COMMUNICATIONS
mate 1 sun light intensity. FTIR measurements were performed on a
6030 Mattson Galaxy Series FTIR spectrometer. Spectroscopic char-
acterization was performed using a pressure cell equipped with CaF2
windows.
Received: December 22, 2003
Final version: April 1, 2004
± Architectures**
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______________________
Adv. Mater. 2004, 16, No. 19, October 4 DOI: 10.1002/adma.200400337
Transparent Solid-State Lithiated
Neutron Scintillators Based on Self-
Assembly of Polystyrene-block-
poly(ethylene oxide) Copolymer
By Hee-Jung Im, Suree Saengkerdsub,
Andrew C. Stephan, Michelle D. Pawel,
David E. Holcomb, and Sheng Dai*
Neutrons generated via either nuclear reactors or spallation
sources are widely used as unique photon sources to charac-
terize structures of nanomaterials and magnetic materials
through various spectroscopic techniques and to diagnose sol-
id-state structures through neutron tomography techniques.
These measurement methods depend greatly on the sensitiv-
ities of neutron detectors and/or neutron fluxes from nuclear
reactors or spallation sources. The increase of neutron fluxes
is an extremely costly process and therefore the improvement
of the measurement sensitivities lies in the development of
sensitive neutron detectors. Another recent important appli-
cation of neutron detectors is in the area of the prevention of
international nuclear smuggling. Because fissile materials
(plutonium-239 and uranium-235) emit neutrons via sponta-
neous fissions, the development of improved neutron scintilla-
tors for security and safe-guard applications is of obvious val-
ue.
Currently, neutrons are mainly detected by scintillation or
gas ionization.[1] Because of the low density of gas, gas-ioniza-
tion detectors are either quite large or operate at high pres-
sure in order to obtain good neutron-detection efficiency. In
addition, the response times of the gas-ionization detectors
are relatively slow. Liquid scintillators can avoid the problems
of gas-based detectors but must be handled carefully (e.g.,
some must be stored and handled in an oxygen and water-free
environment) and are difficult to be integrated for field appli-
cations. Thus, a major trend in radiation sensor research em-
phasizes the development of efficient solid-state scintillating
±
[*] Dr. S. Dai, Dr. H.-J. Im, Dr. S. Saengkerdsub
Dr. A. C. Stephan, M. D. Pawel
Chemical Sciences Division, Oak Ridge National Laboratory
Oak Ridge, TN 37831 (USA)
E-mail: dais@ornl.gov
Dr. D. E. Holcomb
Nuclear Science and Technology Division
Oak Ridge National Laboratory
Oak Ridge, TN 37831 (USA)
[**] The Oak Ridge National Laboratory is managed for the Department
of Energy under contract No. DE-AC05-00OR22725 by UT-Battelle,
LLC. Funding for this work is through the support of the Department
of Energy NA-22. This research was supported in part by the appoint-
ments for H.-J. Im and S. Saengkerdsub to the ORNL Research
Associate Program, administered jointly by ORNL and Oak Ridge
Institute for Science and Education. The authors thank Carl Willis for
assembling a portable pulse-height analysis system.
 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 1757
COMMUNICATIONS
materials,[2] which will significantly enhance general capabili-
ties for in-situ monitoring and imaging of radioactive contami-
nants in the environment.
Because neutrons have no charge, neutron absorbers such
as 6Li or 10B are required to convert neutrons to detectable
charged particles. The 6Li(n, a)H-3 conversion reaction has a
large Q value (4.79 MeV), significantly larger than that which
resulted from 10B(n, a)7Li (2.79 MeV). Accordingly, 6Li is a
desirable neutron absorber for scintillation applications due
to its highly energetic nuclear reaction products. All air-stable
lithium compounds are extremely polar and hydrophilic. Thus,
the current solid-state neutron scintillators using the 6Li neu-
tron absorber are based on inorganic materials such as 6Li-
doped silica glasses and solid mixtures of 6LiF and ZnS/Ag.
These scintillators are prepared by high-temperature pro-
cesses and are therefore difficult to directly integrate into
