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In situ ultra‐small‐angle X‐ray scattering study of the solution‐mediated formation and growth of nanocrystalline ceria
Author(s) -
Allen Andrew J.,
Hackley Vincent A.,
Jemian Pete R.,
Ilavsky Jan,
Raitano Joan M.,
Chan SiuWai
Publication year - 2008
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889808023078
Subject(s) - nucleation , small angle x ray scattering , nanocrystalline material , materials science , nanoparticle , chemical engineering , suspension (topology) , scattering , synchrotron , isothermal process , in situ , chemical physics , nanotechnology , analytical chemistry (journal) , chemistry , optics , thermodynamics , chromatography , physics , mathematics , engineering , homotopy , pure mathematics , organic chemistry
Results are presented for an in situ synchrotron‐based ultra‐small‐angle X‐ray scattering (USAXS) study of the solution‐mediated formation and growth of nanocrystalline ceria (n‐CeO 2 ) using a new remote‐controlled, isothermal, circulating fluid flow cell. The fluid flow mitigates or reduces X‐ray beam‐induced damage, air bubbles or particulate flocculation within the bulk solution, but prevents any coarse particulates that do form from settling out from suspension. Combined with the large‐scale range accessible in USAXS studies, the flow cell has enabled measurement, in situ and in real time, of structural characteristics from 10 Å to a few micrometres in size as a function of the changing physical and chemical conditions. By applying a multi‐component model, the nanoparticle formation and growth component has been identified. Control and online monitoring of flow rate, temperature and pH suspension conditions have permitted real‐time studies of the formation and growth of the individual n‐CeO 2 particles from homogeneous dilute solution over several hours. Aspects of the nanoparticle nucleation and growth are revealed that have not been observed directly in measurements on this system.