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Updated: Nov 18, 2025

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
Published on: June 7, 2018
Hard x-ray methods for studying the structure of amorphous thin films and bulk glassy oxides
C J Benmore1,2, G B González3, O L G Alderman4
1X-Ray Science Division, Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, United States of America.
Abstract:
High-energy photon diffraction minimizes many of the corrections associated with laboratory x-ray diffractometers, and enables structure factor measurements to be made over a wide range of momentum transfers. The method edges us closer toward an ideal experiment, in which coordination numbers can be extracted without knowledge of the sample density. Three case studies are presented that demonstrate new hard x-ray methods for studying the structure of glassy and amorphous materials. First, the methodology and analysis of high-energy grazing incidence on thin films is discussed for the case of amorphous In2O3. The connectivity of irregular InO6polyhedra are shown to exist in face-, edge- and corner-shared configurations in the approximate ratio of 1:2:3. Secondly, the technique of high-energy small and wide angle scattering has been carried out on laser heated and aerodynamically levitated samples of silica-rich barium silicate (20BaO:80SiO2), from the single phase melt at 1500oC to the phase separated glass at room temperature. Based on Ba-O coordination numbers of 6 to 7, it is argued that the although the potential of Ba is ionic, it is weak enough to cause the liquid-liquid immiscibility to become metastable. Lastly, high-energy small and wide angle scattering has also been applied to high water content (up to 12 wt.%) samples of hydrous SiO2glass quenched from 1500oC at 4 GPa. An increase of Si1-O2correlations at 4.3 Å is found to be consistent with an increase in the population of three-membered SiO4rings at the expense of larger rings.
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