SURFACE AND INTERFACE ANALYSIS

Surf. Interface Anal. 2001; 31: 39–45

Tapping mode and phase imaging of biaxially oriented

polyester films
Ben D. Beake,† Graham J. Leggett1 * and Philip H. Shipway2
1
Department of Chemistry, The University of Manchester Institute of Science and Technology, PO Box 88, Manchester M60 1QD, UK
2
School of Mechanical, Materials, Manufacturing Engineering and Management, The University of Nottingham, University Park, Nottingham NG7 2RD,
UK

Received 21 July 2000; Revised 13 October 2000; Accepted 15 October 2000

The surface morphology and mechanical properties of biaxially drawn poly(ethylene terephthalate) film
surfaces have been investigated with tapping mode scanning force microscopy. Imaging with high tapping
forces caused tip-induced wear of the polymer surface. The damage was avoided by tapping at lower force.
It is then possible to utilize phase detection imaging to provide ready access to surface properties such as
stiffness and adhesion. Phase imaging has revealed a wealth of detailed surface structure information not
seen in previous studies of heterogeneous polyester film materials. Not only are the different components
of heterogeneous materials resolved with remarkable clarity, but detailed information is also provided on
the phase morphology of individual components and on homogeneous polyester film materials. Copyright
 2001 John Wiley & Sons, Ltd.

KEYWORDS: atomic force microscopy; tapping mode; phase imaging; poly(ethylene terephthalate); polyester film

INTRODUCTION Phase images reflect differences in energy dissipa-

Scanning force microscopy (SFM) has led to significant
advances in the determination of the surface structure
and chemical and mechanical properties of commercial
polymeric materials at the nanoscale.1 – 3 Polymers are fragile
materials that can be damaged easily in conventional contact
mode SFM.4 – 17 To obtain high-resolution data it is necessary
to avoid these tip-induced wear processes. We have shown
recently that minimization of the tip–sample interfacial
free energy by chemical modification of the tip is one
successful strategy for wear-free imaging of delicate plasma-
modified polyester films.18 Another popular approach is to
use intermittent contact techniques, such as tapping mode.2,11
Imaging forces in tapping mode are significantly lower19 than
in conventional contact mode imaging, and this, combined
with the intermittent contact, effectively eliminates the lateral
(or shear) forces that are responsible for surface damage of
soft samples.
As part of a wider study into the surface properties
(friction, adhesion and wear) of polyester films,16 – 18,20 – 23 in
this publication we report our investigations into the surface
structure and properties of two well-characterized biaxially
oriented materials using tapping mode with phase detection
imaging.
tion19,24 – 29 and are thought to probe variations in adhe-
sive30 – 33 and mechanical34 – 39 properties over heterogeneous
surfaces, depending on the tapping strength. A possible
viscoelastic contribution also has been considered.40 – 43 We
have investigated how tapping mode with phase imaging
can be used as a tool for compositional mapping. Mylar
D, a poly(ethylene terephthalate) film treated to incorporate
silicate additives at the surface, has been used as a model
material with which to investigate the usefulness of tapping
mode on a commercial film. For comparative purposes, an
additive-free material, Melinex O, also has been studied. We
have investigated the effect of tapping force on the phase
image contrast by controlling the level of the tip–sample
interaction force. The tapping strength varies with the
amplitude of the free oscillation of the cantilever .A0 / and
the ratio of the amplitude of set-point oscillation to this free
oscillation .rsp /.
We were interested also in investigating how infor-
mative the phase information is in revealing the surface
microstructure of chemically homogeneous and inhomoge-
neous materials. We were interested to observe whether
phase images could resolve nanoscale surface structures on
the polyester films, and if these structures could be related
to the processing history of the films.

*Correspondence to: G. J. Leggett, Department of Chemistry, The EXPERIMENTAL

University of Manchester Institute of Science and Technology, PO
Box 88, Manchester M60 1QD, UK.
†Present address: MicroMaterials Ltd, Unit 3, The Byre, Wrexham
Technology Park, Wrexham LL13 7YP, UK.
Contract/grant sponsor: EPSRC; Contract/grant number:
GR/L/78529
The poly(ethylene terephthalate) (PET) films used in this
study were Mylar D and Melinex ‘O’. Mylar D, a biaxially
oriented PET film treated during manufacture to incorporate
a particulate silicate additive at regular intervals in the

Copyright  2001 John Wiley & Sons, Ltd.

