Epitaxial Transition Metal Oxide Nanostructures Fabricated by a

Combination of AFM Lithography and Molybdenum Lift-Off**

By Naoki Suzuki, Hidekazu Tanaka,* and Tomoji Kawai*
In recent years, transition metal oxide films have attracted
much research interest because of their remarkable physical
properties such as ferroelectricity, ferromagnetism, high Tc
superconductivity, and colossal magnetoresistance. These useful
characteristics make oxide films potential candidates for novel
functional devices. For example, great advances have been
made in the application of half-metallic oxide materials in magnetic random access memory (MRAM)[1] with a large tunneling
magnetoresistance (TMR) ratio.[2,3] Nanostructures of half-metal magnetic oxides are especially of interest for the current-driven magnetization reversal of TMR devices. Ferroelectric oxides
provide another example of a useful oxide material with superior properties for non-volatile data storage (Fe-RAM). Obtaining nanostructures of these materials is of paramount importance for realizing a highly integrated Fe-RAM device.
The controlled nanofabrication of metal oxides is also important for the investigation of novel nanoscale properties.
For example, Yanagisawa et al.[4] have recently demonstrated
that the resistivity of a ca. 500 nm wide perovskite (La, Pr,
Ca)MnO3 channel structure rapidly falls off over three orders
of magnitude upon the application of a magnetic field, which
is very different from the behavior of a large-area thin film.
These authors have suggested that (La, Pr, Ca)MnO3 with a
strongly correlated electron system forms an electrical multidomain structure with a grain size of several hundreds of
nanometers; as the width of the oxide nanochannel is reduced
to the dimensions of the domain size, a single ferromagnetic
metal domain in the channel acts as a gate by transforming itself into a charge-ordered insulator.
Further discoveries of such novel properties of transition
metal oxides are expected upon scaling them down to nanoscale dimensions. Nevertheless, not much progress has been
achieved in this area. One of the reasons for this is that the

[*] Prof. H. Tanaka, Prof. T. Kawai

The Institute of Scientific and Industrial Research, Osaka University
8-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan)
E-mail: h-tanaka@sanken.osaka-u.ac.jp;
kawai@sanken.osaka-u.ac.jp
Dr. N. Suzuki
Japan Science and Technology Agency
4-1-8 Honmachi, Kawaguchi, Saitama 332-0012 (Japan)
[**] This work was supported by the Core Research for Evolutional
Science and Technology (CREST) of the Japan Science and Technology Agency (JST). The authors thank Dr. Takanori Tanaka, Dr. Masaki
Kanai, Dr. Issei Sato, and Dr. Yoshihiko Yanagisawa (ISIR Osaka University) for supporting the experiments being reported in this work.

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DOI: 10.1002/adma.200700646

fine fabrication of oxide films with nanoscale control still remains remarkably challenging. At this moment, the lower limit for the fine fabrication of oxides using photolithography is
only ca. 1 lm, notwithstanding the remarkable advances in
processing silicon surfaces with better than 100 nm resolution.
Recently, there have been several reports in the literature
dealing with the nanofabrication of transition metal oxides
using top-down approaches such as focused ion beam (FIB) lithography,[57] atomic force microscopy (AFM) lithography,[418] and electron-beam (e-beam) lithography.[19,20] These
methods have been used to achieve feature sizes less than ca.
100 nm. However, each of these top-down methods suffers
from some serious drawback. For example, FIB and AFM lithography are suitable for making holes and grooves in selected regions within an oxide film, but are not as useful for
defining isolated oxide islands and lines, because such patterns need to be defined by removing all sections of the film
that reside outside the pattern. However, for the application
of oxide nanopatterns to integrated memories and sensors, island and dot morphologies tend to be preferred over holes
and grooves. Although e-beam lithography is a feasible alternative for defining not only holes and grooves but also islands
and lines, it is generally necessary to perform some kind of
wet or dry etching after the patterning of the resist. In general,
it can be incredibly challenging to process oxides by most conventional wet or dry etching approaches because these materials are usually very hard and chemically stable. As a result,
the etching conditions depend strongly on the materials used.
Notably, it has been almost impossible to process some oxide
films (e.g., Pb(Zr,Ti)O3, SrTiO3) by wet etching.
The fabrication of oxide nanostructures by lift-off techniques, essentially involving some combination of top-down
and bottom-up approaches (i.e., preparation of an area-selective film by deposition using a patterned mask, followed by removal of the masked area), presents some intriguing possibilities by obviating the need to etch the oxide film. For example,
Donthu et al.[21,22] have recently developed a scheme to fabricate oxide nanostructures using soft e-beam lithography combined with a lift-off technique. These authors have patterned a
polymer e-beam resist by e-beam lithography and cast a solution of sol-gel precursors to the oxides onto the pattern by spin
coating. The sol-gel solution has then been dried by heat treatment at low temperature (less than 150 C). The patterned oxide has been obtained by removing the organic resist with acetone. The residual pattern has been annealed at 700 C in order
to crystallize the film. Donthu et al. have successfully prepared
ca. 40 nm oxide line patterns by this approach. However, the

