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Title: Phase control in the colloidal synthesis of well-defined nickel sulfide nanocrystals

Abstract

In this work, morphologically well-defined colloidal nanocrystals of Ni 3S 4, NiS, Ni 9S 8, and Ni 3S 2 were independently prepared through a solution-phase synthesis using N, N'-disubstituted thioureas as the sulfur precursor. Synthetic control over phase and composition of the resulting colloidal nickel sulfide nanocrystals was achieved by primarily adjusting the reactivity of substituted thioureas as well as tuning the key reaction parameters of temperature and precursor ratio. In general, the more reactive N, N'-diphenyl thiourea yields more sulfur-rich phases (Ni 3S 4 and NiS) while less reactive N, N'-dibutyl thiourea yields sulfur-poor phases (Ni 9S 8 and Ni 3S 2). This phase control can be further tuned through the use of 1-dodecanethiol as an important secondary reactivity-directing agent. In the presence of 1-dodecanethiol, nanocrystals of more sulfur-deficient phases are prepared, while in the absence of 1-dodecanethiol, more sulfur-rich phases are prepared. Under the most sulfur-rich synthetic conditions ( i.e., with N, N'-diphenyl thiourea and no thiol) a phase progression from Ni 3S 4 to the α-NiS and β-NiS phases was observed upon an increase in reaction temperature and sulfur-to-nickel precursor ratio. In conclusion, this study establishes, for the first time, a systematic evaluation of factors that simultaneouslymore » control the phase and yield well-defined nickel sulfide nanocrystals.« less

Authors:
ORCiD logo [1];  [1];  [1];  [1]; ORCiD logo [1]
  1. Univ. of Southern California, Los Angeles, CA (United States)
Publication Date:
Research Org.:
Univ. of Southern California, Los Angeles, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1582647
Alternate Identifier(s):
OSTI ID: 1465600
Grant/Contract Number:  
SC0006812; FG02-11ER46826
Resource Type:
Accepted Manuscript
Journal Name:
Nanoscale
Additional Journal Information:
Journal Volume: 10; Journal Issue: 34; Journal ID: ISSN 2040-3364
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 77 NANOSCIENCE AND NANOTECHNOLOGY

Citation Formats

Barim, Gözde, Smock, Sara R., Antunez, Priscilla D., Glaser, Daniela, and Brutchey, Richard L. Phase control in the colloidal synthesis of well-defined nickel sulfide nanocrystals. United States: N. p., 2018. Web. doi:10.1039/c8nr05208e.
Barim, Gözde, Smock, Sara R., Antunez, Priscilla D., Glaser, Daniela, & Brutchey, Richard L. Phase control in the colloidal synthesis of well-defined nickel sulfide nanocrystals. United States. doi:10.1039/c8nr05208e.
Barim, Gözde, Smock, Sara R., Antunez, Priscilla D., Glaser, Daniela, and Brutchey, Richard L. Thu . "Phase control in the colloidal synthesis of well-defined nickel sulfide nanocrystals". United States. doi:10.1039/c8nr05208e. https://www.osti.gov/servlets/purl/1582647.
@article{osti_1582647,
title = {Phase control in the colloidal synthesis of well-defined nickel sulfide nanocrystals},
author = {Barim, Gözde and Smock, Sara R. and Antunez, Priscilla D. and Glaser, Daniela and Brutchey, Richard L.},
abstractNote = {In this work, morphologically well-defined colloidal nanocrystals of Ni3S4, NiS, Ni9S8, and Ni3S2 were independently prepared through a solution-phase synthesis using N,N'-disubstituted thioureas as the sulfur precursor. Synthetic control over phase and composition of the resulting colloidal nickel sulfide nanocrystals was achieved by primarily adjusting the reactivity of substituted thioureas as well as tuning the key reaction parameters of temperature and precursor ratio. In general, the more reactive N,N'-diphenyl thiourea yields more sulfur-rich phases (Ni3S4 and NiS) while less reactive N,N'-dibutyl thiourea yields sulfur-poor phases (Ni9S8 and Ni3S2). This phase control can be further tuned through the use of 1-dodecanethiol as an important secondary reactivity-directing agent. In the presence of 1-dodecanethiol, nanocrystals of more sulfur-deficient phases are prepared, while in the absence of 1-dodecanethiol, more sulfur-rich phases are prepared. Under the most sulfur-rich synthetic conditions (i.e., with N,N'-diphenyl thiourea and no thiol) a phase progression from Ni3S4 to the α-NiS and β-NiS phases was observed upon an increase in reaction temperature and sulfur-to-nickel precursor ratio. In conclusion, this study establishes, for the first time, a systematic evaluation of factors that simultaneously control the phase and yield well-defined nickel sulfide nanocrystals.},
doi = {10.1039/c8nr05208e},
journal = {Nanoscale},
number = 34,
volume = 10,
place = {United States},
year = {2018},
month = {8}
}

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