Here we report the adaptation of formaldehyde crosslinked phenolic resin-based aerogel and xerogel synthesis to ethanolbased solvent systems. Three specific formulations, namely one resorcinol-formaldehyde (RF) and two resorcinolmelamine-formaldehyde (RMF) systems were studied. As-prepared resins were characterized in terms of envelope and skeletal density. Furthermore, resin samples were pyrolyzed and activated in a CO 2 gas atmosphere using a single-step protocol. The corresponding carbon materials featured high surface areas, moderate water uptake capacity and thermal conductivities in the 0.1 W.m −1 K −1 range, in line with comparable activated carbons. The amount of formaldehyde in the synthesis of the RMF derived carbons proved to be a critical parameter in terms of both structural features and amount of N dopant in the carbonaceous matrix. Furthermore, a high formaldehyde concentration also has a drastic effect on the pore structure of the corresponding RMF carbons, leading primarily to mesopore formation without almost any macropore formation. Perhaps more importantly, the effect of the ammonia curing catalyst concentration on the material microstructure showed the opposite effect as observed in classical, water-based phenolic resin preparations. The ethanol-based synthesis clearly affects the pore structure of the resulting materials but also opens up the possibility to create inorganic/organic hybrid materials by simple combination with classical alkoxide-based silica sol-gel chemistry.
The design and discovery of three-dimensional crystalline metal–organic frameworks (MOFs) from linkers with phosphonate coordinating groups and even alkaline earth metals is largely undeveloped. Herein, we report a strategy for realizing new, stable, and robust barium phosphonate MOFs, termed Empa-1 and Empa-2. The two-dimensional (2D) Empa-1 or three-dimensional (3D) Empa-2 could be realized by way of systematically modulating the ratio of Ba2+ with a tetratopic phosphonate-based linker that was crafted to incorporate nitrogen-rich triazine units bridged by a fixed piperazine core. In addition to this synthetic approach, temperature-dependent synchrotron-radiation powder X-ray diffraction analysis demonstrated that the 2D Empa-1 undergoes an irreversible phase transition upon heating and subsequent dehydration to form the 3D Empa-2. Given the presence of uncoordinated phosphonic acid moieties within the structure of 3D Empa-2, the CO2 sorption capabilities are reported. We believe our ability to link the alkaline earth metal barium with a novel tetratopic phosphonate linker, as evidenced by the robust structures of Empa-1 and -2, paves the way for further exploration and discovery of new crystalline, porous frameworks with greater structural diversity, stability, and wide-scale practical applicability.
Here, we report the gelation and supercritical drying of ethanol-based silica–resorcinol–melamine–formaldehyde (RMF) composite aerogels with relative concentrations of initial reagents ranging from neat silica to neat RMF alcogels. The as-prepared materials are subsequently supercritically dried with carbon dioxide. Their properties include a thermal conductivity in the 15–20 mW·m –1 ·K –1 range even with a silica content as low as 20% wt . The possible reasons behind this interesting insulation performance and the mechanisms leading to the underlying gel structure are discussed in depth. A focus is made on the different gelation modes happening between the RMF and silica phases, from a coating of silica surfaces with RMF species to discontinuous RMF particles within a silica backbone and a continuous RMF backbone with isolated silica particles. The implications in terms of mechanical properties and thermal conductivity are elaborated upon. The initial ratio of silica–RMF species in this ethanol-based synthesis affects the micro- and macrostructure of the composites, resulting in materials with drastically different pore structures and thus an interesting array of possibilities for a new class of silica-organic composite aerogels, based on a sol–gel process.
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