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910

post-crystallization process leads to polycrystalline growth and

precludes the epitaxial growth of single-crystalline nanostructures. These films thus may form multi-domain structures with
a domain size of ca. 100 nm[22] and the presence of grain
boundaries or deleterious cracks. Moreover, it is almost impossible to control the thickness of these films at the atomic scale,
which makes it difficult to integrate these structures into functional nanodevices since the properties of many functional oxide films are strongly dependant on the film thickness.[2330]
Atomically controlled 3D oxide nanostructures are indispensable to the field of nanooxide electronics.
Dry thin-film deposition methods (e.g., pulsed laser deposition (PLD) and chemical vapor deposition (CVD)) are ideal
for obtaining high-quality epitaxial metal oxide films with a flat
surface and well-defined thickness controllable at the atomic
scale.[11] The combination of thin film metal oxide deposition
techniques with lift-off processes will provide access to interesting structures and enable the use of advances in thin film
metal oxide deposition to obtain nanoscale control of the resulting films. Moreover, lift-off techniques are generally compatible with the fabrication of oxide lines and islands even
when top-down methods such as AFM lithography and FIB lithography are used to pattern the polymer resist. However, the
dry deposition of transition metal oxides is generally performed at temperatures as high as several hundreds of degrees
to ensure the epitaxial growth of crystalline films. It is thus virtually impossible to use conventional lift-off techniques with a
polymer resist as the patterned mask, since the polymer pattern
will be destroyed at temperatures ranging from 100 to 200 C.
In this study, we have developed a lift-off technique based
on the use of patterned Mo films as resists to fabricate oxide
nanostructures. The Mo films are stable at high temperatures
that destroy polymer resists. Furthermore, the Mo films can
be easily removed by H2O2 or sublimation at high temperatures under ambient conditions.
There have been two previous reports in the literature[31,32]
pertaining to the patterning of thin films using Mo or Mo oxide resists for lift-off. In these reports, a-SiO2 micropatterns
have been fabricated by Mo lift-off. However, neither report
makes any mention of extending this technique to oxide nanostructures. Mo lift-off clearly has some distinct advantages as
compared to conventional oxide processing techniques. For
example, unlike sol-gel-based techniques for patterning organic resists, this approach is applicable to any well-defined
oxide film including artificial lattices. Since the oxides grow
directly from the surface of the substrate, the films are able to
grow epitaxially. As explained above, conditions for processing oxide films strongly depend on the materials used, which
is a serious problem for obtaining nanoscale control of the
films. However, using the Mo lift-off technique, the pattern of
the Mo mask is precisely transferred to the oxide film, and
thus the only factor that needs to be adjusted is the processing
of the Mo film, which is infinitely easier than direct processing
of the oxide film, and is furthermore independent of the
nature of the oxide. To prepare a nanometer-sized patterned
Mo mask, we have used AFM anodic oxidation lithography.

