Selectivity of the Chemisorption of Vinylacetic Acid on the Si(001)2×1 Surface
Han-Na Hwang, Jae Y. Baik, Ki-Seok An, Sun S. Lee, and Yunsoo Kim*
Thin Film Materials Laboratory, AdVanced Materials DiVision, Korea Research Institute of
Chemical Technology, Daejeon 305-600, Korea
Chan C. Hwang and Bongsoo Kim
Beamline Research DiVision, Pohang Accelerator Laboratory, Pohang UniVersity of Science and Technology,
Pohang 790-784, Korea
ReceiVed: January 10, 2004; In Final Form: April 7, 2004
The adsorption of vinylacetic acid (VAA) on the Si(001)2×1 surface has been investigated using low-energy
electron diffraction, X-ray photoelectron spectroscopy, and synchrotron radiation photoemission spectroscopy.
VAA adsorbs on the Si(001)2×1 surface at room temperature, not through the reaction of the vinyl group
(CH
2
dCH-) but through the dissociative adsorption of RCOOH (R ) CH
2
dCHCH
2
) into RCOO(ad) as a
unidentate adsorbate and H(ad) without breaking the Si dimers. Curve-fitting of the Si 2p core level spectra
taken after VAA exposures shows the development of two new surface components, S
O
and S
H
, shifted by
+0.93 and +0.40 eV, respectively, from the bulk component. The binding energy shifts indicate that the S
O
and S
H
components are due to the Si-OOC-R and Si-H species formed by the dissociative adsorption of
VAA. The adsorption behavior was confirmed by the analysis of the C 1s and O 1s core level spectra. The
C1s core level spectrum for the VAA-saturated surface clearly shows three components contributed by carbon
atoms in the OdC-O, -C-C-, and -CdC- groups, while the O 1s core level spectrum consists of two
components due to oxygen atoms in the Si-O- and -CdO groups. There is no evidence for the bonding
between the Si dimer and the -CdC- bond of VAA through the [2+2] cycloaddition reaction, which is
expected in the adsorption of unsaturated hydrocarbon compounds on the Si(001)2×1 surface, nor for the
hetero-[2+2] reaction of the -CdO group with the Si dimer. This selectivity in the reacting group is discussed
on the basis of the differences in reaction barriers between the Si dimers and the functional groups of the
VAA molecule.
I. Introduction
Covalent attachment chemistry of organic molecules on
silicon surfaces has been of great interest in surface science.
Apart from the fundamental interest, the attachment of organic
molecules to the Si surfaces has been one of promising subjects
for integrating the wide range of available chemical function-
alities of organic molecules with micro- and nano-electronic
technology.
1
The Si(001)2×1 reconstruction is induced by dimerization
of the top layer Si atoms in order to reduce the number of surface
dangling bonds of the ideal bulk-terminated Si(001) surface,
which results in a strong σ and a weak π bonds on the surface
because of the strained geometry.
2-4
The weak π bond is very
reactive in molecule adsorption.
5,6
Several examples of molecule
attachment chemistry on the Si(001)2×1 surface have been
reported for organic molecules having various single- and multi-
functional groups, such as alkenyl,
7-12
hydroxyl,
13-15
mer-
capto,
16
carboxyl,
17-21
and amino
18,22,23
groups, etc., which can
be employed as important building blocks for attaching organic
molecules to the Si surface.
In this study, the adsorption of vinylacetic acid on the Si-
(001)2×1 surface has been investigated. Vinylacetic acid
(VAA), as a typical monomer having both a vinyl (H
2
CdCH-)
and a carboxyl (-COOH) groups, is a bifunctional organic
molecule having usable single and double bonds. Thus, VAA
may be chosen to demonstrate the chemical selectivity and
reactivity of the functional groups with the Si dimers on the
Si(001)2×1 surface.
Dissociative chemical interactions of carboxyl and hydroxyl
groups with the dangling bonds of the Si(001)2×1 surface at
room temperature have been reported from high-resolution
electron energy loss spectroscopy (HREELS), near-edge X-ray
absorption fine structure (NEXAFS), low-energy electron dif-
fraction (LEED), and/or photoemission spectroscopy measure-
ments for the adsorption of formic acid (HCOOH),
17,20
methanol
(CH
3
OH),
14
ethanol (CH
3
CH
2
OH),
13,15
2-propanol (
i
PrOH),
15
tert-butyl alcohol (
t
BuOH),
15
benzoic acid (C
6
H
5
COOH),
18,19
and 4-aminobenzoic acid (H
2
NC
6
H
4
COOH)
21
on the Si(001)2×1
surface. It was confirmed that chemical interactions induce the
HCOO-Si (or CH
3
O-Si, CH
3
CH
2
O-Si, R-C
6
H
4
-COO-Si,
etc.) and the H-Si bonds on the surface. The adsorption of an
unsaturated hydrocarbon on the Si(001)2×1 surface was identi-
fied as the [2+2] cycloaddition reaction (or Diels-Alder
reaction) between the CdC bond and the Si-Si dimer.
7-12
In
addition, the hetero [2+2] cycloaddition reaction of simple
carbonyl-containing compounds on the Si(001)2×1 surface has
been observed.
24-26
Recently, experimental and theoretical
studies of the unsaturated ketones including ethyl vinyl ketone
on the Si(001)2×1 surface showed that the ene and the hetero
Diels-Alder reactions are favored.
27
On the other hand, maleic
anhydride adsorbed preferentially on inter-dimer sites of the
* Author to whom correspondence should be addressed. Tel: 82-42-
860-7350. Fax: 82-42-861-4245. E-mail: yunsukim@krict.re.kr.
8379 J. Phys. Chem. B 2004, 108, 8379-8384
10.1021/jp0498769 CCC: $27.50 © 2004 American Chemical Society
Published on Web 05/25/2004