Abstract

First responders and military personnel require protection against multiple hazards. However, the structure of conventional materials only provides protection against a single threat. By combining a porous network with aligned fibers, this work demonstrates a multifunctional material with a high insulation and high ballistic resistance. Overcoming the limitations of conventional materials, this approach enables simultaneous thermal insulation and mechanical protection, serving as an ideal material platform for the design of high-performance protective equipment for aerospace and warfare applications.

Noble metal aerogels offer a wide range of catalytic applications due to their high surface area and tunable porosity. Control over monolith shape, pore size, and nanofiber diameter is desired in order to optimize electronic conductivity and mechanical integrity for device applications. However, common aerogel synthesis techniques such as solvent mediated aggregation, linker molecules, sol–gel, hydrothermal, and carbothermal reduction are limited when using noble metal salts. Here, we present the synthesis of palladium aerogels using carboxymethyl cellulose nanofiber (CNF) biotemplates that provide control over aerogel shape, pore size, and conductivity. Biotemplate hydrogels were formed via covalent cross linking using 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) with a diamine linker between carboxymethylated cellulose nanofibers. Biotemplate CNF hydrogels were equilibrated in precursor palladium salt solutions, reduced with sodium borohydride, and rinsed with water followed by ethanol dehydration, and supercritical drying to produce freestanding aerogels. Scanning electron microscopy indicated three-dimensional nanowire structures, and X-ray diffractometry confirmed palladium and palladium hydride phases. Gas adsorption, impedance spectroscopy, and cyclic voltammetry were correlated to determine aerogel surface area. These self-supporting CNF-palladium aerogels demonstrate a simple synthesis scheme to control porosity, electrical conductivity, and mechanical robustness for catalytic, sensing, and energy applications.

Here gelatin biotemplated platinum aerogels were prepared from gelatin hydrogels equilibrated in K2PtCl4solutions ranging from 1-250 mM and reduced with sodium borohydride before supercritical drying in liquid CO2. Scanning electron microscopy revealed an average ligament diameter of 40.6 ± 9.7 nm and a pore size range of ∼10 – 200 nm. Thermogravimetric analysis correlated the ratio of metal content to biotemplate mass as a function of equilibrated platinum ion solution, and X-ray diffractometry indicated platinum metal with no detectable oxide phases. Electrochemical impedance spectroscopy indicated a specific capacitance of 1.92 F/g, with a corresponding specific electrochemical accessible surface area of 6.39 m2/g. Cyclic voltammetry performed in H2SO4demonstrated biotemplated platinum aerogel potential for catalytic and energy storage applications.

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various precursor noble metal ions with reducing agents in a 1:1 (v/v) ratio results in the formation of metal gels within seconds to minutes compared to much longer synthesis times for other techniques such as sol-gel. Conducting the reduction step in a microcentrifuge tube or small volume conical tube facilitates a proposed nucleation, growth, densification, fusion, equilibration model for gel formation, with final gel geometry smaller than the initial reaction volume. This method takes advantage of the vigorous hydrogen gas evolution as a by-product of the reduction step, and as a consequence of reagent concentrations. The solvent accessible specific surface area is determined with both electrochemical impedance spectroscopy and cyclic voltammetry. After rinsing and freeze drying, the resulting aerogel structure is examined with scanning electron microscopy, X-ray diffractometry, and nitrogen gas adsorption. The synthesis method and characterization techniques result in a close correspondence of aerogel ligament sizes. This synthesis method for noble metal aerogels demonstrates that high specific surface area monoliths may be achieved with a rapid and direct reduction approach.

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