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AFM lithography is now a well-developed tool for surface

nanofabrication. In this approach, the surface of the material
or film is partially oxidized by an electrochemical reaction induced by a voltage-biased conductive AFM tip.[3335] Since
these processes allow direct monitoring of the surface, it is
possible to position the pattern with great accuracy. In most
cases, AFM-oxidized areas can be selectively removed by wet
etching with little or no damage to the unpatterned regions.
AFM lithography enables the processing of the Mo film
with high resolution because Mo is strongly conductive. In this
case, MoO3 mounds formed by local oxidation are easily removed by dissolution in water because MoO3 is water soluble.
As a result, patterned holes or grooves remain in the Mo
film.[36] By combining this Mo mask with the lift-off process,
sub-100 nm lines and dots should be achievable.
In the present study, we have realized ca. 150 nm Fe2.5Mn0.5O4 (FMO) nanoscale lines on an Al2O3 (0001) (ALO)
single-crystalline substrate by combining PLD, AFM nanofabrication, and the Mo lift-off technique. FMO thin films are
known to be ferromagnetic oxide semiconductors with a very
high Tc,[37] and may be applicable to advanced spin electronic
devices for room-temperature operation.
Figure 1 schematically illustrates the fabrication of oxide
nanostructures by combining Mo lift-off with AFM lithography. In the first step, a ca. 20 nm thick Mo film has been deposited onto the ALO substrate by magnetron sputtering.
MoO3 lines with widths of about ca. 150 nm have then been
defined using the AFM tip (Fig. 1a). The newly formed MoO3
mounds have been easily removed by immersion in water for
3 min, and ca. 150 nm grooves remain intact in the Mo film
(Fig. 1b). The obtained Mo pattern has been used as a resist
for the lift-off process. After slight dry etching with CF4+ to
eliminate residual Mo remnant on the grooves, a ca. 10 nm
thick FMO film has been deposited onto the pattern by PLD.
The deposition has been performed at 340 C in a 104 Pa oxygen atmosphere; these conditions ensure the epitaxial growth
of the film on the ALO substrate.[33] Since Mo is stable under
these conditions, the Mo mask retains its shape during deposition. After cooling down the sample to room temperature, the
Mo layer has been removed by ultrasonic treatment in
10 vol% H2O2 solution for 5 min. Figure 1c indicates that ca.
150 nm FMO nanoscale lines have been successfully defined
in the designated area, reflecting the shape of the Mo pattern.
Figure 2 shows 3D AFM images of the FMO stripe pattern
(the bottom panel is identical with Fig. 1c). The top panel
shows an enlarged AFM image of the enclosed area in the
bottom image. It is clearly apparent in the bottom panel that
uniform lines with a flat surface have been realized on the
ALO substrate, and its roughness is smaller than the typical
grain size (100300 nm)[22,38] of polycrystalline oxides.
Although some sharp mounds are visible in the bottom panel,
the top image indicates that these mounds exist only at the
edges of the lines and that the area between the edges is perfectly flat. The mounds at the edges are so-called rabbit ear
in shape, and are similar to features occasionally observed
after conventional lift-off processes. Notably, no distinct

2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

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AFM t i p
(b)
3

Mo
O

Mo

ALO

ALO

10

2
3
4
Distance/ m

ALO

Height / nm

Height / nm

Height / nm

20

0
0

(c)
FM
O

(a)

-10
0

2
3
4
Distance/ m

10

0
0

2
3
4
Distance/ m

Figure 1. Mo lift-off process used for the fabrication of oxide nanostructures. The top panel schematically illustrates the steps involved in the process.
The middle panel shows topographic images of line patterns fabricated by this process. The bottom panels depict the cross sections of the line patterns shown in the middle panels along the yellow lines.

Figure 2. 3D AFM images of a FMO pattern fabricated by the Mo lift-off process. The top panel
shows an enlarged AFM image of the demarcated area in the bottom image.