40 B. D. Beake et al.
polymer surface (manufactured by Du Pont, USA), was
obtained from Goodfellow Advanced Materials (Cambridge,
UK) and used as received. The additives are thought to
be present to stop the film sticking (‘blocking’) during
winding. Melinex ‘O’, a biaxially oriented additive-free PET
film of low surface roughness, was obtained from ICI and
was used as received. The SFM images of the polymer
film surface were obtained under ambient conditions with
a Nanoscope IIIa MultiMode scanning probe microscope
(Digital Instruments, UK). Height and phase shift images
of the film surfaces were acquired in tapping mode
using ‘Nanosensors’, which are silicon cantilevers with
resonant frequencies of ¾280–300 kHz obtained in wafer
form from LOT Oriel, (Leatherhead, UK). According to the
specifications, the probes had typical tip radii of 10 nm and a
cone half-angle of 18° front to back. Tapping was performed
in air at the cantilevers’ resonant frequency. The level of the
tip–sample interaction force was controlled by adjustment
of two parameters: the amplitude of the free oscillation of
the cantilever and the ratio of the amplitude of set-point
oscillation to this free oscillation. The amplitude of the free
oscillation of the cantilever was typically 1.2–2V; calibration
of the detector sensitivity shows that this is equivalent to
¾22–36 nm. Exact values are given in the figure captions.
Scan speeds were in the range 0.5–2 Hz, except for the images
in Fig. 1, which were acquired using a scan speed of 5 Hz.
RESULTS AND DISCUSSION
Compositional mapping
In phase imaging, a driving oscillation is applied to the
cantilever. The phase lag between the driving frequency and
the cantilever response is measured and used to generate an
Figure 1. Variation of phase contrast with tapping force on Mylar D with A0 D 38 nm and rsp D 0.95 (a), 0.71 (b), 0.29 (c), 0.24 (d)
and 0.48 (e). Image size is 1 µm ð 1 µm in (a)–(d) and 2 µm ð 2 µm in (e). The z-scale is 50° in all images.
Copyright  2001 John Wiley & Sons, Ltd.
image. The phase image is a map of relative differences in
phase shift over the scanned area, and is a measure of energy
dissipation on contact of the tip with the surface during
the oscillation cycle. Regions of the surface that dissipate
less of the energy in the tip–sample contact are shown with
bright contrast. Because phase images reflect the variations
in energy dissipation across the surface, they are thought to
probe variations in stiffness or adhesion over different areas
dependent on the strength of the interaction force during
tapping.29,33 – 38
The interaction force is less easily quantified in phase
imaging than in conventional contact mode imaging. Broadly
speaking, however, the greater the amplitude of the driving
oscillation, the higher the energy of the oscillation and (effec-
tively) the greater the capacity for energy dissipation in the
sample. High-amplitude oscillations are therefore analogous
with high forces in conventional imaging modes. Qualita-
tively, we may define ‘light tapping’ conditions to involve
smaller oscillations than ‘heavy tapping’ conditions. Practi-
cally, the tapping strength was varied by the adjustment of
two parameters: the amplitude of the free oscillation of the
cantilever .A0 / and the ratio of the amplitude of set-point
oscillation to this free oscillation .rsp /. The effective tip-to-
sample force increases as rsp is reduced or as A0 is increased.
We have used Mylar D—a polyester film with silicate
additives present at the surface—as a model, well-
characterized20 – 22 heterogeneous surface with which to
investigate the effect of tapping force on image contrast.
Figure 1 shows the variation of phase contrast with tapping
force. In the phase image, areas of low-energy dissipation
exhibit bright contrast and regions of high-energy dissipation
exhibit dark contrast.
Surf. Interface Anal. 2001; 31: 39–45

