Supported Co catalysts prepared as thin films by magnetron sputtering for sodium borohydride and ammonia borane hydrolysis

Supported Co catalysts were prepared for sodium borohydride and ammonia borane hydrolysis by magnetron sputtering for the first time under different conditions. Ni foam was selected as support. Deposition conditions (time, pressure, and power) were varied to improve catalytic activity. A decrease in deposition power from 200 to 50 W, leads to a decrease in crystallite and column size and a higher activity of catalysts. The increase in deposition pressure from 1.5 × 10−2 to 4.5 × 10−2 mbar produces same effect but in this case the enhancement in activity is higher because amorphous materials were obtained. The highest activity for SB hydrolysis was 2650 ml min−1 gcat−1 for the 50 W Co 4.5 (4 h) sample (Ea = 60 ± 2 kJ mol−1). For AB hydrolysis activity for the 50 W Co 3.2 (4 h) sample was similar. Durability of the thin films was tested for both reactions upon cycling (14 cycles). Diluted acid washing was effective to recover the activity for sodium borohydride reaction but not for ammonia borane hydrolysis. The strong Co–NH3 interactions explain the non-efficiency of the acid washing

Nanoscale characterization of Co and Co-B catalytic coatings before and after catalytic tests for the sodium borohydride hydrolysis

Capítulo tomado de https://onlinelibrary.wiley.com/doi/pdf/10.1002/9783527808465.EMC2016.5347Spanish MINECO (CTQ2012-32519 and CTQ2015-65918)CONSOLIDER FUNCOAT+ (MAT2015-69035-REDC)Junta de Andalucía (PE2012-TEP862)CSIC (PIE201460E018)Laboratory for Nanoscopies and Spectroscopies (LANE) at the ICMSTalent-Hub Program funded by the Junta de Andalucía and the European Commission under the Co-funding of the 7thFramework Program in the People Program (Marie Curie Special Action

Characterization and Validation of a‑Si Magnetron-Sputtered Thin Films as Solid He Targets with High Stability for Nuclear Reactions

In this work, we present our magnetron sputtering based methodology to produce amorphous silicon coatings with closed porosity, as a strategy to fabricate solid helium targets, in the form of supported or self-supported thin films, for nuclear reactions. We show how by changing the He working pressure it is possible to obtain highly porous homogeneous structures incorporating different He amounts. These porous coatings (a- Si:He) are very reproducible from run to run, and the high He amount incorporated makes them excellent candidates for solid He targets. The possibility of producing self-supported films is illustrated here, and its potential use in inverse kinematics experiments with radioactive beams is shown through the dispersion in forward geometry of a stable 6Li beam. Also the elastic scattering cross-sections for proton from helium were determined using an a-Si:He coating. The results agree well with the ones reported in the literature. These two examples validate our coatings as good candidates to be used as solid He targets in nuclear reactions. The stability of He inside the coatings, fundamental for its use as solid He targets, was investigated, both over time and after irradiation. The coatings proved to be very stable, and the amount of He inside the pores remains unaltered at least 2 years after deposition and after high irradiation fluence (5 × 1017 particles/cm2; with a dose rate of 5 × 1012 particles/(cm2 s)).Ministerio de Economía y Competitividad FPA2013-47327-C2-1-R, MAT2015-69035- REDCConsejo Superior de Investigaciones Científicas 201460E018European Union CT-REGPOT-2011-28589

Development of porous silver nanoparticle/polycaprolactone/polyvinyl alcohol coatings for prophylaxis in titanium interconnected samples for dental implants

Stress shielding phenomenon, poor osseointegration, or bacterial infections of titanium dental implants are widely recognized as key problems that deeply affect their survival rate. In this work, a joint solution to solve these three limitations is proposed. The first two issues were minimized applying porous Ti samples. This substrate exhibits an appropriated biomechanical equilibrium (stiffness and mechanical resistance) and good biofunctionality (ability to promote bone ingrowth). On the other hand, the porous Ti disc was coated with biocompatible and non-toxic polymeric composites matrices using poly-ε-caprolactone and partially acetylated polyvinyl alcohol, combined with silver nanoparticles as a therapeutic antimicrobial agent. The optimization of the best blend composition and optimal nanoparticles concentration were investigated. Finally, the two composites with the best antimicrobial activity were infiltrated into porous Ti discs. The deposited coatings presented good adhesion and a honeycomb-like surface structure that could promote vascularization of the implant and enhance osseointegration.Ministry of Science and Innovation of Spain grant PID2019-109371GB-I00Junta de Andalucía (Spain) PAIDI P20_00671FEDER Andalucía US-1380878Universidad de Sevilla, Spain PPI505/2020Universidad de Sevilla, Spain PPI532/202