Adv. Mater. 2008, 20, 909913

grains have been observed in the FMO

pattern. This result clearly shows that
the FMO lines fabricated by the Mo
lift-off process do not form a grain
structure, indicating that they have
grown epitaxially on the ALO substrate.
FMO thin films typically grow epitaxially on ALO substrates under the deposition conditions used here.[37]
Figure 3a shows a scanning electron
microscopy (SEM) image of a FMO
pattern fabricated by the Mo lift-off
technique after the mask has been processed by AFM lithography. FMO
blocks of ca. 5 lm squares are seen to
be distinctively defined on the substrate.
Figure 3bd shows electron probe microanalysis (EPMA) maps indicating
the distribution of Mn and Fe atoms in
the pattern. The EPMA maps clearly indicate that both Mn and Fe atoms are
spatially confined only within the patterns. On the other hand, no signal has
been detected for Mo atoms. This result
shows that the FMO film on the Mo
mask has been completely lifted-off
upon removal of the Mo layer.

2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

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gap

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10m

FMO lines
Pt electrode

ALO substrate
Pt electrode

Figure 4. Optical microscopy image of FMO stripes between Pt electrodes fabricated by the Mo lift-off process. The locations of the FMO
lines are indicated by arrows.

Figure 3. a) Scanning electron microscopy (SEM) image of a FMO pattern fabricated by the Mo lift-off process; b) SEM image of the same pattern obtained while performing electron probe microanalysis (EPMA)
measurements. Spatial distribution of c) Mn and d) Fe derived from
EPMA measurements.

resistivity/ cm

10 1

10 0

150

In order to verify the quality of the nanoscale FMO lines,

we have measured their resistivity. For this measurement, we
have prepared FMO stripes with a width of ca. 200 nm spanning across two Pt electrodes. A hundred FMO lines have
been fabricated since the resistivity of a single FMO line is
too large for these measurements. It has already been reported that the electrical transport properties of FMO channels
processed by AFM lithography do not show any significant
size effect even for ca. 100 nm widths.
Figure 4 shows an optical microscopy image (Olympus
BX51) of FMO stripes connecting two Pt electrodes with a
ca. 10 lm gap. The Mo lift-off technique easily enables the
preparation of many flat oxide stripes in the designated area.
This enables electrical measurements of the nanoscale line
structures, which would have been far more difficult to accomplish using a top-down patterning approach.
The resistivity of the FMO stripes at room temperature has
been determined to be 0.50.6 X cm, whereas the resistivity of
the unpatterned FMO thin film is ca. 0.35 X cm. Figure 5 shows
a plot of the electrical resistivity versus temperature (RTcurve) for both the unpatterned FMO thin film and FMO lines
fabricated by the Mo lift-off technique. Both curves decline as
the temperature rises, and there does not appear to be a significant difference between the stripes and the unpatterned film.
Considering that the resistivity values at room temperature are
of the same order of magnitude and that the tendency of the
RT-curves is similar, it is clear that the patterned FMO film retains the physical properties of the unpatterned film.

912

www.advmat.de

: FMO nano lines

: FMO thin film

200
250
temperature/K

300

Figure 5. Plots indicating the dependence of the electrical resistivity on

temperature for an unpatterned FMO thin film (open circles) and FMO
lines (closed circles) fabricated by the Mo lift-off process.

In summary, nanoscale lines of a FMO thin film have been

defined by combining PLD with a Mo lift-off technique. The
ca. 150 nm wide grooves in the Mo mask for the lift-off resist
have been fabricated using AFM lithography. The Mo mask is
stable during the deposition of FMO at 340 C. After the deposition of FMO, the Mo mask has been ultrasonically removed in a H2O2 solution for 5 min. At the end of this process, ca. 150 nm wide FMO stripes remain on the substrate.
AFM measurements show that the FMO stripes have a flat
surface without any grain structure. EPMA measurements
confirm that the FMO film is confined to the area defined by
the Mo nanomask processed by AFM lithography. These measurements further indicate that FMO on the mask has been
completely removed during the lift-off process. The RT-curve
measurements show that the patterned FMO has not been seriously damaged by the Mo lift-off process. We have further
confirmed that the Mo nanomask is able to survive the film
deposition process at temperatures as high as 700 C. This Mo
lift-off process with the capacity for high-temperature film deposition opens new avenues for the fabrication of many different kinds of well-defined metal oxide nanostructures in combination with thin film deposition techniques such as PLD,
CVD, and radiofrequency (RF) sputtering.

