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Plasma-based VAD process for multiply doped glass powders and high-performance fiber preforms with outstanding homogeneity
An innovative approach using the vapor axial deposition (VAD), for the preparation of silica-based high-power fiber laser preforms, is described in this study. The VAD uses a plasma deposition system operating at atmospheric pressure, fed by a single, chemically adapted solution containing precursors of laser-active dopants (e.g., Yb2O3), glass-modifier species (e.g., Al2O3), and the silica matrix. The approach enables simultaneous doping with multiple optically active species and overcomes some of the current technological limitations encountered with well-established fiber preform technologies in terms of dopant distribution, doping levels, and achievable active core diameter. The deposition of co-doped silica with outstanding homogeneity is proven by Raman spectroscopy and electron probe microanalysis. Yb2O3 concentrations are realized up to 0.3 mol% in SiO2, with simultaneous doping of 3 mol% of Al2O3.
Application of Thermal Response Measurements to Investigate Enhanced Water Adsorption Kinetics in Ball-Milled C2N-Type Materials
Sorption-based water capture is an attractive solution to provide potable water in arid regions. Heteroatom-decorated microporous carbons with hydrophilic character are promising candidates for water adsorption at low humidity, but the strong affinity between the polar carbon pore walls and water molecules can hinder the water transport within the narrow pore system. To reduce the limitations of mass transfer, C2N-type carbon materials obtained from the thermal condensation of a molecular hexaazatriphenylene-hexacarbonitrile (HAT-CN) precursor were treated mechanochemically via ball milling. Scanning electron microscopy as well as static light scattering reveal that large pristine C2N-type particles were split up to a smaller size after ball milling, thus increasing the pore accessibility which consequently leads to faster occupation of the water vapor adsorption sites. The major aim of this work is to demonstrate the applicability of thermal response measurements to track these enhanced kinetics of water adsorption. The adsorption rate constant of a C2N material condensed at 700 °C remarkably increased from 0.026 s−1 to 0.036 s−1 upon ball milling, while maintaining remarkably high water vapor capacity. This work confirms the advantages of small particle sizes in ultramicroporous materials on their vapor adsorption kinetics. It is demonstrated that thermal response measurements are a valuable and time-saving method to investigate water adsorption kinetics, capacities, and cycling stability.
Porous spherical gold nanoparticles via a laser induced process
Nanoparticles consisting of a mixture of several metals and also porous nanoparticles due to their special structure exhibit properties that find applications in spectroscopic detection or catalysis. Different approaches of top down or bottom up technologies exist for the fabrication of such particles. We present a novel combined approach for the fabrication of spherical porous gold nanoparticles on low-cost glass substrates under ambient conditions using a UV-laser induced particle preparation process with subsequent wet chemical selective etching. In this preparation route, nanometer-sized branched structures are formed in spherical particles. The laser process, which is applied to a silver/gold bilayer system with different individual layer thicknesses, generates spherical mixed particles in a nanosecond range and influences the properties of the fabricated nanoparticles, such as the size and the mixture and thus the spectral response. The subsequent etching process is performed by selective wet chemical removal of silver from the nanoparticles with diluted nitric acid. The gold to silver ratio was investigated by energy-dispersive X-ray spectroscopy. The porosity depends on laser parameters and film thickness as well as on etching parameters such as time. After etching, the surface area of the remaining Au nanoparticles increases which makes these particles interesting for catalysis and also as carrier particles for substances. Such substances can be positioned at defined locations or be released in appropriate environments. Absorbance spectra are also analyzed to show how the altered fractured shape of the particles changes localized plasmon resonances of the resultingt particles.
Electrochemical growth mechanism of nanoporous platinum layers
Porous platinum is a frequently used catalyst material in electrosynthesis and a robust broadband absorber in thermoelectrics. Pore size distribution and localization determine its properties by a large extent. However, the pore formation mechanism during the growth of the material remains unclear. In this work we elucidate the mechanism underlying electrochemical growth of nanoporous platinum layers and its control by ionic concentration and current density during electrolysis. The electrode kinetics and reduction steps of PtCl4 on platinum electrodes are investigated by cyclic voltammetry and impedance measurements. Cyclic voltammograms show three reduction steps: two steps relate to the platinum cation reduction, and one step relates to the hydrogen reduction. Hydrogen is not involved in the reduction of PtCl4, however it enables the formation of nanopores in the layers. These findings contribute to the understanding of electrochemical growth of nanoporous platinum layers in isopropanol with thickness of 100 nm to 500 nm.
Modification of Surface Bond Au Nanospheres by Chemically and Plasmonically Induced Pd Deposition
In this work we investigated methods of modifying gold nanospheres bound to a silicon surface by depositing palladium onto the surfaces of single nanoparticles. Bimetallic Au-Pd nanoparticles can thus be gained for use in catalysis or sensor technology. For Pd deposition, two methods were chosen. The first method was the reduction of palladium acetate by ascorbic acid, in which the amounts of palladium acetate and ascorbic acid were varied. In the second method we utilized light-induced metal deposition by making use of the plasmonic effect. Through this method, the surface bond nanoparticles were irradiated with light of wavelengths capable of inducing plasmon resonance. The generation of hot electrons on the particle surface then reduced the palladium acetate in the vicinity of the gold nanoparticle, resulting in palladium-covered gold nanospheres. In our studies we demonstrated the effect of both enhancement methods by monitoring the particle heights over enhancement time by atomic force microscopy (AFM), and investigated the influence of ascorbic acid/Pd acetate concentration as well as the impact of the irradiated wavelengths on the enhancement effect. It could thus be proven that both methods were valid for obtaining a deposition of Pd on the surface of the gold nanoparticles. Deposition of Pd on the gold particles using the light-assisted method could be observed, indicating the impact of the plasmonic effect and hot electron for Pd acetate reduction on the gold particle surface. In the case of the reduction method with ascorbic acid, in addition to Pd deposition on the gold nanoparticle surface, larger pure Pd particles and extended clusters were also generated. The reduction with ascorbic acid however led to a considerably thicker Pd layer of up to 54 nm in comparison to up to 11 nm for the light-induced metal deposition with light resonant to the particle absorption wavelength. Likewise, it could be demonstrated that light of non-resonant wavelengths was not capable of initiating Pd deposition, since a growth of only 1.6 nm (maximum) was observed for the Pd layer.