Resolving the Evolution of Atomic Layer-Deposited Thin-Film Growth by Continuous In Situ X-Ray Absorption Spectroscopy

Qu, Xiaohui; Yan, Danhua; Li, Ruoshui; Cen, Jiajie; Zhou, Chenyu; Zhang, Wenrui; Lu, Deyu; Attenkofer, Klaus; Stacchiola, Dario J.; Hybertsen, Mark S.; Stavitski, Eli; Liu, Mingzhao

doi:10.1021/acs.chemmater.0c04547

Title: Resolving the Evolution of Atomic Layer-Deposited Thin-Film Growth by Continuous In Situ X-Ray Absorption Spectroscopy

Journal Article · Mon Feb 08 00:00:00 EST 2021 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.0c04547· OSTI ID:1766780

Qu, Xiaohui ^[1]; Yan, Danhua ^[2]; Li, Ruoshui ^[2]; Cen, Jiajie ^[3];

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^[1]; Attenkofer, Klaus ^[4];

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^[1]; Stavitski, Eli ^[1];

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Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN); Stony Brook Univ., NY (United States)
Stony Brook Univ., NY (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)

In situ synchrotron X-ray absorption near-edge structure characterization of thin-film titania growth by atomic layer deposition (ALD) over ZnO nanowires reveals persistent low-coordinated Ti motifs leading to a new picture of ALD growth. Through the design of growth and measurement cycles, Ti K-edge spectral data are continuously recorded so as to characterize the film evolution as a function of ALD cycle number and the surface changes within the time scale of the ALD cycle. A unified set of analysis tools is developed to interpret the time-series of spectral data. A prenucleation stage of growth, a transition region, and then a steady-state growth stage are observed with distinguishable features. Multivariate curve resolution analysis, that is physically constrained, demonstrates two specific spectral components with associated, time-dependent concentrations. The bulk-film component tracks the stages of growth. The surface and interface components, present throughout the stages of growth, reveal a significant coverage of relatively isolated or loosely networked tetrahedrally coordinated Ti atomic motifs. Lastly, spectral signatures for the intra-cycle growth kinetics are reconstructed at a time resolution of ~1 s and demonstrate that the transient Ti motifs on the growing surface stabilize within a few seconds of the Ti precursor pulse.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II) and Center for Functional Nanomaterials (CFN); Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Laboratory Directed Research and Development (LDRD) Program

Grant/Contract Number:: SC0012704; 19-008

OSTI ID:: 1766780

Alternate ID(s):: OSTI ID: 1764595

Report Number(s):: BNL-221045-2021-JAAM; BNL-220997-2021-JAAM

Journal Information:: Chemistry of Materials, Vol. 33, Issue 5; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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36 MATERIALS SCIENCE
thickness
x-ray absorption near edge spectroscopy
oxides
precursors
atomic layer deposition

Title: Resolving the Evolution of Atomic Layer-Deposited Thin-Film Growth by Continuous In Situ X-Ray Absorption Spectroscopy

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