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IOP PUBLISHING NANOTECHNOLOGY
Nanotechnology 20 (2009) 045301 (6pp) doi:10.1088/0957-4484/20/4/045301

Nanoindents produced by nanobubbles on

ultrathin polystyrene films in water
Yuliang Wang1,2 , Bharat Bhushan1,3 and Xuezeng Zhao2
1
Nanoprobe Laboratory for Bio- & Nanotechnology and Biomimetics (NLB2 ),
The Ohio State University, 201 West 19th Avenue, Columbus, OH 43210-1142, USA
2
School of Mechanical Engineering, Harbin Institute of Technology, Harbin 150001,
People’s Republic of China

E-mail: Bhushan.2@osu.edu

Received 16 September 2008, in final form 14 November 2008

Published 18 December 2008
Online at stacks.iop.org/Nano/20/045301

Abstract
Nanobubbles are produced on hydrophobic surfaces when they are immersed in aqueous
solutions. The effect of nanobubbles on the immersed surface is of interest in many
applications. In the study presented here, immersion of the polystyrene film in de-ionized water
for several hours produces nanoindents on the film surface. The typical diameter of the
nanoindents is around 20 nm, and the density is about 2.0 × 108 mm−2 . The location and
formation of nanoindents show strong correlation with the size and location of nanobubbles.
A mechanism of nanobubble-induced formation of nanoindents is proposed. The influences of
film thickness and nanobubble size on the nanoindents are also discussed.
(Some figures in this article are in colour only in the electronic version)

1. Introduction traditional non-slip boundary condition (Watts et al 1990, Ou

During wetting of a hydrophobic surface with an aqueous
solvent, nanobubbles with a height of 5–100 nm and a diameter
of 100–800 nm are produced (Ishida et al 2000, Lou et al 2000,
Tyrrell and Attard 2002, Holmberg et al 2003, Simonsen et al
2004, Agrawal et al 2005, Bhushan et al 2008). Nanobubbles
can exist for more than 20 h (Yang et al 2003) and are stable
not only under ambient conditions but also under enormous
reduction of the water pressure down to −6 MPa (Borkent
et al 2007). Under mechanical perturbation of tapping AFM
(atomic force microscopy) tip, coalescences of nanobubbles
can occur (Yang et al 2003, Simonsen et al 2004, Bhushan
et al 2008). By tracking the movement of nanobubbles
and the consequent coalescence during scanning with tapping
mode AFM (TMAFM), Bhushan et al (2008) have shown
that the spherical features formed on hydrophobic surfaces
are indeed nanobubbles. In micro/nanofluidic applications
of relevance to various applications including biosensor
applications (Bhushan 2007), the presence of nanobubbles
reduces the drag force between flowing fluid and solid surface
and is believed to be responsible for the breakdown of
3 Author to whom any correspondence should be addressed.
et al 2004, Maali and Bhushan 2008). Although nanobubbles
show potential in many applications, little is known about
the physical interaction of nanobubbles with the substrate
supporting them, which are both fundamentally interesting and
practically important.
Physical interaction of nanobubbles with ultrathin
polymer films in the presence of nanobubbles has seldom
been done, which could be important in life science,
micro/nanofluidics and biosensors (Bhushan 2007). Here we
report our finding of a novel phenomenon observed as a
result of the formation of nanobubbles on ultrathin polystyrene
(PS) films immersed in de-ionized (DI) water. As soon
as the sample was immersed in water, nanobubbles were
formed on the PS surface. With time, the morphology
of the PS surface continuously changed. A time-series
imaging was performed to study the evolution of nanoindents
on PS surface in water. A strong correlation between
the changes in surface morphology of the PS surface
and the presence of nanobubbles was observed. Their
correlation will be discussed in detail by considering the
interaction between the nanobubbles and the PS surface.
Various factors that could influence the structure of the PS
surface, such as film thickness and nanobubble size, will be
examined.

