RESUMO
Amongst the more than 18 different forms of water ice, only the common hexagonal phase and the cubic phase are present in nature on Earth. Nonetheless, it is now widely recognized that all samples of 'cubic ice' discovered so far do not have a fully cubic crystal structure but instead are stacking-disordered forms of ice I (namely, ice Isd), which contain both hexagonal and cubic stacking sequences of hydrogen-bonded water molecules. Here, we describe a method to obtain large quantities of cubic ice Ic with high structural purity. Cubic ice Ic is formed by heating a powder of D2O ice XVII obtained from annealing of pristine C0 hydrate samples under dynamic vacuum. Neutron diffraction experiments performed on two different instruments and Raman spectroscopy measurements confirm the structural purity of the cubic ice, Ic. These findings contribute to a better understanding of ice I polymorphism and the existence of the two natural ice forms.
RESUMO
Deuterated ice XVII, a metastable solid water polymorph, was filled with Ne and O2 at p ≈ 100 kPa and studied by in situ neutron diffraction (ILL, France). Powder patterns were collected in the ranges of 20-50 K (Ne) and 4.6-90 K (O2). Rietveld refinement and difference Fourier techniques showed that the gas molecules were located inside the hexagonal channels of the host ice. Both Ne atoms and O2 molecules are arranged in a spiral-like configuration off the channel axis, preserving the P6122 symmetry of the host in the case of Ne, but reducing it to P61 in O2. A larger Ne absorption compared to Ne-filled ice II is observed, which is consistent with longer host-guest contacts producing smaller hydrophobic repulsion. In O2-filled ice XVII, instead, short O-D distances (2.37 Å) have attractive character and stabilize the structure.
RESUMO
Distribution, penetration depth and amount of new mineralogical phases formed after the interaction between an inorganic treatment and a matrix are key factors for the evaluation of the conservation treatment behaviour. Nowadays, the conventional analytical methodologies, such as vibrational spectroscopies, scanning electron microscopy and X-ray diffraction, provide only qualitative and spot information. Here, we report, for the first time, the proof of concept of a methodology based on neutron imaging able to achieve quantitative data useful to assess the formation of calcium oxalate in a porous carbonatic stone treated with ammonium oxalate. Starting from the neutron attenuation coefficient of Noto stone-treated specimens, the concentrations of newly formed calcium oxalate and the diffusion coefficient have been calculated for both sound and decayed substrates. These outcomes have been also used for a comparative study between different treatment modalities. Graphical abstract Horizontal slice at 300 mm depth and CaOx molar density profile by NEUTRA output.
RESUMO
Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 µm resolution) distribution of some microstructure properties, such as residual strain, texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. In addition, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.
RESUMO
VESPA, Vibrational Excitation Spectrometer with Pyrolytic-graphite Analysers, aims to probe molecular excitations via inelastic neutron scattering. It is a thermal high resolution inverted geometry time-of-flight instrument designed to maximise the use of the long pulse of the European Spallation Source. The wavelength frame multiplication technique was applied to provide simultaneously a broad dynamic range (about 0-500 meV) while a system of optical blind choppers allows to trade flux for energy resolution. Thanks to its high flux, VESPA will allow the investigation of dynamical and in situ experiments in physical chemistry. Here we describe the design parameters and the corresponding McStas simulations.
RESUMO
Neutron resonance capture analysis (NRCA) is a nuclear technique that is used to determine the elemental composition of materials and artifacts (e.g., bronze objects) of archaeological interest. NRCA experiments are mostly performed at the GELINA facility in Belgium, a pulsed neutron source operating with an electron linear accelerator. Very intense fluxes of epithermal neutrons are also provided by spallation neutron sources, such as the ISIS spallation neutron source in the United Kingdom. In the present study, the suitability of the Italian Neutron Experimental Station (INES) beam line for NRCA measurements is assessed using a compact (n, γ) resonance detector made of a Yttrium-Aluminum-Perovskite (YAP) scintillation crystal coupled with a silicon photomultiplier (SiPM) readout. The measurements provided a qualitative recognition of the composition of the standard sample, a lower limit for the sensitivity for NRCA for almost-in-traces elements, and an estimation of the relative isotopic concentration in the sample.