Advances in Materials Physics and Chemistry, 2013, 3, 299-306
Published Online November 2013 (
Open Access AMPC
Effect of Switching on Metal-Organic Interface
Adhesion Relevant to Organic Electronic Devices
Babaniyi Babatope1*, Akogwu Onobu2, Olusegun O. Adewoye3, Winston O. Soboyejo2,3
1Department of Physics, Obafemi Awolowo University, Ile-Ife, Nigeria
2Department of Mechanical and Aerospace Engineering, Princeton University, Princeton, USA
3Materials Science and Engineering Department, African University of Science and Technology, Abuja, Nigeria
Email: *
Received September 4, 2013; revised October 8, 2013; accepted October 16, 2013
Copyright © 2013 Babaniyi Babatope et al. This is an open access article distributed under the Creative Commons Attribution Li-
cense, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Considerable efforts are currently being devoted to investigation of metal-organic, organic-organic and organic-inor-
ganic interfaces relevant to organic electronic devices such as organic light emitting diode (OLEDs), organic photo-
voltaic solar cells, organic field effect transistors (OFETs), organic spintronic devices and organic-based Write Once
Read Many times (WORM) memory devices on both rigid and flexible substrates in laboratories around the world. The
multilayer structure of these devices makes interfaces between dissimilar materials in contact and plays a prominent
role in charge transport and injection efficiency which inevitably affect device performance. This paper presents results
of an initial study on how switching between voltage thresholds and chemical surface treatment affects adhesion prop-
erties of a metal-organic (Au-PEDOT:PSS) contact interface in a WORM device. Contact and Tapping-mode Atomic
Force Microscopy (AFM) gave surface topography, phase imaging and interface adhesion properties in addition to
SEM/EDX imaging which showed that surface treatment, switching and surface roughness all appeared to be key fac-
tors in increasing interface adhesion with implications for increased device performance.
Keywords: AFM; Interface; Adhesion Force; Organic Electronics; Voltage Switching; Organic Memory Devices;
Surface Treatment
1. Introduction
The investigation of interfaces between dissimilar or-
ganic-metal, organic-organic and organic-inorganic ma-
terials which are inherent in the devices made from them
has been intensified in recent times. The interface phe-
nomena are thus crucial towards the development, under-
standing and improvement of organic-based semicon-
ductor electronic device [1-14] applications such as or-
ganic light emitting devices (OLEDs) [15-18], organic
photovoltaic devices [19-21], organic thin film transistor
devices [22-27] and organic spin electronic devices in
which the transport and control of spin polarized infor-
mation are represented [28-30]. The interface between
the different materials that make them up determines the
charge transport and charge injection efficiency, with
implications for the performance of the devices.
Interfacial phenomena are particularly crucial towards
the development and improvement of applications of
these devices and in order to effectively investigate mul-
tilayer structured devices, the overall flexibility becomes
very critical. This, in addition to their molecular nature,
makes the study of organic thin films interfaces to be
more intensified compared to inorganic semiconductors.
The type of interaction at the interface is either physi-
cal or chemical and progress in organic electronics re-
quires their detail understanding [31]. Investigations of
the chemical nature of interfaces are common in thin film
characterization, but not much attention has been directed
at measuring physical interaction until recently when
advanced characterization tools are becoming more widely
available. However, in a work reported on the nanoscale
adhesion between organic-organic, organic-inorganic, and
inorganic-inorganic thin film interfaces [32], the AFM
technique was used in quantifying the interfaces, though
with some limitations. The pull-off forces and surface
parameters were measured and incorporated into theo-
*Corresponding author.
retical models for the estimation of surface energies. Ob-
viously, therefore, the improvement of performance of
organic electronic devices depends on a clear under-
standing of the principles underlying organic-film/metal-
electrode interfaces.
Data-storage and switching applications of conjugated
polymer-based devices in which, depending on the volt-
age-sweep direction, two different current-voltage (I-V)
characteristics, and hence low and high conducting states
are used, have been observed and reported (e.g. [33-39]).
