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High-Resolution X-ray Photoelectron Spectroscopic Studies of Alkylated Silicon(111) Surfaces

Webb, Lauren J. and Nemanick, E. Joseph and Biteen, Julie S. and Knapp, David W. and Michalak, David J. and Traub, Matthew C. and Chan, Ally S. Y. and Brunschwig, Bruce S. and Lewis, Nathan S. (2005) High-Resolution X-ray Photoelectron Spectroscopic Studies of Alkylated Silicon(111) Surfaces. Journal of Physical Chemistry B, 109 (9). pp. 3930-3937. ISSN 1520-6106. https://resolver.caltech.edu/CaltechAUTHORS:20170524-150224153

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Abstract

Hydrogen-terminated, chlorine-terminated, and alkyl-terminated crystalline Si(111) surfaces have been characterized using high-resolution, soft X-ray photoelectron spectroscopy from a synchrotron radiation source. The H-terminated Si(111) surface displayed a Si 2p_(3/2) peak at a binding energy 0.15 eV higher than the bulk Si 2p_(3/2) peak. The integrated area of this shifted peak corresponded to one equivalent monolayer, consistent with the assignment of this peak to surficial Si−H moieties. Chlorinated Si surfaces prepared by exposure of H-terminated Si to PCl_5 in chlorobenzene exhibited a Si 2p_(3/2) peak at a binding energy of 0.83 eV above the bulk Si peak. This higher-binding-energy peak was assigned to Si−Cl species and had an integrated area corresponding to 0.99 of an equivalent monolayer on the Si(111) surface. Little dichloride and no trichloride Si 2p signals were detected on these surfaces. Silicon(111) surfaces alkylated with C_nH_(2n+1)^− (n = 1 or 2) or C_6H_5CH_2^− groups were prepared by exposing the Cl-terminated Si surface to an alkylmagnesium halide reagent. Methyl-terminated Si(111) surfaces prepared in this fashion exhibited a Si 2p_(3/2) signal at a binding energy of 0.34 eV above the bulk Si 2p_(3/2) peak, with an area corresponding to 0.85 of a Si(111) monolayer. Ethyl- and C_6H_5CH_2-terminated Si(111) surfaces showed no evidence of either residual Cl or oxidized Si and exhibited a Si 2p_(3/2) peak ∼0.20 eV higher in energy than the bulk Si 2p_(3/2) peak. This feature had an integrated area of ∼1 monolayer. This positively shifted Si 2p_(3/2) peak is consistent with the presence of Si−C and Si−H surface functionalities on such surfaces. The SXPS data indicate that functionalization by the two-step chlorination/alkylation process proceeds cleanly to produce oxide-free Si surfaces terminated with the chosen alkyl group.


Item Type:Article
Related URLs:
URLURL TypeDescription
http://dx.doi.org/10.1021/jp047199cDOIArticle
http://pubs.acs.org/doi/abs/10.1021/jp047199cPublisherArticle
ORCID:
AuthorORCID
Brunschwig, Bruce S.0000-0002-6135-6727
Lewis, Nathan S.0000-0001-5245-0538
Additional Information:© 2005 American Chemical Society. Received 28 June 2004. Published online 12 February 2005. Published in print 1 March 2005. We gratefully acknowledge the National Science Foundation, Grant CHE-0213589, for support of this work and for providing a graduate research fellowship to L.J.W. A.C. acknowledges support from the Army Research Office. This research was carried out in part at the National Synchrotron Light Source, Brookhaven National Laboratory, which is supported by the U.S. Department of Energy, Division of Materials Sciences and Division of Chemical Sciences, under Contract DE-AC02-98CH10886. We thank Michael Sullivan for use of the N_2(g)-purged glovebox at the NSLS.
Funders:
Funding AgencyGrant Number
NSFCHE-0213589
Army Research Office (ARO)UNSPECIFIED
Department of Energy (DOE)DE-AC02-98CH10886
Issue or Number:9
Record Number:CaltechAUTHORS:20170524-150224153
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20170524-150224153
Official Citation:High-Resolution X-ray Photoelectron Spectroscopic Studies of Alkylated Silicon(111) Surfaces Lauren J. Webb, E. Joseph Nemanick, Julie S. Biteen, David W. Knapp, David J. Michalak, Matthew C. Traub, Ally S. Y. Chan, Bruce S. Brunschwig, and Nathan S. Lewis The Journal of Physical Chemistry B 2005 109 (9), 3930-3937 DOI: 10.1021/jp047199c
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:77731
Collection:CaltechAUTHORS
Deposited By: Ruth Sustaita
Deposited On:25 May 2017 21:40
Last Modified:03 Oct 2019 18:01

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