Depth-selective x-ray diffraction using energy-dispersive x-ray detector and straight capillary optics.

Depth-selective x-ray diffraction (XRD) technique was developed. In this technique, XRD spectra were measured using an energy dispersive (ED) x-ray detector at fixed angles. A straight capillary optic was used to define the incident x-ray beam, and a second straight capillary defined the beam path from the sample to detector. Thereby, only the XRD spectrum at the small intersection of two capillary optics could be obtained. A depth-selective XRD is possible by changing the sample position in depth. Many XRD peaks appear in a high-energy range more than 10 keV in the ED spectrum. The detection of these peaks will be advantageous for depth analysis because of low absorption in the sample. Depth-selective measurement would be advantageous over general XRD. In this study, depth-selective and ED-XRD spectra are demonstrated for the layered sample, which consisted of film-like Si powder and a muscovite film.

Mechanically stable, hierarchically porous Cu3(btc)2 (HKUST-1) monoliths via direct conversion of copper(II) hydroxide-based monoliths.

The synthesis of highly crystalline macro-meso-microporous monolithic Cu3(btc)2 (HKUST-1; btc(3-) = benzene-1,3,5-tricarboxylate) is demonstrated by direct conversion of Cu(OH)2-based monoliths while preserving the characteristic macroporous structure. The high mechanical strength of the monoliths is promising for possible applications to continuous flow reactors.

Mesoscopic superstructures of flexible porous coordination polymers synthesized via coordination replication.

The coordination replication technique is employed for the direct conversion of a macro- and mesoporous Cu(OH)2-polyacrylamide composite to three-dimensional superstructures consisting of the flexible porous coordination polymers, Cu2(bdc)2(MeOH)2 and Cu2(bdc)2(bpy) (bdc2- = 1,4-benzenedicarboxylate, bpy = 4,4'-bipyridine). Detailed characterization of the replicated systems reveals that the structuralization plays an important role in determining the adsorptive properties of the replicated systems, and that the immobilization of the crystals within a higher-order architecture also affects its structural and dynamic properties. The polyacrylamide polymer is also found to be crucial for maintaining the structuralization of the monolithic systems, and in providing the mechanical robustness required for manual handling. In all, the results discussed here demonstrate a significant expansion in the scope of the coordination replication strategy, and further confirms its utility as a highly versatile platform for the preparation of functional three-dimensional superstructures of porous coordination polymers.