These devices have an associated memory effect for
data-storage applications especially the bistable archi-
tectures (e.g. [21,26,38,40-47]). The bistable and multi-
ple-layer stacking structures have therefore emerged as a
viable technology for flexible, ultrafast, and ultrahigh-
density memory devices in the field of organic electron-
ics [48].
In a multilayer organic electronic device structure
(Figure 1), charges often move from one layer to another
by either injecting holes and/or electrons or transporting
the same in one direction or the other. In the emissive
layers, injected charges produce localized charge carry-
ing species which move through the device under the
influence of external field (bias) across the interface [49].
Charge injection transport efficiency through the inter-
faces is thus critical to device performance. However,
there are problems of adhesion, morphological inho-
mogeneities and conductivity anisotropy at these inter-
faces which are not yet properly understood [50].
Charge transport efficiency could be enhanced by re-
ducing the number of interfaces in organic devices. This
is often done using the standard polymer processing
method of blending in which organic materials, forming
individual layers, are innovatively blended, thereby re-
ducing the number of layers. This has been recognized as
one of the possible ways forwarded for improved charge
transport efficiency [51], as illustrated in Figure 2.
This investigation was therefore motivated by the need
to explore additional interface reengineering techniques
Figure 1. Typical device structure for sun harvesting (Poly-
mer Solar Cells) and light emission (OLEDs). The figure
shows the contacts and the emissive layers made up of dif-
ferent carefully selected conducting (conjugated) polymers.
Figure 2. Device structure that reduced the number of in-
terfaces using conventional polymer blending technique in
which each phase would be expecte d to independently their
different roles of charge transportation and injection.
using a combination of memory switching, adhesion and
surface treatment. Also, this type of study could be in-
corporated into device performance improvement studies
in view of recent reported improving power conversion
efficiency of conjugated polymer-based solar cells [52],
which remains largely unsatisfactory for large-scale
commercial production in competition with its amor-
phous silicon-based devices. There are indications that
charge transportation at the interface could be improved
by a better understanding of the physical phenomena at
the interface [32]. This has brought into the fore, an in-
tensified investigation of the physical interaction be-
tween the dissimilar materials in direct contact, which is
vital to sustainable device performance.
2. Experimental Details
2.1. Materials and Equipment
The materials used in this investigation include AL 4083
PEDOT:PSS suitable for OLED fabrication (H. C. Starck,
MA, Newton, USA) as the organic layer, n-doped silicon
wafer (Eagle-Picher, Miami, OK, USA) as the substrate,
gold (Au) as the metal contact layer (Alfa Aesar, USA),
hydrochloric acid (Aldrich, USA) for the surface treat-
ment of the organic layer, Hydrofluoric acid (Aldrich,
USA) and standard assorted reagents for substrate clean-
ing. The thermal deposition of the gold contact on the
organic layer was carried out using an Edwards E306A
deposition system (Edwards, Sussex, UK), the switching
was done with an HP semiconductor parameter analyzer
(HP 4145B) for the current-voltage measurement, etched
silicon contact AFM tips were purchased from Veeco
Instruments (Woodbury, NY, USA), Digital Instruments
Dimension 3000 Atomic Force Microscope (AFM)
(Digital Instruments, Plainview, NY), Scanning Electron
Microscope (SEM-EDX) (Philips FEI XL30 FEG-SEM,
Hillsboro, USA), a standard Fishers ultrasonic bath, an
ultra violet ozone cleaning system and a drying chamber
were all used in the course of this study.
2.2. Experimental Procedure
A Write Once Read Many times (WORM) device was
fabricated by direct spin-casting of PEDOT:PSS on a
suitably cleaned n-Si substrate followed by vacuum
deposition of Au Contact. The cleaning procedure for the
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substrate includes the use of a combination of different
solvents including acetone, trichloroethylene (TCE), iso-
propanol, hydrofluoric acid (HF), a detergent and deion-
ized water under different temperature conditions in an
ultrasonic bath. The substrate was then transferred to an
ultra violet ozone cleaning system for 5 min for further
cleaning after which it was transferred to a glove box for
safe keeping, ready for spin coating of the organic layer.
