Microporous materials, (materials with pore sizes with widths <2 nm) were prepared by pillaring of smectites obtained from different soil deposits. The materials were prepared by intercalation with oligomeric cations of aluminum, which were transformed to aluminum-oxide pillars by calcination. The adsorption of n-hexane in the pillared clays was studied by the determination of heats of adsorption. Heats of adsorption were measured using either a static microcalorimeter or differential scanning calorim-etry coupled with thermogravimetry (TG-DSC). In this latter case, two different procedures were used that differ on the introduction of the (n-hexane) molecules that are to be adsorbed. The results obtained by the (standard) static microcalorimeter method and the TG-DSC method were compared. This comparison showed the heats of adsorption obtained by TG-DSC are differential heats of adsorption, and it showed the range of adsorption. Characterizing the texture of pillared clays, especially microporosity, is important for monitoring the intercalation process and for determining potential applications of these materials. Correlations between the obtained heats of adsorption and the dimensions of micropores suggest that TG-DSC is a semi-quantitative method for characterizing micropores in aluminum-pillared clays.

A commercially available combined X-ray diffraction – differential scanning calorimetry (XRD-DSC) stage was adapted for studies of gas loading in microporous materials, including metal organic frameworks (MOFs). Insertion of a custom-built humid atmosphere swing chamber (HASC) between a humidity generator and the XRD-DSC stage facilitates both humid atmosphere and vacuum swing gas loading. The HASC is necessary to buffer between the humidity generator and the XRD-DSC stage, allowing the gas mixture to homogenize prior to sample exposure, so that both humid atmosphere and vacuum swings could be performed. The changes in XRD can be used to follow structural changes, including collapse, which is indicative of a lack of microporosity upon activation, and the flexibity of frameworks upon gas sorption–desorption cycles. Measurements of the area under the DSC curve allows for calculation of the isosteric heat of adsorption (Qst; kJ molGAS−1). Vacuum-atmosphere swing experiments performed at different pressure steps allow for the reconstruction of the enthalpy of gas adsorption before and after a phase transition. These modes of operation are illustrated in three case studies from a program of exploratory MOF synthesis used to discover novel materials for selective gas sorption from humid gas streams: (1) gas binding in Stony Brook metal organic framework-1, (2) zeolitic imidazolate framework-7 response to variable pressure vacuum-atmosphere swing, and (3) high throughput evaluation of the selectivity of novel MOFs synthesized from customized linkers.

We have reported the chemical blending carbonization method to obtain microporous carbon with high surface area for application as electrode materials in supercapacitors. Aliphatic dicarboxylic acids with different methylene numbers (n = 2, 4, 6, and 8) react with phenolic resin (PF) during curing process. Abundant micropores are created in the carbon matrix after the decomposition of grafted or blocked diacids at temperature higher than 400 °C. The specific surface area (SSA) of the carbonized blending system increases with the diacid chain length, but decreases after n > 4 of the chain length. The maximum SSA of the blending system is up to 605.9 m2/g, which increased approximately 68% compared to that of the neat carbonized PF. Electrochemical investigation indicates that the highest specific capacitances of the blending system reaches 175 F/g at a specific current of 0.1 A/g in 30 wt% KOH aqueous electrolyte. Furthermore, the capacitance maintenance achieves 82.8% as the current density enlarged 55 times.

Ni20[(C6H8O4)20(H2O)8]∙33H2O, a new nickel(II) 3-methylglutarate, was prepared hydrothermally (180 °C, 48 h, autogenous pressure) from a 1:1.5:2:180 mixture of nickel (II) sulphate hexahydrate, 3-methylglutaric acid, sodium hydroxide, and water. It crystallizes in the cubic system (space group P4332, Z=1) with a=16.8488(5) Å and V=4783.1(4) Å3. Its structure was solved from conventional X-ray powder diffraction data. It presents a three-dimensional network of edge-sharing nickel octahedra, lined by deprotonated organic anions. This remarkable oxide network with corrugated 20-membered rings is constructed from homochiral helices. The rings intersect each other to generate large crossing channels full of water along [111].