Solvent-Free Synthesis of Quaternary Metal Sulfide Nanoparticles Derived from Thiourea

Abstract
The synthesis of metal sulfide (MS) materials with sizes in the sub-10 nm regime often requires capping agents with long hydrocarbon chains that affect their structures and properties. Herein, this study presents a molten-state synthesis method for a series of transition-MS nanoparticles using thiourea as a reactive precursor without capping agents. This study also reports the synthesis of MS with single metals (Fe, Co, Ni, Cu, and Zn) and quaternary CuGa2In3S8 using the same synthesis protocol. Thiourea first melts to form a molten-state condition to serve as the reaction medium at a relatively low temperature (<200 °C), followed by its thermal decomposition to induce a reaction with the metal precursor to form different MS. This synthesis protocol, owing to its dynamic characteristics, involves the formation of a variety of organic carbon nitride polymeric complexes around the MS particles. Dynamic nuclear polarization surface-enhanced nuclear magnetic resonance spectroscopy is effective to identify the polymeric compositions and structures as well as their interactions with the MS. These results provided thorough structural descriptions of the MS nanoparticles surrounded by the carbon nitride species derived from thiourea, which may find various applications, including photocatalytic water splitting.

Citation
Bhunia MK, Abou-Hamad E, Anjum DH, Gurinov A, Takanabe K (2017) Solvent-Free Synthesis of Quaternary Metal Sulfide Nanoparticles Derived from Thiourea. Particle & Particle Systems Characterization: 1700183. Available: http://dx.doi.org/10.1002/ppsc.201700183.

Acknowledgements
The research reported in this publication was supported by King Abdullah University of Science and Technology (KAUST). The authors are grateful to Dr. Ahmed Ziani at KAUST for assistance with the SEM observations.

Publisher
Wiley

Journal
Particle & Particle Systems Characterization

DOI
10.1002/ppsc.201700183

Additional Links
http://onlinelibrary.wiley.com/doi/10.1002/ppsc.201700183/full

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