It has been suggested that at very low tapping forces
the probe response is dominated by capillary and adhesive
interactions.19,30 – 33 By operating with very low tapping forces
(rsp close to unity) we have observed a reduction in image
resolution when compared with scans at moderate tapping
forces. Some streaking in the scan direction is also observed,
as illustrated in Fig. 1(a), which shows a silicate additive
in the centre of the image surrounded by the PET matrix.
Poor image quality in this regime (which has been termed
‘ultralight tapping’19 ) has been reported in studies of other
polymeric and thin-film systems, and was interpreted as a
consequence of the greater relative influence of adhesive and
meniscus forces (in this light tapping regime).
A large phase shift difference is observed between the
silicate additive and the polymer background, with the
silicates exhibiting brighter contrast .30–40° /. Previously
we have performed friction force microscopy and force
volume imaging (adhesion mapping) of the Mylar D surface22
and the results clearly showed that the additives were less
adhesive. The observed image contrast is thus explained by
the expected differences in adhesiveness over the surface,
in agreement with the postulate of Sauer and co-workers,
that at very low tapping forces phase imaging possesses an
‘indirect chemical sensitivity’.19
As the imaging force is increased, it is reasonable to
assume that we are probing the mechanical properties.27
Figures 1(a)–(d) show the effect of lowering rsp and hence
increasing the imaging force. As the tapping force is
increased, the influence of topography on the phase shift is
lessened. There is a clear difference in phase shift between the
additive and the polymer under all the tapping conditions
employed here .0.95 > rsp > 0.24/. The silicates exhibit
high contrast and there is no inversion of this contrast with
the imaging conditions as has been reported for polymer
blends33 – 35 and micropatterned surfaces.36 Some structure
in the polymer background can be seen; when sharper
tips are used, this structure can be resolved clearly and
is discussed below. Typically, the phase shift over the silicate
Figure 2. Tapping (left) and phase (right) images showing wear on Mylar D: 2 µm ð 2 µm; 2 Hz; phase range 0–20° ; A0 D 36 nm;
rsp D 0.30.
Copyright  2001 John Wiley & Sons, Ltd.
Tapping mode and phase imaging of polyester films 41
regions is ¾25–30° greater than that over the surrounding
polymer for 0.6 > rsp > 0.4, the ‘moderate tapping’ regime
as defined by Magonov and co-workers.29,34 – 38 By operating
under conditions of moderate tapping, we have sought to
use phase imaging to probe variations in stiffness on the
Mylar surface. In this regime, the differences in phase shift
are thought to be determined by the relative moduli of the
components. Because the modulus of the silicate additives
is expected to be over an order of magnitude larger than
that of the polymer, our results in Figs 1(c)–(e) are consistent
with this explanation. The level of tapping force also can
be adjusted by altering the amplitude of the free oscillation
of the cantilever .A0 /. Typically, we have used A0 values
of 20–35 nm and find that this gives sufficient sensitivity to
stiffness variations and morphological details. If the A0 value
is reduced to ¾18 nm the phase images become dominated
by topographic effects, whereas if it is enlarged to ¾90 nm
the resolution decreases.
Figure 1(d) shows that it is possible to decrease the set
point too far. The dark contrast horizontal streaking over the
polymer background is most likely to be either the result
of the tip being unable to break free of the sample during
the oscillation cycle (and thus the experiment becomes sim-
ilar to force modulation microscopy) and/or due to surface
damage. Figure 1(e) is an image of the Mylar surface at
rsp D 0.48, after previously scanning the central 1 µm ð 1 µm
area at higher tapping force [Figs 1(c) and (d)]. The effect
of previously decreasing the set-point to a very low value
.rsp D 0.24/ can be seen; the central region exhibits a lower
phase shift and appears ‘smoothed out’, which is indica-
tive of surface damage. To obtain high-resolution images,
it is important to define a level of tapping force where the
imaging process does not induce wear of the sample surface.
We have investigated this and found that although repeated
scanning at moderate tapping forces .0.6 > rsp > 0.4/ does
not induce wear, harder tapping of the PET film surface
.0.35 > rsp > 0.2/ results in a decrease in image resolution
in the scanned region as shown in Figs 1(e) and 2. Figure 2
