A High‐Yield Synthesis of Chalcopyrite CuInS₂ Nanoparticles with Exceptional Size Control

Abstract

We report high-yield and efficient size-controlled syntheses of Chalcopyrite CuInS2nanoparticles by decomposing molecular single source precursors (SSPs) via microwave irradiation in the presence of 1,2-ethanedithiol at reaction temperatures as low as 100°C and times as short as 30 minutes. The nanoparticles sizes were 1.8 nm to 10.8 nm as reaction temperatures were varied from 100°C to 200°C with the bandgaps from 2.71 eV to 1.28 eV with good size control and high yields (64%–95%). The resulting nanoparticles were analyzed by XRD, UV-Vis, ICP-OES, XPS, SEM, EDS, and HRTEM. Titration studies by1H NMR using SSP1with 1,2-ethanedithiol and benzyl mercaptan were conducted to elucidate the formation of Chalcopyrite CuInS2nanoparticles.

Controlled Stoichiometry for Quaternary CuInxGa1−xS2 Chalcopyrite Nanoparticles from Single-Source Precursors via Microwave Irradiation

“…9,10 Uses of SSPs in preparation of nanomaterials present distinct advantages such as precise control in reaction conditions and stoichiometry as SSPs contain all necessary elements in a single molecule. Despite the obvious advantages of SSPs, to the best of our knowledge, no studies have been conducted using combinations of SSPs to form quaternary or multinary chalcopyrite nanoparticles.…”

“…10 As we looked to expand our method to prepare quaternary nanoparticles, we discovered that mixing of two SSPs containing In and Ga can provide desired products without sacrificing stoichiometric control in resulting nanoparticles. In recent years, there have been a limited number of reports describing the preparation of related multinary nanoparticles from multiple sources.…”

“…18 This allows for the preparation of nanoparticles with diameters of a few nanometers, 19 dramatic decreases in reaction times, improved product purities, the use of many forms of precursors, and reactions exhibiting good reproducibility and high yields. 10,20 Herein, we report efficient syntheses of the quaternary CuIn x Ga 1-x S 2 (0 e x e 1) chalcopyrite nanoparticles with precise stoichiometric control by decomposition of a mixture of two I-III bimetallic SSPs in the presence of 1,2-ethanedithiol via microwave irradiation.…”

“…The high level of control is most likely due to the fact that 1,2-ethanedithiol acts as a bridging unit between two SSP units. 10 This process produces cross-linked random polymers of SSPs, which undergo rapid decomposition to produce the resulting CuIn x Ga 1-x S 2 nanoparticles. 10 This is supported by the fact that replacing 1,2-ethanedithiol with 1-hexanethiol resulted in poor metal ratio control (see the Supporting Information).…”

Facile Microwave Approach for Synthesis of Copper–Indium Sulfide Nanoparticles and Study of Their Behavior in Solar Cell

“…Also, There are several reports in the literature of rapid synthesis and size control of CIS semiconductor nps using microwave irradiation [16,17]. Microwave radiation is a fast and low-cost method for the production of CIS nps [18].…”