Open AccessA reaction cell for time‐resolved in situ XAS studies during wet chemical synthesis: the Cu 2 (OH) 3 Cl case
Author(s) -
Boita Jocenir,
do Carmo Martins Alves Maria,
Morais Jonder
Publication year - 2014
Publication title -
journal of synchrotron radiation
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.172
H-Index - 99
ISSN - 1600-5775
DOI - 10.1107/s1600577513028786
Subject(s) - x ray absorption spectroscopy , x ray photoelectron spectroscopy , spectroscopy , absorption spectroscopy , xanes , aqueous solution , extended x ray absorption fine structure , synchrotron radiation , in situ , analytical chemistry (journal) , absorption (acoustics) , chemistry , crystallography , materials science , chemical engineering , optics , organic chemistry , quantum mechanics , composite material , engineering , physics
The use of in situ time‐resolved dispersive X‐ray absorption spectroscopy (DXAS) to monitor the formation of Cu 2 (OH) 3 Cl particles in an aqueous solution is reported. The measurements were performed using a dedicated reaction cell, which enabled the evolution of the Cu K ‐edge X‐ray absorption near‐edge spectroscopy to be followed during mild chemical synthesis. The formed Cu 2 (OH) 3 Cl particles were also characterized by synchrotron‐radiation‐excited X‐ray photoelectron spectroscopy, X‐ray diffraction and scanning electron microscopy. The influence of polyvinylpyrrolidone (PVP) on the electronic and structural properties of the formed particles was investigated. The results indicate clearly the formation of Cu 2 (OH) 3 Cl, with or without the use of PVP, which presents very similar crystalline structures in the long‐range order. However, depending on the reaction, dramatic differences were observed by in situ DXAS in the vicinities of the Cu atoms.