electronic detection devices as thin films. We have recently
developed efficient room-temperature solid-state di-ureasil
neutron detectors using a silica sol±gel process.[3] These sol±
gel neutron detectors have non-hygroscopic, elastic, transpar-
ent, crack-free, and thick monolithic properties, and can be
directly fabricated onto electrical and optical devices. How-
ever, the photon-conversion yields of the sol±gel scintillators
have not been as high as expected. The quenching effects
induced by hydroxy and other polar groups associated with
silica sol±gel and self-absorption of scintillating light caused
by the very pale yellowish color are considered to be the main
reasons for the limited light yield. These deficiencies with the
current neutron scintillators using 6Li neutron absorbers
prompted us to develop lithiated-organic-polymer neutron
scintillators.
The key challenge in synthesizing lithiated-organic-polymer
scintillators is how to incorporate hydrophilic lithium salts
into hydrophobic organic media at a
sufficient concentration without de-
stroying the scintillator's light yield and
CH2-CH
optical transparency. Recent break- n m
throughs in polymer synthesis have re-
sulted in the development of a number
of novel methodologies for the prepa- Polystyrene-block-poly(ethylene oxide)
ration of block copolymers with well-
defined amphiphilic properties and
ordered mesostructures.[4] Polystyrene-
block-poly(ethylene oxide) is an exam-
ple of an amphiphilic copolymer, con-
sisting of hydrophilic poly(ethylene
oxide) and hydrophobic polystyrene
domains through self-assembly.[5] The
hydrophilic domain is ideal for doping
lithium salts while the hydrophobic
polystyrene domain can be loaded with
hydrophobic organic scintillators. In
fact, poly(ethylene oxide)s are exten-
sively used as electrolytes to solubilize
lithium salts in lithium batteries. Simi- Scheme 1. Preparation of the lithiated scintillator based on the self-assembly of the block copoly-
larly, polystyrenes are widely employed mer.
1758  2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
as matrices in order to dope scintillating dyes for alpha and
beta radiation sensors.[6] For example, BC-400 (Bicron Direct,
Saint-Gobain, MA), a polyvinyltoluene-based scintillator
doped with 2,5-diphenyloxazole (PPO) and 1,4-bis-2-(5-phe-
nyloxazolyl)-benzene (POPOP), is the best existing plastic
scintillator for alpha particle detection.[7] Because 6Li emits
an alpha and a triton (H-3) particle upon absorption of a neu-
tron, a logical approach to synthesizing a neutron scintillator
is to place 6Li in a matrix material similar to that of BC-400 or
other existing organic scintillators without affecting the trans-
parency of the resulting materials. Our approach involves this
amphiphilic design strategy toward new neutron scintillators
with the introduction of a poly(ethylene oxide) functional
group into an aromatic ring-containing backbone for lithium
complexation.
The block copolymer used in our investigation is polysty-
rene-b-poly(ethylene oxide) with the molecular weights of the
polystyrene and poly(ethylene oxide) blocks at 2300 and 3200,
respectively. The volume fraction of PEO is 0.56, leading to
the formation of lamellar microdomains upon the self-assem-
bly of block copolymer.[8] Homogeneous, transparent, and
crack-free monolithic films with the thickness of 0.67 (±0.17)
mm were fabricated upon drying of the block copolymer solu-
tions on quartz discs at room temperature. The orientation of
lamellae close to the surface of the quartz disc is expected to
be parallel to the surface due to the preferential segregation
of one component (PEO) to the interface.[9]
The PEO hydrophilic domain is expected to complex with
lithium cations and its crystallinity is expected to be sup-
pressed.[10] The PS hydrophobic domain provides the ideal en-
vironment for dissolution of the organic scintillators (PPO
and POPOP), as well as increases the scintillating efficiency
via the energy transfer mediated by phenyl rings. Scheme 1
N
CH2-CH2-O + O O
+ O + 6LiCl
N N
POPOP PPO
N
O
O O
N N
O
CH2-CH O
n 6 +
O
Li Cl-
O
O
m/5
Samples 1-6, 1A, and 1B
http://www.advmat.de Adv. Mater. 2004, 16, No. 19, October 4

