Photograph of the sample chamber. Only the parts made by brass are shown. The larger part is the cryochamber, and the smaller part that appears on the inside is the liquid cell.
Cross sections of the sample chamber. (a) Schematic view of the sample chamber perpendicular to the direction of x-ray radiation. (b) Schematic view of the sample chamber parallel to the direction of x-ray radiation.
Top view of the phase-contrast x-ray imaging with skew-symmetric two-crystal x-ray interferometer and the sample chamber.
Three dimensional (3D) image of the spheroid-shaped ice sample including air hydrate crystals measured by the phase-contrast x-ray imaging technique. The dark gray circles in the ice sample indicate the areas where the densities are higher than that of the surrounding ice, which correspond to air hydrate crystals. The internal part of the ice was made transparent to show the air hydrate more clearly.
Optical image of a section of ice sample including air hydrate crystals measured by a microscope. The thickness of the sample was reduced to for the observation without dissociation of air hydrates in a cold room at .
Density difference between the air hydrate crystal and the surrounding ice plotted against the size of the air hydrate crystal. The size of the air hydrate crystal expresses the diameter, which was estimated by a spherical approximation using the voxel size of . Only the air hydrates, which are larger than six voxels in volume size, were used for the analysis. The density difference of one of the data points is much higher than that of the other points, thus it might not be an air hydrate but another kind of hydrate such as a hydrate of sulfate salt as reported in Ref. 26.
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