A thin layer of PEDOT:PSS (about 500 nm) deter-
mined based on standard calibration curves obtained by
plotting series of spinning speeds, accelerations and
thicknesses and after drying (H. C. Starck, Newton, MA
USA suppliers of PEDOT:PSS) was then deposited on
the substrate by spin coating in ambient air condition
followed by baking in an oven at 200˚C for about 60 min.
The sample was again transferred to a glove box ready
for the Au deposition. Some of the spin-coated samples
were chemically treated with dilute HCl (0.1 N) prior to
deposition of the Au contact (approximately 100 nm,
preceded by a thin layer, about 5 nm, of Cr) which was
carried out by thermal evaporation under a vacuum of 1
× 10–6 Torr (1 Torr = 133.32 Pa).
A selection of the Au/PEDOT:PSS/Si device was qua-
sistatically switched or “blown” using a pulsed voltage
ramp with 10 ms long 100 mV steps and applied for 0.5 -
4 ms as necessary The switching was carried out by use
of current transients to change the polymer fuse (PE-
DOT:PSS) from a conducting (“1” or “ON”) to a non-
conducting (“0” or “OFF”) state. Quasistatic (continuous)
condition (J~10 A/cm2): 0 V - 10 V - 0 V and rapid volt-
age pulsed transient condition (J~1 kA/cm2): 10 V, 2 μs
were used for this purpose [53,54].
The Au contact was deposited either before or after the
polymer surface treatment and was carefully removed by
a peeling process before and after switching. The same
was done before and after polymer surface treatment.
Phase imaging, surface topography and force calibration
curves were obtained for the different surfaces by AFM
in contact and tapping modes to quantify the physical
interaction at the polymer interface using Au-coated can-
tilever tips. Interaction force response between the sam-
ple and cantilever tip [32,55] was measured for each
sample. The surface roughness for each surface was re-
corded and related to adhesion data as measured by the
deflection as recorded from the interaction between
Au-coated cantilever tip and the polymer surface.
The differently deposited, treated or untreated, switched
or unswitched surfaces before or after peeling the Au-
contact, were separately investigated by SEM/EDX to
qualitatively correlate the effectiveness of the peeling
process, and the relative degree of polymer-metal inter-
face adhesion. These tips were coated with Au the com-
plementary materials that make direct contact with the
surfaces. The purpose is also to investigate whether part
of the polymer peeled with the gold contact.
3. Result and Discussion
Figures 3 and 4 show the surface topography (Figures
3(a)-(d)) as determined by the degree of roughness ob-
tained in the tapping mode; and the force calibration
plots (Figures 3(a)-(d)) obtained in contact mode for the
unswitched (Figures 4(a) and (c)) and switched (Figures
3(b) and (d)) devices when untreated (Figure 3) and
treated (Figure 4). The values for the respective rough-
ness are as shown in Table 1.
Analysis of the force calibration curves shows that in
the unswitched mode, when untreated (Figure 3(b)), the
Au-coated cantilever tips dragged on the polymer surface
prior to disengagement whereas, after switching, the dis-
engagement of the tip was without dragging (Figure
3(d)). This was accompanied with a reduced adhesion
force by almost 50%. Upon surface treatment, this effect
combined with that of switching to give the highest ad-
hesion force in the samples under consideration with a
much greater dragging prior to cantilever tip disengage-
ment. This appears to suggest that surface treatment and
switching are significant to improved interface adhesion
between the Au contact and the polymer. This is ex-
pected to lead to an improvement in device performance;
the next in the on-going work.
The summary of the deflection on the force calibration
curve (a direct measure of adhesion force) as estimated
directly from the calibration plots under different surface
treatment and switching conditions, is shown in Ta bl e 2.
Figures 5 and 6 show the SEM/EDX images for an
untreated surface in the unswitched state (Figure 5) and
in the treated and switched state (the two extremes).
Figure 5 indicates that peeling the Au contact from the
PEDOT:PSS surface was “harder” with more of the Au
remaining adhered to the polymer under similar peeling
This qualitatively suggests that adhesion force would
be high. However, upon surface treatment (which is ex-
pected to make the surface to be more even, due to re-
moval of surface peat, hence minimizing conductivity
anisotropy and heterogeneity at the interface), the Au
peeled off neatly leaving a smooth polymer surface,
(Figure 6).
