effect of filler size and content in the thermal, mechanical, and electrical response of poly(vinylidene fluoride) (PVDF)/BaTiO3 nanocomposites has been investigated. Dielectric constant increases significantly with increasing filler content and decreasing filler size. Space charge effects at the interface between BaTiO3 and PVDF strongly influence the dielectric response. The electroactive β-phase of PVDF is nucleated by the presence of the ceramic filler, the effect being strongly dependent on filler size and independent on filler content. This filler/matrix interaction is also responsible for the variations observed in the activation energy of the thermal degradation of the polymer. Smaller particles lead to larger relative contact areas and are responsible for the main variations observed in the thermal, mechanical, and electrical properties of the composites.

Effect of the carbon nanotube surface characteristics on the conductivity and dielectric constant of carbon nanotube/poly(vinylidene fluoride) composites

Commercial multi-walled carbon nanotubes (CNT) were functionalized by oxidation with HNO3, to introduce oxygen-containing surface groups, and by thermal treatments at different temperatures for their selective removal. The obtained samples were characterized by adsorption of N2 at -196°C, temperature-programmed desorption and determination of pH at the point of zero charge. CNT/poly(vinylidene fluoride) composites were prepared using the above CNT samples, with different filler fractions up to 1 wt%. It was found that oxidation reduced composite conductivity for a given concentration, shifted the percolation threshold to higher concentrations, and had no significant effect in the dielectric response.

Development of inkjet printed strain sensors

Strain sensors with different architectures, such as single sensors, sensor arrays and a sensor matrix have been developed by inkjet printing technology. Sensors with gauge factors up to 2.48, dimensions of 1.5 mm × 1.8 mm and interdigitated structures with a distance of 30 μm between the finger lines have been achieved based on PeDOT (poly(3,4-ethylenedioxythiophene) and conductive ink. Strain gauges based on silver ink have also been achieved with a gauge factor of 0.35. Performance tests including 1000 mechanical cycles have been successfully carried out for the development of smart prosthesis applications.

The effect of nanotube surface oxidation on the electrical properties of multiwall carbon nanotube/poly(vinylidene fluoride) composites

Carbon nanotube/poly(vinylidene fluoride) (CNT/PVDF) composites were prepared using CNT with different oxidation and thermal treatments. The oxidation procedure leads to CNT with the most acidic characteristics that lower the degree of crystallinity of the polymer and contribute to a large increase of the dielectric constant. The surface treatments, in general, increase the percolation threshold and decrease conductivity. The surface treatments do not seem to affect CNT interactions and similar degrees of dispersion are achieved in all cases, as shown by the SEM results. The maximum value of the dielectric constant is ~630. It is demonstrated that the composite conductivity can be attributed to a hopping mechanism that is strongly affected by the surface treatment of the CNT.

Design and characterization of Ni2+ and Co2+ decorated Porous Magnetic Silica spheres synthesized by hydrothermal-assisted modified-Stöber method for His-tagged proteins separation

The complete elimination of enzymes from the reaction mixture and the possibility of its recycling for several rounds result in great benefits, allowing the reduction of the enzyme consumption and their usability in continuous processes. In this work, it is evaluated the capture of a H6-tagged green fluorescence protein (GFP-H6) on porous magnetic spheres using the Co(2+) and Ni(2+) affinity adsorption as a possible cost-effective and up-scaled alternative way for the immobilization of His-tagged proteins. For this purpose, Porous Magnetic Silica (PMS) spheres were synthesized by one-step hydrothermal-assisted modified-Stöber method. The obtained spheres have a homogenous size distribution of 400 nm diameter. The γ-Fe(2)O(3) nanoparticles are homogenously distributed in the silica matrix. The obtained PMS spheres have a saturation magnetization of about 10 emu/g. Magnetophoresis measurements show a total separation time of 16 min at 60 T/m. The obtained PMS spheres were successfully and homogenously decorated with Co(2+) and Ni(2+) and then evaluated for the capture of a GFP-H6 protein. The results were compared with the performance of the commercial beads Dynabeads® His-Tag Isolation & Pulldown.

Influence of zeolite structure and chemistry on the electrical response and crystallization phase of poly(vinylidene fluoride)

Zeolites with framework types LTL, LTA, FAU, and MFI were synthesized and used as fillers to prepare PVDF/zeolite composites. The obtained composites showed structural and electrical dependence on the pore system and chemical content of the inorganic host. The larger polymer-zeolite electrostatic interactions of the Y and A zeolites lead the polymer to crystallize in the electroactive γ-phase, which in the case of the L zeolite is prevented due to the reduced interaction area. The solvent and water encapsulation ability of the zeolite as well as improve of the dielectric response of the composite is directly related to the Si/Al ratio, leading zeolites with lower Si/Al ratios to larger dielectric responses and encapsulation efficiencies in the composites. These effects show also some dependency on the dimensionality of the pore system; the zeolite L-containing 1D channels showing superior dielectric performance than the 3D pore system of zeolite Y.