Development of porous silver nanoparticle/polycaprolactone/polyvinyl alcohol coatings for prophylaxis in titanium interconnected samples for dental implants

Stress shielding phenomenon, poor osseointegration, or bacterial infections of titanium dental implants are widely recognized as key problems that deeply affect their survival rate. In this work, a joint solution to solve these three limitations is proposed. The first two issues were minimized applying porous Ti samples. This substrate exhibits an appropriated biomechanical equilibrium (stiffness and mechanical resistance) and good biofunctionality (ability to promote bone ingrowth). On the other hand, the porous Ti disc was coated with biocompatible and non-toxic polymeric composites matrices using poly-ε-caprolactone and partially acetylated polyvinyl alcohol, combined with silver nanoparticles as a therapeutic antimicrobial agent. The optimization of the best blend composition and optimal nanoparticles concentration were investigated. Finally, the two composites with the best antimicrobial activity were infiltrated into porous Ti discs. The deposited coatings presented good adhesion and a honeycomb-like surface structure that could promote vascularization of the implant and enhance osseointegration.Ministerio de Ciencia e Innovación PID2019-109371GB-I00Junta de Andalucía PAIDI 2020, P20_00671Universidad de Sevilla US-138087, PPI505/2020, PPI532/202

Pd-C catalytic thin films prepared by magnetron sputtering for the decomposition of formic acid

Formic acid is an advantageous liquid organic hydrogen carrier. It is relatively nontoxic and can be synthesized by the reaction of CO2 with sustainable hydrogen or by biomass decompo-sition. As an alternative to more widely studied powdery catalysts, supported Pd-C catalytic thin films with controlled nanostructure and compositions were newly prepared in this work by mag-netron sputtering on structured supports and tested for the formic acid decomposition reaction. A two-magnetron configuration (carbon and tailored Pd-C targets) was used to achieve a reduction in Pd consumption and high catalyst surface roughness and dispersion by increasing the carbon con-tent. Activity and durability tests were carried out for the gas phase formic acid decomposition reaction on SiC foam monoliths coated with the Pd-C films and the effects of column width, surface roughness and thermal pre-reduction time were investigated. Activity of 5.04 molH2∙gPd−1∙h−1 and 92% selectivity to the dehydrogenation reaction were achieved at 300 °C for the catalyst with a lower column width and higher carbon content and surface roughness. It was also found that deactivation occurs when Pd is sintered due to the elimination of carbon and/or the segregation and agglomera-tion of Pd upon cycling. Magnetron sputtering deposition appears as a promising and scalable route for the one-step preparation of Pd-C catalytic films by overcoming the different deposition characteristics of Pd and C with an appropriate experimental design.Ministerio de Ciencia, Innovación y Universidades RTI2018-093871-B-I0

Simultaneous quantification of light elements in thin films deposited on Si substrates using proton EBS (Elastic Backscattering Spectroscopy)

Quantification of light elements content in thin films is an important and difficult issue in many technological fields such as polymeric functional thin films, organic thin film devices, biomaterials, and doped semiconducting structures. Light elements are difficult to detect with techniques based on X-ray emission, such as energy dispersive analysis of X-rays (EDAX). Other techniques, like X-ray photoelectron spectroscopy (XPS), can easily quantify the content of light elements within a surface but often these surface measurements are not representative of the lights elements global composition of the thin film. Standard Rutherford backscattering spectroscopy (RBS), using alpha particles as probe projectiles, is not a good option to measure light elements deposited on heavier substrates composed of heavier elements like Si or glass. Nuclear Reaction Analysis (NRA) offers a good quantification method, but most of the nuclear reactions used are selective for the quantification of only one element, so several reactions and analysis are necessary to measure different elements. In this study, Elastic Backscattering Spectroscopy (EBS) using proton beams of 2.0 MeV simultaneously quantified different light elements (helium, carbon, nitrogen, oxygen, and fluorine) contained in thin films supported on silicon substrates. The capabilities of the proposed quantification method are illustrated with examples of the analysis for a series of thin film samples: amorphous silicon with helium bubbles, fluorinated silica, fluorinated diamond-like carbon and organic thin films. It is shown that this simple and versatile procedure allows the simultaneous quantification of light elements in thin films with thicknesses in the 200-500 nm range and contents lower than 10 at.%.España Mineco CSD2007- 42 CSD2008-00023 MAT2010-21228 MAT2010-1844

