Focused electron beam induced deposition (FEBID) is an important synthesis method as it is an extremely flexible tool for fabricating functional (3D) structures with nanometer spatial resolution. However, FEBID has historically suffered from carbon impurities up to 90 at %, which significantly limits the intended functionalities. In this study we demonstrate that MeCpPtIVMe3 deposits can be fully purified by an electron-beam assisted approach using H2O vapor at room temperature, which eliminates sample and/or gas heating and complicated gas delivery systems, respectively. We demonstrate that local pressures of 10 Pa results in an electron-limited regime, thus enabling high purification rates of better than 5 min·nA–1·μm–2 (30 C·cm–2) for initially 150 nm thick deposits. Furthermore, TEM measurements suggest the purification process for the highly compact deposits occurs via a bottom-up process.
The conversion of various polymer substrates into laserinduced graphene (LIG) with a CO 2 laser in ambient condition is recently emerging as a simple method for obtaining patterned porous graphene conductors, with a myriad of applications in sensing, actuation, and energy. In this paper, a method is presented for embedding porous LIG (LIG-P) or LIG fibers (LIG-F) into a thin (about 50 μm) and soft medical grade polyurethane (MPU) providing excellent conformal adhesion on skin, stretchability, and maximum breathability to boost the development of various unperceivable monitoring systems on skin. The effect of varying laser fluence and geometry of the laser scribing on the LIG micro−nanostructure morphology and on the electrical and electromechanical properties of LIG/ MPU composites is investigated. A peculiar and distinct behavior is observed for either LIG-P or LIG-F. Excellent stretchability without permanent impairment of conductive properties is revealed up to 100% strain and retained after hundreds of cycles of stretching tests. A distinct piezoresistive behavior, with an average gauge factor of 40, opens the way to various potential strain/ pressure sensing applications. A novel method based on laser scribing is then introduced for providing vertical interconnect access (VIA) into LIG/MPU conformable epidermal sensors. Such VIA enables stable connections to an external measurement device, as this represents a typical weakness of many epidermal devices so far. Three examples of minimally invasive LIG/MPU epidermal sensing proof of concepts are presented: as electrodes for electromyographic recording on limb and as piezoresistive sensors for touch and respiration detection on skin. Long-term wearability and functioning up to several days and under repeated stretching tests is demonstrated.
Aqueous iodine based electrochemical energy storage is considered a potential candidate to improve sustainability and performance of current battery and supercapacitor technology. It harnesses the redox activity of iodide, iodine, and polyiodide species in the confined geometry of nanoporous carbon electrodes. However, current descriptions of the electrochemical reaction mechanism to interconvert these species are elusive. Here we show that electrochemical oxidation of iodide in nanoporous carbons forms persistent solid iodine deposits. Confinement slows down dissolution into triiodide and pentaiodide, responsible for otherwise significant self-discharge via shuttling. The main tools for these insights are in situ Raman spectroscopy and in situ small and wide-angle X-ray scattering (in situ SAXS/WAXS). In situ Raman confirms the reversible formation of triiodide and pentaiodide. In situ SAXS/WAXS indicates remarkable amounts of solid iodine deposited in the carbon nanopores. Combined with stochastic modeling, in situ SAXS allows quantifying the solid iodine volume fraction and visualizing the iodine structure on 3D lattice models at the sub-nanometer scale. Based on the derived mechanism, we demonstrate strategies for improved iodine pore filling capacity and prevention of self-discharge, applicable to hybrid supercapacitors and batteries.
Herein a convenient synthetic method to obtain 2,2,3,3-tetrasilyltetrasilane 3 and 2,2,3,3,4,4-hexasilylpentasilane 4 on a multigram scale is presented. Proton-coupled Si NMR spectroscopy and single-crystal X-ray crystallography enabled unequivocal structural assignment. Owing to their unique properties, which are reflected in their nonpyrophoric character on contact with air and their enhanced light absorption above 250 nm, 3 and 4 are valuable precursors for liquid-phase deposition (LPD) and the processing of thin silicon films. Amorphous silicon (a-Si:H) films of excellent quality were deposited starting from 3 and characterized by conductivity measurements, ellipsometry, optical microscopy, and Raman spectroscopy.
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