depicts schematic presentations of the composite neutron
scintillators based on the self-assembly of the block copoly-
mer. The doping concentrations for 6Li+ were 0.80, 1.49, 2.70,
3.70, 4.70 and 5.86 wt.-% for samples 1, 2, 3, 4, 5 and 6, respec-
tively. Films 1A and 1B were four and eight times thicker than
film 1, respectively. Control monolithic films C1 (without 6Li+,
PPO and POPOP) and C2 (without 6Li+) were also prepared.
As a primary fluor, PPO absorbs resonance energy from the
block copolymer substrate during radiation ionization and
emits energy as fluorescent light. The secondary fluor (PO-
POP, wavelength shifter) shifts the wavelength of the emitted
light to a wavelength that is more suitable for photomultiplier
tube (PMT) detection. As a result, samples 1±6, 1A, 1B, and
C2 all produced peak light emission in the range of 409 nm
under UV excitation, suitable for use with PMTs (Fig. 1). The
control samples C1 and blank quartz disc did not show any
detectable wavelength emission peak in this range due to the
absence of PPO and POPOP.
The comparative measurements of intrinsic peak efficiency,
light yield, and peak resolution for thermal neutrons from a
thermalized AmBe and Cf neutron source were made using
the various lithiated-block-copolymer scintillator samples.
Figure 2 shows the superimposed pulse-height spectra from
experimental monolithic films 1, 1A, and 1B and quartz. In-
spection of the pulse-height spectra shows that the three ex-
perimental films all exhibit a peak around a relative pulse am-
plitude of 1.7. This peak is attributed to thermal neutron
capture events by 6Li+. This peak is noticeably absent in the
quartz data, which supports this conclusion. All of the experi-
Emission [a.u.]
290 340 390
Wavelength [nm]
Figure 1. Scaled emission spectra of the polystyrene-b-poly(ethylene oxide) substrate and the lithiated organic polymer scintillator 3 at 284 nm excita-
tion.
Adv. Mater. 2004, 16, No. 19, October 4 http://www.advmat.de
COMMUNICATIONS
mental films also show a significant number of events below
the neutron peak. These events are attributed to gamma rays
interacting in the scintillators and PMT and fast neutrons scat-
tering off of hydrogen atoms in the scintillators. Although
most neutrons from the source are thermalized, some fast
neutron leakage can occur. Although quartz is not a scintilla-
tor, there is significant low-amplitude noise in the quartz
pulse-height spectrum. The noise is attributed to gamma rays
producing pulses by interacting inside the PMT. Because our
lithiated organic scintillators are colorless, homogeneous, and
transparent films, increasing the thickness of the monolithic
films (1: 0.5 mm thickness; 1A: 1.21 mm thickness; 1B:
1.95 mm thickness) should increase the neutron count rate
without losing light output (relative pulse height). As seen
from Figure 2, this assertion is consistent with the experimen-
tal observation.
Figure 3 shows total peak counts versus pulse height for a
set of the scintillating films after removal of the background
determined with the quartz disc. All data were based on
0.67 ± 0.17 mm thick film samples. This format uses the inte-
grated peak area (error bar is ca. 10 %) for total counts, avoid-
ing the visually misleading peak heights encountered in the
spectra plot. Counts are proportional to the intrinsic peak effi-
ciency, and pulse height is proportional to light yield. Accord-
ingly, the better detectors yield higher neutron counts and rel-
ative pulse height. As can be seen from Figure 3, the increase
of 6Li+ concentration up to approximately 4.7 %, leads to an
increase in the intrinsic peak efficiency (net counts) even
though the pulse height is reduced. The reduction of the pulse
Poly(styrene-b-ethylene oxide)
Sample 3
440 490 540
 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 1759
COMMUNICATIONS