0957-4484/09/045301+06$30.00 1 © 2009 IOP Publishing Ltd Printed in the UK

Nanotechnology 20 (2009) 045301
2. Experimental details
A polystyrene (PS) sample was prepared by spin-coating
a thin film of PS on a silicon (100) substrate at a speed
of 500 rpm. The substrate was cleaned in a sonication
bath of acetone and then water. Polystyrene particles
(molecular weight 350 000, Sigma-Aldrich) were dissolved
in toluene (Mallinckrodt Chemical) to a concentration of
0.046% (weight) to obtain the solution for spin-coating.
After spin-coating, the PS samples were put into an oven at
temperature 45 ± 3 ◦ C for about 4 h to remove the remaining
toluene. The thickness of the PS coating was measured to be
2.8 ± 0.3 nm with an ellipsometer (Model L116C, Gaertner
Scientific Corporation). The contact angle of the PS surface
with water was measured to be 95◦ ± 3◦ using a sessile drop
method.
A commercial AFM (MultiMode III, Digital Instruments)
operating in tapping mode was used for imaging the sample
in water (Bhushan 2008). To obtain an improved signal-to-
noise ratio, a modified tapping mode tip holder (Maali et al
2006) was used to directly drive the cantilever in fluid with
the embedded piezo-driver. A horizontal slot was carved out
in the opening of the commercially available tip holder above
the piezo-element in order to insert a glass slide. When
the liquid is added between the glass slide and the substrate,
the liquid meniscus is formed between the glass and sample
surface for fluid imaging. A silicon RFESP cantilever (Digital
Instruments) with a tip radius <10 nm and a quoted stiffness
of 3 N m−1 was used. The measured resonance frequencies
of the cantilever in air and water were about 75 KHz and
26 KHz, respectively. The sample was first imaged in air using
TMAFM and then immersed into DI water for time-series
imaging. To minimize the force applied on the nanobubbles
and sample surface, the setpoint was set to be only 95% of
the free amplitude. While imaging in air and liquid, the drive
frequency was chosen to be the resonance frequency. The tip
was scanned at a rate of 2 Hz and an angle of 90◦ .
3. Results and discussion
In this section, we will first show the evidence of nanobubble
existence by imaging the PS surface in DI water with TMAFM.
Then time-series images with the evolution of nanobubbles and
morphological changes in the PS surface will be presented.
Based on the experimental observations, a mechanism of
nanobubble-induced nanoindented surface will be given, and
the influence of film thickness and nanobubble size on
formation of the nanoindented surface will be discussed.
3.1. Formation of nanobubbles on the PS surface in DI water
Before it is immersed in water, the surface of the PS film is
observed to be uniform and smooth with a RMS roughness
of about 0.22 nm (figure 1(a)). Here one should note that in
all section profiles shown in figure 1, the horizontal scale is
different from the vertical one. After being immersed in water
for 10 min, the PS surface was imaged and nanobubbles were
observed to emerge on the surface (figure 1(b)). The roughness
2
Y Wang et al
Figure 1. Comparison of images of PS coated silicon wafer using
tapping mode AFM in (a) air and (b) DI water. Two groups of size of
nanobubbles can be observed. The section profiles, which are plotted
at different scales along horizontal and vertical directions, show
structures of nanobubbles.
increased to 1.3 nm, significantly larger than that in air. The
nanobubbles on this substrate are not uniform in their size and
roughly distribute around two peaks. The large nanobubbles
have a diameter around 100 nm and a height around 6 nm. The
small nanobubbles have a diameter around 50 nm and a height
of 1.5 nm. The densities for the small and large nanobubbles
are estimated to be about 2.0×108 mm−2 and 0.68×108 mm−2 ,
respectively. The diversity of the nanobubble size appears to be
related to the heterogeneous surface property of the PS film, in
particular, the roughness. It has been reported that nanobubbles
on the rough surface are much less densely populated and their
sizes are relatively larger than those on the smooth surface
(Yang et al 2003).
3.2. Formation of nanoindents
Time-series images of the PS sample immersed in water for
a duration of several hours are shown in figure 2. It is
clear that the morphologies of the nanobubbles and the PS
surface experienced continuous change with time. At the
time of 10 min, spherical nanobubbles with smooth profiles
are observed (figure 2(a)), which can be seen through the
section profile of figure 2(a). Similar to figure 1, for all
section profiles shown in figure 2, the horizontal scale is
different from the vertical one. After 40 min, both small
nanobubbles and large nanobubbles appear to shrink in their
size. Most distinctively, circular rims emerged at the perimeter
of the large bubbles (figure 2(b)). Typical height of the
rims is about 1.0 nm. After 150 min, typical height of
rims increased to about 2.0 nm (figure 2(c)). Most of
small nanobubbles have disappeared in figure 2(c), leaving
small impressions at their original positions with a diameter
of about 20 nm. After 225 min, another scan area was
chosen to exclude the possibility of cantilever tip influence on
evolution of nanobubbles and formation of nanoindents. All
Nanotechnology 20 (2009) 045301 Y Wang et al