This study is significant in the quest to finding ways of
improving the lifetimes of organic electronic devices
through interface reengineering which is vital to better
device performance. It has also qualitatively and quanti-
tatively revealed the possibility of using this technique in
combination with established packaging (or encapsulat-
ing methods to significantly contribute to general im-
provement in device performance). It was observed that
peeling the gold contact in the untreated, unswitched
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(a) (b)
(c) (d)
Figure 3. Surface roughness ((a) and (c)) and force displacement curves ((b) and (d)) for untreated PEDOT:PSS on silicon
substrate when in the unswitched ((a), (b)) and switched ((c), (d)) modes. (a) Surface roughness in the untreated and
unswitched mode; (b) Force-displacement curve in untreated and unswitched mode; (c) Surface roughness in the untreated
and switched mode; (d) Force-displacement curve in the untreated and switched mode.
(a) (b)
(c) (d)
Figure 4. Surface roughness ((a) and (c)) and force displacement curves ((b) and (d)) for untreated PEDOT:PSS on silicon
substrate when in the unswitched ((a), (b)) and switched ((c), (d)) modes. (a) Surface roughness in the treated and unswitched
mode; (b) Force-displacement curve in the treated and unswitched mode; (c) Surface roughness in the treated and switched
mode; (d) Force-displacement curve in the treated and switched mode.
Figure 5. SEM/EDX images for an Untreated sample in the
unswitched mode show ing the surface of PEDOT:PSS after
peeling off the Au contact (top and bottom right), the Au
surface (inset) and the EDX for the contact showing that no
polymer adhered to it.
Figure 6. SEM/EDX images for an treated sample in the
switched mode showing the surface of PEDOT:PSS after
peeling off the Au contact (bottom right), the Au surface
(top right) and the EDX for the contact showing that no
polymer adhered to it.
Table 1. Summary data showing the effect of surface treat-
ment and switching on the Au-PEDOT:PSS interface adhe-
Unswitched Switched
Adhesion Force
Untreated Rough
(13.667 nm)
(5.609 nm) Increased
Treated Rough
(9.739 nm)
(1.434 nm) Increased
Force Not
sample was “harder” compared to the switched and
treated samples that peeled more easily with the highest
interface adhesion. Since this is more or less an explora-
tory study, the concept of switching especially the effect
of treating the surface with different reagents requires
Table 2. Summary of adhesion data show ing deflection val-
Untreated Treated
Unswitched 140.00 nm Unswitched 70.00 nm
Switched 78.00 nm Switched 185.50 nm
Unswitched Switched
Treated 70.00 nm Treated 185.50 nm
Untreated 140.00 nm Untreated 78.00 nm
further detailed investigation.
The quantitative analysis of the micrographs consis-
tently showed convincingly that there was no evidence of
the presence of the polymer, PEDOT:PSS, on the gold
surface as all the specimens investigated showed that
each time the Au contact was peeled, no polymer ad-
hered to it (Figures 5 and 6). The adhesive force at the
interface is thought to be a combination of Van Der Waal
and electrostatic forces in view of the involvement of
different interacting ions from the reagent used in surface
treatment together with that of the polyelectrolyte dopant
in PEDOT. The physics and chemistry of the interaction
are thus very crucial to further understanding of this
phenomenon as it would complement this initial result of
the study.
4. Conclusions
From this preliminary investigation, it can be suggested
1) Surface treatment, switching and surface roughness
all appear to be key factors in increasing interface adhe-
sion, hence device performance.
2) Switching an untreated PEDOT:PSS surface re-
sulted in reduced interface adhesion.
3) Switching a surface-treated specimen significantly
increased interface adhesion most probably because of
reduced surface roughness.
These results require more detailed investigations, es-
pecially in relation to the actual device performance.
5. Acknowledgements
The authors wish to acknowledge the invaluable assis-
tance offered by staff of the nano-fabrication laboratory,
Department of Electrical Engineering, Princeton Univer-
sity, New Jersey, USA. BB acknowledges the authorities
of Obafemi Awolowo University for kindly granting
leave of absence for the Fellowship at Princeton Univer-
sity where the experimental work was carried out.
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