3,5 quartz

1(0.8 weight% Li, 0.5 mm thickness)

3 1A(4 times the amount of 1, 1.21 mm thickness)

1B(8 times the amount of 1, 1.95 mm thickness)

2,5
Log (Counts)

1,5

0,5

0
0 0.5 1 1.5 2 2.5

Relative Pulse Height [(Channel #) / (Amplifier Gain)]

Figure 2. Comparison of neutron pulse-height spectra of experimental samples (quartz, samples 1, 1A, and 1B).

height with the increase of 6Li+ concentration indicates that
the polarity of 6Li+ has a negative effect on ionization events
in the domain of polystyrene. Further work will be focused on
synthesizing and testing scintillators based on different combi-
nations of polystyrene and poly(ethylene oxide) blocks and
also exploration of new block copolymer matrix materials
consisting of poly(ethylene oxide) and polyvinylxylene. The
work on polystyrene-b-poly(ethylene oxide) with a wide
range of PEO volume fractions will represent various micro-
domain morphologies and their correlation (if any) with the
efficiency of films as neutron scintillators.
In conclusion, a new class of organic neutron scintillators
containing organic fluors and 6Li+ has been developed based
on a room-temperature synthesis method with block copoly-
mers. The detecting efficiency achieved with such thin-film
neutron scintillators is very promising for the fabrication of
large-scale position-sensitive neutron scintillators. The unique
self-assembly nanostructure of block polymers makes it possi-
ble to homogenize hydrophilic neutron absorbers and hydro-
phobic organic scintillators in nanometer scale. The use of na-
noscopic materials highlights new opportunities in the
development of highly sensitive radiation sensors.

4000

3500 1(0.80% Li)

3000
2(1.49% Li)
Net Counts

2500
3(2.70% Li)
2000

4(3.70% Li)
1500

5(4.70% Li)
1000

500 6(5.86% Li)

Figure 3. Experimental total peak counts
plotted against pulse height (peak centroid)
0 based on 0.67 (± 0.17) mm thick samples. This
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 format is less misleading and easier to read
but contains essentially the same information
Relative Pulse Height as Figure 2.

1760  2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim http://www.advmat.de Adv. Mater. 2004, 16, No. 19, October 4