Surf. Interface Anal. 2001; 31: 39–45
42 B. D. Beake et al.
shows the effect of scan size on surface damage. The cen-
tral region .1 µm ð 1 µm/ has been scanned previously at
rsp D 0.30 and poor resolution was observed (not shown).
The image shown in Fig. 2 has been rescanned at the same rsp
value of 0.3 but this time at lower magnification. It has been
noted that at high magnifications the tip resides longer at
each given point on the surface, contributing to larger effec-
tive tapping forces.19 In this case it appears that, at lower
magnifications, it is possible to reduce rsp below 0.4 and avoid
obvious wear. In general, however, we suggest that for a free
amplitude of 35 nm rsp should be ¾0.4–0.5 for the optimum
combination of wear-free imaging of polyester materials at
the submicron scale and stiffness-controlled phase contrast.
Surface morphology
Traditionally, electron microscopic methods for the deter-
mination of polymer surface morphology have relied on
surface pretreatments such as deposition of a conductive
coating, ultramicrotomy, heavy metal ion staining, chromic
acid etching and gas plasma ablation.45 These techniques
reveal information about near-surface structure by providing
image contrast based on variations in the crystallinity of dif-
ferent areas. A potential problem with these approaches
is that it is not always known to what extent the outer-
most region of the surface is modified or removed in the
pretreatment stage, and it is unclear how this relates to the
morphological organization at the interface itself. In contrast,
tapping mode with phase imaging provides direct access to
the interfacial morphology without the need for surface pre-
treatment. We have shown that by operating in the so-called
moderate tapping regime we can image the polymer surface
non-destructively and resolve structures in the polymeric
background. By intermittent contact imaging at moderate
force we can avoid tip-induced wear more easily than when
using contact mode mechanical techniques such as force
modulation microscopy, where lateral or shear forces are
appreciable.19,22,29
In addition to being a tool for compositional mapping
on multi-component surfaces, tapping and phase detection
Figure 3. Tapping (left) and phase (right) images of Melinex ‘O’: 1.5 µm ð 1.5 µm; A0 D 22 nm; rsp D 0.42.
Copyright  2001 John Wiley & Sons, Ltd.
imaging can readily provide unique insights into the
organization of crystallites at the interface. Figure 3 shows
tapping and phase images of Melinex ‘O’ under conditions
of moderate tapping. Comparison of these images reveals
variations in the polyester film topography from region to
region. Typically, the surface topography shows little or no
obvious orientation, as shown in the tapping mode image
in Fig. 3, and the topography resembles ‘rolling hills’ as
has been described previously. The phase image reveals
the surface microstructure. Small features exhibiting bright
contrast are seen to be distributed densely and evenly across
the whole of the polymer surface. Large-area phase images
of Mylar D exhibited very similar features to those observed
for Melinex O (see Fig. 2). On careful inspection of the
corresponding tapping mode images, there was sometimes
evidence for topographical structure that correlated with the
features observed in the phase images. However, the features
were very much less easy to distinguish than they were in
the phase images, indicating that the phase contrast arises
from inhomogeneities in properties rather than nanoscale
topographical detail.
It is clear from the images shown in Figs 2 and 3 that
tapping mode and phase imaging provide complementary
information about the film surface. As a first approxima-
tion, tapping mode can reveal topographic variations in
the 100 nm to micrometre range, whereas phase imaging
provides more detailed morphological information in the
10–100 nm range. Phase images can provide clearer insights
into the nanoscale structures on polymer surfaces than topo-
graphical data, because the inherent roughness of the sample
does not significantly influence the image resolution. To
obtain well-resolved images of this microstructure it was
necessary to use very sharp probe tips. The AFM tips used
in this study had a quoted radius of curvature of ¾10 nm.
Blunt tips or tips dulled through prolonged use overestimate
the width of the high phase contrast features, as has been
reported on other polyester surfaces.22
It is of obvious interest to identify the surface features
clearly seen in the phase images. We believe that they are
Surf. Interface Anal. 2001; 31: 39–45
 Tapping mode and phase imaging of polyester films 43

