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The formation of hierarchically porous metal and metal oxide monoliths by replication of hierarchically porous silica templates is reviewed. The various factors that impact the structure and properties of the synthesized materials are discussed and illustrated by the formation of new α‐Fe2O3, ZrO2, nickel, silver, and silver silicate porous monoliths. The impact of the atmosphere is addressed in the formation of Co3O4 and silver monoliths. For Co3O4, formation of the monolith under vacuum, air, argon, or nitrogen was found to dramatically change the structure of the final material. For silver, decomposition of the silver nitrate under air resulted in porous monoliths composed of silver silicates. Decomposition of silver nitrate under vacuum produced monoliths for which the chemical composition of the monolith was predominantly silver on the exterior of the monolith consisted of silver silicates in the interior of the monolith.

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Abstract

Hierarchically porous materials are of interest in a wide range of applications. If the materials are electronic or ionic conductors such materials are of interest as electrodes for use in fuel cells, flow batteries, electrocatalysis, and pseudo/supercapacitors. We have demonstrated the synthesis of hierarchically porous carbon, metal and metal oxide monoliths. Hierarchically porous silica with porosity at three length scales: 0.5-30 micrometer, 200-500 nm, and 3-8 nm, is used as a template to form these materials. The porosity of the silica template is produced by spinodal decomposition (0.5-30 micrometer), particle agglomeration (200-500 nm) and addition of surfactant or block copolymer (3-8 nm). Nanocasting: replication of all or part of the structure via one of a number of chemical replication techniques has been used to produce the carbon, metal oxide and metal replicas. The final surface areas of the materials can be as high as 1200 m2/g for carbon replicas, and >300 m2/g for metals and metal oxides. The use of the nanocasting technique allows for formation of materials that are compositionally or spatially heterogeneous.We report here results on the synthesis and characterization of hierarchically porous monoliths of carbon and, nickel and the use of some of these monoliths in catalysis and electrochemical capacitors.

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We report on a pair of MSP (Mathematics & Science Partnership) START pilot projects designed to identify nanoscience experiments that will fit within the Alabama course of study for use in Alabama K-12 classrooms. As part of the first project we are testing the development, refinement and evaluation of an activity already partly developed. The form of this activity has had input from a focus group of RETs who were tasked to provide input into the activity and how it can be matched to components of the Alabama Course of Study. This activity consists of using sparks generated by abrasion of misch metal by sand paper of different grit size. Different grit sizes produce metal particles of different sizes, resulting in sparks of different size and length. If done in a dry box no sparks are produced and the powder left is not pyrophoric, demonstrating that high surface area, heat and oxygen are all required to produce sparks. SEM characterization of the powder allows the particle sizes to be determined, giving the correlation between size, grit size and spark track length. The activity was tested on groups of middle school science campers at McWane Science Center, and after evaluation, further modified to increase student interest and impact. The activity was then tested on grades 6-8 in a middle school classroom by a graduate student/undergraduate student team.

Hierarchically porous silica monoliths were introduced into liquid phase chromatography at the beginning of the last decade. The high surface area, high void volume and bicontinuous nature of the porosity of the materials are significant advantages over existing chromatographic supports and have resulted in rapid acceptance of these materials into the chromatography market.We report here on the synthesis of 3-D porous silver, cobalt oxide and zinc oxide monoliths, their materials characterization, fabrication as liquid chromatographic columns and initial chromatographic characterization. The, as prepared, columns gave very low back pressure, consistent with the bicontinuous nature of the columns. Cobalt oxide and zinc oxide both demonstrated retention of a number of nitrogen heterocycles, providing the basis for molecular separation.