Silicon nanocrystals exhibit size-dependent optical and electronic properties that may be exploited for applications ranging from sensors to photovoltaics. In addition, they can be utilized in biological and environmental systems thanks to the nontoxicity of silicon. Synthesis of silicon nanocrystals has been accomplished using a variety of methods. However, creating near monodisperse systems of high purity has been a challenge. The high temperature processing of hydrogen silsesquioxane method of particle synthesis reproducibly provides pure, near monodisperse particles in scalable quantities. These particles can then be liberated using HF etching and functionalized using a variety of methods. This paper outlines our lab procedures for creating silicon nanocrystals, the various functionalization methods and the most commonly used characterization techniques.
Exploiting the chemical compatibility of transparent high surface area silica aerogels and environmentally benign luminescent silicon nanocrystals (SiNCs) opens the door to a new class of silicon-based hybrid materials. Hydrophilic SiNCs of various sizes and surface groups that photoluminesce throughout the visible and NIR spectral regions were synthesized and incorporated into tetramethyl orthosilicate containing solution to produce luminescent aerogels of varied transparency. Photoluminescence (PL) spectroscopy performed on solutions and aerogel monoliths containing SiNCs reveal that the optical properties of SiNCs are dependent on their size and surface chemistry. Furthermore, the incorporation of SiNCs into aerogels does not influence their PL response. The nitrogen adsorption-desorption measurements indicate that the physical properties of aerogels may be tailored by changing the SiNC size and surface chemistry.Adding to the appeal of the present work, PL quenching of SiNC-loaded aerogel upon exposure to nitrobenzene confirms that SiNCs remain chemically accessible.
Alkoxy-terminated silicon quantum dots (SiQDs) were synthesized via hydrosilylation of aliphatic ketones on hydride-terminated SiQD (H-SiQD) surfaces under microwave-irradiation. Aromatic ketones undergo hydrosilylation on H-SiQD surfaces at room temperature without requiring any catalyst. The alkoxy-terminated SiQDs are soluble in organic solvents, colloidally stable, and show bright and size dependent photoluminescence (PL). The alkoxy-functionalized silicon surfaces were used as reactive platform for further functionalization via unprecedented ligand exchange of the alkoxy-surface groups with alkyl or alkenyl-surface groups in the presence of BH3·THF. Proton nuclear magnetic resonance ((1)H NMR), Fourier transform infrared (FTIR), and X-ray photoelectron spectroscopy (XPS) spectroscopy confirmed alkoxy-terminated surfaces and their ligand exchange reactions in the presence of various alkenes and alkynes.
Materials based upon porous carbon have gained considerable attention due to their high surface area, electric conductivity, thermal and chemical stability, low density, and availability. These superior properties make them ideal for diverse applications. Doping these carbon nanostructures holds promise of designing the properties of these structures and opening the door to practical applications. Herein, we report the preparation of hollow N-doped mesoporous carbon (HMC) spheres fabricated via polymerization and carbonization of dopamine on a sacrificial spherical SiO(2) template that is removed upon hydrofluoric acid etching. The morphology and structural features of these HMCs were evaluated using scanning electron microscopy and transmission electron microscopy and the N-doping (7.1 at%) was confirmed by X-ray photoelectron spectroscopy (XPS). The oxygen reduction/evolution reaction (ORR/OER) performance of N-doped HMC was evaluated using rotating disk electrode (RDE) voltammetry in an alkaline electrolyte. N-doped HMC demonstrated a high ORR onset potential of -0.055 V (vs. Hg/HgO) and excellent stability. The outstanding bifunctional activity was implemented in a practical Zn-air battery (ZAB), which exhibited a small charge-discharge voltage polarization of 0.89 V and high stability over repeated cycling.
FeO nanorods coated with nitrogen-doped mesoporous carbon (ND-FeO@mC) shells of defined thicknesses have been prepared via a new microwave-assisted approach. Microstructural characterization of these ND-FeO@mC structures was performed using x-ray diffraction, x-ray photoelectron spectroscopy, transmission electron microscopy, and scanning electron microscopy. Following identification, the electrochemical performance of the catalysts was evaluated using linear sweep voltammetry with a rotating disc electrode system. The present investigation reveals enhanced oxygen reduction reaction catalytic activity and the carbon layer thickness influences oxygen diffusion to the active FeO nanorod core.
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