crystalline lamellae imaged edge-on at the surface of the film.

Such an interpretation certainly would be consistent with the
findings of other workers who have undertaken extensive
investigations of the morphologies of biaxially oriented
PET films.46,47 Their studies suggest that the crystallites
are typically small lamellae, of the order of only a few
nanometres in size. The relative proportions of the light
and dark contrast areas on the polymer surface .¾50 : 50/
are in accordance with the technical specifications of the
film (Melinex is ¾56% crystalline in the bulk and possibly
more so at the surface;48 Mylar D is also thought be
¾50% crystalline). The width of the high-contrast features
is typically ¾8–10 nm. In comparison, lamellae with widths
as low as 5 nm have been resolved using phase imaging
on other polymer surfaces.44 The average repeat distance
between bright regions along the raised features on the
surface of both Mylar D and Melinex has been measured
Figure 4. Phase image showing structure surrounding silicate
and found to vary very little from region to region, with
additive on Mylar D: 0.6 µm ð 0.6 µm; contrast 0–15° ; A0 D
values of 16–17 nm. This compares very reasonably with
25 nm; rsp D 0.40.
values of the long period (lamellar periodicity) on other
drawn PET films, 13–15 nm, as measured by small-angle x-
ray methods.49,50 On Mylar D, the long axes of these features image from top left to bottom right. The difference in phase
were usually oriented close to parallel to the nearest edge between these features is ¾2–4° . If, as expected from the data
of the silicate inclusions, as shown in Figs 2 and 4. This shown in Fig. 1, variations in stiffness dominate the phase
ordering generally decreased with increasing distance from contrast under these tapping conditions, the bright contrast
the additives, although it was commonly observed in the (higher phase) features can be identified as stiffer. Most
thin raised features that connect the larger additives. likely they are composed of crystalline material, whereas the
Many of the tapping mode images exhibited larger, lower phase-shift regions between them contain amorphous
radial features around the larger silicate particles on Mylar material. There is some correlation between the height and
D surfaces. These have been reported already elsewhere the phase data; the bright contrast features in the phase image
in contact mode studies and tentatively ascribed to strain- are typically 1–2 nm higher than the intervening (dark phase
induced crystallization.20 Figure 5 shows tapping and phase contrast) material in the tapping image. Longer features, of
images of some of these features. A periodic light–dark similar width, were also observed in images of Melinex O.
contrast can be seen clearly running diagonally across the Phase images revealed similar plate-like features, oriented

Figure 5. Tapping and phase images showing raised connecting features on Mylar D: 0.5 µm ð 0.5 µm; z-scale is 5 nm in the height
image and 5° in the phase image; A0 D 36 nm; rsp D 0.50.

Copyright  2001 John Wiley & Sons, Ltd. Surf. Interface Anal. 2001; 31: 39–45
44 B. D. Beake et al.
Figure 6. Tapping (left) and phase (right) images of a sample of Melinex O, with an enlarged region of the phase image shown at the
bottom of the figure. The main images are 1.5 µm ð 1.5 µm. Raised features may be seen in the tapping mode image. Plate-like
features may be seen in the phase image, the axes of the plates being aligned perpendicular to the direction of the raised feature.
The enlarged region clearly shows the plate-like features.
perpendicular to their long axes (Fig. 6). The arrow in Fig. 6
marks out one particular feature in both the phase and the
tapping mode images; detail of this feature is shown in the
expansion of the area marked by a box. In this case, as in
the case of the radial features around the larger silicates, it
seems most likely that phase imaging is revealing crystal
structures at the film surface. The features that are oriented
perpendicular to the direction of the arrow in Fig. 6 are most
likely to be plate-like cyrstallites.
The phase images of Melinex have indicated that there
is little or no overall preferred orientation at the surface of
the biaxially drawn film. Although some local orientation in
the film is often observed, it does not extend over such large
distances as has been observed in images of near-surface
structure obtained by ultramicrotoming50 or low-power
argon plasma etching17 of the sample. In contrast, the silicate
additives present in the Mylar surface appear to direct the
orientation of the surrounding polymeric material. The direct
visualization of nanoscale crystal structures represents a
significant advance in our ability to characterize the film
structure and could facilitate significant future advances
in our understanding of the relationship between film
processing conditions and polymer morphology.
CONCLUSIONS
We have used tapping mode AFM to investigate biaxially
drawn PET film surfaces. Phase detection imaging has
Copyright  2001 John Wiley & Sons, Ltd.
clearly revealed compositional differences on heterogeneous
materials and has provided a unique insight into the
crystallite structure at the surface of homogeneous materials
and within single phases of multicomponent films. By
avoiding the tip-induced surface damage that readily
occurs in conventional contact mode imaging of polymeric
materials, phase imaging can, provided that the tip does not
tap too hard, yield ready access to surface properties such as
stiffness and adhesion.
Acknowledgements
We thank the EPSRC (grant GR/L/78529) for financial support.
Professor D. Briggs (ICI, Wilton) is thanked for supplying Melinex
‘O’ with known processing history and for many useful discussions.
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