Swift Morphosynthesis of Hierarchical Nanostructures of CdS via Microwave-Induced Semisolvothermal Route

Abstract

For the swift generation of hierarchical nanostructures of CdS, we propose herein a docile microwave-induced semi-solvothermal reaction (i.e., involving simultaneous usage of nonaqueous and aqueous solvents) between cadmium acetate and thiourea in binary solution of diethylenetriamine and deionized water. Typically, such microwave-assisted reaction was accomplished within 5 minutes as against 12 h required in conventional approach. The resultant products were characterized by X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, energy dispersive analysis by X-rays, laser Raman spectroscopy and photoluminescence spectroscopy. X-ray diffraction data indicates occurrence of hexagonal CdS with strong (002) preferred orientation. SEM images reveal formation of solvent-ratio dependent complex morphological (i.e., hierarchical) features both at the microscale and nanoscale. Fine-scale microstructure examination by TEM discloses formation of entangled nanorods, nano(potato)sticks, nanoflowers etc. Elemental analysis facility (equipped with TEM) suggests presence of Cd rich product. Raman spectroscopy shows the fundamental and overtone bands pertaining to hexagonal CdS with remarkable enhancement in relative intensities of such bands in case of sample corresponding to diethylenetriamine(DETA)/deionized water(DI) volume ratio of 6:1. Room temperature photoluminescence spectra mainly reveal broad asymmetric emission background composed of classical band edge and trap-induced emission in CdS.

Microwave-Assisted Preparation of Inorganic Nanostructures in Liquid Phase

“…Shinde et al 953 prepared CdS nanorod bundles as well as sea urchin-like and starfish-like hierarchical nanostructures using Cd(CH 3 COO) 2 and thiourea in diethylene triamine and water by the microwave-assisted method at 140 °C for 10 min. Amalnerkar et al 954 reported the microwave-assisted solvothermal synthesis of hierarchical CdS nanostructures including entangled nanorods, nanosticks, and nanoflowers using Cd(CH 3 COO) 2 and thiourea in binary solvents of diethylenetriamine and deionized water typically within 5 min. Patra et al 955 reported a microwave-assisted route to nanoflakes and dendrite-type β-In 2 S 3 in high yield (>97%) using InCl 3 and thiourea in mixed solvents of EG and PEG-400, and the length and width of the resulting nanoflakes were in the range of 70−600 and 4−10 nm, respectively.…”

Porous Chromium Terephthalate MIL‐101 with Coordinatively Unsaturated Sites: Surface Functionalization, Encapsulation, Sorption and Catalysis

“…Recently, Chang and co-workers established a microwave route of MOFs, [61,62] which was already utilized for the synthesis of porous materials [63,64] as well as condensed solids. [65] In addition to the above-mentioned methods, ionothermal synthesis [66] with ionic liquids as both a solvent and ligand and high-throughput synthesis by combinatorial approach have also been studied. [67,68] …”

Synthesis and properties of bismuth ferrite multiferroic flowers

“…One of the most rarely met nanobjects are nanoclusters in the form of nanoflowers reported in a nice review by Kharisov [1]. Nanoflowers can be composed of various elements and compounds like: metals (Au [2], Ni [3], Zn [4], Sn [5], Co [6]) and carbon [7,8], metal oxides (ZnO [9,10], MgO [11], CuO [12], α-MnO 2 [13], SnO 2 [14]), hydroxides and oxosalts (Mg(OH) 2 [15], Cu 2 (OH) 3 Cl [16]), sulphides, selenides and tellurides (CdS [17], ZnSe [18], PbTe [19]), nitrides and phosphides (lnN [20], GaP [21]), organic and coordination compounds (CdQ 2 complexes [22], alkali earth phenylphosphonates [23]).…”

“…However, it seems that the solvothermal and hydrothermal techniques are here especially effective [5,13,15,27,28,[34][35][36][37]. In some cases the hydrothermal process was activated by microwave heating [3,17,38].…”