2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Adv. Mater. 2008, 20, 909913

Experimental
The FMO patterns were fabricated as follows: first, a ca. 20 nm Mo
layer was deposited onto an ALO substrate. Next, a MoO3 pattern
was formed by the local anodic oxidation of Mo induced by a voltagebiased AFM tip. The MoO3 regions were then removed by immersion
in water for 3 min. After slight dry etching with CF4+ to eliminate the
residual Mo layer, a FMO film with a thickness of ca. 10 nm was deposited onto the pattern at an elevated temperature and then cooled
down to room temperature. The Mo layer was subsequently removed
by ultrasonic treatment with 10 vol% H2O2 solution for 5 min.
ALO substrates were supplied by Furuuchi Chemicals and used
after ultrasonic cleaning in ethanol without any further treatment.
The Mo layer was deposited by magnetron sputtering using a Quick
Coater SC-701HMC system (Sanyu Electron). During deposition, argon
was used as the sputtering gas. The purity of the Mo target was 99.9%.
AFM lithography was performed with a Dimension 3100 AFM microscope (Veeco) using Olympus OMCL-AC240TM AFM tips with a
resonant frequency of ca. 70 kHz and a spring constant of 2 N m-1. In
order to achieve good uniformity of the pattern, the lithography process was performed with a constant current.[14] Control over the current was obtained by connecting the AFM tip and the sample to an
external setup comprising a picoammeter and a feedback circuit.
The FMO thin film was deposited by PLD (arc excimer laser;
k = 193 nm). The target was prepared by sintering a FMO pellet
synthesized by a conventional solid reaction process. The PO2 was set at
1.0104 Pa, and the temperature of the substrate was kept at 340 C.
In order to measure the spatial atomic distribution, EPMA measurements were performed using an electron probe microanalyzer JXA8800R (JEOL). For this measurement, ca. 50 nm thick FMO was deposited on a ca. 70 nm thick Mo mask to improve the sensitivity of EPMA.
The resistivity of FMO stripes fabricated as described above was
also measured. FMO stripes were prepared between a ca. 10 lm gap
between Pt electrodes on an ALO substrate. The Pt electrodes were
fabricated by sputtering Pt onto a substrate wound with a 10 lmU
tungsten wire and removing the wire after completion of the sputtering process. In order to obtain measurable conductivity, 100 FMO
lines were fabricated between the Pt gap electrodes. The resistivity of
the system was measured using a Physical Property Measurement System Model 6000 (Quantum Design).
Received: March 18, 2007
Revised: November 13, 2007
Published online: January 30, 2008

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Although the ca. 150 nm widths of the lines shown in this

study are larger than that of nanochannels (ca. 30 nm[15] and
50 nm[16]) reported previously by our group using top-down removal AFM lithography, the present nanoscale lines are completely isolated and no remnants of the film are present outside
the lines, as corroborated by Figure 4. This represents a big advantage for the application of these lines in integrated oxide
devices. To the best of our knowledge, this is the first report of
the fabrication of isolated thin lines of a transition metal oxide
by a dry method with a line-width less than 150 nm.
The Mo lift-off process is also compatible with other fabrication methods that allow fine control such as e-beam lithography, FIB, and photolithography. In particular, it is worth
noting that it is much easier to process metals by photolithography as compared to oxides. Thus, even large-area oxide
nanopatterns should be accessible by combining photolithography with the Mo lift-off technique.

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