Experimental
Synthesis Protocol: Polystyrene-b-poly(ethylene oxide) [P1503-
SEO, Mn: PS (2300) -PEO (3100), Mw/Mn: 1.08, PEO volume fraction:
0.56, calculated using known densities of polystyrene and poly(ethyl-
ene oxide) at room temperature (rPS = 1.05 g cm±3, rPEO = 1.13 g cm±3)
[11] Polymer Source, Inc.], liquid scintillation mixture containing 1,4-
bis-2-(5-phenyloxazolyl)-benzene (POPOP) and 2,5-diphenyloxazole
(PPO) in toluene (Aldrich, 1 L contains 1.25 g POPOP and 100 g
PPO in toluene), 6LiOH.H2O (95 %), HCl (12.2 M, EM Science), tol-
uene (Aldrich, anhydrous, 99.8 %), and methyl alcohol (MeOH, Bur-
dick & Jackson, HPLC grade) were used as received. The liquid scin-
tillation mixture (600 lL) was diluted (to 2500 lL) with toluene
beforehand. In a typical synthesis, 40.6 mg of P1503-SEO was dis-
solved in 500 lL of MeOH with varying amounts (1, 2.4 mg; 2,
4.7 mg; 3, 9.4 mg; 4,14.1 mg; 5,18.8 mg; 6, 28.3 mg) of 6LiCl. Subse-
quently, 20 lL of the diluted PPO/POPOP solution was added to each
solution. The control samples (C1 and C2) were prepared with P1503-
SEO (40.6 mg) in MeOH (500 lL) for C1 and P1503-SEO (40.6 mg)
in MeOH (500 lL) containing diluted PPO/POPOP (20 lL) for C2.
Each precursor solution was sonicated for about 10 min. The viscous
solutions were then applied to 1 in. (1 in. = 2.54cm) diameter quartz
discs to give thick monolithic films. After drying for one week at
room-temperature, these monolithic films were tested for neutron de-
tection capabilities.
Characterization: The pulse-height analysis system consisted of a
one-inch-diameter PMT (Hamamatsu R1924A), amplifiers (Ortec
113 preamplifier and 575A shaping main amplifier), and a computer-
interfaced multichannel analyzer (Spectrum Techniques UCS-20).
The procedure for neutron measurements involved placing a specific
scintillator near a neutron source storage drum containing a 3 Ci
AmBe neutron source and a 3 mCi 252Cf spontaneous fission neutron
source. The drum uses a thick neutron moderator/absorber shield, so
that thermal neutrons predominate in the energy distribution outside
the drum. The scintillator and PMT were shielded from fission gamma
radiation by 5 cm lead bricks, and an additional 3 cm of high-density
polyethylene moderator was interposed between the bricks and the
source drum. Pulse-height spectra were accumulated over 1.5 ” 104 s
for each neutron detector sample.
Fluorescence emission and excitation spectra were recorded on a
SPEX Fluorolog spectrofluorometer Model FL3-22, equipped with
two double-grating monochromators and a 450 W xenon lamp as an
excitation source.
Received: March 6, 2004
Final version: May 3, 2004
± Consiglio Nazionale delle Ricerche
[1] J. B. Birks, in The Theory and Practice of Scintillation Counting,
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[2] G. Blasse, Chem. Mater. 1994, 6, 1465.
[3] H.-J. Im, C. Willis, A. C. Stephan, M. D. Pawel, S. Saengkerdsub,
S. Dai, Appl. Phys. Lett. 2004, 84, 2448.
[4] H.-A. Klok, S. Lecommandoux, Adv. Mater. 2001, 13, 1217.
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meritakis, K. Yu, N. Liu, H. Fan, R. A. Assink, C. A. Drewien,
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COMMUNICATIONS
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[10] T. H. Epps, T. S. Bailey, R. Waletzko, F. S. Bates, Macromolecules
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Molecular-Scale Tracking of the
Self-Healing of Polycrystalline
Monolayers at the Solid±Liquid
Interface**
By Paolo Samorí,* Klaus Müllen,* and Jürgen P. Rabe*
Dedicated to Professor Roeland J. M. Nolte on the occasion of
his 60th birthday
Since thin films grown under non-equilibrium conditions
are always prone to rearrangement,[1,2] understanding the
mechanisms and kinetics of such a reorganization is necessary
to predict film stability. The temporal evolution towards the
equilibrium state involves coarsening, i.e., an increase in the
characteristic length-scale of the dominant structure. Previous
studies have been mainly devoted to the dynamics of metallic
or semiconducting thin films.[3±6] At organic interfaces, the
underlying processes still need to be better understood at the
molecular level.[2] In particular, little is known of the pro-
cesses occurring at the liquid±solid interface.
A scanning tunneling microscopy (STM) study of Ostwald
ripening in two dimensions revealed that the underlying mo-
lecular process is a reaction-controlled phenomenon that
±
[*] Dr. P. Samorí
Istituto per la Sintesi Organica e la Fotoreattività
via Gobetti 101, I-40129 Bologna (Italy)
E-mail: samori@isof.cnr.it
Dr. P. Samorí
Institut de Science et d'IngØnierie SupramolØculaires
UniversitØ Louis Pasteur
8, allØe Gaspard Monge, F-67083 Strasbourg Cedex (France)
Prof. K. Müllen
Max-Planck-Institute for Polymer Research
Postfach 3148, D-55021 Mainz (Germany)
E-mail: muellen@mpip-mainz.mpg.de
Prof. J. P. Rabe
Department of Physics, Humboldt University Berlin
Newtonstrasse 15, D-12489 Berlin (Germany)
E-mail: rabe@physik.hu-berlin.de
[**] We thank Dr. Viola Francke for the synthesis of the molecule and
Dr. N. Severin for his assistance with Molecular Modeling. This
work was supported by TMR project SISITOMAS (project reference
FMRX970099) and by the European Science Foundation through
SMARTON and SONS-BIONICS. P. S. wishes to thank the EU for a
Marie Curie fellowship.
 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 1761