Premium
In situ energy‐dispersive X‐ray diffraction of local phase dynamics during solvothermal growth of Cu 4 O 3
Author(s) -
Jiang Zhelong,
Sharma Jai,
Okasinski John S.,
Chen Haiyan,
Shoemaker Daniel P.
Publication year - 2021
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/s1600576720014806
Subject(s) - in situ , solvothermal synthesis , diffraction , crystallography , materials science , phase (matter) , powder diffraction , analytical chemistry (journal) , chemistry , optics , physics , organic chemistry
Using in situ methods to characterize the state of a system during reactions is critical to understanding and improving solvothermal syntheses. This work demonstrates the use of in situ energy‐dispersive X‐ray diffraction (EDXRD) to investigate the local dynamics during solvothermal formation of Cu 4 O 3 using a general‐purpose full‐sized laboratory oven. This allows for direct comparison of in situ data with laboratory‐based reactions. Using in situ EDXRD, changes in the local amounts of Cu 4 O 3 , Cu 2 O and CuO within approximately 100 × 100 × 700 µm gauge volumes during solvothermal Cu 4 O 3 formation were recorded. Fast conversion between Cu 2 O and CuO was observed in the solvothermal environment, whereas Cu 4 O 3 was found to be chemically stable against disturbances once formed. The observed differences in local dynamics give further support to the differences in formation mechanisms between Cu 4 O 3 and Cu 2 O/CuO proposed here.