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Microwave‐assisted synthesis of CuInSe 2 nanoparticles in low‐absorbing solvents
Author(s) -
Oleksak Richard P.,
Flynn Brendan T.,
Schut David M.,
Herman Gregory S.
Publication year - 2014
Publication title -
physica status solidi (a)
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.532
H-Index - 104
eISSN - 1862-6319
pISSN - 1862-6300
DOI - 10.1002/pssa.201330070
Subject(s) - nanoparticle , fourier transform infrared spectroscopy , materials science , transmission electron microscopy , tetragonal crystal system , chemical engineering , microwave , infrared spectroscopy , energy dispersive x ray spectroscopy , oleic acid , spectroscopy , indium , scanning electron microscope , analytical chemistry (journal) , nuclear chemistry , chemistry , nanotechnology , crystallography , organic chemistry , crystal structure , biochemistry , physics , quantum mechanics , engineering , metallurgy , composite material
Copper indium diselenide (CIS) nanoparticles were synthesized using a microwave‐assisted one‐pot solvothermal approach. For these studies high microwave‐absorbing precursors were used in combination with low microwave absorbing solvents tri‐ n ‐octylphosphine (TOP) and oleic acid (OA) to investigate the effect of selective heating of the precursors on nanoparticle synthesis. High‐resolution transmission electron microscopy (TEM) results indicated that the nanoparticles were spherical, crystalline and 4–5 nm in diameter. X‐ray diffraction (XRD) results indicated that the nanoparticles had a body‐centered tetragonal structure with planar defects that decreased in concentration with increasing reaction temperature and reaction time. The nanoparticle compositions varied depending on the reaction conditions and the compositions were found to approach stoichiometry for increased reaction times. Fourier transform infrared (FTIR) spectroscopy indicated both solvents adsorbed to the nanoparticle surface and energy dispersive spectroscopy indicated that these ligands became chlorinated during the reaction. The uniform temperature profile offered by the microwave heating allowed for highly reproducible batch‐to‐batch reactions, allowing for tight control over composition and defect concentration.