Influence of Femtosecond Laser Modification on Biomechanical and Biofunctional Behavior of Porous Titanium Substrates

Bone resorption and inadequate osseointegration are considered the main problems of titanium implants. In this investigation, the texture and surface roughness of porous titanium samples obtained by the space holder technique were modified with a femtosecond Yb-doped fiber laser. Different percentages of porosity (30, 40, 50, and 60 vol.%) and particle range size (100–200 and 355–500 μm) were compared with fully-dense samples obtained by conventional powder metallurgy. After femtosecond laser treatment the formation of a rough surface with micro-columns and micro-holes occurred for all the studied substrates. The surface was covered by ripples over the micro-metric structures. This work evaluates both the influence of the macro-pores inherent to the spacer particles, as well as the micro-columns and the texture generated with the laser, on the wettability of the surface, the cell behavior (adhesion and proliferation of osteoblasts), micro-hardness (instrumented micro-indentation test, P–h curves) and scratch resistance. The titanium sample with 30 vol.% and a pore range size of 100–200 μm was the best candidate for the replacement of small damaged cortical bone tissues, based on its better biomechanical (stiffness and yield strength) and biofunctional balance (bone in-growth and in vitro osseointegration).Ministerio de Ciencia e Innovación del Gobierno de España PID2019-109371GB-100Junta de Andalucía (Spain) PAIDI P20-0067

Procedimiento de obtención de recubrimientos mediante pulverización catódica y recubrimiento obtenible mediante dicho procedimiento

Procedimiento de obtención de recubrimientos mediante pulverización catódica y recubrimiento obtenible mediante dicho procedimiento.El objeto de la invención es un procedimiento de obtención de recubrimientos realizado por deposición de capas mediante pu

Electropolymerized polypyrrole silver nanocomposite coatings on porous Ti substrates with enhanced corrosion and antibacterial behavior for biomedical applications

This work proposes an innovative strategy that combines two well-known easy and economical preparation techniques: powder metallurgy based space-holder (SH) technique to provide porous biocompatible Ti substrates with balanced biomechanical behavior (for cortical bone tissue substitution) promoting bone ingrowth and biocoating infiltration, and electropolymerization to coat these substrates with the polypyrrole–silver nanoparticles (PPy-AgNPs) composite conductive polymers improving its corrosion resistance, biocompatibility with enhanced antibacterial activity. The deposited PPy-based coatings present a cauliflower-like structure well adhered to the porous substrates. The macroporosity of and rough inner pore surface of Ti SH substrates are responsible for the superior adhesion of the conductive polymer comparing to typical denser substrates obtained by powder metallurgy or forging. The corrosion protection properties of the coatings were investigated by open circuit potential and Anodic Polarization in PBS media to simulate possible implant conditions, revealing improved corrosion resistance for the composite coatings. The bioactivity of the coatings was evaluated by immersion tests, revealing the formation of Hydroxyapatite after 90-day immersion in PBS. In both PPy and PPy-AgNPs composite coatings, a displacement of the polarization curves to more noble potentials and a decrease in the current density, indicated that the coating's protective character is maintained after 90-day immersion in PBS. The antibacterial activity was assessed by using the Kirby–Bauer disk-diffusion method against Staphylococcus aureus (ATCC 25923). The inhibition halo increased from 5.5 ± 0.4 mm for the bare substrate to 8.2 ± 0.6 mm for the PPy-coated substrate and to 12.5 ± 0.7 mm for the PPy-AgNPs-coated porous Ti. This feature associated to the improved corrosion protection and biocompatibility would significantly contribute to the success of the potential use of porous Ti implants by SH technique envisaging substitution of small damaged bone tissues for example in tumors