Figure 2. Sequence of nanobubble height images and phase shift images as a function of time immersed in DI water in 1 μm × 1 μm scan
area: (a) 10 min; (b) 40 min; (c) 150 min; and (d) 225 min. Rims appear in (b). Small nanobubbles gradually disappear in (c), leaving
nanoindents at corresponding sites, and finally small nanobubbles disappear in (d). The section profiles, which are plotted at different scales
along horizontal and vertical directions, show structures of nanobubbles and rims around the nanobubbles.

the small nanobubbles disappeared and left densely distributed

nanoindents. However, bigger nanobubbles were still on the
surface. The presence and evolution of nanobubbles can
also been observed through phase images. The phase shift
data is important to reveal mechanical properties in TMAFM
(Bhushan 2008). Using phase shift data, Bhushan et al (2008)
studied the viscoelastic properties of cantilever–tip interaction.
Here, phase shift images are shown to help us distinguish
surface features on the PS surface. In figure 2, the black
circular objects in phase shift images represent the existence
of nanobubbles. The phase images reveal that the density
of small nanobubbles gradually reduced with time and finally Figure 3. 3D images of a nanobubble circled in figures 2(a) and (c)
at 10 min (a) and 150 min (c) after the PS sample was immersed into
disappeared at 225 min. 3D images for a certain nanobubble DI water. The profile of the nanobubble is smooth at 10 min and a
circled in figures 2(a) and (c) after 10 and 150 min are given rim appeared around the nanobubble at 150 min.
in figures 3(a) and (b) to illustrate the topography change.
At the time of 10 min, the nanobubble has a smooth profile.
However, a rim appeared around the nanobubble at the time of
the PS film are induced by the nanobubbles. To further explore
150 min. The diameter of the nanobubble lightly shrinks after
why nanobubbles can induce nanoindents on the PS film, the
appearance of the rim.
relevant forces on the locations of nanobubbles are analyzed.
A schematic diagram is given in figure 4(a), where p and R
3.3. Mechanism of formation of nanoindents are Laplace pressure and radius of curvature of nanobubbles,
The strong correlation between the nanobubbles and the Fst is the surface tension force of water, h is the thickness of
nanoindents indicates the nanoindented structures observed on the PS film, and θ is the water contact angle at nano-scale.

