Template-free vapor-phase growth of patrónite by atomic layer deposition

Weimer, Matthew S.; McCarthy, Robert F.; Emery, Jonathan D.; Bedzyk, Michael J.; Sen, Fatih G.; Kinaci, Alper; Chan, Maria K. Y.; Hock, Adam S.; Martinson, Alex B. F.

doi:10.1021/acs.chemmater.6b05084

Title: Template-free vapor-phase growth of patrónite by atomic layer deposition

Journal Article · Thu Mar 09 00:00:00 EST 2017 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.6b05084· OSTI ID:1352533

^[1]; McCarthy, Robert F. ^[2];

^[3];

^[3]; Sen, Fatih G. ^[4]; Kinaci, Alper ^[4];

^[4];

^[1];

^[4]

Illinois Institute of Technology, Chicago, IL (United States); Argonne National Lab. (ANL), Argonne, IL (United States)
Argonne National Lab. (ANL), Argonne, IL (United States); Microlink Devices, Inc., Niles, IL (United States)
Northwestern Univ., Evanston, IL (United States)
Argonne National Lab. (ANL), Argonne, IL (United States)

Despite challenges to control stoichiometry in the vanadium-sulfur system, template-free growth of patrónite, VS₄, thin films is demonstrated for the first time. A novel atomic layer deposition (ALD) process enables the growth of phase pure films and the study of electrical and vibrational properties of the quasi-one-dimensional (1D) transition metal sulfide. Self-limiting surface chemistry during ALD of VS4 is established via in situ quartz crystal microbalance and quadrupole mass spectrometry between 150 to 200 °C. The V precursor, unconventionally, sheds all organic components in the first half-cycle, while the H₂S half-cycle generates the disulfide dimer moiety, S₂^-2, and oxidizes V³⁺ to V⁴⁺. X-ray analysis establishes VS₄ crystallinity and phase purity, as well as a self-limiting growth rate of 0.33 Å/cy, modest roughness (2.4 nm) and expected density (2.7g/cm³ ). Phase pure films enable a new assignment of vibrational modes and corresponding Raman activity of VS4 that is corroborated by density functional theory (DFT) calculations. Lastly, at elevated growth temperatures, a change in the surface mechanism provides a synthetic route to a second vanadium-sulfur phase, V₂S₃.

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Research Organization:: Argonne National Lab. (ANL), Argonne, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Argonne-Northwestern Solar Energy Research Center (ANSER)

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

Grant/Contract Number:: AC02-06CH11357; SC0001059

OSTI ID:: 1352533

Journal Information:: Chemistry of Materials, Vol. 29, Issue 7; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 30 works

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36 MATERIALS SCIENCE
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Atomic Layer Deposition
Density Functional Theory
In Situ Quartz Crystal Microbalance
Patrónite
Raman Spectroscopy
V(V2 -2)2
VS4

Title: Template-free vapor-phase growth of patrónite by atomic layer deposition

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