Rapid Microwave-Enhanced Solvothermal Process for Synthesis of CuInSe₂ Particles and Its Morphologic Manipulation

Abstract

CuInSe2 nanoparticles are prepared using a microwave-assisted solvothermal method with ethylenediamine as a solvent. The morphology of the as-prepared CuInSe2 nanoparticles has been successful manipulated by controlling the morphology of selenium seeds. We achieved this through a systematic treatment of selenium powders before the addition of indium and copper precursors. This pretreatment of selenium powders, under microwave heating, converts the morphologies of selenium seed from spherical to nanorod. As a result, this nanorod morphology of selenium seeds are responsible for the formation of crystalline CuInSe2 particles with rodlike morphology, while the crystalline CuInSe2 particles with platelike morphology are obtained without pretreatment of selenium powders. The XRD data and SEM images show that pure chalcopyrite CuInSe2 particles with good crystallinity are obtained with the pretreatment of selenium and ethylenediamine mixture in the microwave heating for 30 min and followed by further microwave-enhanced reaction with indium and copper precursors for 30 min. We proposed the reaction mechanism based on XRD and SEM data, which includes the intermediate products. The Raman spectrum of the chalcopyrite CuInSe2 nanoparticle shows an intense peak at 175 cm−1 corresponds to the A1 phonon mode of tetragonal CuInSe2 chalcopyrite. The compositions of the products consistent very well with their nominal value are confirmed by energy-dispersive X-ray analysis.

Microwave‐Assisted Synthesis of Colloidal Inorganic Nanocrystals

“…Under these experimental conditions, an accurate control of the stoichiometry and band gap was achieved for NCs in the 2.5–4.5 nm range. Nano‐ to micron‐sized CuInSe 2 particles with variable shapes were obtained by MW‐supported solvothermal synthesis in EDA 304. The particle evolution was controlled by in‐situ formation of nanocrystal seeds of different types.…”

Microwave-assisted hydrothermal synthesis and characterization of ZnO nanorods

“…In most cases, the high synthesis temperature leads to the formation of strong aggregates in the ZnO nanomaterials, which subsequently have to be excessively milled resulting in poor control of particle morphology and size distribution [14] Among of the various synthesis methods of nanomaterials; the hydrothermal technique has several advantages over others synthetic methods, among which are: the one-step synthesis without high temperature calcinations and milling, low aggregation levels and narrow crystallite size distributions, in addition to high purity and excellent control of particle morphology and size [14]. Recently, the hydrothermal microwave-assisted synthesis has attracted wide interests as a novel heating model in material science due to its various advantages including normal atmospheric pressure reacting, short reaction time, rapid heating, low reaction temperature, homogeneous thermal transmission, and the phase purity with better yield [15][16][17][18].…”

Mikrowellen‐unterstützte Synthese von kolloidalen anorganischen Nanokristallen

“…Unter diesen experimentellen Bedingungen wurde eine präzise Steuerung der Stöchiometrie und Bandlücke für Nanokristalle in einem Größenbereich von 2.5–4.5 nm erzielt. Nano‐ bis mikrometergroße CuInSe 2 ‐Nanokristalle mit verschiedenen Formen wurden durch MW‐unterstützte solvothermale Synthesen in EDA erhalten 304. Die NK‐Entwicklung wurde durch die In‐situ‐Bildung von Nanokristallkeimen verschiedener Arten gesteuert.…”