Size Dependent Optical Properties and Structure of ZnS Nanocrystals Prepared from a Library of Thioureas

Bennett, Ellie; Greenberg, Matthew W.; Jordan, Abraham J.; Hamachi, Leslie S.; Banerjee, Soham; Billinge, Simon J. L.; Owen, Jonathan S.

doi:10.1021/acs.chemmater.1c03432

Size Dependent Optical Properties and Structure of ZnS Nanocrystals Prepared from a Library of Thioureas

Journal Article · Wed Jan 05 23:00:00 EST 2022 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.1c03432· OSTI ID:1842802

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Columbia Univ., New York, NY (United States)
Columbia Univ., New York, NY (United States); California Polytechnic State Univ. (CalPoly), San Luis Obispo, CA (United States)
Columbia Univ., New York, NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)

Here, ZnS nanocrystals (λ_max(1S_e-1S_3/2h) = 260 - 320 nm, d = 1.7 - 10.0 nm) are synthesized from Zn(O₂CR)₂ (O₂CR = tetra-decanoate, oleate and 2-hexyldecanoate), N,N'-disubstituted and N,N',N'-trisubstituted thioureas, and P,P,N-trisubstituted phos-phanecarbothioamides. The influence of precursor substitution, ligand sterics, and reaction temperature on the final nanocrystal size were evaluated. By using saturated hydrocarbon solvents and saturated aliphatic carboxylate ligands, polymeric byproducts could be avoided and pure ZnS nanocrystals isolated. Elevated temperatures, slower precursor conversion reactivity and branched zinc 2-hexyldecanoate yield the largest ZnS nanocrystals. Carefully purified zinc carboxylate, rapidly converting precursors, and cooling the synthesis mixture following complete precursor conversion provide quasi spherical nanocrystals with the narrowest shape dispersity. Nanocrystal sizes were measured using pair distribution function (PDF) analysis of X-ray scattering and scanning transmission electron microscopy (STEM) and plotted versus the energy of their first excitonic optical absorption. The resulting empirical relationship provides a useful method to characterize the nanocrystal size from 1.7-4.0 nm using optical absorption spectroscopy.

View Accepted Manuscript (DOE)

Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704

OSTI ID:: 1842802

Report Number(s):: BNL--222668-2022-JAAM

Journal Information:: Chemistry of Materials, Journal Name: Chemistry of Materials Journal Issue: 2 Vol. 34; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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