Thermal Properties of Electrospun Poly(Lactic Acid) Membranes

Poly(lactic acid) (PLA) electrospun membranes were obtained by electrospinning and characterized by scanning electron microscopy (SEM) and thermal analysis. The polymer membranes showed a random fiber distribution with a mean diameter of 1 μm (±300 nm). Differential scanning calorimetry (DSC) experiments showed that the membranes had a glass transition, cold crystallization, and melting temperatures of 54, 90, and 151°C, respectively. The kinetic study of thermal degradation of PLA under a nitrogen atmosphere was performed by means of thermogravimetry (TGA). It was found that the thermal decomposition kinetics of PLA could be interpreted in terms of a multi-step degradation mechanism. Several theoretical models were applied to the TGA data. The activation energies obtained by the Broido and Ozawa–Flynn–Wall (OFW) models were in good agreement with the value of the activation energy calculated by the Kissinger method.

Bioactive macroporous titanium implants highly interconnected.

Intervertebral implants should be designed with low load requirements, high friction coefficient and low elastic modulus in order to avoid the stress shielding effect on bone. Furthermore, the presence of a highly interconnected porous structure allows stimulating bone in-growth and enhancing implant-bone fixation. The aim of this study was to obtain bioactive porous titanium implants with highly interconnected pores with a total porosity of approximately 57 %. Porous Titanium implants were produced by powder sintering route using the space holder technique with a binder phase and were then evaluated in an in vivo study. The size of the interconnection diameter between the macropores was about 210 μm in order to guarantee bone in-growth through osteblastic cell penetration. Surface roughness and mechanical properties were analyzed. Stiffness was reduced as a result of the powder sintering technique which allowed the formation of a porous network. Compression and fatigue tests exhibited suitable properties in order to guarantee a proper compromise between mechanical properties and pore interconnectivity. Bioactivity treatment effect in novel sintered porous titanium materials was studied by thermo-chemical treatments and were compared with the same material that had undergone different bioactive treatments. Bioactive thermo-chemical treatment was confirmed by the presence of sodium titanates on the surface of the implants as well as inside the porous network. Raman spectroscopy results suggested that the identified titanate structures would enhance in vivo apatite formation by promoting ion exchange for the apatite formation process. In vivo results demonstrated that the bioactive titanium achieved over 75 % tissue colonization compared to the 40 % value for the untreated titanium.

Improving the binding capacity of Ni2+ decorated porous magnetic silica spheres for histidine-rich protein separation

Biomagnetic immobilization of histidine-rich proteins based on the single-step affinity adsorption of transition metal ions continues to be a suitable practice as a cost effective and a up scaled alternative to the to multiple-step chromatographic separations. In our previous work, we synthesised Porous Magnetic silica (PMS) spheres by one-step hydrothermal-assisted modified-stöber method. The obtained spheres were decorated with Ni(2+) and Co(2+), and evaluated for the capture of a H6-Tagged green fluorescence protein (GFP-H6) protein. The binding capacity of the obtained spheres was found to be slightly higher in the case Ni(2+) decorated PMS spheres (PMSNi). However, comparing with commercial products, the binding capacity was found to be lower than the expected. In this way, the present work is an attempt to improve the binding capacity of PMSNi to histidine-rich proteins. We find that increasing the amount of Ni(2+) onto the surface of the PMS spheres leads to an increment of the binding capacity to GFP-H6 by a factor of two. On the other hand, we explore how the size of histidine-rich protein can affect the binding capacity comparing the results of the GFP-6H to those of the His-tagged α-galactosidase (α-GLA). Finally, we demonstrate that the optimization of the magnetophoresis parameters during washing and eluting steps can lead to an additional improvement of the binding capacity.

Treatment of cotton with an alkaline Bacillus spp cellulase: Activity towards crystalline cellulose

We analysed the influence of several enzymatic treatment processes using an alkaline cellulase enzyme from Bacillus spp. on the sorption properties of cotton fabrics. Although cellulases are commonly applied in detergent formulations due to their anti‐redeposition and depilling benefits, determining the mechanism of action of alkaline cellulases on cotton fibres requires a deeper understanding of the morphology and structure of cotton fibres in terms of fibre cleaning. The accessibility of cellulose fibres was studied by evaluating the iodine sorption value and by fluorescent‐labelled enzyme microscopy; the surface morphology of fabrics was analysed by scanning microscopy. The action of enzyme hydrolysis over short time periods can produce fibrillation on cotton fibre surface without any release of cellulosic material. The results indicate that several short consecutive treatments were more effective in increasing the fibre accessibility than one long treatment. In addition, no detectable hydrolytic activity, in terms of reducing sugar production, was found.