3
Nanotechnology 20 (2009) 045301
Figure 4. (a) Schematic of a nanobubble on the ultrathin PS film in
water. The surface tension force Fst can be decomposed into
perpendicular force Fp and horizontal force Fh . The inside pressure
uniformly applies on the PS surface inside the nanobubble. (b) Cross
section profile of a nanobubble marked by an arrow in figure 2(a)
through apex of the nanobubble and corresponding least-square fit
curves (solid) by fitting the profile as circular arcs.
A nanobubble of moderate size is taken as an example
as marked by an arrow in figure 2(a). The cross section
through the center of the nanobubble is fitted with a circular
arc as shown in figure 4(b) and the radius of the nanobubble
is estimated to be 83.5 nm. The contact angle θ of water
is derived to be about 162.5◦ , which is close to 168.4◦
reported by Simonsen et al (2004) for nanobubbles on a
similar PS surface. The presence of the nanobubble clearly
introduces two important factors to the PS film: the high
inside pressure and surface tension force due to solid–liquid–
gas (three phase) contact line, which combine together and
increase the instability of PS film nearby nanobubbles.
3.3.1. Influence of inside pressure. According to the
Laplace–Young equation, the pressure difference p across
a nanobubble can be calculated using the following equation:
(Israelachvili 1992, Bhushan 1999, 2002):
p = 2γ /R, (1)
where γ is surface tension of water (72 mN m−1 ), and R is
the radius of curvature of a bubble. For the nanobubble shown
in figure 4(b), the inside pressure is about 1.85 MPa, which is
substantially larger than the ambient pressure (101 kPa). For
the nanobubbles with diameters smaller than 40 nm, the inside
pressure should be even higher than that of the nanobubbles
marked in figure 2. As illustrated in figure 4(a), the large inside
4
Y Wang et al
pressure would squeeze PS chains out of the nanobubble,
contributing to the formation of rims around nanobubbles.
To demonstrate the contribution of inside pressure to
the formation of rims and nanoindents, nanoindentation
experiments using a silicon nitride AFM tip were carried out on
a PS surface using a tip radius of about 50 nm. A normal load
of 0.84 nN was continuously applied on the surface for about
30 min. After that, an apparent deformation was observed to
the PS film. The mean contact pressure applied on the contact
area is about 55.3 MPa based on Hertz analysis with the bulk
value of elastic modulus of 3.2–3.4 GPa (Brandrup et al 1999)
and Poisson’s ratio of 0.325 (Boundy and Boyer 1952) for PS.
The actual value of elastic modulus for ultrathin PS film may
be smaller than the bulk value, which would predict a lower
Hertz stress. Thus the data suggest that indentation of the PS
film is possible with rather small loads.
Here one should note that the thickness of PS film also
contributes to the formation of rims and nanoindents. In
the bulk state, polymer chains are entangled with each other,
and the mobility of polymer chains is greatly impeded (Si
et al 2005). Near the surface or interface, the degree of
entanglement is greatly reduced and the mobility of polymer
chains is enhanced, leading to relatively weak interaction
between PS chains. The polymer chain packing theory (Brown
and Russell 1996), dynamic molecular simulation (Meyer et al
2007) together with a recent experiment (Si et al 2005) reveal
that the entanglement density in an ultrathin polymer surface
is significantly reduced, which reduces the interaction between
different chains. Hence, PS chains move towards the outside of
the nanobubbles with high inside pressure p and perpendicular
component Fp (to be described later) of surface tension force,
resulting in the appearance of rims around nanobubbles.
3.3.2. Influence of three phase contact line. The total surface
tension force Fst along the contact line can be decomposed
into two sub-components: the perpendicular force Fp and the
horizontal force Fh . Both Fp and Fh increase the instability
of the PS films near the three phase contact line. The
perpendicular component of surface tension force Fp works
collaboratively with the inside pressure to pile up the PS
chains at the perimeter of the nanobubble, contributing to the
formation of rims as shown in the height images of figure 2.
However, the horizontal component Fh is likely to stretch the
PS film and lead to fracture. Here we will check whether Fh
will lead to fracture.
The total horizontal force Fh acting along the three phase
contact line is given as:
Fh = Fst cos(180 − θ ) = γ π D cos(180 − θ ), (2)
where D is the diameter of the circular contact line and γ is
surface tension of water (72 mN m−1 ). With equation (2), the
tensile stress σ induced by three phase contact line around the
nanobubble can be given as:
σ = Fh /(π Dh) = γ cos(180 − θ )/ h. (3)
Therefore, the thicker the PS film h , the smaller the tensile
stress σ and the more stable the PS film. From equation (3), the
Nanotechnology 20 (2009) 045301 Y Wang et al

