DMEX Centre for X-ray Imaging

Hydroquinone (HQ) is known to form organic clathrates with some gaseous species such as CO2 and CH4. This work presents spectroscopic data, surface and internal morphologies, gas storage capacities, guest release temperatures, and structural transition temperatures for HQ clathrates obtained from pure CO2, pure CH4, and an equimolar CO2/CH4 mixture. All analyses are performed on clathrates formed by direct gas–solid reaction after 1 month’s reaction at ambient temperature conditions and under a pressure of 3.0 MPa. A collection of spectroscopic data (Raman, FT-IR, and 13C NMR) is presented, and the results confirm total conversion of the native HQ (α-HQ) into HQ clathrates (β-HQ) at the end of the reaction. Optical microscopy and SEM analyses reveal morphology changes after the enclathration reaction, such as the presence of surface asperities. Gas porosimetry measurements show that HQ clathrates and native HQ are neither micro- nor mesoporous materials. However, as highlighted by TEM analyses and X-ray tomography, α- and β-HQ contain unsuspected macroscopic voids and channels, which create a macroporosity inside the crystals that decreases due to the enclathration reaction. TGA and in situ Raman spectroscopy give the guest release temperatures as well as the structural transition temperatures from β-HQ to α-HQ. The gas storage capacity of the clathrates is also quantified by means of different types of gravimetric analyses (mass balance and TGA). After having been formed under pressure, the characterized clathrates exhibit exceptional metastability: the gases remain in the clathrate structure at ambient conditions over time scales of more than 1 month. Consequently, HQ gas clathrates display very interesting properties for gas storage and sequestration applications.

The investigation of destruction processes in composite materials is a current problem for their structural application and the improvement of their functional properties. This work aimed to visualize structural changes induced in layered carbon fiber reinforced plastics (CFRP) with the help of synchrotron X-ray microtomography. This article presents the details of destructive processes in the early stages of the deformation of reinforced polymers under uniaxial stretching, investigated at the micro level. Individual structural elements of the composite-filaments, parallel fiber bundles, the nonuniformity of the polymer binder distribution, and continuity defects-were observed under an external load. We have considered the influence of the material architecture and technological defects on fracture evolution in cross-ply and quasi-isotropic fiber-reinforced plastics. The results indicate the sequence of irreversible structural changes before the destruction of the material.

International audience

International audience

International audience

International audience

Abstract We document the evolution of the 3D fabric of shale along a km-long strain gradient in the Jaca basin (Southern Pyrenees, Spain). With respect to the distance from a thrust, samples were collected in the cleavage-free domain, at the onset of the pencil-cleavage domain, within the pencil-cleavage domain and within the slaty-cleavage domain. By combining high resolution X-ray computed tomography (XCT) and energy dispersive X-ray spectroscopy (EDS), the morphology and the Shape Preferred Orientation (SPO) of thousands of quartz grains, calcite grains and pores was studied. In the least deformed samples, quartz and calcite display mean foliation parallel to bedding with comparable dispersion. In the pencil-cleavage domain, quartz foliation still follows the bedding while calcite foliation is mostly governed by cleavage. In the slaty-cleavage domain, calcite shows a much better organization, with foliation parallel to cleavage, mimicking closely the pore fabric. By contrast, the quartz shape fabric is much less defined, scattered between bedding and cleavage planes. This suggests that quartz grain act as rigid marker in the ductile matrix, while calcite grain orientation is governed by dissolution-precipitation processes.

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