Formation and characterization of crystalline iron oxide films
on self-assembled organic monolayers and their in
situ patterning
Hyunjung Shin and Jong Up Jeon
Nano System Laboratory, Samsung Advanced Institute of Technology and CRI, P.O. Box 111,
Suwon, Korea 440-600
Y. Eugene Pak
Micro Electro-Mechanical System (MEMS) Laboratory, Samsung Advanced Institute of Technology,
P.O. Box 111, Suwon, Korea
Hyejin Im
Department of Ceramic Engineering, YonSei University, Seoul, Korea
Eung Soo Kim
Department of Materials Engineering, Kyonggi University, Suwon, Korea
(Received 14 July 2000; accepted 14 November 2000)
Crystalline and pore-free films of a–Fe
2
O
3
were prepared on hydrophilic
self-assembled organic monolayers (DTT-SAMs) at 80 °C. Subsequently, Fe
3
O
4
and
g–Fe
2
O
3
films were synthesized via post annealing of as-deposited a–Fe
2
O
3
. In situ
patterning of crystalline iron oxide thin layers was achieved via microcontact printing
(mCP) and selective deposition. mCP was used to pattern two different surface moieties
of self-assembled organic monolayers (SAMs) on Au–Cr–Si substrates. An elastomeric
stamp was used to transfer either hexadecanethiol (HDT) SAMs, which are to sustain
deposition of iron oxide precipitates, or hydrophilic SAMs [e.g., dithiothreitol (DTT)].
Selective deposition was realized through precipitation of iron oxide phases. Iron oxide
films were deposited onto hydrophilic SAMs, but not onto HDT surfaces. Line (width
of <1 mm) patterns in crystalline a–Fe
2
O
3
thin films were obtained.
I. INTRODUCTION
Magnetic oxides, mainly g–Fe
2
O
3
(maghemite) and
Fe
3
O
4
(magnetite), have been used most widely for the
last few decades in magnetic recording media.
1–3
Be-
cause Fe
2
O
3
is polymorphic and can exist in a thermo-
dynamically stable antiferromagnetic form (a–Fe
2
O
3
,
hematite), and a metastable ferrimagnetic form
(g–Fe
2
O
3
), the properties of the films are largely depen-
dent on film preparation methods and conditions.
4
In
most cases a–Fe
2
O
3
is a precursor to Fe
3
O
4
and g–Fe
2
O
3
via reduction in H
2
followed by controlled oxidation at
elevated temperatures in air.
5
Our primary interest was in fabrication of crystalline
as well as in situ patterned iron oxide film using self-
assembled organic monolayers (SAMs)
6
as a promoter
and/or inhibitor of its formation. SAMs are functional-
ized, siloxane- and/or thiolate-anchored, organic thin
films formed spontaneously on surfaces by immersion
into solutions of alkyl-chain surfactant molecules. Often
the terminal functionality can be chemically modified to
dramatically alter the surface’s reactivity and physical
characteristics, for example, charge, wetability, and ad-
hesion. Substrates derivatized with organic functional
groups can be used to control the deposition of inorganic
and/or mineral thin films from aqueous solutions, as re-
ported by several research groups.
7–9
Deposition and pat-
terning of iron oxyhydroxide in the form of FeOOH
(goethite) on sulfonic acid terminated SAMs from iron
nitrate aqueous solutions has been investigated.
10,11
No
reports, however, were found in the literature on the
deposition of crystalline iron oxide films onto function-
alized SAMs at ambient temperatures (<100 °C).
Microcontact printing (mCP) is a broadly applicable
technique for derivatizing surfaces.
12–14
Patterns of or-
ganic layers having dimensions <0.5 mm can be routinely
prepared on metals such as gold,
15,16
silver,
17
or copper
and on Si/SiO
2
18
by using an elastomeric stamp [usually
polydimethylsiloxane (PDMS)]. In the case of gold sur-
faces, alkanethiols are often used. By using different ter-
minal groups, it is possible to define areas on the surfaces
having well-controlled properties. For example, hydro-
phobic surfaces can be generated with hexadecanethiols
(HDT), hydrophilic surfaces with dithiothreitol (DTT),
and so on.
Our strategy for the fabrication of patterned iron oxide
films was to combine two key technologies: mCP to gen-
erate mixed surface moieties and selective deposition of
crystalline iron oxide films onto specific areas. There are
significant advantages in our strategy. First, patterned
oxide films can be generated directly without any post-
J. Mater. Res., Vol. 16, No. 2, Feb 2001 © 2001 Materials Research Society 564