tensile stress induced by three phase contact line on the 2.8 nm

thickness PS film is obtained as σ = 24.8 MPa, which is
smaller than the bulk value of tensile strength st of 30–60 MPa
(Mark 1999). As mentioned earlier, the reduced entanglement
density of PS chains in ultrathin films decreases interaction
between different chains. Therefore, the tensile strength for
ultrathin PS film is expected to be lower than that of the
bulk value. However, experimental observation reveals the
relationship σ  st should be satisfied during the experiment.
If the horizontal component Fh is the main reason for the
formation of nanoindents, there should be more nanoindents
appearing around nanobubbles. From the height image of
figure 2(c), one can find that most of the nanoindents appear
on the sites of small nanobubbles and very few nanoindents Figure 5. Schematic of the process for nanoindents formed on the
appear around the bigger nanobubbles, which means it is high PS surface. The whole process is divided into three stages. Stage 1:
inside pressure p combining with perpendicular component nanobubbles formation; stage 2: rims appear and nanobubbles shrink,
and stage 3: rims grows around large nanobubbles and small
Fp , but not Fh , dominating the process of the generation of
nanobubbles disappear with appearance of nanoindents.
rims and nanoindents. This can also been observed through
the structure of rims around bigger nanobubbles, as shown
in section profiles of figure 2 and 3D image of figure 3(b).
have totally disappeared because the changed topography is no
After rims appear around the nanobubbles, the topography of
longer favorable for them to stay on.
PS film outside of rims remains flat. From the conservation
It is clear that the size of nanobubbles is strongly
of materials of PS chains, the appearance of rims should be
correlated with the speed of nanobubble disappearance and
mainly because of PS chain movement from inside to outside
nanoindent formation. Smaller nanobubbles have greater
of nanobubbles due to high inside pressure.
inside pressure. Therefore, the speed of topography change
is expected to be faster than bigger ones. Additionally,
3.4. Detailed process of formation of nanoindents smaller nanobubbles are much more sensitive to the change
The advantage of the sample studied in this experiment is of topography. Once the nanoindents grow up to a size
that different sizes of nanobubbles appeared simultaneously comparable to the diameter of nanobubbles, small nanobubbles
will disappear. However, bigger nanobubbles are not as
during the experiment, and the nanobubble size impact can
be determined during the experiment. Through the process sensitive as smaller ones to the topography change. As revealed
through experimental observation, the rims around bigger
of nanobubble evolution in figure 2, it can be found that
the influence of big nanobubbles on the ultrathin PS film is nanobubbles gradually grow and the nanobubbles continue to
different from that of small nanobubbles. Small nanobubbles stay on the rims.
first shrink and finally disappear at about 150 min, leaving In summary, the presence of nanobubbles is crucial for
nanoindents at their locations. Big bubbles lasted during the the formation of nanoindents, and the size of nanobubbles can
liquid experiment with growing rims around them. greatly influence the process. Based on this experiment, it
is found that nanobubbles with diameters larger than 100 nm
Based on the experimental observation, a schematic
and smaller than 40 nm hinder the process. When the
diagram is given to demonstrate the detailed process
diameters of nanobubbles are larger than 100 nm, the inside
of nanoindented surface formation and the influence of
pressure is low and they cannot be dissolved easily during
nanobubble size during this process, as shown in figure 5.
At stage 1, different sizes of nanobubbles appear on the PS experiment. In contrast, when the diameters are smaller than
50 nm, the nanobubbles will dissolve quickly and leave smaller
sample which is immersed into DI water for several min.
nanoindents sitting on the sites. Nanobubbles with diameters
Both nanobubbles and PS sample surface are not changed yet,
of about 60–80 nm should be desirable for the process. In
corresponding to the image of figure 2(a). At stage 2, the
view of its ease of use, the phenomenon revealed in this
sample has stayed in DI water for several decade min. Because
of the existence of inside Laplace pressure of nanobubbles paper could be applied to fabricate nanopattern structures on
polystyrene surfaces. Additionally, this work should also
and surface tension force along three phase contact line, the
provide instructive information for the application of polymer
PS chains below the nanobubbles are under an imbalance
thin films in aqueous solutions.
condition, which leads to fracture of the PS film. Rims appear
around the nanobubbles. At the same time, the rims confine
the nanobubbles and make them shrink. Stage 2 corresponds 4. Conclusions
to the image of figures 2(b) and (c), where round rims appear
around the nanobubbles and gradually grow up, and parts of A novel phenomenon is reported during the immersion of
the small nanobubbles begin to disappear. At stage 3, which an ultrathin PS film spin-coating on a silicon substrate in
corresponds to the image of figure 2(d), the PS sample has DI water. The time-series images obtained using TMAFM
been in DI water for over 200 min. The smaller nanobubbles show that after immersion, nanobubbles of various size

5
Nanotechnology 20 (2009) 045301
form immediately on the surface of PS film. With time,
nanobubbles first shrank and rims appeared around them.
Small nanobubbles with diameters less than 50 nm gradually
disappeared, leaving nanoindents at their sites. However,
bigger nanobubbles with diameters larger than 70 nm were
more stable and still remained there after 200 min with
growing rims around them. The mechanism for the formation
of nanoindents and rims is studied by analyzing the inside
pressure of nanobubbles and the interfacial forces at the
perimeter of nanobubbles. The combination of high inside
pressure and the perpendicular component of surface tension
force along three phase contact line is believed to be
responsible for the appearance of rims and formation of
nanoindents. The size of nanobubbles is greatly correlated
with the speed of nanobubble disappearance and nanoindents
formation. Small nanobubbles disappeared at about 150 min.
In contrast, big nanobubbles continue to stay on the rims during
the experiment. This is believed to be due to higher inside
pressure of small nanobubbles than that of big nanobubbles.
Small nanobubbles are also more sensitive to topography
change than bigger ones. The nanoindented surface as formed
using this simple method has impressions with a diameter
around 20 nm and a density as high as 2.0 × 108 mm−2 , which
may find practical applications in fabrication of nanopatterned
surfaces.
Acknowledgments
Yuliang Wang acknowledges financial support from Chinese
Scholarship Council. Suggestions from Dr Xing Ling are
warmly acknowledged.
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